Predicting solid-state phase transformations during metal additive manufacturing: A case study on electron-beam powder bed fusion of Inconel-738

Predicting solid-state phase transformations during metal additive manufacturing: A case study on electron-beam powder bed fusion of Inconel-738

금속 적층 제조 중 고체 상 변형 예측: Inconel-738의 전자빔 분말층 융합에 대한 사례 연구

Nana Kwabena Adomako a, Nima Haghdadi a, James F.L. Dingle bc, Ernst Kozeschnik d, Xiaozhou Liao bc, Simon P. Ringer bc, Sophie Primig a

Abstract

Metal additive manufacturing (AM) has now become the perhaps most desirable technique for producing complex shaped engineering parts. However, to truly take advantage of its capabilities, advanced control of AM microstructures and properties is required, and this is often enabled via modeling. The current work presents a computational modeling approach to studying the solid-state phase transformation kinetics and the microstructural evolution during AM. Our approach combines thermal and thermo-kinetic modelling. A semi-analytical heat transfer model is employed to simulate the thermal history throughout AM builds. Thermal profiles of individual layers are then used as input for the MatCalc thermo-kinetic software. The microstructural evolution (e.g., fractions, morphology, and composition of individual phases) for any region of interest throughout the build is predicted by MatCalc. The simulation is applied to an IN738 part produced by electron beam powder bed fusion to provide insights into how γ′ precipitates evolve during thermal cycling. Our simulations show qualitative agreement with our experimental results in predicting the size distribution of γ′ along the build height, its multimodal size character, as well as the volume fraction of MC carbides. Our findings indicate that our method is suitable for a range of AM processes and alloys, to predict and engineer their microstructures and properties.

Graphical Abstract

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Keywords

Additive manufacturing, Simulation, Thermal cycles, γ′ phase, IN738

1. Introduction

Additive manufacturing (AM) is an advanced manufacturing method that enables engineering parts with intricate shapes to be fabricated with high efficiency and minimal materials waste. AM involves building up 3D components layer-by-layer from feedstocks such as powder [1]. Various alloys, including steel, Ti, Al, and Ni-based superalloys, have been produced using different AM techniques. These techniques include directed energy deposition (DED), electron- and laser powder bed fusion (E-PBF and L-PBF), and have found applications in a variety of industries such as aerospace and power generation [2][3][4]. Despite the growing interest, certain challenges limit broader applications of AM fabricated components in these industries and others. One of such limitations is obtaining a suitable and reproducible microstructure that offers the desired mechanical properties consistently. In fact, the AM as-built microstructure is highly complex and considerably distinctive from its conventionally processed counterparts owing to the complicated thermal cycles arising from the deposition of several layers upon each other [5][6].

Several studies have reported that the solid-state phases and solidification microstructure of AM processed alloys such as CMSX-4, CoCr [7][8], Ti-6Al-4V [9][10][11]IN738 [6]304L stainless steel [12], and IN718 [13][14] exhibit considerable variations along the build direction. For instance, references [9][10] have reported that there is a variation in the distribution of α and β phases along the build direction in Ti-alloys. Similarly, the microstructure of an L-PBF fabricated martensitic steel exhibits variations in the fraction of martensite [15]. Furthermore, some of the present authors and others [6][16][17][18][19][20] have recently reviewed and reported that there is a difference in the morphology and fraction of nanoscale precipitates as a function of build height in Ni-based superalloys. These non-uniformities in the as-built microstructure result in an undesired heterogeneity in mechanical and other important properties such as corrosion and oxidation [19][21][22][23]. To obtain the desired microstructure and properties, additional processing treatments are utilized, but this incurs extra costs and may lead to precipitation of detrimental phases and grain coarsening. Therefore, a through-process understanding of the microstructure evolution under repeated heating and cooling is now needed to further advance 3D printed microstructure and property control.

It is now commonly understood that the microstructure evolution during printing is complex, and most AM studies concentrate on the microstructure and mechanical properties of the final build only. Post-printing studies of microstructure characteristics at room temperature miss crucial information on how they evolve. In-situ measurements and modelling approaches are required to better understand the complex microstructural evolution under repeated heating and cooling. Most in-situ measurements in AM focus on monitoring the microstructural changes, such as phase transformations and melt pool dynamics during fabrication using X-ray scattering and high-speed X-ray imaging [24][25][26][27]. For example, Zhao et al. [25] measured the rate of solidification and described the α/β phase transformation during L-PBF of Ti-6Al-4V in-situ. Also, Wahlmann et al. [21] recently used an L-PBF machine coupled with X-ray scattering to investigate the changes in CMSX-4 phase during successive melting processes. Although these techniques provide significant understanding of the basic principles of AM, they are not widely accessible. This is due to the great cost of the instrument, competitive application process, and complexities in terms of the experimental set-up, data collection, and analysis [26][28].

Computational modeling techniques are promising and more widely accessible tools that enable advanced understanding, prediction, and engineering of microstructures and properties during AM. So far, the majority of computational studies have concentrated on physics based process models for metal AM, with the goal of predicting the temperature profile, heat transfer, powder dynamics, and defect formation (e.g., porosity) [29][30]. In recent times, there have been efforts in modeling of the AM microstructure evolution using approaches such as phase-field [31], Monte Carlo (MC) [32], and cellular automata (CA) [33], coupled with finite element simulations for temperature profiles. However, these techniques are often restricted to simulating the evolution of solidification microstructures (e.g., grain and dendrite structure) and defects (e.g., porosity). For example, Zinovieva et al. [33] predicted the grain structure of L-PBF Ti-6Al-4V using finite difference and cellular automata methods. However, studies on the computational modelling of the solid-state phase transformations, which largely determine the resulting properties, remain limited. This can be attributed to the multi-component and multi-phase nature of most engineering alloys in AM, along with the complex transformation kinetics during thermal cycling. This kind of research involves predictions of the thermal cycle in AM builds, and connecting it to essential thermodynamic and kinetic data as inputs for the model. Based on the information provided, the thermokinetic model predicts the history of solid-state phase microstructure evolution during deposition as output. For example, a multi-phase, multi-component mean-field model has been developed to simulate the intermetallic precipitation kinetics in IN718 [34] and IN625 [35] during AM. Also, Basoalto et al. [36] employed a computational framework to examine the contrasting distributions of process-induced microvoids and precipitates in two Ni-based superalloys, namely IN718 and CM247LC. Furthermore, McNamara et al. [37] established a computational model based on the Johnson-Mehl-Avrami model for non-isothermal conditions to predict solid-state phase transformation kinetics in L-PBF IN718 and DED Ti-6Al-4V. These models successfully predicted the size and volume fraction of individual phases and captured the repeated nucleation and dissolution of precipitates that occur during AM.

In the current study, we propose a modeling approach with appreciably short computational time to investigate the detailed microstructural evolution during metal AM. This may include obtaining more detailed information on the morphologies of phases, such as size distribution, phase fraction, dissolution and nucleation kinetics, as well as chemistry during thermal cycling and final cooling to room temperature. We utilize the combination of the MatCalc thermo-kinetic simulator and a semi-analytical heat conduction model. MatCalc is a software suite for simulation of phase transformations, microstructure evolution and certain mechanical properties in engineering alloys. It has successfully been employed to simulate solid-state phase transformations in Ni-based superalloys [38][39], steels [40], and Al alloys [41] during complex thermo-mechanical processes. MatCalc uses the classical nucleation theory as well as the so-called Svoboda-Fischer-Fratzl-Kozeschnik (SFFK) growth model as the basis for simulating precipitation kinetics [42]. Although MatCalc was originally developed for conventional thermo-mechanical processes, we will show that it is also applicable for AM if the detailed time-temperature profile of the AM build is known. The semi-analytical heat transfer code developed by Stump and Plotkowski [43] is used to simulate these profile throughout the AM build.

1.1. Application to IN738

Inconel-738 (IN738) is a precipitation hardening Ni-based superalloy mainly employed in high-temperature components, e.g. in gas turbines and aero-engines owing to its exceptional mechanical properties at temperatures up to 980 °C, coupled with high resistance to oxidation and corrosion [44]. Its superior high-temperature strength (∼1090 MPa tensile strength) is provided by the L12 ordered Ni3(Al,Ti) γ′ phase that precipitates in a face-centered cubic (FCC) γ matrix [45][46]. Despite offering great properties, IN738, like most superalloys with high γ′ fractions, is challenging to process owing to its propensity to hot cracking [47][48]. Further, machining of such alloys is challenging because of their high strength and work-hardening rates. It is therefore difficult to fabricate complex INC738 parts using traditional manufacturing techniques like casting, welding, and forging.

The emergence of AM has now made it possible to fabricate such parts from IN738 and other superalloys. Some of the current authors’ recent research successfully applied E-PBF to fabricate defect-free IN738 containing γ′ throughout the build [16][17]. The precipitated γ′ were heterogeneously distributed. In particular, Haghdadi et al. [16] studied the origin of the multimodal size distribution of γ′, while Lim et al. [17] investigated the gradient in γ′ character with build height and its correlation to mechanical properties. Based on these results, the present study aims to extend the understanding of the complex and site-specific microstructural evolution in E-PBF IN738 by using a computational modelling approach. New experimental evidence (e.g., micrographs not published previously) is presented here to support the computational results.

2. Materials and Methods

2.1. Materials preparation

IN738 Ni-based superalloy (59.61Ni-8.48Co-7.00Al-17.47Cr-3.96Ti-1.01Mo-0.81W-0.56Ta-0.49Nb-0.47C-0.09Zr-0.05B, at%) gas-atomized powder was used as feedstock. The powders, with average size of 60 ± 7 µm, were manufactured by Praxair and distributed by Astro Alloys Inc. An Arcam Q10 machine by GE Additive with an acceleration voltage of 60 kV was used to fabricate a 15 × 15 × 25 mm3 block (XYZ, Z: build direction) on a 316 stainless steel substrate. The block was 3D-printed using a ‘random’ spot melt pattern. The random spot melt pattern involves randomly selecting points in any given layer, with an equal chance of each point being melted. Each spot melt experienced a dwell time of 0.3 ms, and the layer thickness was 50 µm. Some of the current authors have previously characterized the microstructure of the very same and similar builds in more detail [16][17]. A preheat temperature of ∼1000 °C was set and kept during printing to reduce temperature gradients and, in turn, thermal stresses [49][50][51]. Following printing, the build was separated from the substrate through electrical discharge machining. It should be noted that this sample was simultaneously printed with the one used in [17] during the same build process and on the same build plate, under identical conditions.

2.2. Microstructural characterization

The printed sample was longitudinally cut in the direction of the build using a Struers Accutom-50, ground, and then polished to 0.25 µm suspension via standard techniques. The polished x-z surface was electropolished and etched using Struers A2 solution (perchloric acid in ethanol). Specimens for image analysis were polished using a 0.06 µm colloidal silica. Microstructure analyses were carried out across the height of the build using optical microscopy (OM) and scanning electron microscopy (SEM) with focus on the microstructure evolution (γ′ precipitates) in individual layers. The position of each layer being analyzed was determined by multiplying the layer number by the layer thickness (50 µm). It should be noted that the position of the first layer starts where the thermal profile is tracked (in this case, 2 mm from the bottom). SEM images were acquired using a JEOL 7001 field emission microscope. The brightness and contrast settings, acceleration voltage of 15 kV, working distance of 10 mm, and other SEM imaging parameters were all held constant for analysis of the entire build. The ImageJ software was used for automated image analysis to determine the phase fraction and size of γ′ precipitates and carbides. A 2-pixel radius Gaussian blur, following a greyscale thresholding and watershed segmentation was used [52]. Primary γ′ sizes (>50 nm), were measured using equivalent spherical diameters. The phase fractions were considered equal to the measured area fraction. Secondary γ′ particles (<50 nm) were not considered here. The γ′ size in the following refers to the diameter of a precipitate.

2.3. Hardness testing

A Struers DuraScan tester was utilized for Vickers hardness mapping on a polished x-z surface, from top to bottom under a maximum load of 100 mN and 10 s dwell time. 30 micro-indentations were performed per row. According to the ASTM standard [53], the indentations were sufficiently distant (∼500 µm) to assure that strain-hardened areas did not interfere with one another.

2.4. Computational simulation of E-PBF IN738 build

2.4.1. Thermal profile modeling

The thermal history was generated using the semi-analytical heat transfer code (also known as the 3DThesis code) developed by Stump and Plotkowski [43]. This code is an open-source C++ program which provides a way to quickly simulate the conductive heat transfer found in welding and AM. The key use case for the code is the simulation of larger domains than is practicable with Computational Fluid Dynamics/Finite Element Analysis programs like FLOW-3D AM. Although simulating conductive heat transfer will not be an appropriate simplification for some investigations (for example the modelling of keyholding or pore formation), the 3DThesis code does provide fast estimates of temperature, thermal gradient, and solidification rate which can be useful for elucidating microstructure formation across entire layers of an AM build. The mathematics involved in the code is as follows:

In transient thermal conduction during welding and AM, with uniform and constant thermophysical properties and without considering fluid convection and latent heat effects, energy conservation can be expressed as:(1)��∂�∂�=�∇2�+�̇where � is density, � specific heat, � temperature, � time, � thermal conductivity, and �̇ a volumetric heat source. By assuming a semi-infinite domain, Eq. 1 can be analytically solved. The solution for temperature at a given time (t) using a volumetric Gaussian heat source is presented as:(2)��,�,�,�−�0=33�����32∫0�1������exp−3�′�′2��+�′�′2��+�′�′2����′(3)and��=12��−�′+��2for�=�,�,�(4)and�′�′=�−���′Where � is the vector �,�,� and �� is the location of the heat source.

The numerical integration scheme used is an adaptive Gaussian quadrature method based on the following nondimensionalization:(5)�=��xy2�,�′=��xy2�′,�=��xy,�=��xy,�=��xy,�=���xy

A more detailed explanation of the mathematics can be found in reference [43].

The main source of the thermal cycling present within a powder-bed fusion process is the fusion of subsequent layers. Therefore, regions near the top of a build are expected to undergo fewer thermal cycles than those closer to the bottom. For this purpose, data from the single scan’s thermal influence on multiple layers was spliced to represent the thermal cycles experienced at a single location caused by multiple subsequent layers being fused.

The cross-sectional area simulated by this model was kept constant at 1 × 1 mm2, and the depth was dependent on the build location modelled with MatCalc. For a build location 2 mm from the bottom, the maximum number of layers to simulate is 460. Fig. 1a shows a stitched overview OM image of the entire build indicating the region where this thermal cycle is simulated and tracked. To increase similarity with the conditions of the physical build, each thermal history was constructed from the results of two simulations generated with different versions of a random scan path. The parameters used for these thermal simulations can be found in Table 1. It should be noted that the main purpose of the thermal profile modelling was to demonstrate how the conditions at different locations of the build change relative to each other. Accurately predicting the absolute temperature during the build would require validation via a temperature sensor measurement during the build process which is beyond the scope of the study. Nonetheless, to establish the viability of the heat source as a suitable approximation for this study, an additional sensitivity analysis was conducted. This analysis focused on the influence of energy input on γ′ precipitation behavior, the central aim of this paper. This was achieved by employing varying beam absorption energies (0.76, 0.82 – the values utilized in the simulation, and 0.9). The direct impact of beam absorption efficiency on energy input into the material was investigated. Specifically, the initial 20 layers of the build were simulated and subsequently compared to experimental data derived from SEM. While phase fractions were found to be consistent across all conditions, disparities emerged in the mean size of γ′ precipitates. An absorption efficiency of 0.76 yielded a mean size of approximately 70 nm. Conversely, absorption efficiencies of 0.82 and 0.9 exhibited remarkably similar mean sizes of around 130 nm, aligning closely with the outcomes of the experiments.

Fig. 1

Table 1. A list of parameters used in thermal simulation of E-PBF.

ParameterValue
Spatial resolution5 µm
Time step0.5 s
Beam diameter200 µm
Beam penetration depth1 µm
Beam power1200 W
Beam absorption efficiency0.82
Thermal conductivity25.37 W/(m⋅K)
Chamber temperature1000 °C
Specific heat711.756 J/(kg⋅K)
Density8110 kg/m3

2.4.2. Thermo-kinetic simulation

The numerical analyses of the evolution of precipitates was performed using MatCalc version 6.04 (rel 0.011). The thermodynamic (‘mc_ni.tdb’, version 2.034) and diffusion (‘mc_ni.ddb’, version 2.007) databases were used. MatCalc’s basic principles are elaborated as follows:

The nucleation kinetics of precipitates are computed using a computational technique based on a classical nucleation theory [54] that has been modified for systems with multiple components [42][55]. Accordingly, the transient nucleation rate (�), which expresses the rate at which nuclei are formed per unit volume and time, is calculated as:(6)�=�0��*∙�xp−�*�∙�∙exp−��where �0 denotes the number of active nucleation sites, �* the rate of atomic attachment, � the Boltzmann constant, � the temperature, �* the critical energy for nucleus formation, τ the incubation time, and t the time. � (Zeldovich factor) takes into consideration that thermal excitation destabilizes the nucleus as opposed to its inactive state [54]. Z is defined as follows:(7)�=−12�kT∂2∆�∂�2�*12where ∆� is the overall change in free energy due to the formation of a nucleus and n is the nucleus’ number of atoms. ∆�’s derivative is evaluated at n* (critical nucleus size). �* accounts for the long-range diffusion of atoms required for nucleation, provided that the matrix’ and precipitates’ composition differ. Svoboda et al. [42] developed an appropriate multi-component equation for �*, which is given by:(8)�*=4��*2�4�∑�=1��ki−�0�2�0��0�−1where �* denotes the critical radius for nucleation, � represents atomic distance, and � is the molar volume. �ki and �0� represent the concentration of elements in the precipitate and matrix, respectively. The parameter �0� denotes the rate of diffusion of the ith element within the matrix. The expression for the incubation time � is expressed as [54]:(9)�=12�*�2

and �*, which represents the critical energy for nucleation:(10)�*=16�3�3∆�vol2where � is the interfacial energy, and ∆Gvol the change in the volume free energy. The critical nucleus’ composition is similar to the γ′ phase’s equilibrium composition at the same temperature. � is computed based on the precipitate and matrix compositions, using a generalized nearest neighbor broken bond model, with the assumption of interfaces being planar, sharp, and coherent [56][57][58].

In Eq. 7, it is worth noting that �* represents the fundamental variable in the nucleation theory. It contains �3/∆�vol2 and is in the exponent of the nucleation rate. Therefore, even small variations in γ and/or ∆�vol can result in notable changes in �, especially if �* is in the order of �∙�. This is demonstrated in [38] for UDIMET 720 Li during continuous cooling, where these quantities change steadily during precipitation due to their dependence on matrix’ and precipitate’s temperature and composition. In the current work, these changes will be even more significant as the system is exposed to multiple cycles of rapid cooling and heating.

Once nucleated, the growth of a precipitate is assessed using the radius and composition evolution equations developed by Svoboda et al. [42] with a mean-field method that employs the thermodynamic extremal principle. The expression for the total Gibbs free energy of a thermodynamic system G, which consists of n components and m precipitates, is given as follows:(11)�=∑���0��0�+∑�=1�4���33��+∑�=1��ki�ki+∑�=1�4���2��.

The chemical potential of component � in the matrix is denoted as �0�(�=1,…,�), while the chemical potential of component � in the precipitate is represented by �ki(�=1,…,�,�=1,…,�). These chemical potentials are defined as functions of the concentrations �ki(�=1,…,�,�=1,…,�). The interface energy density is denoted as �, and �� incorporates the effects of elastic energy and plastic work resulting from the volume change of each precipitate.

Eq. (12) establishes that the total free energy of the system in its current state relies on the independent state variables: the sizes (radii) of the precipitates �� and the concentrations of each component �ki. The remaining variables can be determined by applying the law of mass conservation to each component �. This can be represented by the equation:(12)��=�0�+∑�=1�4���33�ki,

Furthermore, the global mass conservation can be expressed by equation:(13)�=∑�=1���When a thermodynamic system transitions to a more stable state, the energy difference between the initial and final stages is dissipated. This model considers three distinct forms of dissipation effects [42]. These include dissipations caused by the movement of interfaces, diffusion within the precipitate and diffusion within the matrix.

Consequently, �̇� (growth rate) and �̇ki (chemical composition’s rate of change) of the precipitate with index � are derived from the linear system of equation system:(14)�ij��=��where �� symbolizes the rates �̇� and �̇ki [42]. Index i contains variables for precipitate radius, chemical composition, and stoichiometric boundary conditions suggested by the precipitate’s crystal structure. Eq. (10) is computed separately for every precipitate �. For a more detailed description of the formulae for the coefficients �ij and �� employed in this work please refer to [59].

The MatCalc software was used to perform the numerical time integration of �̇� and �̇ki of precipitates based on the classical numerical method by Kampmann and Wagner [60]. Detailed information on this method can be found in [61]. Using this computational method, calculations for E-PBF thermal cycles (cyclic heating and cooling) were computed and compared to experimental data. The simulation took approximately 2–4 hrs to complete on a standard laptop.

3. Results

3.1. Microstructure

Fig. 1 displays a stitched overview image and selected SEM micrographs of various γ′ morphologies and carbides after observations of the X-Z surface of the build from the top to 2 mm above the bottom. Fig. 2 depicts a graph that charts the average size and phase fraction of the primary γ′, as it changes with distance from the top to the bottom of the build. The SEM micrographs show widespread primary γ′ precipitation throughout the entire build, with the size increasing in the top to bottom direction. Particularly, at the topmost height, representing the 460th layer (Z = 22.95 mm), as seen in Fig. 1b, the average size of γ′ is 110 ± 4 nm, exhibiting spherical shapes. This is representative of the microstructure after it solidifies and cools to room temperature, without experiencing additional thermal cycles. The γ′ size slightly increases to 147 ± 6 nm below this layer and remains constant until 0.4 mm (∼453rd layer) from the top. At this position, the microstructure still closely resembles that of the 460th layer. After the 453rd layer, the γ′ size grows rapidly to ∼503 ± 19 nm until reaching the 437th layer (1.2 mm from top). The γ′ particles here have a cuboidal shape, and a small fraction is coarser than 600 nm. γ′ continue to grow steadily from this position to the bottom (23 mm from the top). A small fraction of γ′ is > 800 nm.

Fig. 2

Besides primary γ′, secondary γ′ with sizes ranging from 5 to 50 nm were also found. These secondary γ′ precipitates, as seen in Fig. 1f, were present only in the bottom and middle regions. A detailed analysis of the multimodal size distribution of γ′ can be found in [16]. There is no significant variation in the phase fraction of the γ′ along the build. The phase fraction is ∼ 52%, as displayed in Fig. 2. It is worth mentioning that the total phase fraction of γ′ was estimated based on the primary γ′ phase fraction because of the small size of secondary γ′. Spherical MC carbides with sizes ranging from 50 to 400 nm and a phase fraction of 0.8% were also observed throughout the build. The carbides are the light grey precipitates in Fig. 1g. The light grey shade of carbides in the SEM images is due to their composition and crystal structure [52]. These carbides are not visible in Fig. 1b-e because they were dissolved during electro-etching carried out after electropolishing. In Fig. 1g, however, the sample was examined directly after electropolishing, without electro-etching.

Table 2 shows the nominal and measured composition of γ′ precipitates throughout the build by atom probe microscopy as determined in our previous study [17]. No build height-dependent composition difference was observed in either of the γ′ precipitate populations. However, there was a slight disparity between the composition of primary and secondary γ′. Among the main γ′ forming elements, the primary γ′ has a high Ti concentration while secondary γ′ has a high Al concentration. A detailed description of the atom distribution maps and the proxigrams of the constituent elements of γ′ throughout the build can be found in [17].

Table 2. Bulk IN738 composition determined using inductively coupled plasma atomic emission spectroscopy (ICP-AES). Compositions of γ, primary γ′, and secondary γ′ at various locations in the build measured by APT. This information is reproduced from data in Ref. [17] with permission.

at%NiCrCoAlMoWTiNbCBZrTaOthers
Bulk59.1217.478.487.001.010.813.960.490.470.050.090.560.46
γ matrix
Top50.4832.9111.591.941.390.820.440.80.030.030.020.24
Mid50.3732.6111.931.791.540.890.440.10.030.020.020.010.23
Bot48.1034.5712.082.141.430.880.480.080.040.030.010.12
Primary γ′
Top72.172.513.4412.710.250.397.780.560.030.020.050.08
Mid71.602.573.2813.550.420.687.040.730.010.030.040.04
Bot72.342.473.8612.500.260.447.460.500.050.020.020.030.04
Secondary γ′
Mid70.424.203.2314.190.631.035.340.790.030.040.040.05
Bot69.914.063.6814.320.811.045.220.650.050.100.020.11

3.2. Hardness

Fig. 3a shows the Vickers hardness mapping performed along the entire X-Z surface, while Fig. 3b shows the plot of average hardness at different build heights. This hardness distribution is consistent with the γ′ precipitate size gradient across the build direction in Fig. 1Fig. 2. The maximum hardness of ∼530 HV1 is found at ∼0.5 mm away from the top surface (Z = 22.5), where γ′ particles exhibit the smallest observed size in Fig. 2b. Further down the build (∼ 2 mm from the top), the hardness drops to the 440–490 HV1 range. This represents the region where γ′ begins to coarsen. The hardness drops further to 380–430 HV1 at the bottom of the build.

Fig. 3

3.3. Modeling of the microstructural evolution during E-PBF

3.3.1. Thermal profile modeling

Fig. 4 shows the simulated thermal profile of the E-PBF build at a location of 23 mm from the top of the build, using a semi-analytical heat conduction model. This profile consists of the time taken to deposit 460 layers until final cooling, as shown in Fig. 4a. Fig. 4b-d show the magnified regions of Fig. 4a and reveal the first 20 layers from the top, a single layer (first layer from the top), and the time taken for the build to cool after the last layer deposition, respectively.

Fig. 4

The peak temperatures experienced by previous layers decrease progressively as the number of layers increases but never fall below the build preheat temperature (1000 °C). Our simulated thermal cycle may not completely capture the complexity of the actual thermal cycle utilized in the E-PBF build. For instance, the top layer (Fig. 4c), also representing the first deposit’s thermal profile without additional cycles (from powder heating, melting, to solidification), recorded the highest peak temperature of 1390 °C. Although this temperature is above the melting range of the alloy (1230–1360 °C) [62], we believe a much higher temperature was produced by the electron beam to melt the powder. Nevertheless, the solidification temperature and dynamics are outside the scope of this study as our focus is on the solid-state phase transformations during deposition. It takes ∼25 s for each layer to be deposited and cooled to the build temperature. The interlayer dwell time is 125 s. The time taken for the build to cool to room temperature (RT) after final layer deposition is ∼4.7 hrs (17,000 s).

3.3.2. MatCalc simulation

During the MatCalc simulation, the matrix phase is defined as γ. γ′, and MC carbide are included as possible precipitates. The domain of these precipitates is set to be the matrix (γ), and nucleation is assumed to be homogenous. In homogeneous nucleation, all atoms of the unit volume are assumed to be potential nucleation sitesTable 3 shows the computational parameters used in the simulation. All other parameters were set at default values as recommended in the version 6.04.0011 of MatCalc. The values for the interfacial energies are automatically calculated according to the generalized nearest neighbor broken bond model and is one of the most outstanding features in MatCalc [56][57][58]. It should be noted that the elastic misfit strain was not included in the calculation. The output of MatCalc includes phase fraction, size, nucleation rate, and composition of the precipitates. The phase fraction in MatCalc is the volume fraction. Although the experimental phase fraction is the measured area fraction, it is relatively similar to the volume fraction. This is because of the generally larger precipitate size and similar morphology at the various locations along the build [63]. A reliable phase fraction comparison between experiment and simulation can therefore be made.

Table 3. Computational parameters used in the simulation.

Precipitation domainγ
Nucleation site γ′Bulk (homogenous)
Nucleation site MC carbideBulk (Homogenous)
Precipitates class size250
Regular solution critical temperature γ′2500 K[64]
Calculated interfacial energyγ′ = 0.080–0.140 J/m2 and MC carbide = 0.410–0.430 J/m2
3.3.2.1. Precipitate phase fraction

Fig. 5a shows the simulated phase fraction of γ′ and MC carbide during thermal cycling. Fig. 5b is a magnified view of 5a showing the simulated phase fraction at the center points of the top 70 layers, whereas Fig. 5c corresponds to the first two layers from the top. As mentioned earlier, the top layer (460th layer) represents the microstructure after solidification. The microstructure of the layers below is determined by the number of thermal cycles, which increases with distance to the top. For example, layers 459, 458, 457, up to layer 1 (region of interest) experience 1, 2, 3 and 459 thermal cycles, respectively. In the top layer in Fig. 5c, the volume fraction of γ′ and carbides increases with temperature. For γ′, it decreases to zero when the temperature is above the solvus temperature after a few seconds. Carbides, however, remain constant in their volume fraction reaching equilibrium (phase fraction ∼ 0.9%) in a short time. The topmost layer can be compared to the first deposit, and the peak in temperature symbolizes the stage where the electron beam heats the powder until melting. This means γ′ and carbide precipitation might have started in the powder particles during heating from the build temperature and electron beam until the onset of melting, where γ′ dissolves, but carbides remain stable [28].

Fig. 5

During cooling after deposition, γ′ reprecipitates at a temperature of 1085 °C, which is below its solvus temperature. As cooling progresses, the phase fraction increases steadily to ∼27% and remains constant at 1000 °C (elevated build temperature). The calculated equilibrium fraction of phases by MatCalc is used to show the complex precipitation characteristics in this alloy. Fig. 6 shows that MC carbides form during solidification at 1320 °C, followed by γ′, which precipitate when the solidified layer cools to 1140 °C. This indicates that all deposited layers might contain a negligible amount of these precipitates before subsequent layer deposition, while being at the 1000 °C build temperature or during cooling to RT. The phase diagram also shows that the equilibrium fraction of the γ′ increases as temperature decreases. For instance, at 1000, 900, and 800 °C, the phase fractions are ∼30%, 38%, and 42%, respectively.

Fig. 6

Deposition of subsequent layers causes previous layers to undergo phase transformations as they are exposed to several thermal cycles with different peak temperatures. In Fig. 5c, as the subsequent layer is being deposited, γ′ in the previous layer (459th layer) begins to dissolve as the temperature crosses the solvus temperature. This is witnessed by the reduction of the γ′ phase fraction. This graph also shows how this phase dissolves during heating. However, the phase fraction of MC carbide remains stable at high temperatures and no dissolution is seen during thermal cycling. Upon cooling, the γ′ that was dissolved during heating reprecipitates with a surge in the phase fraction until 1000 °C, after which it remains constant. This microstructure is similar to the solidification microstructure (layer 460), with a similar γ′ phase fraction (∼27%).

The complete dissolution and reprecipitation of γ′ continue for several cycles until the 50th layer from the top (layer 411), where the phase fraction does not reach zero during heating to the peak temperature (see Fig. 5d). This indicates the ‘partial’ dissolution of γ′, which continues progressively with additional layers. It should be noted that the peak temperatures for layers that underwent complete dissolution were much higher (1170–1300 °C) than the γ′ solvus.

The dissolution and reprecipitation of γ′ during thermal cycling are further confirmed in Fig. 7, which summarizes the nucleation rate, phase fraction, and concentration of major elements that form γ′ in the matrix. Fig. 7b magnifies a single layer (3rd layer from top) within the full dissolution region in Fig. 7a to help identify the nucleation and growth mechanisms. From Fig. 7b, γ′ nucleation begins during cooling whereby the nucleation rate increases to reach a maximum value of approximately 1 × 1020 m−3s−1. This fast kinetics implies that some rearrangement of atoms is required for γ′ precipitates to form in the matrix [65][66]. The matrix at this stage is in a non-equilibrium condition. Its composition is similar to the nominal composition and remains unchanged. The phase fraction remains insignificant at this stage although nucleation has started. The nucleation rate starts declining upon reaching the peak value. Simultaneously, diffusion-controlled growth of existing nuclei occurs, depleting the matrix of γ′ forming elements (Al and Ti). Thus, from (7)(11), ∆�vol continuously decreases until nucleation ceases. The growth of nuclei is witnessed by the increase in phase fraction until a constant level is reached at 27% upon cooling to and holding at build temperature. This nucleation event is repeated several times.

Fig. 7

At the onset of partial dissolution, the nucleation rate jumps to 1 × 1021 m−3s−1, and then reduces sharply at the middle stage of partial dissolution. The nucleation rate reaches 0 at a later stage. Supplementary Fig. S1 shows a magnified view of the nucleation rate, phase fraction, and thermal profile, underpinning this trend. The jump in nucleation rate at the onset is followed by a progressive reduction in the solute content of the matrix. The peak temperatures (∼1130–1160 °C) are lower than those in complete dissolution regions but still above or close to the γ′ solvus. The maximum phase fraction (∼27%) is similar to that of the complete dissolution regions. At the middle stage, the reduction in nucleation rate is accompanied by a sharp drop in the matrix composition. The γ′ fraction drops to ∼24%, where the peak temperatures of the layers are just below or at γ′ solvus. The phase fraction then increases progressively through the later stage of partial dissolution to ∼30% towards the end of thermal cycling. The matrix solute content continues to drop although no nucleation event is seen. The peak temperatures are then far below the γ′ solvus. It should be noted that the matrix concentration after complete dissolution remains constant. Upon cooling to RT after final layer deposition, the nucleation rate increases again, indicating new nucleation events. The phase fraction reaches ∼40%, with a further depletion of the matrix in major γ′ forming elements.

3.3.2.2. γ′ size distribution

Fig. 8 shows histograms of the γ′ precipitate size distributions (PSD) along the build height during deposition. These PSDs are predicted at the end of each layer of interest just before final cooling to room temperature, to separate the role of thermal cycles from final cooling on the evolution of γ′. The PSD for the top layer (layer 460) is shown in Fig. 8a (last solidified region with solidification microstructure). The γ′ size ranges from 120 to 230 nm and is similar to the 44 layers below (2.2 mm from the top).

Fig. 8

Further down the build, γ′ begins to coarsen after layer 417 (44th layer from top). Fig. 8c shows the PSD after the 44th layer, where the γ′ size exhibits two peaks at ∼120–230 and ∼300 nm, with most of the population being in the former range. This is the onset of partial dissolution where simultaneously with the reprecipitation and growth of fresh γ′, the undissolved γ′ grows rapidly through diffusive transport of atoms to the precipitates. This is shown in Fig. 8c, where the precipitate class sizes between 250 and 350 represent the growth of undissolved γ′. Although this continues in the 416th layer, the phase fractions plot indicates that the onset of partial dissolution begins after the 411th layer. This implies that partial dissolution started early, but the fraction of undissolved γ′ was too low to impact the phase fraction. The reprecipitated γ′ are mostly in the 100–220 nm class range and similar to those observed during full dissolution.

As the number of layers increases, coarsening intensifies with continued growth of more undissolved γ′, and reprecipitation and growth of partially dissolved ones. Fig. 8d, e, and f show this sequence. Further down the build, coarsening progresses rapidly, as shown in Figs. 8d, 8e, and 8f. The γ′ size ranges from 120 to 1100 nm, with the peaks at 160, 180, and 220 nm in Figs. 8d, 8e, and 8f, respectively. Coarsening continues until nucleation ends during dissolution, where only the already formed γ′ precipitates continue to grow during further thermal cycling. The γ′ size at this point is much larger, as observed in layers 361 and 261, and continues to increase steadily towards the bottom (layer 1). Two populations in the ranges of ∼380–700 and ∼750–1100 nm, respectively, can be seen. The steady growth of γ′ towards the bottom is confirmed by the gradual decrease in the concentration of solute elements in the matrix (Fig. 7a). It should be noted that for each layer, the γ′ class with the largest size originates from continuous growth of the earliest set of the undissolved precipitates.

Fig. 9Fig. 10 and supplementary Figs. S2 and S3 show the γ′ size evolution during heating and cooling of a single layer in the full dissolution region, and early, middle stages, and later stages of partial dissolution, respectively. In all, the size of γ′ reduces during layer heating. Depending on the peak temperature of the layer which varies with build height, γ′ are either fully or partially dissolved as mentioned earlier. Upon cooling, the dissolved γ′ reprecipitate.

Fig. 9
Fig. 10

In Fig. 9, those layers that underwent complete dissolution (top layers) were held above γ′ solvus temperature for longer. In Fig. 10, layers at the early stage of partial dissolution spend less time in the γ′ solvus temperature region during heating, leading to incomplete dissolution. In such conditions, smaller precipitates are fully dissolved while larger ones shrink [67]. Layers in the middle stages of partial dissolution have peak temperatures just below or at γ′ solvus, not sufficient to achieve significant γ′ dissolution. As seen in supplementary Fig. S2, only a few smaller γ′ are dissolved back into the matrix during heating, i.e., growth of precipitates is more significant than dissolution. This explains the sharp decrease in concentration of Al and Ti in the matrix in this layer.

The previous sections indicate various phenomena such as an increase in phase fraction, further depletion of matrix composition, and new nucleation bursts during cooling. Analysis of the PSD after the final cooling of the build to room temperature allows a direct comparison to post-printing microstructural characterization. Fig. 11 shows the γ′ size distribution of layer 1 (460th layer from the top) after final cooling to room temperature. Precipitation of secondary γ′ is observed, leading to the multimodal size distribution of secondary and primary γ′. The secondary γ′ size falls within the 10–80 nm range. As expected, a further growth of the existing primary γ′ is also observed during cooling.

Fig. 11
3.3.2.3. γ′ chemistry after deposition

Fig. 12 shows the concentration of the major elements that form γ′ (Al, Ti, and Ni) in the primary and secondary γ′ at the bottom of the build, as calculated by MatCalc. The secondary γ′ has a higher Al content (13.5–14.5 at% Al), compared to 13 at% Al in the primary γ′. Additionally, within the secondary γ′, the smallest particles (∼10 nm) have higher Al contents than larger ones (∼70 nm). In contrast, for the primary γ′, there is no significant variation in the Al content as a function of their size. The Ni concentration in secondary γ′ (71.1–72 at%) is also higher in comparison to the primary γ′ (70 at%). The smallest secondary γ′ (∼10 nm) have higher Ni contents than larger ones (∼70 nm), whereas there is no substantial change in the Ni content of primary γ′, based on their size. As expected, Ti shows an opposite size-dependent variation. It ranges from ∼ 7.7–8.7 at% Ti in secondary γ′ to ∼9.2 at% in primary γ′. Similarly, within the secondary γ′, the smallest (∼10 nm) have lower Al contents than the larger ones (∼70 nm). No significant variation is observed for Ti content in primary γ′.

Fig. 12

4. Discussion

A combined modelling method is utilized to study the microstructural evolution during E-PBF of IN738. The presented results are discussed by examining the precipitation and dissolution mechanism of γ′ during thermal cycling. This is followed by a discussion on the phase fraction and size evolution of γ′ during thermal cycling and after final cooling. A brief discussion on carbide morphology is also made. Finally, a comparison is made between the simulation and experimental results to assess their agreement.

4.1. γ′ morphology as a function of build height

4.1.1. Nucleation of γ′

The fast precipitation kinetics of the γ′ phase enables formation of γ′ upon quenching from higher temperatures (above solvus) during thermal cycling [66]. In Fig. 7b, for a single layer in the full dissolution region, during cooling, the initial increase in nucleation rate signifies the first formation of nuclei. The slight increase in nucleation rate during partial dissolution, despite a decrease in the concentration of γ′ forming elements, may be explained by the nucleation kinetics. During partial dissolution and as the precipitates shrink, it is assumed that the regions at the vicinity of partially dissolved precipitates are enriched in γ′ forming elements [68][69]. This differs from the full dissolution region, in which case the chemical composition is evenly distributed in the matrix. Several authors have attributed the solute supersaturation of the matrix around primary γ′ to partial dissolution during isothermal ageing [69][70][71][72]. The enhanced supersaturation in the regions close to the precipitates results in a much higher driving force for nucleation, leading to a higher nucleation rate upon cooling. This phenomenon can be closely related to the several nucleation bursts upon continuous cooling of Ni-based superalloys, where second nucleation bursts exhibit higher nucleation rates [38][68][73][74].

At middle stages of partial dissolution, the reduction in the nucleation rate indicates that the existing composition and low supersaturation did not trigger nucleation as the matrix was closer to the equilibrium state. The end of a nucleation burst means that the supersaturation of Al and Ti has reached a low level, incapable of providing sufficient driving force during cooling to or holding at 1000 °C for further nucleation [73]. Earlier studies on Ni-based superalloys have reported the same phenomenon during ageing or continuous cooling from the solvus temperature to RT [38][73][74].

4.1.2. Dissolution of γ′ during thermal cycling

γ′ dissolution kinetics during heating are fast when compared to nucleation due to exponential increase in phase transformation and diffusion activities with temperature [65]. As shown in Fig. 9Fig. 10, and supplementary Figs. S2 and S3, the reduction in γ′ phase fraction and size during heating indicates γ′ dissolution. This is also revealed in Fig. 5 where phase fraction decreases upon heating. The extent of γ′ dissolution mostly depends on the temperature, time spent above γ′ solvus, and precipitate size [75][76][77]. Smaller γ′ precipitates are first to be dissolved [67][77][78]. This is mainly because more solute elements need to be transported away from large γ′ precipitates than from smaller ones [79]. Also, a high temperature above γ′ solvus temperature leads to a faster dissolution rate [80]. The equilibrium solvus temperature of γ′ in IN738 in our MatCalc simulation (Fig. 6) and as reported by Ojo et al. [47] is 1140 °C and 1130–1180 °C, respectively. This means the peak temperature experienced by previous layers decreases progressively from γ′ supersolvus to subsolvus, near-solvus, and far from solvus as the number of subsequent layers increases. Based on the above, it can be inferred that the degree of dissolution of γ′ contributes to the gradient in precipitate distribution.

Although the peak temperatures during later stages of partial dissolution are much lower than the equilibrium γ′ solvus, γ′ dissolution still occurs but at a significantly lower rate (supplementary Fig. S3). Wahlmann et al. [28] also reported a similar case where they observed the rapid dissolution of γ′ in CMSX-4 during fast heating and cooling cycles at temperatures below the γ′ solvus. They attributed this to the γ′ phase transformation process taking place in conditions far from the equilibrium. While the same reasoning may be valid for our study, we further believe that the greater surface area to volume ratio of the small γ′ precipitates contributed to this. This ratio means a larger area is available for solute atoms to diffuse into the matrix even at temperatures much below the solvus [81].

4.2. γ′ phase fraction and size evolution

4.2.1. During thermal cycling

In the first layer, the steep increase in γ′ phase fraction during heating (Fig. 5), which also represents γ′ precipitation in the powder before melting, has qualitatively been validated in [28]. The maximum phase fraction of 27% during the first few layers of thermal cycling indicates that IN738 theoretically could reach the equilibrium state (∼30%), but the short interlayer time at the build temperature counteracts this. The drop in phase fraction at middle stages of partial dissolution is due to the low number of γ′ nucleation sites [73]. It has been reported that a reduction of γ′ nucleation sites leads to a delay in obtaining the final volume fraction as more time is required for γ′ precipitates to grow and reach equilibrium [82]. This explains why even upon holding for 150 s before subsequent layer deposition, the phase fraction does not increase to those values that were observed in the previous full γ′ dissolution regions. Towards the end of deposition, the increase in phase fraction to the equilibrium value of 30% is as a result of the longer holding at build temperature or close to it [83].

During thermal cycling, γ′ particles begin to grow immediately after they first precipitate upon cooling. This is reflected in the rapid increase in phase fraction and size during cooling in Fig. 5 and supplementary Fig. S2, respectively. The rapid growth is due to the fast diffusion of solute elements at high temperatures [84]. The similar size of γ′ for the first 44 layers from the top can be attributed to the fact that all layers underwent complete dissolution and hence, experienced the same nucleation event and growth during deposition. This corresponds with the findings by Balikci et al. [85], who reported that the degree of γ′ precipitation in IN738LC does not change when a solution heat treatment is conducted above a certain critical temperature.

The increase in coarsening rate (Fig. 8) during thermal cycling can first be ascribed to the high peak temperature of the layers [86]. The coarsening rate of γ′ is known to increase rapidly with temperature due to the exponential growth of diffusion activity. Also, the simultaneous dissolution with coarsening could be another reason for the high coarsening rate, as γ′ coarsening is a diffusion-driven process where large particles grow by consuming smaller ones [78][84][86][87]. The steady growth of γ′ towards the bottom of the build is due to the much lower layer peak temperature, which is almost close to the build temperature, and reduced dissolution activity, as is seen in the much lower solute concentration in γ′ compared to those in the full and partial dissolution regions.

4.2.2. During cooling

The much higher phase fraction of ∼40% upon cooling signifies the tendency of γ′ to reach equilibrium at lower temperatures (Fig. 4). This is due to the precipitation of secondary γ′ and a further increase in the size of existing primary γ′, which leads to a multimodal size distribution of γ′ after cooling [38][73][88][89][90]. The reason for secondary γ′ formation during cooling is as follows: As cooling progresses, it becomes increasingly challenging to redistribute solute elements in the matrix owing to their lower mobility [38][73]. A higher supersaturation level in regions away from or free of the existing γ′ precipitates is achieved, making them suitable sites for additional nucleation bursts. More cooling leads to the growth of these secondary γ′ precipitates, but as the temperature and in turn, the solute diffusivity is low, growth remains slow.

4.3. Carbides

MC carbides in IN738 are known to have a significant impact on the high-temperature strength. They can also act as effective hardening particles and improve the creep resistance [91]. Precipitation of MC carbides in IN738 and several other superalloys is known to occur during solidification or thermal treatments (e.g., hot isostatic pressing) [92]. In our case, this means that the MC carbides within the E-PBF build formed because of the thermal exposure from the E-PBF thermal cycle in addition to initial solidification. Our simulation confirms this as MC carbides appear during layer heating (Fig. 5). The constant and stable phase fraction of MC carbides during thermal cycling can be attributed to their high melting point (∼1360 °C) and the short holding time at peak temperatures [75][93][94]. The solvus temperature for most MC carbides exceeds most of the peak temperatures observed in our simulation, and carbide dissolution kinetics at temperatures above the solvus are known to be comparably slow [95]. The stable phase fraction and random distribution of MC carbides signifies the slight influence on the gradient in hardness.

4.4. Comparison of simulations and experiments

4.4.1. Precipitate phase fraction and morphology as a function of build height

A qualitative agreement is observed for the phase fraction of carbides, i.e. ∼0.8% in the experiment and ∼0.9% in the simulation. The phase fraction of γ′ differs, with the experiment reporting a value of ∼51% and the simulation, 40%. Despite this, the size distribution of primary γ′ along the build shows remarkable consistency between experimental and computational analyses. It is worth noting that the primary γ′ morphology in the experimental analysis is observed in the as-fabricated state, whereas the simulation (Fig. 8) captures it during deposition process. The primary γ′ size in the experiment is expected to experience additional growth during the cooling phase. Regardless, both show similar trends in primary γ′ size increments from the top to the bottom of the build. The larger primary γ’ size in the simulation versus the experiment can be attributed to the fact that experimental and simulation results are based on 2D and 3D data, respectively. The absence of stereological considerations [96] in our analysis could have led to an underestimation of the precipitate sizes from SEM measurements. The early starts of coarsening (8th layer) in the experiment compared to the simulation (45th layer) can be attributed to a higher actual γ′ solvus temperature than considered in our simulation [47]. The solvus temperature of γ′ in a Ni-based superalloy is mainly determined by the detailed composition. A high amount of Cr and Co are known to reduce the solvus temperature, whereas Ta and Mo will increase it [97][98][99]. The elemental composition from our experimental work was used for the simulation except for Ta. It should be noted that Ta is not included in the thermodynamic database in MatCalc used, and this may have reduced the solvus temperature. This could also explain the relatively higher γ′ phase fraction in the experiment than in simulation, as a higher γ′ solvus temperature will cause more γ′ to precipitate and grow early during cooling [99][100].

Another possible cause of this deviation can be attributed to the extent of γ′ dissolution, which is mainly determined by the peak temperature. It can be speculated that individual peak temperatures at different layers in the simulation may have been over-predicted. However, one needs to consider that the true thermal profile is likely more complicated in the actual E-PBF process [101]. For example, the current model assumes that the thermophysical properties of the material are temperature-independent, which is not realistic. Many materials, including IN738, exhibit temperature-dependent properties such as thermal conductivityspecific heat capacity, and density [102]. This means that heat transfer simulations may underestimate or overestimate the temperature gradients and cooling rates within the powder bed and the solidified part. Additionally, the model does not account for the reduced thermal diffusivity through unmelted powder, where gas separating the powder acts as insulation, impeding the heat flow [1]. In E-PBF, the unmelted powder regions with trapped gas have lower thermal diffusivity compared to the fully melted regions, leading to localized temperature variations, and altered solidification behavior. These limitations can impact the predictions, particularly in relation to the carbide dissolution, as the peak temperatures may be underestimated.

While acknowledging these limitations, it is worth emphasizing that achieving a detailed and accurate representation of each layer’s heat source would impose tough computational challenges. Given the substantial layer count in E-PBF, our decision to employ a semi-analytical approximation strikes a balance between computational feasibility and the capture of essential trends in thermal profiles across diverse build layers. In future work, a dual-calibration strategy is proposed to further reduce simulation-experiment disparities. By refining temperature-independent thermophysical property approximations and absorptivity in the heat source model, and by optimizing interfacial energy descriptions in the kinetic model, the predictive precision could be enhanced. Further refining the simulation controls, such as adjusting the precipitate class size may enhance quantitative comparisons between modeling outcomes and experimental data in future work.

4.4.2. Multimodal size distribution of γ′ and concentration

Another interesting feature that sees qualitative agreement between the simulation and the experiment is the multimodal size distribution of γ′. The formation of secondary γ′ particles in the experiment and most E-PBF Ni-based superalloys is suggested to occur at low temperatures, during final cooling to RT [16][73][90]. However, so far, this conclusion has been based on findings from various continuous cooling experiments, as the study of the evolution during AM would require an in-situ approach. Our simulation unambiguously confirms this in an AM context by providing evidence for secondary γ′ precipitation during slow cooling to RT. Additionally, it is possible to speculate that the chemical segregation occurring during solidification, due to the preferential partitioning of certain elements between the solid and liquid phases, can contribute to the multimodal size distribution during deposition [51]. This is because chemical segregation can result in variations in the local composition of superalloys, which subsequently affects the nucleation and growth of γ′. Regions with higher concentrations of alloying elements will encourage the formation of larger γ′ particles, while regions with lower concentrations may favor the nucleation of smaller precipitates. However, it is important to acknowledge that the elevated temperature during the E-PBF process will largely homogenize these compositional differences [103][104].

A good correlation is also shown in the composition of major γ′ forming elements (Al and Ti) in primary and secondary γ′. Both experiment and simulation show an increasing trend for Al content and a decreasing trend for Ti content from primary to secondary γ′. The slight composition differences between primary and secondary γ′ particles are due to the different diffusivity of γ′ stabilizers at different thermal conditions [105][106]. As the formation of multimodal γ′ particles with different sizes occurs over a broad temperature range, the phase chemistry of γ′ will be highly size dependent. The changes in the chemistry of various γ′ (primary, secondary, and tertiary) have received significant attention since they have a direct influence on the performance [68][105][107][108][109]. Chen et al. [108][109], reported a high Al content in the smallest γ′ precipitates compared to the largest, while Ti showed an opposite trend during continuous cooling in a RR1000 Ni-based superalloy. This was attributed to the temperature and cooling rate at which the γ′ precipitates were formed. The smallest precipitates formed last, at the lowest temperature and cooling rate. A comparable observation is evident in the present investigation, where the secondary γ′ forms at a low temperature and cooling rate in comparison to the primary. The temperature dependence of γ′ chemical composition is further evidenced in supplementary Fig. S4, which shows the equilibrium chemical composition of γ′ as a function of temperature.

5. Conclusions

A correlative modelling approach capable of predicting solid-state phase transformations kinetics in metal AM was developed. This approach involves computational simulations with a semi-analytical heat transfer model and the MatCalc thermo-kinetic software. The method was used to predict the phase transformation kinetics and detailed morphology and chemistry of γ′ and MC during E-PBF of IN738 Ni-based superalloy. The main conclusions are:

  • 1.The computational simulations are in qualitative agreement with the experimental observations. This is particularly true for the γ′ size distribution along the build height, the multimodal size distribution of particles, and the phase fraction of MC carbides.
  • 2.The deviations between simulation and experiment in terms of γ′ phase fraction and location in the build are most likely attributed to a higher γ′ solvus temperature during the experiment than in the simulation, which is argued to be related to the absence of Ta in the MatCalc database.
  • 3.The dissolution and precipitation of γ′ occur fast and under non-equilibrium conditions. The level of γ′ dissolution determines the gradient in γ′ size distribution along the build. After thermal cycling, the final cooling to room temperature has further significant impacts on the final γ′ size, morphology, and distribution.
  • 4.A negligible amount of γ′ forms in the first deposited layer before subsequent layer deposition, and a small amount of γ′ may also form in the powder induced by the 1000 °C elevated build temperature before melting.

Our findings confirm the suitability of MatCalc to predict the microstructural evolution at various positions throughout a build in a Ni-based superalloy during E-PBF. It also showcases the suitability of a tool which was originally developed for traditional thermo-mechanical processing of alloys to the new additive manufacturing context. Our simulation capabilities are likely extendable to other alloy systems that undergo solid-state phase transformations implemented in MatCalc (various steels, Ni-based superalloys, and Al-alloys amongst others) as well as other AM processes such as L-DED and L-PBF which have different thermal cycle characteristics. New tools to predict the microstructural evolution and properties during metal AM are important as they provide new insights into the complexities of AM. This will enable control and design of AM microstructures towards advanced materials properties and performances.

CRediT authorship contribution statement

Primig Sophie: Writing – review & editing, Supervision, Resources, Project administration, Funding acquisition, Conceptualization. Adomako Nana Kwabena: Writing – original draft, Writing – review & editing, Visualization, Software, Investigation, Formal analysis, Conceptualization. Haghdadi Nima: Writing – review & editing, Supervision, Project administration, Methodology, Conceptualization. Dingle James F.L.: Methodology, Conceptualization, Software, Writing – review & editing, Visualization. Kozeschnik Ernst: Writing – review & editing, Software, Methodology. Liao Xiaozhou: Writing – review & editing, Project administration, Funding acquisition. Ringer Simon P: Writing – review & editing, Project administration, Funding acquisition.

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Acknowledgements

This research was sponsored by the Department of Industry, Innovation, and Science under the auspices of the AUSMURI program – which is a part of the Commonwealth’s Next Generation Technologies Fund. The authors acknowledge the facilities and the scientific and technical assistance at the Electron Microscope Unit (EMU) within the Mark Wainwright Analytical Centre (MWAC) at UNSW Sydney and Microscopy Australia. Nana Adomako is supported by a UNSW Scientia PhD scholarship. Michael Haines’ (UNSW Sydney) contribution to the revised version of the original manuscript is thankfully acknowledged.

Appendix A. Supplementary material

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Supplementary material.

Data Availability

Data will be made available on request.

References

Thermo-fluid modeling of influence of attenuated laser beam intensity profile on melt pool behavior in laser-assisted powder-based direct energy deposition

레이저 보조 분말 기반 직접 에너지 증착에서 용융 풀 거동에 대한 감쇠 레이저 빔 강도 프로파일의 영향에 대한 열유체 모델링

Thermo-fluid modeling of influence of attenuated laser beam intensity profile on melt pool behavior in laser-assisted powder-based direct energy deposition

Mohammad Sattari, Amin Ebrahimi, Martin Luckabauer, Gert-willem R.B.E. Römer

Research output: Chapter in Book/Conference proceedings/Edited volume › Conference contribution › Professional

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Abstract

A numerical framework based on computational fluid dynamics (CFD), using the finite volume method (FVM) and volume of fluid (VOF) technique is presented to investigate the effect of the laser beam intensity profile on melt pool behavior in laser-assisted powder-based directed energy deposition (L-DED). L-DED is an additive manufacturing (AM) process that utilizes a laser beam to fuse metal powder particles. To assure high-fidelity modeling, it was found that it is crucial to accurately model the interaction between the powder stream and the laser beam in the gas region above the substrate. The proposed model considers various phenomena including laser energy attenuation and absorption, multiple reflections of the laser rays, powder particle stream, particle-fluid interaction, temperature-dependent properties, buoyancy effects, thermal expansion, solidification shrinkage and drag, and Marangoni flow. The latter is induced by temperature and element-dependent surface tension. The model is validated using experimental results and highlights the importance of considering laser energy attenuation. Furthermore, the study investigates how the laser beam intensity profile affects melt pool size and shape, influencing the solidification microstructure and mechanical properties of the deposited material. The proposed model has the potential to optimize the L-DED process for a variety of materials and provides insights into the capability of numerical modeling for additive manufacturing optimization.

Original languageEnglish
Title of host publicationFlow-3D World Users Conference
Publication statusPublished – 2023
EventFlow-3D World User Conference – Strasbourg, France
Duration: 5 Jun 2023 → 7 Jun 2023

Conference

ConferenceFlow-3D World User Conference
Country/TerritoryFrance
CityStrasbourg
Period5/06/23 → 7/06/23
Numerical simulation on molten pool behavior of narrow gap gas tungsten arc welding

좁은 간격 가스 텅스텐 아크 용접의 용융 풀 거동에 대한 수치 시뮬레이션

Numerical simulation on molten pool behavior of narrow gap gas tungsten arc welding

The International Journal of Advanced Manufacturing Technology (2023)Cite this article

Abstract

As a highly efficient thick plate welding resolution, narrow gap gas tungsten arc welding (NG-GTAW) is in the face of a series of problems like inter-layer defects like pores, lack of fusion, inclusion of impurity, and the sensitivity to poor sidewall fusion, which is hard to be repaired after the welding process. This study employs numerical simulation to investigate the molten pool behavior in NG-GTAW root welding. A 3D numerical model was established, where a body-fitted coordinate system was applied to simulate the electromagnetic force, and a bridge transition model was developed to investigate the wire–feed root welding. The simulated results were validated experimentally. Results show that the molten pool behavior is dominated by electromagnetic force when the welding current is relatively high, and the dynamic change of the vortex actually determines the molten pool morphology. For self-fusion welding, there are two symmetric inward vortices in the cross-section and one clockwise vortex in the longitudinal section. With the increasing welding current, the vortices in the cross-section gradually move to the arc center with a decreasing range, while the vortex in the longitudinal section moves backward. With the increasing traveling speed, the vortices in the cross-section move toward the surface of the molten pool with a decreasing range, and the horizontal component of liquid metal velocity changes in the longitudinal section. For wire–feed welding, the filling metal strengthens the downward velocity component; as a result, the vortex formation is blocked in the cross-section and is strengthened in the longitudinal section.

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Figure 14. Defects: (a) Unmelt defects(Scheme NO.4);(b) Pores defects(Scheme NO.1); (c); Spattering defect (Scheme NO.3); (d) Low overlapping rate defects(Scheme NO.5).

Molten pool structure, temperature and velocity
flow in selective laser melting AlCu5MnCdVA alloy

용융 풀 구조, 선택적 온도 및 속도 흐름 레이저 용융 AlCu5MnCdVA 합금

Pan Lu1 , Zhang Cheng-Lin2,6,Wang Liang3, Liu Tong4 and Liu Jiang-lin5
1 Aviation and Materials College, Anhui Technical College of Mechanical and Electrical Engineering, Wuhu Anhui 241000, People’s
Republic of China 2 School of Engineering Science, University of Science and Technology of China, Hefei Anhui 230026, People’s Republic of China 3 Anhui Top Additive Manufacturing Technology Co., Ltd., Wuhu Anhui 241300, People’s Republic of China 4 Anhui Chungu 3D Printing Institute of Intelligent Equipment and Industrial Technology, Anhui 241300, People’s Republic of China 5 School of Mechanical and Transportation Engineering, Taiyuan University of Technology, Taiyuan Shanxi 030024, People’s Republic of
China 6 Author to whom any correspondence should be addressed.
E-mail: ahjdpanlu@126.com, jiao__zg@126.com, ahjdjxx001@126.com,tongliu1988@126.com and liujianglin@tyut.edu.cn

Keywords

SLM, molten pool, AlCu5MnCdVA alloy, heat flow, velocity flow, numerical simulation

Abstract

선택적 레이저 용융(SLM)은 열 전달, 용융, 상전이, 기화 및 물질 전달을 포함하는 복잡한 동적 비평형 프로세스인 금속 적층 제조(MAM)에서 가장 유망한 기술 중 하나가 되었습니다. 용융 풀의 특성(구조, 온도 흐름 및 속도 흐름)은 SLM의 최종 성형 품질에 결정적인 영향을 미칩니다. 이 연구에서는 선택적 레이저 용융 AlCu5MnCdVA 합금의 용융 풀 구조, 온도 흐름 및 속도장을 연구하기 위해 수치 시뮬레이션과 실험을 모두 사용했습니다.

그 결과 용융풀의 구조는 다양한 형태(깊은 오목 구조, 이중 오목 구조, 평면 구조, 돌출 구조 및 이상적인 평면 구조)를 나타냈으며, 용융 풀의 크기는 약 132 μm × 107 μm × 50 μm였습니다. : 용융풀은 초기에는 여러 구동력에 의해 깊이 15μm의 깊은 오목형상이었으나, 성형 후기에는 장력구배에 의해 높이 10μm의 돌출형상이 되었다. 용융 풀 내부의 금속 흐름은 주로 레이저 충격력, 금속 액체 중력, 표면 장력 및 반동 압력에 의해 구동되었습니다.

AlCu5MnCdVA 합금의 경우, 금속 액체 응고 속도가 매우 빠르며(3.5 × 10-4 S), 가열 속도 및 냉각 속도는 각각 6.5 × 107 K S-1 및 1.6 × 106 K S-1 에 도달했습니다. 시각적 표준으로 표면 거칠기를 선택하고, 낮은 레이저 에너지 AlCu5MnCdVA 합금 최적 공정 매개변수 창을 수치 시뮬레이션으로 얻었습니다: 레이저 출력 250W, 부화 공간 0.11mm, 층 두께 0.03mm, 레이저 스캔 속도 1.5m s-1 .

또한, 실험 프린팅과 수치 시뮬레이션과 비교할 때, 용융 풀의 폭은 각각 약 205um 및 약 210um이었고, 인접한 두 용융 트랙 사이의 중첩은 모두 약 65um이었다. 결과는 수치 시뮬레이션 결과가 실험 인쇄 결과와 기본적으로 일치함을 보여 수치 시뮬레이션 모델의 정확성을 입증했습니다.

Selective Laser Melting (SLM) has become one of the most promising technologies in Metal Additive Manufacturing (MAM), which is a complex dynamic non-equilibrium process involving heat transfer, melting, phase transition, vaporization and mass transfer. The characteristics of the molten pool (structure, temperature flow and velocity flow) have a decisive influence on the final forming quality of SLM. In this study, both numerical simulation and experiments were employed to study molten pool structure, temperature flow and velocity field in Selective Laser Melting AlCu5MnCdVA alloy. The results showed the structure of molten pool showed different forms(deep-concave structure, double-concave structure, plane structure, protruding structure and ideal planar structure), and the size of the molten pool was approximately 132 μm × 107 μm × 50 μm: in the early stage, molten pool was in a state of deep-concave shape with a depth of 15 μm due to multiple driving forces, while a protruding shape with a height of 10 μm duo to tension gradient in the later stages of forming. The metal flow inside the molten pool was mainly driven by laser impact force, metal liquid gravity, surface tension and recoil pressure. For AlCu5MnCdVA alloy, metal liquid solidification speed was extremely fast(3.5 × 10−4 S), the heating rate and cooling rate reached 6.5 × 107 K S−1 and 1.6 × 106 K S−1 , respectively. Choosing surface roughness as a visual standard, low-laser energy AlCu5MnCdVA alloy optimum process parameters window was obtained by numerical simulation: laser power 250 W, hatching space 0.11 mm, layer thickness 0.03 mm, laser scanning velocity 1.5 m s−1 . In addition, compared with experimental printing and numerical simulation, the width of the molten pool was about 205 um and about 210 um, respectively, and overlapping between two adjacent molten tracks was all about 65 um. The results showed that the numerical simulation results were basically consistent with the experimental print results, which proved the correctness of the numerical simulation model.

Figure 1. AlCu5MnCdVA powder particle size distribution.
Figure 1. AlCu5MnCdVA powder particle size distribution.
Figure 2. AlCu5MnCdVA powder
Figure 2. AlCu5MnCdVA powder
Figure 3. Finite element model and calculation domains of SLM.
Figure 3. Finite element model and calculation domains of SLM.
Figure 4. SLM heat transfer process.
Figure 4. SLM heat transfer process.
Figure 14. Defects: (a) Unmelt defects(Scheme NO.4);(b) Pores defects(Scheme NO.1); (c); Spattering defect (Scheme NO.3); (d) Low
overlapping rate defects(Scheme NO.5).
Figure 17. Two-pass molten tracks overlapping for Scheme NO.2.
Figure 17. Two-pass molten tracks overlapping for Scheme NO.2.

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Figure 4.24 - Model with virtual valves in the extremities of the geometries to simulate the permeability of the mold promoting a more uniformed filling

Optimization of filling systems for low pressure by Flow-3D

Dissertação de Mestrado
Ciclo de Estudos Integrados Conducentes ao
Grau de Mestre em Engenharia Mecânica
Trabalho efectuado sob a orientação do
Doutor Hélder de Jesus Fernades Puga
Professor Doutor José Joaquim Carneiro Barbosa

ABSTRACT

논문의 일부로 튜터 선택 가능성과 해결해야 할 주제가 설정되는 매개변수를 염두에 두고 개발 주제 ‘Flow- 3D ®에 의한 저압 충전 시스템 최적화’가 선택되었습니다. 이를 위해서는 달성해야 할 목표와 이를 달성하기 위한 방법을 정의하는 것이 필요했습니다.

충전 시스템을 시뮬레이션하고 검증할 수 있는 광범위한 소프트웨어에도 불구하고 Flow-3D®는 시장에서 최고의 도구 중 하나로 표시되어 전체 충전 프로세스 및 행동 표현과 관련하여 탁월한 정확도로 시뮬레이션하는 능력을 입증했습니다.

이를 위해 관련 프로세스를 더 잘 이해하고 충진 시스템 시뮬레이션을 위한 탐색적 기반 역할을 하기 위해 이 도구를 탐색하는 것이 중요합니다. 지연 및 재료 낭비에 반영되는 실제적인 측면에서 충전 장치의 치수를 완벽하게 만드는 비용 및 시간 낭비. 이러한 방식으로 저압 주조 공정에서 충진 시스템을 설계하고 물리적 모델을 탐색하여 특성화하는 방법론을 검증하기 위한 것입니다.

이를 위해 다음 주요 단계를 고려하십시오.

시뮬레이션 소프트웨어 Flow 3D® 탐색;
충전 시스템 모델링;
모델의 매개변수를 탐색하여 모델링된 시스템의 시뮬레이션, 검증 및 최적화.

따라서 연구 중인 압력 곡선과 주조 분석에서 가장 관련성이 높은 정보의 최종 마이닝을 검증하기 위한 것입니다.

사용된 압력 곡선은 수집된 문헌과 이전에 수행된 실제 작업을 통해 얻었습니다. 결과를 통해 3단계 압력 곡선이 층류 충진 체계의 의도된 목적과 관련 속도가 0.5 𝑚/𝑠를 초과하지 않는다는 결론을 내릴 수 있었습니다.

충전 수준이 2인 압력 곡선은 0.5 𝑚/𝑠 이상의 속도로 영역을 채우는 더 난류 시스템을 갖습니다. 열전달 매개변수는 이전에 얻은 값이 주물에 대한 소산 거동을 확증하지 않았기 때문에 연구되었습니다.

이러한 방식으로 주조 공정에 더 부합하는 새로운 가치를 얻었습니다. 달성된 결과는 유사한 것으로 나타난 NovaFlow & Solid®에 의해 생성된 결과와 비교되어 시뮬레이션에서 설정된 매개변수를 검증했습니다. Flow 3D®는 주조 부품 시뮬레이션을 위한 강력한 도구로 입증되었습니다.

As part of the dissertation and bearing in mind the parameters in which the possibility of a choice of tutor and the subject to be addressed is established, the subject for development ’Optimization of filling systems for low pressure by Flow 3D ®’ was chosen. For this it was necessary to define the objectives to achieve and the methods to attain them. Despite the wide range of software able to simulate and validate filling systems, Flow 3D® has been shown as one of the best tools in the market, demonstrating its ability to simulate with distinctive accuracy with respect to the entire process of filling and the behavioral representation of the fluid obtained. To this end, it is important to explore this tool for a better understanding of the processes involved and to serve as an exploratory basis for the simulation of filling systems, simulation being one of the great strengths of the current industry due to the need to reduce costs and time waste, in practical terms, that lead to the perfecting of the dimensioning of filling devices, which are reflected in delays and wasted material. In this way it is intended to validate the methodology to design a filling system in lowpressure casting process, exploring their physical models and thus allowing for its characterization. For this, consider the following main phases: The exploration of the simulation software Flow 3D®; modeling of filling systems; simulation, validation and optimization of systems modeled by exploring the parameters of the models. Therefore, it is intended to validate the pressure curves under study and the eventual mining of the most relevant information in a casting analysis. The pressure curves that were used were obtained through the gathered literature and the practical work previously performed. Through the results it was possible to conclude that the pressure curve with 3 levels meets the intended purpose of a laminar filling regime and associated speeds never exceeding 0.5 𝑚/𝑠. The pressure curve with 2 filling levels has a more turbulent system, having filling areas with velocities above 0.5 𝑚/𝑠. The heat transfer parameter was studied due to the values previously obtained didn’t corroborate the behavior of dissipation regarding to the casting. In this way, new values, more in tune with the casting process, were obtained. The achieved results were compared with those generated by NovaFlow & Solid®, which were shown to be similar, validating the parameters established in the simulations. Flow 3D® was proven a powerful tool for the simulation of casting parts.

키워드

저압, Flow 3D®, 시뮬레이션, 파운드리, 압력-시간 관계,Low Pressure, Flow 3D®, Simulation, Foundry, Pressure-time relation

Figure 4.24 - Model with virtual valves in the extremities of the geometries to simulate the permeability of the mold promoting a more uniformed filling
Figure 4.24 – Model with virtual valves in the extremities of the geometries to simulate the permeability of the mold promoting a more uniformed filling
Figure 4.39 - Values of temperature contours using full energy heat transfer parameter for simula
Figure 4.39 – Values of temperature contours using full energy heat transfer parameter for simula
Figure 4.40 – Comparison between software simulations (a) Flow 3D® simulation,
(b) NovaFlow & Solid® simulation
Figure 4.40 – Comparison between software simulations (a) Flow 3D® simulation, (b) NovaFlow & Solid® simulation

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Figure 1: Mold drawings

3D Flow and Temperature Analysis of Filling a Plutonium Mold

플루토늄 주형 충전의 3D 유동 및 온도 분석

Authors: Orenstein, Nicholas P. [1]

Publication Date:2013-07-24
Research Org.: Los Alamos National Lab. (LANL), Los Alamos, NM (United States)
Sponsoring Org.: DOE/LANL
OSTI Identifier: 1088904
Report Number(s): LA-UR-13-25537
DOE Contract Number: AC52-06NA25396
Resource Type: Technical Report
Country of Publication: United States
Language: English
Subject: Engineering(42); Materials Science(36); Radiation Chemistry, Radiochemistry, & Nuclear Chemistry(38)

Introduction

The plutonium foundry at Los Alamos National Laboratory casts products for various special nuclear applications. However, plutonium’s radioactivity, material properties, and security constraints complicate the ability to perform experimental analysis of mold behavior. The Manufacturing Engineering and Technologies (MET-2) group previously developed a graphite mold to vacuum cast small plutonium disks to be used by the Department of Homeland Security as point sources for radiation sensor testing.

A two-stage pouring basin consisting of a funnel and an angled cavity directs the liquid into a vertical runner. A stack of ten disk castings connect to the runner by horizontal gates. Volumetric flow rates were implemented to limit overflow into the funnel and minimize foundry returns. Models using Flow-3D computational fluid dynamics software are employed here to determine liquid Pu flow paths, optimal pour regimes, temperature changes, and pressure variations.

Setup

Hardcopy drawings provided necessary information to create 3D .stl models for import into Flow-3D (Figs. 1 and 2). The mesh was refined over several iterations to isolate the disk cavities, runner, angled cavity, funnel, and input pour. The final flow and mold-filling simulation utilizes a fine mesh with ~5.5 million total cells. For the temperature study, the mesh contained 1/8 as many cells to reduce computational time and set temperatures to 850 °C for the molten plutonium and 500 °C for the solid graphite mold components (Fig. 3).

Flow-3D solves mass continuity and Navier-Stokes momentum equations over the structured rectangular grid model using finite difference and finite volume numerical algorithms. The solver includes terms in the momentum equation for body and viscous accelerations and uses convective heat transfer.

Simulation settings enabled Flow-3D physics calculations for gravity at 980.665 cm/s 2 in the negative Z direction (top of mold to bottom); viscous, turbulent, incompressible flow using dynamically-computed Renormalized Group Model turbulence calculations and no-slip/partial slip wall shear, and; first order, full energy equation heat transfer.

Mesh boundaries were all set to symmetric boundary conditions except for the Zmin boundary set to outflow and the Zmax boundary set to a volume flow. Vacuum casting conditions and the high reactivity of remaining air molecules with Pu validate the assumption of an initially fluidless void.

Results

The flow follows a unique three-dimensional path. The mold fills upwards with two to three disks receiving fluid in a staggered sequence. Figures 5-9 show how the fluid fills the cavity, and Figure 7 includes the color scale for pressure levels in these four figures. The narrow gate causes a high pressure region which forces the fluid to flow down the cavity centerline.

It proceeds to splash against the far wall and then wrap around the circumference back to the gate (Figs. 5 and 6). Flow in the angled region of the pouring basin cascades over the bottom ledge and attaches to the far wall of the runner, as seen in Figure 7.

This channeling becomes less pronounced as fluid volume levels increase. Finally, two similar but non-uniform depressed regions form about the centerline. These regions fill from their perimeter and bottom until completion (Fig. 8). Such a pattern is counter, for example, to a steady scenario in which a circle of molten Pu encompassing the entire bottom surface rises as a growing cylinder.

Cavity pressure becomes uniform when the cavity is full. Pressure levels build in the rising well section of the runner, where impurities were found to settle in actual casting. Early test simulations optimized the flow as three pours so that the fluid would never overflow to the funnel, the cavities would all fill completely, and small amounts of fluid would remain as foundry returns in the angled cavity.

These rates and durations were translated to the single 2.7s pour at 100 cm 3 per second used here. Figure 9 shows anomalous pressure fluctuations which occurred as the cavities became completely filled. Multiple simulations exhibited a rapid change in pressure from positive to negative and back within the newly-full disk and surrounding, already-full disks.

The time required to completely fill each cavity is plotted in Figure 10. Results show negligible temperature change within the molten Pu during mold filling and, as seen in Figure 11, at fill completion.

Figure 1: Mold drawings
Figure 1: Mold drawings
Figure 2: Mold Assembly
Figure 2: Mold Assembly
Figure 4: Actual mold and cast Pu
Figure 4: Actual mold and cast Pu
Figure 5: Bottom cavity filling
from runner
Figure 5: Bottom cavity filling from runner
Figure 6: Pouring and filling
Figure 6: Pouring and filling
Figure 8: Edge detection of cavity fill geometry. Two similar depressed areas form
about the centerline. Top cavity shown; same pressure scale as other figures
Figure 8: Edge detection of cavity fill geometry. Two similar depressed areas form about the centerline. Top cavity shown; same pressure scale as other figures
Figure 10: Cavity fill times,from first fluid contact with pouring basin, Figure 11:Fluid temperature remains essentially constant
Figure 10: Cavity fill times,from first fluid contact with pouring basin, Figure 11:Fluid temperature remains essentially constant

Conclusions

Non-uniform cavity filling could cause crystal microstructure irregularities during solidification. However, the small temperature changes seen – due to large differences in specific heat between Pu and graphite – over a relatively short time make such problems unlikely in this case.

In the actual casting, cooling required approximately ten minutes. This large difference in time scales further reduces the chance for temperature effects in such a superheated scenario. Pouring basin emptying decreases pressure at the gate which extends fill time of the top two cavities.

The bottom cavity takes longer to fill because fluid must first enter the runner and fill the well. Fill times continue linearly until the top two cavities. The anomalous pressure fluctuations may be due to physical attempts by the system to reach equilibrium, but they are more likely due to numerical errors in the Flow3D solver.

Unsuccessful tests were performed to remove them by halving fluid viscosity. The fine mesh reduced, but did not eliminate, the extent of the fluctuations. Future work is planned to study induction and heat transfer in the full Pu furnace system, including quantifying temporal lag of the cavity void temperature to the mold wall temperature during pre-heat and comparing heat flux levels between furnace components during cool-down.

Thanks to Doug Kautz for the opportunity to work with MET-2 and for assigning an interesting unclassified project. Additional thanks to Mike Bange for CFD guidance, insight of the project’s history, and draft review.

Fig. 6 LH2 isotherms at 1020 s.

액체-수소 탱크를 위한 결합된 열역학-유체-역학 솔루션

Coupled thermodynamic-fluid-dynamic solution for a liquid-hydrogen tank

G. D. Grayson

Published Online:23 May 2012 https://doi.org/10.2514/3.26706

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Introduction

ROPELLANT 열 성층화 및 외부 교란에 대한 유체 역학적 반응은 발사체와 우주선 모두에서 중요합니다. 과거에는 결합된 솔루션을 제공할 수 있는 충분한 계산 기술이 부족하여 이러한 문제를 개별적으로 해결했습니다.1

이로 인해 모델링 기술의 불확실성을 허용하기 위해 큰 안전 계수를 가진 시스템이 과도하게 설계되었습니다. 고중력 환경과 저중력 환경 모두에서 작동하도록 설계된 미래 시스템은 기술적으로나 재정적으로 실현 가능하도록 과잉 설계 및 안전 요소가 덜 필요합니다.

이러한 유체 시스템은 열역학 및 유체 역학이 모두 중요한 환경에서 모델의 기능을 광범위하게 검증한 후에만 고충실도 수치 모델을 기반으로 할 수 있습니다. 상용 컴퓨터 코드 FLOW-3D2는 유체 역학 및 열 모델링 모두에서 가능성을 보여주었으며,1 따라서 열역학-유체-역학 엔지니어링 문제에서 결합된 질량, 운동량 및 에너지 방정식을 푸는 데 적합함을 시사합니다.

발사체의 복잡한 액체 가스 시스템에 대한 포괄적인 솔루션을 달성하기 위한 첫 번째 단계로 액체 유체 역학과 열역학을 통합하는 제안된 상단 단계 액체-수소(Lit) 탱크의 간단한 모델이 여기에 제시됩니다. FLOW-3D FLOW-3D 프로그램은 Los Alamos Scientific Laboratory에서 시작되었으며 마커 및 셀 방법에서 파생된 것입니다.3 현재 상태로 가져오기 위해 수년에 걸쳐 광범위한 코드 수정이 이루어졌습니다.2

프로그램은 다음과 같습니다. 일반 Navier-Stokes 방정식을 풀기 위해 수치 근사의 중앙 유한 차분 방법을 사용하는 3차원 유체 역학 솔버입니다. 모멘텀 및 에너지 방정식의 섹션은 특정 응용 프로그램에 따라 활성화 또는 비활성화할 수 있습니다.

코드는 1994년 9월 13일 접수를 인용하기 위해 무액체 표면, 복잡한 용기 기하학, 여러 점성 모델, 표면 장력, 다공성 매체를 통한 흐름 및 응고와 함께 압축성 또는 비압축성 유동 가정을 제공합니다. 1995년 1월 15일에 받은 개정; 1995년 2월 17일 출판 승인.

ROPELLANT thermal stratification and fluid-dynamic response to external disturbances are of concern in both launch vehicles and spacecraft. In the past these problems have been addressed separately for want of sufficient computational technology to provide for coupled solutions.1 This has resulted in overdesigned systems with large safety factors to allow for the uncertainty in modeling techniques. Future systems designed to perform in both highand low-gravity environments will require less overdesign and safety factors to be technically and financially feasible. Such fluid systems can be based on high-fidelity numerical models only after extensive validation of the models’ capabilities in environments where both the thermodynamics and the fluid dynamics are important. The commercial computer code FLOW-3D2 has shown promise in both fluid-dynamic and thermal modeling,1 thus suggesting suitability for solving the coupled mass, momentum, and energy equations in thermodynamic-fluid-dynamic engineering problems. As a first step to achieving a comprehensive solution for complex liquidgas systems in a launch vehicle, a simple model of a proposed upper-stage liquid-hydrogen (Lit) tank incorporating the liquid fluid dynamics and thermodynamics is presented here. FLOW-3D The FLOW-3D program originated at the Los Alamos Scientific Laboratory and is a derivative of the marker-and-cell method.3 Extensive code modifications have been made over the years to bring it to its present state.2 The program is a three-dimensional fluiddynamic solver that uses a central finite-difference method of numerical approximation to solve the general Navier-Stokes equations. Sections of the momentum and energy equations can be enabled or disabled depending on the particular application. The code provides compressible or incompressible flow assumptions with liquid free surfaces, complex container geometries, several viscosity models, surface tension, flow though porous media, and solidification, to cite Received Sept. 13, 1994; revision received Jan. 15, 1995; accepted for publication Feb. 17, 1995. Copyright © 1995 by the American Institute of Aeronautics and Astronautics, Inc. All rights reserved. *Engineer/Scientist, Propulsion Analysis and Hydraulics, Space Transportation Division, MS 13-3, 5301 Bolsa Avenue. Member AIAA. a few of the possibilities. Further information on FLOW-3D’s capabilities and details of the numerical algorithms can be found in Ref. 2

Fig. 1 Axial-acceleration history.
Fig. 1 Axial-acceleration history.
Fig. 2 Heat flux histories.
Fig. 2 Heat flux histories.
Fig. 3 LHi isotherms at 50 s.
Fig. 3 LHi isotherms at 50 s.
Fig. 4 LH2 isotherms at 300 s
Fig. 4 LH2 isotherms at 300 s
Fig. 5 LH2 isotherms at 880 s.
Fig. 5 LH2 isotherms at 880 s.
Fig. 6 LH2 isotherms at 1020 s.
Fig. 6 LH2 isotherms at 1020 s.
Fig. 7 Tank-outlet temperature history.
Fig. 7 Tank-outlet temperature history.
Development of macro-defect-free PBF-EB-processed Ti–6Al–4V alloys with superior plasticity using PREP-synthesized powder and machine learning-assisted process optimization

Development of macro-defect-free PBF-EB-processed Ti–6Al–4V alloys with superior plasticity using PREP-synthesized powder and machine learning-assisted process optimization

Yunwei GuiabKenta Aoyagib Akihiko Chibab
aDepartment of Materials Processing, Graduate School of Engineering, Tohoku University, 6-6 Aramaki Aza Aoba, Aoba-ku, Sendai, 980-8579, Japan
bInstitute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai, 980-8577, Japan

Received 14 October 2022, Revised 23 December 2022, Accepted 3 January 2023, Available online 5 January 2023.Show lessAdd to MendeleyShareCite

https://doi.org/10.1016/j.msea.2023.144595Get rights and content

Abstract

The elimination of internal macro-defects is a key issue in Ti–6Al–4V alloys fabricated via powder bed fusion using electron beams (PBF-EB), wherein internal macro-defects mainly originate from the virgin powder and inappropriate printing parameters. This study compares different types powders by combining support vector machine techniques to determine the most suitable powder for PBF-EB and to predict the processing window for the printing parameters without internal macro-defects. The results show that powders fabricated via plasma rotating electrode process have the best sphericity, flowability, and minimal porosity and are most suitable for printing. Surface roughness criterion was also applied to determine the quality of the even surfaces, and support vector machine was used to construct processing maps capable of predicting a wide range of four-dimensional printing parameters to obtain macro-defect-free samples, offering the possibility of subsequent development of Ti–6Al–4V alloys with excellent properties. The macro-defect-free samples exhibited good elongation, with the best overall mechanical properties being the ultimate tensile strength and elongation of 934.7 MPa and 24.3%, respectively. The elongation of the three macro-defect-free samples was much higher than that previously reported for additively manufactured Ti–6Al–4V alloys. The high elongation of the samples in this work is mainly attributed to the elimination of internal macro-defects.

Introduction

Additive manufacturing (AM) technologies can rapidly manufacture complex or custom parts, reducing process steps and saving manufacturing time [[1], [2], [3], [4]], and are widely used in the aerospace, automotive, and other precision industries [5,6]. Powder bed fusion using an electron beam (PBF-EB) is an additive manufacturing method that uses a high-energy electron beam to melt metal powders layer by layer to produce parts. In contrast to selective laser melting, PBF-EB involves the preparation of samples in a high vacuum environment, which effectively prevents the introduction of impurities such as O and N. It also involves a preheating process for the print substrate and powder, which reduces residual thermal stress on the sample and subsequent heat treatment processes [[2], [3], [4],7]. Due to these features and advantages, PBF-EB technology is a very important AM technology with great potential in metallic materials. Moreover, PBF-EB is the ideal AM technology for the manufacture of complex components made of many alloys, such as titanium alloys, nickel-based superalloys, aluminum alloys and stainless steels [[2], [3], [4],8].

Ti–6Al–4V alloy is one of the prevalent commercial titanium alloys possessing high specific strength, excellent mechanical properties, excellent corrosion resistance, and good biocompatibility [9,10]. It is widely used in applications requiring low density and excellent corrosion resistance, such as the aerospace industry and biomechanical applications [11,12]. The mechanical properties of PBF-EB-processed Ti–6Al–4V alloys are superior to those fabricated by casting or forging, because the rapid cooling rate in PBF-EB results in finer grains [[12], [13], [14], [15], [16], [17], [18]]. However, the PBF-EB-fabricated parts often include internal macro-defects, which compromises their mechanical properties [[19], [20], [21], [22]]. This study focused on the elimination of macro-defects, such as porosity, lack of fusion, incomplete penetration and unmelted powders, which distinguishes them from micro-defects such as vacancies, dislocations, grain boundaries and secondary phases, etc. Large-sized fusion defects cause a severe reduction in mechanical strength. Smaller defects, such as pores and cracks, lead to the initiation of fatigue cracking and rapidly accelerate the cracking process [23]. The issue of internal macro-defects must be addressed to expand the application of the PBF-EB technology. The main studies for controlling internal macro-defects are online monitoring of defects, remelting and hot isostatic pressing (HIP). The literatures [24,25] report the use of infrared imaging or other imaging techniques to identify defects, but the monitoring of smaller sized defects is still not adequate. And in some cases remelting does not reduce the internal macro-defects of the part, but instead causes coarsening of the macrostructure and volatilization of some metal elements [23]. The HIP treatment does not completely eliminate the internal macro-defects, the original defect location may still act as a point of origin of the crack, and the subsequent treatment will consume more time and economic costs [23]. Therefore, optimizing suitable printing parameters to avoid internal macro-defects in printed parts at source is of great industrial value and research significance, and is an urgent issue in PBF-EB related technology.

There are two causes of internal macro-defects in the AM process: gas pores trapped in the virgin powder and the inappropriate printing parameters [7,23]. Gui et al. [26] classify internal macro-defects during PBF-EB process according to their shape, such as spherical defects, elongated shape defects, flat shape defects and other irregular shape defects. Of these, spherical defects mainly originate from raw material powders. Other shape defects mainly originate from lack of fusion or unmelted powders caused by unsuitable printing parameters, etc. The PBF-EB process requires powders with good flowability, and spherical powders are typically chosen as raw materials. The prevalent techniques for the fabrication of pre-alloyed powders are gas atomization (GA), plasma atomization (PA), and the plasma rotating electrode process (PREP) [27,28]. These methods yield powders with different characteristics that affect the subsequent fabrication. The selection of a suitable powder for PBF-EB is particularly important to produce Ti–6Al–4V alloys without internal macro-defects. The need to optimize several printing parameters such as beam current, scan speed, line offset, and focus offset make it difficult to eliminate internal macro-defects that occur during printing [23]. Most of the studies [11,12,22,[29], [30], [31], [32], [33]] on the optimization of AM processes for Ti–6Al–4V alloys have focused on samples with a limited set of parameters (e.g., power–scan speed) and do not allow for the guidance and development of unknown process windows for macro-defect-free samples. In addition, process optimization remains a time-consuming problem, with the traditional ‘trial and error’ method demanding considerable time and economic costs. The development of a simple and efficient method to predict the processing window for alloys without internal macro-defects is a key issue. In recent years, machine learning techniques have increasingly been used in the field of additive manufacturing and materials development [[34], [35], [36], [37]]. Aoyagi et al. [38] recently proposed a novel and efficient method based on a support vector machine (SVM) to optimize the two-dimensional process parameters (current and scan speed) and obtain PBF-EB-processed CoCr alloys without internal macro-defects. The method is one of the potential approaches toward effective optimization of more than two process parameters and makes it possible for the machine learning techniques to accelerate the development of alloys without internal macro-defects.

Herein, we focus on the elimination of internal macro-defects, such as pores, lack of fusion, etc., caused by raw powders and printing parameters. The Ti–6Al–4V powders produced by three different methods were compared, and the powder with the best sphericity, flowability, and minimal porosity was selected as the feedstock for subsequent printing. The relationship between the surface roughness and internal macro-defects in the Ti–6Al–4V components was also investigated. The combination of SVM and surface roughness indices (Sdr) predicted a wider four-dimensional processing window for obtaining Ti–6Al–4V alloys without internal macro-defects. Finally, we investigated the tensile properties of Ti–6Al–4V alloys at room temperature with different printing parameters, as well as the corresponding microstructures and fracture types.

Section snippets

Starting materials

Three types of Ti–6Al–4V alloy powders, produced by GA, PA, and PREP, were compared. The particle size distribution of the powders was determined using a laser particle size analyzer (LS230, Beckman Coulter, USA), and the flowability was measured using a Hall flowmeter (JIS-Z2502, Tsutsui Scientific Instruments Co., Ltd., Japan), according to the ASTM B213 standard. The powder morphology and internal macro-defects were determined using scanning electron microscopy (SEM, JEOL JCM-6000) and X-ray 

Comparison of the characteristics of GA, PA, and PREP Ti–6Al–4V powders

The particle size distributions (PSDs) and flowability of the three types of Ti–6Al–4V alloy powders produced by GA, PA, and PREP are shown in Fig. 2. Although the average particle sizes are similar (89.4 μm for GA, 82.5 μm for PA, and 86.1μm for PREP), the particle size range is different for the three types of powder (6.2–174.8 μm for GA, 27.3–139.2 μm for PA, and 39.4–133.9 μm for PREP). The flowability of the GA, PA, and PREP powders was 30.25 ± 0.98, 26.54 ± 0.37, and 25.03 ± 0.22 (s/50

Conclusions

The characteristics of the three types of Ti–6Al–4V alloy powders produced via GA, PA, and PREP were compared. The PREP powder with the best sphericity, flowability, and low porosity was found to be the most favorable powder for subsequent printing of Ti–6Al–4V alloys without internal macro-defects. The quantitative criterion of Sdr <0.015 for even surfaces was also found to be applicable to Ti–6Al–4V alloys. The process maps of Ti–6Al–4V alloys include two regions, high beam current/scan speed 

Uncited references

[55]; [56]; [57]; [58]; [59]; [60]; [61]; [62]; [63]; [64]; [65].

CRediT authorship contribution statement

Yunwei Gui: Writing – original draft, Visualization, Validation, Investigation. Kenta Aoyagi: Writing – review & editing, Supervision, Resources, Methodology, Funding acquisition, Conceptualization. Akihiko Chiba: Supervision, Funding acquisition.

Declaration of competing interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Acknowledgments

This study was based on the results obtained from project JPNP19007, commissioned by the New Energy and Industrial Technology Development Organization (NEDO). This work was also supported by JSPS KAKENHI (Proposal No. 21K03801) and the Inter-University Cooperative Research Program (Proposal nos. 18G0418, 19G0411, and 20G0418) of the Cooperative Research and Development Center for Advanced Materials, Institute for Materials Research, Tohoku University. It was also supported by the Council for

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Figure 5: 3D & 2D views of simulated fill sequence of a hollow cylinder at 1000 rpm and 1500 rpm at various time intervals during filling.

Computer Simulation of Centrifugal Casting Process using FLOW-3D

Aneesh Kumar J1, a, K. Krishnakumar1, b and S. Savithri2, c 1 Department of Mechanical Engineering, College of Engineering, Thiruvananthapuram, Kerala, 2 Computational Modelling& Simulation Division, Process Engineering & Environmental Technology Division CSIR-National Institute for Interdisciplinary Science & Technology
Thiruvananthapuram, Kerala, India.
a aneesh82kj@gmail.com, b kkk@cet.ac.in, c sivakumarsavi@gmail.com, ssavithri@niist.res.in Key words: Mold filling, centrifugal casting process, computer simulation, FLOW- 3D™

Abstract

원심 주조 공정은 기능적으로 등급이 지정된 재료, 즉 구성 요소 간에 밀도 차이가 큰 복합 재료 또는 금속 재료를 생산하는 데 사용되는 잠재적인 제조 기술 중 하나입니다. 이 공정에서 유체 흐름이 중요한 역할을 하며 복잡한 흐름 공정을 이해하는 것은 결함 없는 주물을 생산하는 데 필수입니다. 금형이 고속으로 회전하고 금형 벽이 불투명하기 때문에 흐름 패턴을 실시간으로 시각화하는 것은 불가능합니다. 따라서 현재 연구에서는 상용 CFD 코드 FLOW-3D™를 사용하여 수직 원심 주조 공정 중 단순 중공 원통형 주조에 대한 금형 충전 시퀀스를 시뮬레이션했습니다. 수직 원심주조 공정 중 다양한 방사 속도가 충전 패턴에 미치는 영향을 조사하고 있습니다.

Centrifugal casting process is one of the potential manufacturing techniques used for producing functionally graded materials viz., composite materials or metallic materials which have high differences of density among constituents. In this process, the fluid flow plays a major role and understanding the complex flow process is a must for the production of defect-free castings. Since the mold spins at a high velocity and the mold wall being opaque, it is impossible to visualise the flow patterns in real time. Hence, in the present work, the commercial CFD code FLOW-3D™, has been used to simulate the mold filling sequence for a simple hollow cylindrical casting during vertical centrifugal casting process. Effect of various spinning velocities on the fill pattern during vertical centrifugal casting process is being investigated.

Figure 1: (a) Mold geometry and (b) Computational mesh
Figure 1: (a) Mold geometry and (b) Computational mesh
Figure 2: Experimental data on height of
vertex formed [8]  / Figure 3: Vertex height as a function of time
Figure 2: Experimental data on height of vertex formed [8]/Figure 3: Vertex height as a function of time
Figure 4: Free surface contours for water model at 10 s, 15 s and 20 s.
Figure 4: Free surface contours for water model at 10 s, 15 s and 20 s.
Figure 5: 3D & 2D views of simulated fill sequence of a hollow cylinder at 1000 rpm and 1500 rpm at various time intervals during filling.
Figure 5: 3D & 2D views of simulated fill sequence of a hollow cylinder at 1000 rpm and 1500 rpm at various time intervals during filling.

References

[1] W. Shi-Ping, L. Chang-yun, G. Jing-jie, S. Yan-qing, L. Xiu-qiao, F. Heng-zhi, Numerical simulation and
experimental investigation of two filling methods in vertical centrifugal casting, Trans. Nonferrous Met. Soc.
China 16 (2006) 1035-1040.
10.1016/s1003-6326(06)60373-7
[2] G. Chirita, D. Soares, F.S. Silva, Advantages of the centrifugal casting technique for the production of
structural components with Al-Si alloys, Mater. Des. 29 (2008) 20-27.
10.1016/j.matdes.2006.12.011
[3] A. Kermanpur, Sh. Mahmoudi, A. Hajipour, Numerical simulation of metal flow and solidification in the
multi-cavity casting moulds of automotive components, J. Mater. Proc. Tech. 206 (208) 62-68.
10.1016/j.jmatprotec.2007.12.004
[4] D. McBride et. al. Complex free surface flows in centrifugal casting: Computational modelling and
validation experiments, Computers & Fluids 82 (2013) 63-72.
10.1016/j.compfluid.2013.04.021

Fig. 8 Distribution of solidification properties on the yz cross section at the maximum width of the melt pool.(a) thermal gradient G, (b) solidification velocity vT, (c) cooling rate G×vT, and (d) morphology factor G/vT. These profiles are calculated with a laser power 300 W and velocity 400 mm/s using (a1 through d1) analytical Rosenthal simulation and (a2 through d2) high-fidelity CFD simulation. The laser is moving out of the page from the upper left corner of each color map (Color figure online)

Quantifying Equiaxed vs Epitaxial Solidification in Laser Melting of CMSX-4 Single Crystal Superalloy

CMSX -4 단결정 초합금의 레이저 용융에서 등축 응고와 에피택셜 응고 정량화

본 논문은 독자의 편의를 위해 기계번역된 내용이어서 자세한 내용은 원문을 참고하시기 바랍니다.

Abstract

에피택셜 과 등축 응고 사이의 경쟁은 적층 제조에서 실행되는 레이저 용융 동안 CMSX-4 단결정 초합금에서 조사되었습니다. 단일 트랙 레이저 스캔은 레이저 출력과 스캐닝 속도의 여러 조합으로 방향성 응고된 CMSX-4 합금의 분말 없는 표면에서 수행되었습니다. EBSD(Electron Backscattered Diffraction) 매핑은 새로운 방향의 식별을 용이하게 합니다. 영역 분율 및 공간 분포와 함께 융합 영역 내에서 핵을 형성한 “스트레이 그레인”은 충실도가 높은 전산 유체 역학 시뮬레이션을 사용하여 용융 풀 내의 온도 및 유체 속도 필드를 모두 추정했습니다. 이 정보를 핵 생성 모델과 결합하여 용융 풀에서 핵 생성이 발생할 확률이 가장 높은 위치를 결정했습니다. 금속 적층 가공의 일반적인 경험에 따라 레이저 용융 트랙의 응고된 미세 구조는 에피택셜 입자 성장에 의해 지배됩니다. 더 높은 레이저 스캐닝 속도와 더 낮은 출력이 일반적으로 흩어진 입자 감소에 도움이 되지만,그럼에도 불구하고 길쭉한 용융 풀에서 흩어진 입자가 분명했습니다.

The competition between epitaxial vs. equiaxed solidification has been investigated in CMSX-4 single crystal superalloy during laser melting as practiced in additive manufacturing. Single-track laser scans were performed on a powder-free surface of directionally solidified CMSX-4 alloy with several combinations of laser power and scanning velocity. Electron backscattered diffraction (EBSD) mapping facilitated identification of new orientations, i.e., “stray grains” that nucleated within the fusion zone along with their area fraction and spatial distribution. Using high-fidelity computational fluid dynamics simulations, both the temperature and fluid velocity fields within the melt pool were estimated. This information was combined with a nucleation model to determine locations where nucleation has the highest probability to occur in melt pools. In conformance with general experience in metals additive manufacturing, the as-solidified microstructure of the laser-melted tracks is dominated by epitaxial grain growth; nevertheless, stray grains were evident in elongated melt pools. It was found that, though a higher laser scanning velocity and lower power are generally helpful in the reduction of stray grains, the combination of a stable keyhole and minimal fluid velocity further mitigates stray grains in laser single tracks.

Introduction

니켈 기반 초합금은 고온에서 긴 노출 시간 동안 높은 인장 강도, 낮은 산화 및 우수한 크리프 저항성을 포함하는 우수한 특성의 고유한 조합으로 인해 가스 터빈 엔진 응용 분야에서 광범위하게 사용됩니다. CMSX-4는 특히 장기 크리프 거동과 관련하여 초고강도의 2세대 레늄 함유 니켈 기반 단결정 초합금입니다. 1 , 2 ]입계의 존재가 크리프를 가속화한다는 인식은 가스 터빈 엔진의 고온 단계를 위한 단결정 블레이드를 개발하게 하여 작동 온도를 높이고 효율을 높이는 데 기여했습니다. 이러한 구성 요소는 사용 중 마모될 수 있습니다. 즉, 구성 요소의 무결성을 복원하고 단결정 미세 구조를 유지하는 수리 방법을 개발하기 위한 지속적인 작업이 있었습니다. 3 , 4 , 5 ]

적층 제조(AM)가 등장하기 전에는 다양한 용접 공정을 통해 단결정 초합금에 대한 수리 시도가 수행되었습니다. 균열 [ 6 , 7 ] 및 흩어진 입자 8 , 9 ] 와 같은 심각한 결함 이 이 수리 중에 자주 발생합니다. 일반적으로 “스트레이 그레인”이라고 하는 응고 중 모재의 방향과 다른 결정학적 방향을 가진 새로운 그레인의 형성은 니켈 기반 단결정 초합금의 수리 중 유해한 영향으로 인해 중요한 관심 대상입니다. 3 , 10 ]결과적으로 재료의 단결정 구조가 손실되고 원래 구성 요소에 비해 기계적 특성이 손상됩니다. 이러한 흩어진 입자는 특정 조건에서 에피택셜 성장을 대체하는 등축 응고의 시작에 해당합니다.

떠돌이 결정립 형성을 완화하기 위해 이전 작업은 용융 영역(FZ) 내에서 응고하는 동안 떠돌이 결정립 형성에 영향을 미치는 수지상 응고 거동 및 처리 조건을 이해하는 데 중점을 두었습니다. 11 , 12 , 13 , 14 ] 연구원들은 단결정 합금의 용접 중에 표류 결정립 형성에 대한 몇 가지 가능한 메커니즘을 제안했습니다. 12 , 13 , 14 , 15 ]응고 전단에 앞서 국부적인 구성 과냉각은 이질적인 핵 생성 및 등축 결정립의 성장을 유발할 수 있습니다. 또한 용융 풀에서 활발한 유체 흐름으로 인해 발생하는 덴드라이트 조각화는 용융 풀 경계 근처에서 새로운 결정립을 형성할 수도 있습니다. 두 메커니즘 모두에서, 표류 결정립 형성은 핵 생성 위치에 의존하며, 차이점은 수상 돌기 조각화는 수상 돌기 조각이 핵 생성 위치로 작용한다는 것을 의미하는 반면 다른 메커니즘은 재료,  를 들어 산화물 입자에서 발견되는 다른 유형의 핵 생성 위치를 사용한다는 것을 의미합니다. 잘 알려진 바와 같이, 많은 주물에 대한 반대 접근법은 TiB와 같은 핵제의 도입을 통해 등축 응고를 촉진하는 것입니다.22알루미늄 합금에서.

헌법적 과냉 메커니즘에서 Hunt 11 ] 는 정상 상태 조건에서 기둥에서 등축으로의 전이(CET)를 설명하는 모델을 개발했습니다. Gaumann과 Kurz는 Hunt의 모델을 수정하여 단결정이 응고되는 동안 떠돌이 결정립이 핵을 생성하고 성장할 수 있는 정도를 설명했습니다. 12 , 14 ] 이후 연구에서 Vitek은 Gaumann의 모델을 개선하고 출력 및 스캐닝 속도와 같은 용접 조건의 영향에 대한 보다 자세한 분석을 포함했습니다. Vitek은 또한 실험 및 모델링 기술을 통해 표류 입자 형성에 대한 기판 방향의 영향을 포함했습니다. 3 , 10 ]일반적으로 높은 용접 속도와 낮은 출력은 표류 입자의 양을 최소화하고 레이저 용접 공정 중 에피택셜 단결정 성장을 최대화하는 것으로 나타났습니다. 3,10 ] 그러나 Vitek은 덴드라이트 조각화를 고려하지 않았으며 그의 연구는 불균질 핵형성이 레이저 용접된 CMSX -4 단결정 합금에서 표류 결정립 형성을 이끄는 주요 메커니즘임을 나타냅니다. 현재 작업에서 Vitek의 수치적 방법이 채택되고 금속 AM의 급속한 특성의 더 높은 속도와 더 낮은 전력 특성으로 확장됩니다.

AM을 통한 금속 부품 제조 는 지난 10년 동안 급격한 인기 증가를 목격했습니다. 16 ] EBM(Electron Beam Melting)에 의한 CMSX-4의 제작 가능성은 자주 조사되었으나 17 , 18 , 19 , 20 , 21 ] CMSX의 제조 및 수리에 대한 조사는 매우 제한적이었다. – 4개의 단결정 구성요소는 레이저 분말 베드 융합(LPBF)을 사용하며, AM의 인기 있는 하위 집합으로, 특히 표류 입자 형성을 완화하는 메커니즘과 관련이 있습니다. 22 ]이러한 조사 부족은 주로 이러한 합금 시스템과 관련된 처리 문제로 인해 발생합니다. 2 , 19 , 22 , 23 , 24 ] 공정 매개변수( 예: 열원 전력, 스캐닝 속도, 스폿 크기, 예열 온도 및 스캔 전략)의 엄격한 제어는 완전히 조밀한 부품을 만들고 유지 관리할 수 있도록 하는 데 필수적입니다. 단결정 미세구조. 25 ] EBM을 사용하여 단결정 합금의 균열 없는 수리가 현재 가능하지만 19 , 24 ] 표류 입자를 생성하지 않는 수리는 쉽게 달성할 수 없습니다.23 , 26 ]

이 작업에서 LPBF를 대표하는 조건으로 레이저 용융을 사용하여 단결정 CMSX-4에서 표류 입자 완화를 조사했습니다. LPBF는 스캐닝 레이저 빔을 사용하여 금속 분말의 얇은 층을 기판에 녹이고 융합합니다. 층별 증착에서 레이저 빔의 사용은 급격한 온도 구배, 빠른 가열/냉각 주기 및 격렬한 유체 흐름을 경험하는 용융 풀을 생성 합니다 이것은 일반적으로 부품에 결함을 일으킬 수 있는 매우 동적인 물리적 현상으로 이어집니다. 28 , 29 , 30 ] 레이저 유도 키홀의 동역학( 예:, 기화 유발 반동 압력으로 인한 위상 함몰) 및 열유체 흐름은 AM 공정에서 응고 결함과 강하게 결합되고 관련됩니다. 31 , 32 , 33 , 34 ] 기하 구조의 급격한 변화가 발생하기 쉬운 불안정한 키홀은 다공성, 볼링, 스패터 형성 및 흔하지 않은 미세 구조 상을 포함하는 유해한 물리적 결함을 유발할 수 있습니다. 그러나 키홀 진화와 유체 흐름은 자연적으로 다음을 통해 포착 하기 어렵 습니다 .전통적인 사후 특성화 기술. 고충실도 수치 모델링을 활용하기 위해 이 연구에서는 전산유체역학(CFD)을 적용하여 표면 아래의 레이저-물질 상호 작용을 명확히 했습니다. 36 ] 이것은 응고된 용융물 풀의 단면에 대한 오랫동안 확립된 사후 특성화와 비교하여 키홀 및 용융물 풀 유체 흐름 정량화를 실행합니다.

CMSX-4 구성 요소의 레이저 기반 AM 수리 및 제조를 위한 적절한 절차를 개발하기 위해 적절한 공정 창을 설정하고 응고 중 표류 입자 형성 경향에 대한 예측 기능을 개발하는 것부터 시작합니다. 다중 합금에 대한 단일 트랙 증착은 분말 층이 있거나 없는 AM 공정에서 용융 풀 형상 및 미세 구조의 정확한 분석을 제공하는 것으로 나타났습니다. 37 , 38 , 39 ]따라서 본 연구에서는 CMSX-4의 응고 거동을 알아보기 위해 분말을 사용하지 않는 단일 트랙 레이저 스캔 실험을 사용하였다. 이는 CMSX-4 단결정의 LPBF 제조를 위한 예비 실험 지침을 제공합니다. 또한 응고 모델링은 기존 용접에서 LPBF와 관련된 급속 용접으로 확장되어 표류 입자 감소를 위한 최적의 레이저 용융 조건을 식별했습니다. 가공 매개변수 최적화를 위한 추가 지침을 제공하기 위해 용융물 풀의 매우 동적인 유체 흐름을 모델링했습니다.

재료 및 방법

단일 트랙 실험

방전 가공(EDM)을 사용하여 CMSX-4 방향성 응고 단결정 잉곳으로부터 샘플을 제작했습니다. 샘플의 최종 기하학은 치수 20의 직육면체 형태였습니다.××20××6mm. 6개 중 하나⟨ 001 ⟩⟨001⟩잉곳의 결정학적 방향은 레이저 트랙이 이 바람직한 성장 방향을 따라 스캔되도록 절단 표면에 수직으로 위치했습니다. 단일 레이저 용융 트랙은 EOS M290 기계를 사용하여 분말이 없는 샘플 표면에 만들어졌습니다. 이 기계는 최대 출력 400W, 가우시안 빔 직경 100의 이터븀 파이버 레이저가 장착된 LPBF 시스템입니다. μμ초점에서 m. 실험 중에 직사각형 샘플을 LPBF 기계용 맞춤형 샘플 홀더의 포켓에 끼워 표면을 동일한 높이로 유지했습니다. 이 맞춤형 샘플 홀더에 대한 자세한 내용은 다른 곳에서 설명합니다. 실험 은 아르곤 퍼지 분위기에서 수행되었으며 예열은 적용되지 않았습니다 단일 트랙 레이저 용융 실험은 다양한 레이저 출력(200~370W)과 스캔 속도(0.4~1.4m/s)에서 수행되었습니다.

성격 묘사

레이저 스캐닝 후, 레이저 빔 스캐닝 방향에 수직인 평면에서 FZ를 통해 다이아몬드 톱을 사용하여 샘플을 절단했습니다. 그 후, 샘플을 장착하고 220 그릿 SiC 페이퍼로 시작하여 콜로이드 실리카 현탁액 광택제로 마무리하여 자동 연마했습니다. 결정학적 특성화는 20kV의 가속 전압에서 TESCAN MIRA 3XMH 전계 방출 주사 전자 현미경(SEM)에서 수행되었습니다. EBSD 지도는0.4μm _0.4μ미디엄단계 크기. Bruker 시스템을 사용하여 EBSD 데이터를 정리하고 분석했습니다. EBSD 클린업은 그레인을 접촉시키기 위한 그레인 확장 루틴으로 시작한 다음 인덱스되지 않은 회절 패턴과 관련된 검은색 픽셀을 해결하기 위해 이웃 방향 클린업 루틴으로 이어졌습니다. 용융 풀 형태를 분석하기 위해 단면을 광학 현미경으로 분석했습니다. 광학 특성화의 대비를 향상시키기 위해 10g CuSO로 구성된 Marbles 시약의 변형으로 샘플을 에칭했습니다.44, 50mL HCl 및 70mL H22영형.

응고 모델링

구조적 과냉 기준에 기반한 응고 모델링을 수행하여 표유 입자의 성향 및 분포에 대한 가공 매개변수의 영향을 평가했습니다. 이 분석 모델링 접근 방식에 대한 자세한 내용은 이전 작업에서 제공됩니다. 3 , 10 ] 참고문헌 3 에 기술된 바와 같이 , 기본 재료의 결정학적 배향을 가진 용융 풀에서 총 표유 입자 면적 분율의 변화는 최소이므로 기본 재료 배향의 영향은 이 작업에서 고려되지 않았습니다. 우리의 LPBF 결과를 이전 작업과 비교하기 위해 Vitek의 작업에서 사용된 수학적으로 간단한 Rosenthal 방정식 3 ]또한 레이저 매개변수의 함수로 용융 풀의 모양과 FZ의 열 조건을 계산하기 위한 기준으로 여기에서 채택되었습니다. Rosenthal 솔루션은 열이 일정한 재료 특성을 가진 반무한 판의 정상 상태 점원을 통해서만 전도를 통해 전달된다고 가정하며 일반적으로 다음과 같이 표현 됩니다 40 , 41 ] .

티=티0+η피2 파이케이엑스2+와이2+지2———-√경험치[- 브이(엑스2+와이2+지2———-√− 엑스 )2α _] ,티=티0+η피2파이케이엑스2+와이2+지2경험치⁡[-V(엑스2+와이2+지2-엑스)2α],(1)

여기서 T 는 온도,티0티0본 연구에서 313K(  , EOS 기계 챔버 온도)로 설정된 주변 온도, P 는 레이저 빔 파워, V 는 레이저 빔 스캐닝 속도,ηη는 레이저 흡수율, k 는 열전도율,αα베이스 합금의 열확산율입니다. x , y , z 는 각각 레이저 스캐닝 방향, 가로 방향 및 세로 방향의 반대 방향과 정렬된 방향입니다 . 이 직교 좌표는 참조 3 의 그림 1에 있는 시스템을 따랐습니다 . CMSX-4에 대한 고상선 온도(1603K)와 액상선 온도(1669K)의 등온선 평균으로 응고 프런트( 즉 , 고체-액체 계면)를 정의했습니다. 42 , 43 , 44 ] 시뮬레이션에 사용된 열물리적 특성은 표 I 에 나열되어 있습니다.표 I CMSX-4의 응고 모델링에 사용된 열물리적 특성

풀 사이즈 테이블

열 구배는 외부 열 흐름에 의해 결정되었습니다.∇ 티∇티45 ] 에 의해 주어진 바와 같이 :

지 = | ∇ 티| =∣∣∣∂티∂엑스나^^+∂티∂와이제이^^+∂티∂지케이^^∣∣∣=(∂티∂엑스)2+(∂티∂와이)2+(∂티∂지)2————————√,G=|∇티|=|∂티∂엑스나^^+∂티∂와이제이^^+∂티∂지케이^^|=(∂티∂엑스)2+(∂티∂와이)2+(∂티∂지)2,(2)

어디나^^나^^,제이^^제이^^, 그리고케이^^케이^^는 각각 x , y 및 z 방향 을 따른 단위 벡터 입니다. 응고 등온선 속도,V티V티는 다음 관계에 의해 레이저 빔 스캐닝 속도 V 와 기하학적으로 관련됩니다.

V티= V코사인θ =V∂티∂엑스(∂티∂엑스)2+(∂티∂와이)2+(∂티∂지)2——————-√,V티=V코사인⁡θ=V∂티∂엑스(∂티∂엑스)2+(∂티∂와이)2+(∂티∂지)2,(삼)

어디θθ는 스캔 방향과 응고 전면의 법선 방향(  , 최대 열 흐름 방향) 사이의 각도입니다. 이 연구의 용접 조건과 같은 제한된 성장에서 수지상 응고 전면은 고체-액체 등온선의 속도로 성장하도록 강제됩니다.V티V티. 46 ]

응고 전선이 진행되기 전에 새로 핵 생성된 입자의 국지적 비율ΦΦ, 액체 온도 구배 G 에 의해 결정 , 응고 선단 속도V티V티및 핵 밀도N0N0. 고정된 임계 과냉각에서 모든 입자가 핵형성된다고 가정함으로써△티N△티N, 등축 결정립의 반경은 결정립이 핵 생성을 시작하는 시점부터 주상 전선이 결정립에 도달하는 시간까지의 성장 속도를 통합하여 얻습니다. 과냉각으로 대체 시간d (ΔT_) / dt = – _V티G디(△티)/디티=-V티G, 열 구배 G 사이의 다음 관계 , 등축 입자의 국부적 부피 분율ΦΦ, 수상 돌기 팁 과냉각ΔT _△티, 핵 밀도N0N0, 재료 매개변수 n 및 핵생성 과냉각△티N△티N, Gäumann 외 여러분 에 의해 파생되었습니다 . 12 , 14 ] Hunt의 모델 11 ] 의 수정에 기반함 :

지 =1엔 + 1- 4π _N03 인치( 1 − Φ )———√삼ΔT _( 1 -△티엔 + 1N△티엔 + 1) .G=1N+1-4파이N0삼인⁡(1-Φ)삼△티(1-△티NN+1△티N+1).(4)

계산을 단순화하기 위해 덴드라이트 팁 과냉각을 전적으로 구성 과냉각의 것으로 추정합니다.△티씨△티씨, 멱법칙 형식으로 근사화할 수 있습니다.△티씨= ( _V티)1 / 엔△티씨=(ㅏV티)1/N, 여기서 a 와 n 은 재료 종속 상수입니다. CMSX-4의 경우 이 값은a = 1.25 ×106ㅏ=1.25×106 s K 3.4m− 1-1,엔 = 3.4N=3.4, 그리고N0= 2 ×1015N0=2×1015미디엄− 3,-삼,참고문헌 3 에 의해 보고된 바와 같이 .△티N△티N2.5K이며 보다 큰 냉각 속도에서 응고에 대해 무시할 수 있습니다.106106 K/s. 에 대한 표현ΦΦ위의 방정식을 재배열하여 해결됩니다.

Φ= 1 -이자형에스\ 여기서\  S=- 4π _N0삼(1( 엔 + 1 ) (GN/ 아V티)1 / 엔)삼=−2.356×1019(vTG3.4)33.4.Φ=1−eS\ where\ S=−4πN03(1(n+1)(Gn/avT)1/n)3=−2.356×1019(vTG3.4)33.4.

(5)

As proposed by Hunt,[11] a value of Φ≤0.66Φ≤0.66 pct represents fully columnar epitaxial growth condition, and, conversely, a value of Φ≥49Φ≥49 pct indicates that the initial single crystal microstructure is fully replaced by an equiaxed microstructure. To calculate the overall stray grain area fraction, we followed Vitek’s method by dividing the FZ into roughly 19 to 28 discrete parts (depending on the length of the melt pool) of equal length from the point of maximum width to the end of melt pool along the x direction. The values of G and vTvT were determined at the center on the melt pool boundary of each section and these values were used to represent the entire section. The area-weighted average of ΦΦ over these discrete sections along the length of melt pool is designated as Φ¯¯¯¯Φ¯, and is given by:

Φ¯¯¯¯=∑kAkΦk∑kAk,Φ¯=∑kAkΦk∑kAk,

(6)

where k is the index for each subsection, and AkAk and ΦkΦk are the areas and ΦΦ values for each subsection. The summation is taken over all the sections along the melt pool. Vitek’s improved model allows the calculation of stray grain area fraction by considering the melt pool geometry and variations of G and vTvT around the tail end of the pool.

수년에 걸쳐 용융 풀 현상 모델링의 정확도를 개선하기 위해 많은 고급 수치 방법이 개발되었습니다. 우리는 FLOW-3D와 함께 고충실도 CFD를 사용했습니다. FLOW-3D는 여러 물리 모델을 통합하는 상용 FVM(Finite Volume Method)입니다. 47 , 48 ] CFD는 유체 운동과 열 전달을 수치적으로 시뮬레이션하며 여기서 사용된 기본 물리 모델은 레이저 및 표면력 모델이었습니다. 레이저 모델에서는 레이 트레이싱 기법을 통해 다중 반사와 프레넬 흡수를 구현합니다. 36 ]먼저, 레이저 빔은 레이저 빔에 의해 조명되는 각 그리드 셀을 기준으로 여러 개의 광선으로 이산화됩니다. 그런 다음 각 입사 광선에 대해 입사 벡터가 입사 위치에서 금속 표면의 법선 벡터와 정렬될 때 에너지의 일부가 금속에 의해 흡수됩니다. 흡수율은 Fresnel 방정식을 사용하여 추정됩니다. 나머지 에너지는 반사광선 에 의해 유지되며 , 반사광선은 재료 표면에 부딪히면 새로운 입사광선으로 처리됩니다. 두 가지 주요 힘이 액체 금속 표면에 작용하여 자유 표면을 변형시킵니다. 금속의 증발에 의해 생성된 반동 압력은 증기 억제를 일으키는 주요 힘입니다. 본 연구에서 사용된 반동 압력 모델은피아르 자형= 특급 _{ B ( 1- _티V/ 티) }피아르 자형=ㅏ경험치⁡{비(1-티V/티)}, 어디피아르 자형피아르 자형는 반동압력, A 와 B 는 재료의 물성에 관련된 계수로 각각 75와 15이다.티V티V는 포화 온도이고 T 는 키홀 벽의 온도입니다. 표면 흐름 및 키홀 형성의 다른 원동력은 표면 장력입니다. 표면 장력 계수는 Marangoni 흐름을 포함하기 위해 온도의 선형 함수로 추정되며,σ =1.79-9.90⋅10− 4( 티− 1654케이 )σ=1.79-9.90⋅10-4(티-1654년케이)엔엠− 1-1. 49 ] 계산 영역은 베어 플레이트의 절반입니다(2300 μμ미디엄××250 μμ미디엄××500 μμm) xz 평면 에 적용된 대칭 경계 조건 . 메쉬 크기는 8입니다. μμm이고 시간 단계는 0.15입니다. μμs는 계산 효율성과 정확성 간의 균형을 제공합니다.

결과 및 논의

용융 풀 형태

이 작업에 사용된 5개의 레이저 파워( P )와 6개의 스캐닝 속도( V )는 서로 다른 29개의 용융 풀을 생성했습니다.피- 브이피-V조합. P 와 V 값이 가장 높은 것은 그림 1 을 기준으로 과도한 볼링과 관련이 있기 때문에 본 연구에서는 분석하지 않았다  .

단일 트랙 용융 풀은 그림  1 과 같이 형상에 따라 네 가지 유형으로 분류할 수 있습니다 39 ] : (1) 전도 모드(파란색 상자), (2) 키홀 모드(빨간색), (3) 전환 모드(마젠타), (4) 볼링 모드(녹색). 높은 레이저 출력과 낮은 스캐닝 속도의 일반적인 조합인 키홀 모드에서 용융물 풀은 일반적으로 너비/깊이( W / D ) 비율이 0.5보다 훨씬 큰 깊고 가느다란 모양을 나타냅니다 . 스캐닝 속도가 증가함에 따라 용융 풀이 얕아져 W / D 가 약 0.5인 반원형 전도 모드 용융 풀을 나타냅니다. W / D _전환 모드 용융 풀의 경우 1에서 0.5 사이입니다. 스캐닝 속도를 1200 및 1400mm/s로 더 높이면 충분히 큰 캡 높이와 볼링 모드 용융 풀의 특징인 과도한 언더컷이 발생할 수 있습니다.

힘과 속도의 함수로서의 용융 풀 깊이와 너비는 각각 그림  2 (a)와 (b)에 표시되어 있습니다. 용융 풀 폭은 기판 표면에서 측정되었습니다. 그림  2 (a)는 깊이가 레이저 출력과 매우 선형적인 관계를 따른다는 것을 보여줍니다. 속도가 증가함에 따라 깊이  파워 곡선의 기울기는 꾸준히 감소하지만 더 높은 속도 곡선에는 약간의 겹침이 있습니다. 이러한 예상치 못한 중첩은 종종 용융 풀 형태의 동적 변화를 유발하는 유체 흐름의 영향과 레이저 스캔당 하나의 이미지만 추출되었다는 사실 때문일 수 있습니다. 이러한 선형 동작은 그림 2 (b) 의 너비에 대해 명확하지 않습니다  . 그림  2(c)는 선형 에너지 밀도 P / V 의 함수로서 용융 깊이와 폭을 보여줍니다 . 선형 에너지 밀도는 퇴적물의 단위 길이당 에너지 투입량을 측정한 것입니다. 50 ] 용융 풀 깊이는 에너지 밀도에 따라 달라지며 너비는 더 많은 분산을 나타냅니다. 동일한 에너지 밀도가 준공 부품의 용융 풀, 미세 구조 또는 속성에서 반드시 동일한 유체 역학을 초래하지는 않는다는 점에 유의하는 것이 중요합니다. 50 ]

그림 1
그림 1
그림 2
그림 2

레이저 흡수율 평가

레이저 흡수율은 LPBF 조건에서 재료 및 가공 매개변수에 따라 크게 달라진다는 것은 잘 알려져 있습니다. 31 , 51 , 52 ] 적분구를 이용한 전통적인 흡수율의 직접 측정은 일반적으로 높은 비용과 구현의 어려움으로 인해 쉽게 접근할 수 없습니다. 51 ] 그  . 39 ] 전도 모드 용융 풀에 대한 Rosenthal 방정식을 기반으로 경험적 레이저 흡수율 모델을 개발했지만 기본 가정으로 인해 키홀 용융 풀에 대한 정확한 예측을 제공하지 못했습니다. 40 ] 최근 간 . 53 ] Ti–6Al–4V에 대한 30개의 고충실도 다중 물리 시뮬레이션 사례를 사용하여 레이저 흡수에 대한 스케일링 법칙을 확인했습니다. 그러나 연구 중인 특정 재료에 대한 최소 흡수(평평한 용융 표면의 흡수율)에 대한 지식이 필요하며 이는 CMSX-4에 대해 알려지지 않았습니다. 다양한 키홀 모양의 용융 풀에 대한 레이저 흡수의 정확한 추정치를 얻기가 어렵기 때문에 상한 및 하한 흡수율로 분석 시뮬레이션을 실행하기로 결정했습니다. 깊은 키홀 모양의 용융 풀의 경우 대부분의 빛을 가두는 키홀 내 다중 반사로 인해 레이저 흡수율이 0.8만큼 높을 수 있습니다. 이것은 기하학적 현상이며 기본 재료에 민감하지 않습니다. 5152 , 54 ] 따라서 본 연구에서는 흡수율의 상한을 0.8로 설정하였다. 참고 문헌 51 에 나타낸 바와 같이 , 전도 용융 풀에 해당하는 최저 흡수율은 약 0.3이었으며, 이는 이 연구에서 합리적인 하한 값입니다. 따라서 레이저 흡수율이 스트레이 그레인 형성에 미치는 영향을 보여주기 위해 흡수율 값을 0.55 ± 0.25로 설정했습니다. Vitek의 작업에서는 1.0의 고정 흡수율 값이 사용되었습니다. 3 ]

퓨전 존 미세구조

그림  3 은 200~300W 및 600~300W 및 600~300W 범위의 레이저 출력 및 속도로 9가지 다른 처리 매개변수에 의해 생성된 CMSX-4 레이저 트랙의 yz 단면 에서 취한 EBSD 역극점도와 해당 역극점도를 보여 줍니다. 각각 1400mm/s. EBSD 맵에서 여러 기능을 쉽게 관찰할 수 있습니다. 스트레이 그레인은 EBSD 맵에서 그 방향에 해당하는 다른 RGB 색상으로 나타나고 그레인 경계를 묘사하기 위해 5도의 잘못된 방향이 사용되었습니다. 여기, 그림  3 에서 스트레이 그레인은 대부분 용융 풀의 상단 중심선에 집중되어 있으며, 이는 용접된 단결정 CMSX-4의 이전 보고서와 일치합니다. 10 ]역 극점도에서, 점 근처에 집중된 클러스터⟨ 001 ⟩⟨001⟩융합 경계에서 유사한 방향을 유지하는 단결정 기반 및 에피택셜로 응고된 덴드라이트를 나타냅니다. 그러나 흩어진 곡물은 식별할 수 있는 질감이 없는 흩어져 있는 점으로 나타납니다. 단결정 기본 재료의 결정학적 방향은 주로⟨ 001 ⟩⟨001⟩비록 샘플을 절단하는 동안 식별할 수 없는 기울기 각도로 인해 또는 단결정 성장 과정에서 약간의 잘못된 방향이 있었기 때문에 약간의 편차가 있지만. 용융 풀 내부의 응고된 수상 돌기의 기본 방향은 다시 한 번⟨ 001 ⟩⟨001⟩주상 결정립 구조와 유사한 에피택셜 성장의 결과. 그림 3 과 같이 용융 풀에서 수상돌기의 성장 방향은 하단의 수직 방향에서 상단의 수평 방향으로 변경되었습니다  . 이 전이는 주로 온도 구배 방향의 변화로 인한 것입니다. 두 번째 전환은 CET입니다. FZ의 상단 중심선 주변에서 다양한 방향의 흩어진 입자가 관찰되며, 여기서 안쪽으로 성장하는 수상돌기가 서로 충돌하여 용융 풀에서 응고되는 마지막 위치가 됩니다.

더 깊은 키홀 모양을 특징으로 하는 샘플에서 용융 풀의 경계 근처에 침전된 흩어진 입자가 분명합니다. 이러한 새로운 입자는 나중에 모델링 섹션에서 논의되는 수상돌기 조각화 메커니즘에 의해 잠재적으로 발생합니다. 결정립이 강한 열 구배에서 핵을 생성하고 성장한 결과, 대부분의 흩어진 결정립은 모든 방향에서 동일한 크기를 갖기보다는 장축이 열 구배 방향과 정렬된 길쭉한 모양을 갖습니다. 그림 3 의 전도 모드 용융 풀 흩어진 입자가 없는 것으로 입증되는 더 나은 단결정 품질을 나타냅니다. 상대적으로 낮은 출력과 높은 속도의 스캐닝 레이저에 의해 생성된 이러한 더 얕은 용융 풀에서 최소한의 결정립 핵형성이 발생한다는 것은 명백합니다. 더 큰 면적 분율을 가진 스트레이 그레인은 고출력 및 저속으로 생성된 깊은 용융 풀에서 더 자주 관찰됩니다. 국부 응고 조건에 대한 동력 및 속도의 영향은 후속 모델링 섹션에서 조사할 것입니다.

그림 3
그림 3

응고 모델링

서론에서 언급한 바와 같이 연구자들은 단결정 용접 중에 표류 결정립 형성의 가능한 메커니즘을 평가했습니다. 12 , 13 , 14 , 15 , 55 ]논의된 가장 인기 있는 두 가지 메커니즘은 (1) 응고 전단에 앞서 구성적 과냉각에 의해 도움을 받는 이종 핵형성 및 (2) 용융물 풀의 유체 흐름으로 인한 덴드라이트 조각화입니다. 첫 번째 메커니즘은 광범위하게 연구되었습니다. 이원 합금을 예로 들면, 고체는 액체만큼 많은 용질을 수용할 수 없으므로 응고 중에 용질을 액체로 거부합니다. 결과적으로, 성장하는 수상돌기 앞에서 용질 분할은 실제 온도가 국부 평형 액상선보다 낮은 과냉각 액체를 생성합니다. 충분히 광범위한 체질적으로 과냉각된 구역의 존재는 새로운 결정립의 핵형성 및 성장을 촉진합니다. 56 ]전체 과냉각은 응고 전면에서의 구성, 동역학 및 곡률 과냉각을 포함한 여러 기여의 합입니다. 일반적인 가정은 동역학 및 곡률 과냉각이 합금에 대한 용질 과냉각의 더 큰 기여와 관련하여 무시될 수 있다는 것입니다. 57 ]

서로 다른 기본 메커니즘을 더 잘 이해하려면피- 브이피-V조건에서 응고 모델링이 수행됩니다. 첫 번째 목적은 스트레이 그레인의 전체 범위를 평가하는 것입니다(Φ¯¯¯¯Φ¯) 처리 매개 변수의 함수로 국부적 표류 입자 비율의 변화를 조사하기 위해 (ΦΦ) 용융 풀의 위치 함수로. 두 번째 목적은 금속 AM의 빠른 응고 동안 응고 미세 구조와 표류 입자 형성 메커니즘 사이의 관계를 이해하는 것입니다.

그림 4
그림 4

그림  4 는 해석적으로 시뮬레이션된 표류 입자 비율을 보여줍니다.Φ¯¯¯¯Φ¯세 가지 레이저 흡수율 값에서 다양한 레이저 스캐닝 속도 및 레이저 출력에 대해. 결과는 스트레이 그레인 면적 비율이 흡수된 에너지에 민감하다는 것을 보여줍니다. 흡수율을 0.30에서 0.80으로 증가시키면Φ¯¯¯¯Φ¯약 3배이며, 이 효과는 저속 및 고출력 영역에서 더욱 두드러집니다. 다른 모든 조건이 같다면, 흡수된 전력의 큰 영향은 평균 열 구배 크기의 일반적인 감소와 용융 풀 내 평균 응고율의 증가에 기인합니다. 스캐닝 속도가 증가하고 전력이 감소함에 따라 평균 스트레이 그레인 비율이 감소합니다. 이러한 일반적인 경향은 Vitek의 작업에서 채택된 그림 5 의 파란색 영역에서 시뮬레이션된 용접 결과와 일치합니다  . 3 ] 더 큰 과냉각 구역( 즉, 지 /V티G/V티영역)은 용접 풀의 표유 입자의 면적 비율이 분홍색 영역에 해당하는 LPBF 조건의 면적 비율보다 훨씬 더 크다는 것을 의미합니다. 그럼에도 불구하고 두 데이터 세트의 일반적인 경향은 유사합니다.  , 레이저 출력이 감소하고 레이저 속도가 증가함에 따라 표류 입자의 비율이 감소합니다. 또한 그림  5 에서 스캐닝 속도가 LPBF 영역으로 증가함에 따라 표유 입자 면적 분율에 대한 레이저 매개변수의 변화 효과가 감소한다는 것을 추론할 수 있습니다. 그림  6 (a)는 그림 3 의 EBSD 분석에서 나온 실험적 표류 결정립 면적 분율  과 그림 4 의 해석 시뮬레이션 결과를  비교합니다.. 열쇠 구멍 모양의 FZ에서 정확한 값이 다르지만 추세는 시뮬레이션과 실험 데이터 모두에서 일관되었습니다. 키홀 모양의 용융 풀, 특히 전력이 300W인 2개는 분석 시뮬레이션 예측보다 훨씬 더 많은 양의 흩어진 입자를 가지고 있습니다. Rosenthal 방정식은 일반적으로 열 전달이 순전히 전도에 의해 좌우된다는 가정으로 인해 열쇠 구멍 체제의 열 흐름을 적절하게 반영하지 못하기 때문에 이러한 불일치가 실제로 예상됩니다. 39 , 40 ] 그것은 또한 그림  4 의 발견 , 즉 키홀 모드 동안 흡수된 전력의 증가가 표류 입자 형성에 더 이상적인 조건을 초래한다는 것을 검증합니다. 그림  6 (b)는 실험을 비교Φ¯¯¯¯Φ¯수치 CFD 시뮬레이션Φ¯¯¯¯Φ¯. CFD 모델이 약간 초과 예측하지만Φ¯¯¯¯Φ¯전체적으로피- 브이피-V조건에서 열쇠 구멍 조건에서의 예측은 분석 모델보다 정확합니다. 전도 모드 용융 풀의 경우 실험 값이 분석 시뮬레이션 값과 더 가깝게 정렬됩니다.

그림 5
그림 5

모의 온도 구배 G 분포 및 응고율 검사V티V티분석 모델링의 쌍은 그림  7 (a)의 CMSX-4 미세 구조 선택 맵에 표시됩니다. 제공지 /V티G/V티(  , 형태 인자)는 형태를 제어하고지 ×V티G×V티(  , 냉각 속도)는 응고된 미세 구조의 규모를 제어하고 , 58 , 59 ]지 -V티G-V티플롯은 전통적인 제조 공정과 AM 공정 모두에서 미세 구조 제어를 지원합니다. 이 플롯의 몇 가지 분명한 특징은 등축, 주상, 평면 전면 및 이러한 경계 근처의 전이 영역을 구분하는 경계입니다. 그림  7 (a)는 몇 가지 선택된 분석 열 시뮬레이션에 대한 미세 구조 선택 맵을 나타내는 반면 그림  7 (b)는 수치 열 모델의 결과와 동일한 맵을 보여줍니다. 등축 미세구조의 형성은 낮은 G 이상 에서 명확하게 선호됩니다.V티V티정황. 이 플롯에서 각 곡선의 평면 전면에 가장 가까운 지점은 용융 풀의 최대 너비 위치에 해당하는 반면 등축 영역에 가까운 지점의 끝은 용융 풀의 후면 꼬리에 해당합니다. 그림  7 (a)에서 대부분의지 -V티G-V티응고 전면의 쌍은 원주형 영역에 속하고 점차 CET 영역으로 위쪽으로 이동하지만 용융 풀의 꼬리는 다음에 따라 완전히 등축 영역에 도달하거나 도달하지 않을 수 있습니다.피- 브이피-V조합. 그림 7 (a) 의 곡선 중 어느 것도  평면 전면 영역을 통과하지 않지만 더 높은 전력의 경우에 가까워집니다. 저속 레이저 용융 공정을 사용하는 이전 작업에서는 곡선이 평면 영역을 통과할 수 있습니다. 레이저 속도가 증가함에 따라 용융 풀 꼬리는 여전히 CET 영역에 있지만 완전히 등축 영역에서 멀어집니다. CET 영역으로 떨어지는 섹션의 수도 감소합니다.Φ¯¯¯¯Φ¯응고된 물질에서.

그림 6
그림 6

그만큼지 -V티G-V티CFD 모델을 사용하여 시뮬레이션된 응고 전면의 쌍이 그림  7 (b)에 나와 있습니다. 세 방향 모두에서 각 점 사이의 일정한 간격으로 미리 정의된 좌표에서 수행된 해석 시뮬레이션과 달리, 고충실도 CFD 모델의 출력은 불규칙한 사면체 좌표계에 있었고 G 를 추출하기 전에 일반 3D 그리드에 선형 보간되었습니다. 그리고V티V티그런 다음 미세 구조 선택 맵에 플롯됩니다. 일반적인 경향은 그림  7 (a)의 것과 일치하지만 이 방법으로 모델링된 매우 동적인 유체 흐름으로 인해 결과에 더 많은 분산이 있었습니다. 그만큼지 -V티G-V티분석 열 모델의 쌍 경로는 더 연속적인 반면 수치 시뮬레이션의 경로는 용융 풀 꼬리 모양의 차이를 나타내는 날카로운 굴곡이 있습니다(이는 G 및V티V티) 두 모델에 의해 시뮬레이션됩니다.

그림 7
그림 7
그림 8
그림 8

유체 흐름을 통합한 응고 모델링

수치 CFD 모델을 사용하여 유동 입자 형성 정도에 대한 유체 흐름의 영향을 이해하고 시뮬레이션 결과를 분석 Rosenthal 솔루션과 비교했습니다. 그림  8 은 응고 매개변수 G 의 분포를 보여줍니다.V티V티,지 /V티G/V티, 그리고지 ×V티G×V티yz 단면에서 x  FLOW-3D에서 (a1–d1) 분석 열 모델링 및 (a2–d2) FVM 방법을 사용하여 시뮬레이션된 용융 풀의 최대 폭입니다. 그림  8 의 값은 응고 전선이 특정 위치에 도달할 때 정확한 값일 수도 있고 아닐 수도 있지만 일반적인 추세를 반영한다는 의미의 임시 가상 값입니다. 이 프로파일은 출력 300W 및 속도 400mm/s의 레이저 빔에서 시뮬레이션됩니다. 용융 풀 경계는 흰색 곡선으로 표시됩니다. (a2–d2)의 CFD 시뮬레이션 용융 풀 깊이는 342입니다. μμm, 측정 깊이 352와 잘 일치 μμ일치하는 길쭉한 열쇠 구멍 모양과 함께 그림 1 에 표시된 실험 FZ의 m  . 그러나 분석 모델은 반원 모양의 용융 풀을 출력하고 용융 풀 깊이는 264에 불과합니다. μμ열쇠 구멍의 경우 현실과는 거리가 멀다. CFD 시뮬레이션 결과에서 열 구배는 레이저 반사 증가와 불안정한 액체-증기 상호 작용이 발생하는 증기 함몰의 동적 부분 근처에 있기 때문에 FZ 하단에서 더 높습니다. 대조적으로 해석 결과의 열 구배 크기는 경계를 따라 균일합니다. 두 시뮬레이션 결과 모두 그림 8 (a1) 및 (a2) 에서 응고가 용융 풀의 상단 중심선을 향해 진행됨에 따라 열 구배가 점차 감소합니다  . 응고율은 그림 8 과 같이 경계 근처에서 거의 0입니다. (b1) 및 (b2). 이는 경계 영역이 응고되기 시작할 때 국부 응고 전면의 법선 방향이 레이저 스캐닝 방향에 수직이기 때문입니다. 이것은 드라이브θ → π/ 2θ→파이/2그리고V티→ 0V티→0식에서 [ 3 ]. 대조적으로 용융 풀의 상단 중심선 근처 영역에서 응고 전면의 법선 방향은 레이저 스캐닝 방향과 잘 정렬되어 있습니다.θ → 0θ→0그리고V티→ 브이V티→V, 빔 스캐닝 속도. G 와 _V티V티값이 얻어지면 냉각 속도지 ×V티G×V티및 형태 인자지 /V티G/V티계산할 수 있습니다. 그림 8 (c2)는 용융 풀 바닥 근처의 온도 구배가 매우 높고 상단에서 더 빠른 성장 속도로  인해 냉각 속도가 용융 풀의 바닥 및 상단 중심선 근처에서 더 높다는 것을 보여줍니다. 지역. 그러나 이러한 추세는 그림  8 (c1)에 캡처되지 않았습니다. 그림 8 의 형태 요인 (d1) 및 (d2)는 중심선에 접근함에 따라 눈에 띄게 감소합니다. 경계에서 큰 값은 열 구배를 거의 0인 성장 속도로 나누기 때문에 발생합니다. 이 높은 형태 인자는 주상 미세구조 형성 가능성이 높음을 시사하는 반면, 중앙 영역의 값이 낮을수록 등축 미세구조의 가능성이 더 크다는 것을 나타냅니다. Tanet al. 또한 키홀 모양의 용접 풀 59 ] 에서 이러한 응고 매개변수의 분포 를 비슷한 일반적인 경향으로 보여주었습니다. 그림  3 에서 볼 수 있듯이 용융 풀의 상단 중심선에 있는 흩어진 입자는 낮은 특징을 나타내는 영역과 일치합니다.지 /V티G/V티그림  8 (d1) 및 (d2)의 값. 시뮬레이션과 실험 간의 이러한 일치는 용융 풀의 상단 중심선에 축적된 흩어진 입자의 핵 생성 및 성장이 등온선 속도의 증가와 온도 구배의 감소에 의해 촉진됨을 보여줍니다.

그림 9
그림 9

그림  9 는 유체 속도 및 국부적 핵형성 성향을 보여줍니다.ΦΦ300W의 일정한 레이저 출력과 400, 800 및 1200mm/s의 세 가지 다른 레이저 속도에 의해 생성된 3D 용융 풀 전체에 걸쳐. 그림  9 (d)~(f)는 로컬ΦΦ해당 3D 보기에서 밝은 회색 평면으로 표시된 특정 yz 단면의 분포. 이 yz 섹션은 가장 높기 때문에 선택되었습니다.Φ¯¯¯¯Φ¯용융 풀 내의 값은 각각 23.40, 11.85 및 2.45pct입니다. 이들은 그림  3 의 실험 데이터와 비교하기에 적절하지 않을 수 있는 액체 용융 풀의 과도 값이며Φ¯¯¯¯Φ¯그림  6 의 값은 이 값이 고체-액체 계면에 가깝지 않고 용융 풀의 중간에서 취해졌기 때문입니다. 온도가 훨씬 낮아서 핵이 생존하고 성장할 수 있기 때문에 핵 형성은 용융 풀의 중간이 아닌 고체-액체 계면에 더 가깝게 발생할 가능성이 있습니다.

그림  3 (a), (d), (g), (h)에서 위쪽 중심선에서 멀리 떨어져 있는 흩어진 결정립이 있었습니다. 그들은 훨씬 더 높은 열 구배와 더 낮은 응고 속도 필드에 위치하기 때문에 과냉각 이론은 이러한 영역에서 표류 입자의 형성에 대한 만족스러운 설명이 아닙니다. 이것은 떠돌이 결정립의 형성을 야기할 수 있는 두 번째 메커니즘,  수상돌기의 팁을 가로지르는 유체 흐름에 의해 유발되는 수상돌기 조각화를 고려하도록 동기를 부여합니다. 유체 흐름이 열 구배를 따라 속도 성분을 갖고 고체-액체 계면 속도보다 클 때, 주상 수상돌기의 국지적 재용융은 용질이 풍부한 액체가 흐물흐물한 구역의 깊은 곳에서 액상선 등온선까지 이동함으로써 발생할 수 있습니다. . 55] 분리된 수상돌기는 대류에 의해 열린 액체로 운반될 수 있습니다. 풀이 과냉각 상태이기 때문에 이러한 파편은 고온 조건에서 충분히 오래 생존하여 길 잃은 입자의 핵 생성 사이트로 작용할 수 있습니다. 결과적으로 수상 돌기 조각화 과정은 활성 핵의 수를 효과적으로 증가시킬 수 있습니다.N0N0) 용융 풀 15 , 60 , 61 ] 에서 생성된 미세 구조에서 표류 입자의 면적을 증가시킵니다.

그림  9 (a) 및 (b)에서 반동 압력은 용융 유체를 아래쪽으로 흐르게 하여 결과 흐름을 지배합니다. 유체 속도의 역방향 요소는 V = 400 및 800mm/s에 대해 각각 최대값 1.0 및 1.6m/s로 더 느려집니다 . 그림  9 (c)에서 레이저 속도가 더 증가함에 따라 증기 침하가 더 얕고 넓어지고 반동 압력이 더 고르게 분포되어 증기 침강에서 주변 영역으로 유체를 밀어냅니다. 역류는 최대값 3.5m/s로 더 빨라집니다. 용융 풀의 최대 너비에서 yz 단면  의 키홀 아래 평균 유체 속도는 그림에 표시된 경우에 대해 0.46, 0.45 및 1.44m/s입니다.9 (a), (b) 및 (c). 키홀 깊이의 변동은 각 경우의 최대 깊이와 최소 깊이의 차이로 정의되는 크기로 정량화됩니다. 240 범위의 강한 증기 내림 변동 μμm은 그림 9 (a)의 V = 400mm/s 경우에서  발견 되지만 이 변동은 그림  9 (c)에서 16의 범위로  크게 감소합니다.μμ미디엄. V = 400mm/s인 경우 의 유체장과 높은 변동 범위는 이전 키홀 동역학 시뮬레이션과 일치합니다. 34 ]

따라서 V = 400mm/s 키홀 케이스의 무질서한 변동 흐름이 용융 풀 경계를 따라 응고된 주상 수상돌기에서 분리된 조각을 구동할 가능성이 있습니다. V = 1200mm/s의 경우 강한 역류 는 그림 3 에서 관찰되지 않았지만 동일한 효과를 가질 수 있습니다. . 덴드라이트 조각화에 대한 유체 유동장의 영향에 대한 이 경험적 설명은 용융 풀 경계 근처에 떠돌이 입자의 존재에 대한 그럴듯한 설명을 제공합니다. 분명히 하기 위해, 우리는 이 가설을 검증하기 위해 이 현상에 대한 직접적인 실험적 관찰을 하지 않았습니다. 이 작업에서 표유 입자 면적 분율을 계산할 때 단순화를 위해 핵 생성 모델링에 일정한 핵 생성 수 밀도가 적용되었습니다. 이는 그림  9 의 표류 입자 영역 비율 이 수지상정 조각화가 발생하는 경우 이러한 높은 유체 흐름 용융 풀에서 발생할 수 있는 것,  강화된 핵 생성 밀도를 반영하지 않는다는 것을 의미합니다.

위의 이유로 핵 형성에 대한 수상 돌기 조각화의 영향을 아직 배제할 수 없습니다. 그러나 단편화 이론은 용접 문헌 [ 62 ] 에서 검증될 만큼 충분히 개발되지 않았 으므로 부차적인 중요성만 고려된다는 점에 유의해야 합니다. 1200mm/s를 초과하는 레이저 스캐닝 속도는 최소한의 표류 결정립 면적 분율을 가지고 있음에도 불구하고 분명한 볼링을 나타내기 때문에 단결정 수리 및 AM 처리에 적합하지 않습니다. 따라서 낮은 P 및 높은 V 에 의해 생성된 응고 전면 근처에서 키홀 변동이 최소화되고 유체 속도가 완만해진 용융 풀이 생성된다는 결론을 내릴 수 있습니다., 처리 창의 극한은 아니지만 흩어진 입자를 나타낼 가능성이 가장 적습니다.

마지막으로 단일 레이저 트랙의 응고 거동을 조사하면 에피택셜 성장 동안 표류 입자 형성을 더 잘 이해할 수 있다는 점에 주목하는 것이 중요합니다. 우리의 현재 결과는 최적의 레이저 매개변수에 대한 일반적인 지침을 제공하여 최소 스트레이 그레인을 달성하고 단결정 구조를 유지합니다. 이 가이드라인은 250W 정도의 전력과 600~800mm/s의 스캔 속도로 최소 흩어진 입자에 적합한 공정 창을 제공합니다. 각 처리 매개변수를 신중하게 선택하면 과거에 스테인리스강에 대한 거의 단결정 미세 구조를 인쇄하는 데 성공했으며 이는 CMSX-4 AM 빌드에 대한 가능성을 보여줍니다. 63 ]신뢰성을 보장하기 위해 AM 수리 프로세스를 시작하기 전에 보다 엄격한 실험 테스트 및 시뮬레이션이 여전히 필요합니다. 둘 이상의 레이저 트랙 사이의 상호 작용도 고려해야 합니다. 또한 레이저, CMSX-4 분말 및 벌크 재료 간의 상호 작용이 중요하며, 수리 중에 여러 층의 CMSX-4 재료를 축적해야 하는 경우 다른 스캔 전략의 효과도 중요한 역할을 할 수 있습니다. 분말이 포함된 경우 Lopez-Galilea 등 의 연구에서 제안한 바와 같이 분말이 주로 완전히 녹지 않았을 때 추가 핵 생성 사이트를 도입하기 때문에 단순히 레이저 분말과 속도를 조작하여 흩어진 입자 형성을 완화하기 어려울 수 있습니다 . 22 ]결과적으로 CMSX-4 단결정을 수리하기 위한 레이저 AM의 가능성을 다루기 위해서는 기판 재료, 레이저 출력, 속도, 해치 간격 및 층 두께의 조합을 모두 고려해야 하며 향후 연구에서 다루어야 합니다. CFD 모델링은 2개 이상의 레이저 트랙 사이의 상호작용과 열장에 미치는 영향을 통합할 수 있으며, 이는 AM 빌드 시나리오 동안 핵 생성 조건으로 단일 비드 연구의 지식 격차를 해소할 것입니다.

결론

LPBF 제조의 특징적인 조건 하에서 CMSX-4 단결정 의 에피택셜(기둥형)  등축 응고 사이의 경쟁을 실험적 및 이론적으로 모두 조사했습니다. 이 연구는 고전적인 응고 개념을 도입하여 빠른 레이저 용융의 미세 구조 특징을 설명하고 응고 조건과 표유 결정 성향을 예측하기 위해 해석적 및 수치적 고충실도 CFD 열 모델 간의 비교를 설명했습니다. 본 연구로부터 다음과 같은 주요 결론을 도출할 수 있다.

  • 단일 레이저 트랙의 레이저 가공 조건은 용융 풀 형상, 레이저 흡수율, 유체 흐름 및 키홀 요동, 입자 구조 및 표류 입자 형성 민감성에 강한 영향을 미치는 것으로 밝혀졌습니다.
  • 레이저 용접을 위해 개발된 이론적인 표유 결정립 핵형성 분석이 레이저 용융 AM 조건으로 확장되었습니다. 분석 모델링 결과와 단일 레이저 트랙의 미세구조 특성화를 비교하면 예측이 전도 및 볼링 조건에서 실험적 관찰과 잘 일치하는 반면 키홀 조건에서는 예측이 약간 과소하다는 것을 알 수 있습니다. 이러한 불일치는 레이저 트랙의 대표성이 없는 섹션이나 유체 속도 필드의 변화로 인해 발생할 수 있습니다. CFD 모델에서 추출한 열장에 동일한 표유 입자 계산 파이프라인을 적용하면 연구된 모든 사례에서 과대평가가 발생하지만 분석 모델보다 연장된 용융 풀의 실험 데이터와 더 정확하게 일치합니다.
  • 이 연구에서 두 가지 표류 결정립 형성 메커니즘인 불균일 핵형성 및 수상돌기 조각화가 평가되었습니다. 우리의 결과는 불균일 핵형성이 용융 풀의 상단 중심선에서 새로운 결정립의 형성으로 이어지는 주요 메커니즘임을 시사합니다.지 /V티G/V티정권.
  • 용융 풀 경계 근처의 흩어진 입자는 깊은 키홀 모양의 용융 풀에서 독점적으로 관찰되며, 이는 강한 유체 흐름으로 인한 수상 돌기 조각화의 영향이 이러한 유형의 용융 풀에서 고려하기에 충분히 강력할 수 있음을 시사합니다.
  • 일반적으로 더 높은 레이저 스캐닝 속도와 더 낮은 전력 외에도 안정적인 키홀과 최소 유체 속도는 또한 흩어진 입자 형성을 완화하고 레이저 단일 트랙에서 에피택셜 성장을 보존합니다.

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Fig. 1. (a) Dimensions of the casting with runners (unit: mm), (b) a melt flow simulation using Flow-3D software together with Reilly's model[44], predicted that a large amount of bifilms (denoted by the black particles) would be contained in the final casting. (c) A solidification simulation using Pro-cast software showed that no shrinkage defect was contained in the final casting.

AZ91 합금 주물 내 연행 결함에 대한 캐리어 가스의 영향

TianLiabJ.M.T.DaviesaXiangzhenZhuc
aUniversity of Birmingham, Birmingham B15 2TT, United Kingdom
bGrainger and Worrall Ltd, Bridgnorth WV15 5HP, United Kingdom
cBrunel Centre for Advanced Solidification Technology, Brunel University London, Kingston Ln, London, Uxbridge UB8 3PH, United Kingdom

Abstract

An entrainment defect (also known as a double oxide film defect or bifilm) acts a void containing an entrapped gas when submerged into a light-alloy melt, thus reducing the quality and reproducibility of the final castings. Previous publications, carried out with Al-alloy castings, reported that this trapped gas could be subsequently consumed by the reaction with the surrounding melt, thus reducing the void volume and negative effect of entrainment defects. Compared with Al-alloys, the entrapped gas within Mg-alloy might be more efficiently consumed due to the relatively high reactivity of magnesium. However, research into the entrainment defects within Mg alloys has been significantly limited. In the present work, AZ91 alloy castings were produced under different carrier gas atmospheres (i.e., SF6/CO2, SF6/air). The evolution processes of the entrainment defects contained in AZ91 alloy were suggested according to the microstructure inspections and thermodynamic calculations. The defects formed in the different atmospheres have a similar sandwich-like structure, but their oxide films contained different combinations of compounds. The use of carrier gases, which were associated with different entrained-gas consumption rates, affected the reproducibility of AZ91 castings.

연행 결함(이중 산화막 결함 또는 이중막이라고도 함)은 경합금 용융물에 잠길 때 갇힌 가스를 포함하는 공극으로 작용하여 최종 주물의 품질과 재현성을 저하시킵니다. Al-합금 주물을 사용하여 수행된 이전 간행물에서는 이 갇힌 가스가 주변 용융물과의 반응에 의해 후속적으로 소모되어 공극 부피와 연행 결함의 부정적인 영향을 줄일 수 있다고 보고했습니다. Al-합금에 비해 마그네슘의 상대적으로 높은 반응성으로 인해 Mg-합금 내에 포집된 가스가 더 효율적으로 소모될 수 있습니다. 그러나 Mg 합금 내 연행 결함에 대한 연구는 상당히 제한적이었습니다. 현재 작업에서 AZ91 합금 주물은 다양한 캐리어 가스 분위기(즉, SF6/CO2, SF6/공기)에서 생산되었습니다. AZ91 합금에 포함된 연행 결함의 진화 과정은 미세 조직 검사 및 열역학 계산에 따라 제안되었습니다. 서로 다른 분위기에서 형성된 결함은 유사한 샌드위치 구조를 갖지만 산화막에는 서로 다른 화합물 조합이 포함되어 있습니다. 다른 동반 가스 소비율과 관련된 운반 가스의 사용은 AZ91 주물의 재현성에 영향을 미쳤습니다.

Keywords

Magnesium alloy, Casting, Oxide film, Bifilm, Entrainment defect, Reproducibility

1. Introduction

As the lightest structural metal available on Earth, magnesium became one of the most attractive light metals over the last few decades. The magnesium industry has consequently experienced a rapid development in the last 20 years [1,2], indicating a large growth in demand for Mg alloys all over the world. Nowadays, the use of Mg alloys can be found in the fields of automobiles, aerospace, electronics and etc.[3,4]. It has been predicted that the global consumption of Mg metals will further increase in the future, especially in the automotive industry, as the energy efficiency requirement of both traditional and electric vehicles further push manufactures lightweight their design [3,5,6].

The sustained growth in demand for Mg alloys motivated a wide interest in the improvement of the quality and mechanical properties of Mg-alloy castings. During a Mg-alloy casting process, surface turbulence of the melt can lead to the entrapment of a doubled-over surface film containing a small quantity of the surrounding atmosphere, thus forming an entrainment defect (also known as a double oxide film defect or bifilm) [7][8][9][10]. The random size, quantity, orientation, and placement of entrainment defects are widely accepted to be significant factors linked to the variation of casting properties [7]. In addition, Peng et al. [11] found that entrained oxides films in AZ91 alloy melt acted as filters to Al8Mn5 particles, trapping them as they settle. Mackie et al. [12] further suggested that entrained oxide films can act to trawl the intermetallic particles, causing them to cluster and form extremely large defects. The clustering of intermetallic compounds made the entrainment defects more detrimental for the casting properties.

Most of the previous studies regarding entrainment defects were carried out on Al-alloys [7,[13][14][15][16][17][18], and a few potential methods have been suggested for diminishing their negative effect on the quality of Al-alloy castings. Nyahumwa et al.,[16] shows that the void volume within entrainment defects could be reduced by a hot isostatic pressing (HIP) process. Campbell [7] suggested the entrained gas within the defects could be consumed due to reaction with the surrounding melt, which was further verified by Raiszedeh and Griffiths [19].The effect of the entrained gas consumption on the mechanical properties of Al-alloy castings has been investigated by [8,9], suggesting that the consumption of the entrained gas promoted the improvement of the casting reproducibility.

Compared with the investigation concerning the defects within Al-alloys, research into the entrainment defects within Mg-alloys has been significantly limited. The existence of entrainment defects has been demonstrated in Mg-alloy castings [20,21], but their behaviour, evolution, as well as entrained gas consumption are still not clear.

In a Mg-alloy casting process, the melt is usually protected by a cover gas to avoid magnesium ignition. The cavities of sand or investment moulds are accordingly required to be flushed with the cover gas prior to the melt pouring [22]. Therefore, the entrained gas within Mg-alloy castings should contain the cover gas used in the casting process, rather than air only, which may complicate the structure and evolution of the corresponding entrainment defects.

SF6 is a typical cover gas widely used for Mg-alloy casting processes [23][24][25]. Although this cover gas has been restricted to use in European Mg-alloy foundries, a commercial report has pointed out that this cover is still popular in global Mg-alloy industry, especially in the countries which dominated the global Mg-alloy production, such as China, Brazil, India, etc. [26]. In addition, a survey in academic publications also showed that this cover gas was widely used in recent Mg-alloy studies [27]. The protective mechanism of SF6 cover gas (i.e., the reaction between liquid Mg-alloy and SF6 cover gas) has been investigated by several previous researchers, but the formation process of the surface oxide film is still not clearly understood, and even some published results are conflicting with each other. In early 1970s, Fruehling [28] found that the surface film formed under SF6 was MgO mainly with traces of fluorides, and suggested that SF6 was absorbed in the Mg-alloy surface film. Couling [29] further noticed that the absorbed SF6 reacted with the Mg-alloy melt to form MgF2. In last 20 years, different structures of the Mg-alloy surface films have been reported, as detailed below.(1)

Single-layered film. Cashion [30,31] used X-ray Photoelectron Spectroscopy (XPS) and Auger Spectroscopy (AES) to identify the surface film as MgO and MgF2. He also found that composition of the film was constant throughout the thickness and the whole experimental holding time. The film observed by Cashion had a single-layered structure created from a holding time from 10 min to 100 min.(2)

Double-layered film. Aarstad et. al [32] reported a doubled-layered surface oxide film in 2003. They observed several well-distributed MgF2 particles attached to the preliminary MgO film and grew until they covered 25–50% of the total surface area. The inward diffusion of F through the outer MgO film was the driving force for the evolution process. This double-layered structure was also supported by Xiong’s group [25,33] and Shih et al. [34].(3)

Triple-layered film. The triple-layered film and its evolution process were reported in 2002 by Pettersen [35]. Pettersen found that the initial surface film was a MgO phase and then gradually evolved to the stable MgF2 phase by the inward diffusion of F. In the final stage, the film has a triple-layered structure with a thin O-rich interlayer between the thick top and bottom MgF2 layers.(4)

Oxide film consisted of discrete particles. Wang et al [36] stirred the Mg-alloy surface film into the melt under a SF6 cover gas, and then inspect the entrained surface film after the solidification. They found that the entrained surface films were not continues as the protective surface films reported by other researchers but composed of discrete particles. The young oxide film was composed of MgO nano-sized oxide particles, while the old oxide films consist of coarse particles (about 1  µm in average size) on one side that contained fluorides and nitrides.

The oxide films of a Mg-alloy melt surface or an entrained gas are both formed due to the reaction between liquid Mg-alloy and the cover gas, thus the above-mentioned research regarding the Mg-alloy surface film gives valuable insights into the evolution of entrainment defects. The protective mechanism of SF6 cover gas (i.e., formation of a Mg-alloy surface film) therefore indicated a potential complicated evolution process of the corresponding entrainment defects.

However, it should be noted that the formation of a surface film on a Mg-alloy melt is in a different situation to the consumption of an entrained gas that is submerged into the melt. For example, a sufficient amount of cover gas was supported during the surface film formation in the studies previously mentioned, which suppressed the depletion of the cover gas. In contrast, the amount of entrained gas within a Mg-alloy melt is finite, and the entrained gas may become fully depleted. Mirak [37] introduced 3.5%SF6/air bubbles into a pure Mg-alloy melt solidifying in a specially designed permanent mould. It was found that the gas bubbles were entirely consumed, and the corresponding oxide film was a mixture of MgO and MgF2. However, the nucleation sites (such as the MgF2 spots observed by Aarstad [32] and Xiong [25,33]) were not observed. Mirak also speculated that the MgF2 formed prior to MgO in the oxide film based on the composition analysis, which was opposite to the surface film formation process reported in previous literatures (i.e., MgO formed prior to MgF2). Mirak’s work indicated that the oxide-film formation of an entrained gas may be quite different from that of surface films, but he did not reveal the structure and evolution of the oxide films.

In addition, the use of carrier gas in the cover gases also influenced the reaction between the cover gas and the liquid Mg-alloy. SF6/air required a higher content of SF6 than did a SF6/CO2 carrier gas [38], to avoid the ignition of molten magnesium, revealing different gas-consumption rates. Liang et.al [39] suggested that carbon was formed in the surface film when CO2 was used as a carrier gas, which was different from the films formed in SF6/air. An investigation into Mg combustion [40] reported a detection of Mg2C3 in the Mg-alloy sample after burning in CO2, which not only supported Liang’s results, but also indicated a potential formation of Mg carbides in double oxide film defects.

The work reported here is an investigation into the behaviour and evolution of entrainment defects formed in AZ91 Mg-alloy castings, protected by different cover gases (i.e., SF6/air and SF6/CO2). These carrier gases have different protectability for liquid Mg alloy, which may be therefore associated with different consumption rates and evolution processes of the corresponding entrained gases. The effect of the entrained-gas consumption on the reproducibility of AZ91 castings was also studied.

2. Experiment

2.1. Melting and casting

Three kilograms AZ91 alloy was melted in a mild steel crucible at 700 ± 5 °C. The composition of the AZ91 alloy has been shown in Table 1. Prior to heating, all oxide scale on the ingot surface was removed by machining. The cover gases used were 0.5%SF6/air or 0.5%SF6/CO2 (vol.%) at a flow rate of 6 L/min for different castings. The melt was degassed by argon with a flow rate of 0.3 L/min for 15 min [41,42], and then poured into sand moulds. Prior to pouring, the sand mould cavity was flushed with the cover gas for 20 min [22]. The residual melt (around 1 kg) was solidified in the crucible.

Table 1. Composition (wt.%) of the AZ91 alloy used in this study.

AlZnMnSiFeNiMg
9.40.610.150.020.0050.0017Residual

Fig. 1(a) shows the dimensions of the casting with runners. A top-filling system was deliberately used to generate entrainment defects in the final castings. Green and Campbell [7,43] suggested that a top-filling system caused more entrainment events (i.e., bifilms) during a casting process, compared with a bottom-filling system. A melt flow simulation (Flow-3D software) of this mould, using Reilly’s model [44] regarding the entrainment events, also predicted that a large amount of bifilms would be contained in the final casting (denoted by the black particles in Fig. 1b).

Fig. 1. (a) Dimensions of the casting with runners (unit: mm), (b) a melt flow simulation using Flow-3D software together with Reilly's model[44], predicted that a large amount of bifilms (denoted by the black particles) would be contained in the final casting. (c) A solidification simulation using Pro-cast software showed that no shrinkage defect was contained in the final casting.

Shrinkage defects also affect the mechanical properties and reproducibility of castings. Since this study focused on the effect of bifilms on the casting quality, the mould has been deliberately designed to avoid generating shrinkage defects. A solidification simulation using ProCAST software showed that no shrinkage defect would be contained in the final casting, as shown in Fig. 1c. The casting soundness has also been confirmed using a real time X-ray prior to the test bar machining.

The sand moulds were made from resin-bonded silica sand, containing 1wt. % PEPSET 5230 resin and 1wt. % PEPSET 5112 catalyst. The sand also contained 2 wt.% Na2SiF6 to act as an inhibitor [45]. The pouring temperature was 700 ± 5 °C. After the solidification, a section of the runner bars was sent to the Sci-Lab Analytical Ltd for a H-content analysis (LECO analysis), and all the H-content measurements were carried out on the 5th day after the casting process. Each of the castings was machined into 40 test bars for a tensile strength test, using a Zwick 1484 tensile test machine with a clip extensometer. The fracture surfaces of the broken test bars were examined using Scanning Electron Microscope (SEM, Philips JEOL7000) with an accelerating voltage of 5–15 kV. The fractured test bars, residual Mg-alloy solidified in the crucible, and the casting runners were then sectioned, polished and also inspected using the same SEM. The cross-section of the oxide film found on the test-bar fracture surface was exposed by the Focused Ion Beam milling technique (FIB), using a CFEI Quanta 3D FEG FIB-SEM. The oxide film required to be analysed was coated with a platinum layer. Then, a gallium ion beam, accelerated to 30 kV, milled the material substrate surrounding the platinum coated area to expose the cross section of the oxide film. EDS analysis of the oxide film’s cross section was carried out using the FIB equipment at accelerating voltage of 30 kV.

2.2. Oxidation cell

As previously mentioned, several past researchers investigated the protective film formed on a Mg-alloy melt surface [38,39,[46][47][48][49][50][51][52]. During these experiments, the amount of cover gas used was sufficient, thus suppressing the depletion of fluorides in the cover gas. The experiment described in this section used a sealed oxidation cell, which limited the supply of cover gas, to study the evolution of the oxide films of entrainment defects. The cover gas contained in the oxidation cell was regarded as large-size “entrained bubble”.

As shown in Fig. 2, the main body of the oxidation cell was a closed-end mild steel tube which had an inner length of 400 mm, and an inner diameter of 32 mm. A water-cooled copper tube was wrapped around the upper section of the cell. When the tube was heated, the cooling system created a temperature difference between the upper and lower sections, causing the interior gas to convect within the tube. The temperature was monitored by a type-K thermocouple located at the top of the crucible. Nie et al. [53] suggested that the SF6 cover gas would react with the steel wall of the holding furnace when they investigated the surface film of a Mg-alloy melt. To avoid this reaction, the interior surface of the steel oxidation cell (shown in Fig. 2) and the upper half section of the thermocouple were coated with boron nitride (the Mg-alloy was not in contact with boron nitride).

Fig. 2. Schematic of the oxidation cell used to study the evolution of the oxide films of the entrainment defects (unit mm).

During the experiment, a block of solid AZ91 alloy was placed in a magnesia crucible located at the bottom of the oxidation cell. The cell was heated to 100 °C in an electric resistance furnace under a gas flow rate of 1 L/min. The cell was held at this temperature for 20 min, to replace the original trapped atmosphere (i.e. air). Then, the oxidation cell was further heated to 700 °C, melting the AZ91 sample. The gas inlet and exit valves were then closed, creating a sealed environment for oxidation under a limited supply of cover gas. The oxidation cell was then held at 700 ± 10 °C for periods of time from 5 min to 30 min in 5-min intervals. At the end of each holding time, the cell was quenched in water. After cooling to room temperature, the oxidised sample was sectioned, polished, and subsequently examined by SEM.

3. Results

3.1. Structure and composition of the entrainment defects formed in SF6/air

The structure and composition of the entrainment defect formed in the AZ91 castings under a cover gas of 0.5%SF6/air was observed by SEM and EDS. The results indicate that there exist two types of entrainment defects which are sketched in Fig. 3: (1) Type A defect whose oxide film has a traditional single-layered structure and (2) Type B defect, whose oxide film has two layers. The details of these defects were introduced in the following. Here it should be noticed that, as the entrainment defects are also known as biofilms or double oxide film, the oxide films of Type B defect were referred to as “multi-layered oxide film” or “multi-layered structure” in the present work to avoid a confusing description such as “the double-layered oxide film of a double oxide film defect”.

Fig. 3. Schematic of the different types of entrainment defects found in AZ91 castings. (a) Type A defect with a single-layered oxide film and (b) Type B defect with two-layered oxide film.

Fig. 4(a-b) shows a Type A defect having a compact single-layered oxide film with about 0.4 µm thickness. Oxygen, fluorine, magnesium and aluminium were detected in this film (Fig. 4c). It is speculated that oxide film is the mixture of fluoride and oxide of magnesium and aluminium. The detection of fluorine revealed that an entrained cover gas was contained in the formation of this defect. That is to say that the pores shown in Fig. 4(a) were not shrinkage defects or hydrogen porosity, but entrainment defects. The detection of aluminium was different with Xiong and Wang’s previous study [47,48], which showed that no aluminium was contained in their surface film of an AZ91 melt protected by a SF6 cover gas. Sulphur could not be clearly recognized in the element map, but there was a S-peak in the corresponding ESD spectrum.

Fig. 4. (a) A Type A entrainment defect formed in SF6/air and having a single-layered oxide film, (b) the oxide film of this defect, (c) SEM-EDS element maps (using Philips JEOL7000) corresponding to the area highlighted in (b).

Fig. 5(a-b) shows a Type B entrainment defect having a multi-layered oxide film. The compact outer layers of the oxide films were enriched with fluorine and oxygen (Fig. 5c), while their relatively porous inner layers were only enriched with oxygen (i.e., poor in fluorine) and partly grew together, thus forming a sandwich-like structure. Therefore, it is speculated that the outer layer is the mixture of fluoride and oxide, while the inner layer is mainly oxide. Sulphur could only be recognized in the EDX spectrum and could not be clearly identified in the element map, which might be due to the small S-content in the cover gas (i.e., 0.5% volume content of SF6 in the cover gas). In this oxide film, aluminium was contained in the outer layer of this oxide film but could not be clearly detected in the inner layer. Moreover, the distribution of Al seems to be uneven. It can be found that, in the right side of the defect, aluminium exists in the film but its concentration can not be identified to be higher than the matrix. However, there is a small area with much higher aluminium concentration in the left side of the defect. Such an uneven distribution of aluminium was also observed in other defects (shown in the following), and it is the result of the formation of some oxide particles in or under the film.

Fig. 5. (a) A Type B entrainment defect formed in SF6/air and having a multi-layered oxide film, (b) the oxide films of this defect have grown together, (c) SEM-EDS element maps (using Philips JEOL7000) corresponding to the area shown in (b).

Figs. 4 and 5 show cross sectional observations of the entrainment defects formed in the AZ91 alloy sample cast under a cover gas of SF6/air. It is not sufficient to characterize the entrainment defects only by the figures observed from the two-dimensional section. To have a further understanding, the surface of the entrainment defects (i.e. the oxide film) was further studied by observing the fracture surface of the test bars.

Fig. 6(a) shows fracture surfaces of an AZ91 alloy tensile test bar produced in SF6/air. Symmetrical dark regions can be seen on both sides of the fracture surfaces. Fig. 6(b) shows boundaries between the dark and bright regions. The bright region consisted of jagged and broken features, while the surface of the dark region was relatively smooth and flat. In addition, the EDS results (Fig. 6c-d and Table 2) show that fluorine, oxygen, sulphur, and nitrogen were only detected in the dark regions, indicating that the dark regions were surface protective films entrained into the melt. Therefore, it could be suggested that the dark regions were an entrainment defect with consideration of their symmetrical nature. Similar defects on fracture surfaces of Al-alloy castings have been previously reported [7]Nitrides were only found in the oxide films on the test-bar fracture surfaces but never detected in the cross-sectional samples shown in Figs. 4 and 5. An underlying reason is that the nitrides contained in these samples may have hydrolysed during the sample polishing process [54].

Fig. 6. (a) A pair of the fracture surfaces of a AZ91 alloy tensile test bar produced under a cover gas of SF6/air. The dimension of the fracture surface is 5 mm × 6 mm, (b) a section of the boundary between the dark and bright regions shown in (a), (c-d) EDS spectrum of the (c) bright regions and (d) dark regions, (e) schematic of an entrainment defect contained in a test bar.

Table 2. EDS results (wt.%) corresponding to the regions shown in Fig. 6 (cover gas: SF6/air).

Empty CellCOMgFAlZnSN
Dark region in Fig. 6(b)3.481.3279.130.4713.630.570.080.73
Bright region in Fig. 6(b)3.5884.4811.250.68

In conjunction with the cross-sectional observation of the defects shown in Figs. 4 and 5, the structure of an entrainment defect contained in a tensile test bar was sketched as shown in Fig. 6(e). The defect contained an entrained gas enclosed by its oxide film, creating a void section inside the test bar. When the tensile force applied on the defect during the fracture process, the crack was initiated at the void section and propagated along the entrainment defect, since cracks would be propagated along the weakest path [55]. Therefore, when the test bar was finally fractured, the oxide films of entrainment defect appeared on both fracture surfaces of the test bar, as shown in Fig. 6(a).

3.2. Structure and composition of the entrainment defects formed in SF6/CO2

Similar to the entrainment defect formed in SF6/air, the defects formed under a cover gas of 0.5%SF6/CO2 also had two types of oxide films (i.e., single-layered and multi-layered types). Fig. 7(a) shows an example of the entrainment defects containing a multi-layered oxide film. A magnified observation to the defect (Fig. 7b) shows that the inner layers of the oxide films had grown together, presenting a sandwich-like structure, which was similar to the defects formed in an atmosphere of SF6/air (Fig. 5b). An EDS spectrum (Fig. 7c) revealed that the joint area (inner layer) of this sandwich-like structure mainly contained magnesium oxides. Peaks of fluorine, sulphur, and aluminium were recognized in this EDS spectrum, but their amount was relatively small. In contrast, the outer layers of the oxide films were compact and composed of a mixture of fluorides and oxides (Fig. 7d-e).

Fig. 7. (a) An example of entrainment defects formed in SF6/CO2 and having a multi-layered oxide film, (b) magnified observation of the defect, showing the inner layer of the oxide films has grown together, (c) EDS spectrum of the point denoted in (b), (d) outer layer of the oxide film, (e) SEM-EDS element maps (using Philips JEOL7000) corresponding to the area shown in (d).

Fig. 8(a) shows an entrainment defect on the fracture surfaces of an AZ91 alloy tensile test bar, which was produced in an atmosphere of 0.5%SF6/CO2. The corresponding EDS results (Table 3) showed that oxide film contained fluorides and oxides. Sulphur and nitrogen were not detected. Besides, a magnified observation (Fig. 8b) indicated spots on the oxide film surface. The diameter of the spots ranged from hundreds of nanometres to a few micron meters.

Fig. 8. (a) A pair of the fracture surfaces of a AZ91 alloy tensile test bar, produced in an atmosphere of SF6/CO2. The dimension of the fracture surface is 5 mm × 6 mm, (b) surface appearance of the oxide films on the fracture surfaces, showing spots on the film surface.

To further reveal the structure and composition of the oxide film clearly, the cross-section of the oxide film on a test-bar fracture surface was onsite exposed using the FIB technique (Fig. 9). As shown in Fig. 9a, a continuous oxide film was found between the platinum coating layer and the Mg-Al alloy substrate. Fig. 9 (b-c) shows a magnified observation to oxide films, indicating a multi-layered structure (denoted by the red box in Fig. 9c). The bottom layer was enriched with fluorine and oxygen and should be the mixture of fluoride and oxide, which was similar to the “outer layer” shown in Figs. 5 and 7, while the only-oxygen-enriched top layer was similar to the “inner layer” shown in Figs. 5 and 7.

Fig. 9. (a) A cross-sectional observation of the oxide film on the fracture surface of the AZ91 casting produced in SF6/CO2, exposed by FIB, (b) a magnified observation of area highlighted in (a), and (c) SEM-EDS elements map of the area shown in (b), obtained by CFEI Quanta 3D FEG FIB-SEM.

Except the continuous film, some individual particles were also observed in or below the continuous film, as shown in Fig. 9. An Al-enriched particle was detected in the left side of the oxide film shown in Fig. 9b and might be speculated to be spinel Mg2AlO4 because it also contains abundant magnesium and oxygen elements. The existing of such Mg2AlO4 particles is responsible for the high concentration of aluminium in small areas of the observed film and the uneven distribution of aluminium, as shown in Fig. 5(c). Here it should be emphasized that, although the other part of the bottom layer of the continuous oxide film contains less aluminium than this Al-enriched particle, the Fig. 9c indicated that the amount of aluminium in this bottom layer was still non-negligible, especially when comparing with the outer layer of the film. Below the right side of the oxide film shown in Fig. 9b, a particle was detected and speculated to be MgO because it is rich in Mg and O. According to Wang’s result [56], lots of discrete MgO particles can be formed on the surface of the Mg melt by the oxidation of Mg melt and Mg vapor. The MgO particles observed in our present work may be formed due to the same reasons. While, due to the differences in experimental conditions, less Mg melt can be vapored or react with O2, thus only a few of MgO particles formed in our work. An enrichment of carbon was also found in the film, revealing that CO2 was able to react with the melt, thus forming carbon or carbides. This carbon concentration was consistent with the relatively high carbon content of the oxide film shown in Table 3 (i.e., the dark region). In the area next to the oxide film.

Table 3. EDS results (wt.%) corresponding to the regions shown in Fig. 8 (cover gas: SF6/ CO2).

Empty CellCOMgFAlZnSN
Dark region in Fig. 8(a)7.253.6469.823.827.030.86
Bright region in Fig. 8(a)2.100.4482.8313.261.36

This cross-sectional observation of the oxide film on a test bar fracture surface (Fig. 9) further verified the schematic of the entrainment defect shown in Fig. 6(e). The entrainment defects formed in different atmospheres of SF6/CO2 and SF6/air had similar structures, but their compositions were different.

3.3. Evolution of the oxide films in the oxidation cell

The results in Section 3.1 and 3.2 have shown the structures and compositions of entrainment defects formed in AZ91 castings under cover gases of SF6/air and SF6/CO2. Different stages of the oxidation reaction may lead to the different structures and compositions of entrainment defects. Although Campbell has conjectured that an entrained gas may react with the surrounding melt, it is rarely reported that the reaction occurring between the Mg-alloy melt and entrapped cover gas. Previous researchers normally focus on the reaction between a Mg-alloy melt and the cover gas in an open environment [38,39,[46][47][48][49][50][51][52], which was different from the situation of a cover gas trapped into the melt. To further understand the formation of the entrainment defect in an AZ91 alloy, the evolution process of oxide films of the entrainment defect was further studied using an oxidation cell.

Fig. 10 (a and d) shows a surface film held for 5 min in the oxidation cell, protected by 0.5%SF6/air. There was only one single layer consisting of fluoride and oxide (MgF2 and MgO). In this surface film. Sulphur was detected in the EDS spectrum, but its amount was too small to be recognized in the element map. The structure and composition of this oxide film was similar to the single-layered films of entrainment defects shown in Fig. 4.

Fig. 10. Oxide films formed in the oxidation cell under a cover gas of 0.5%SF6/air and held at 700 °C for (a) 5 min; (b) 10 min; (c) 30 min, and (d-f) the SEM-EDS element maps (using Philips JEOL7000) corresponding to the oxide film shown in (a-c) respectively, (d) 5 min; (e) 10 min; (f) 30 min. The red points in (c and f) are the location references, denoting the boundary of the F-enriched layer in different element maps.

After a holding time of 10 min, a thin (O, S)-enriched top layer (around 700 nm) appeared upon the preliminary F-enriched film, forming a multi-layered structure, as shown in Fig. 10(b and e). The thickness of the (O, S)-enriched top layer increased with increased holding time. As shown in Fig. 10(c and f), the oxide film held for 30 min also had a multi-layered structure, but the thickness of its (O, S)-enriched top layer (around 2.5 µm) was higher than the that of the 10-min oxide film. The multi-layered oxide films shown in Fig. 10(b-c) presented a similar appearance to the films of the sandwich-like defect shown in Fig. 5.

The different structures of the oxide films shown in Fig. 10 indicated that fluorides in the cover gas would be preferentially consumed due to the reaction with the AZ91 alloy melt. After the depletion of fluorides, the residual cover gas reacted further with the liquid AZ91 alloy, forming the top (O, S)-enriched layer in the oxide film. Therefore, the different structures and compositions of entrainment defects shown in Figs. 4 and 5 may be due to an ongoing oxidation reaction between melt and entrapped cover gas.

This multi-layered structure has not been reported in previous publications concerning the protective surface film formed on a Mg-alloy melt [38,[46][47][48][49][50][51]. This may be due to the fact that previous researchers carried out their experiments with an un-limited amount of cover gas, creating a situation where the fluorides in the cover gas were not able to become depleted. Therefore, the oxide film of an entrainment defect had behaviour traits similar to the oxide films shown in Fig. 10, but different from the oxide films formed on the Mg-alloy melt surface reported in [38,[46][47][48][49][50][51].

Similar with the oxide films held in SF6/air, the oxide films formed in SF6/CO2 also had different structures with different holding times in the oxidation cell. Fig. 11(a) shows an oxide film, held on an AZ91 melt surface under a cover gas of 0.5%SF6/CO2 for 5 min. This film had a single-layered structure consisting of MgF2. The existence of MgO could not be confirmed in this film. After the holding time of 30 min, the film had a multi-layered structure; the inner layer was of a compact and uniform appearance and composed of MgF2, while the outer layer is the mixture of MgF2 and MgO. Sulphur was not detected in this film, which was different from the surface film formed in 0.5%SF6/air. Therefore, fluorides in the cover gas of 0.5%SF6/CO2 were also preferentially consumed at an early stage of the film growth process. Compared with the film formed in SF6/air, the MgO in film formed in SF6/CO2 appeared later and sulphide did not appear within 30 min. It may mean that the formation and evolution of film in SF6/air is faster than SF6/CO2. CO2 may have subsequently reacted with the melt to form MgO, while sulphur-containing compounds accumulated in the cover gas and reacted to form sulphide in very late stage (may after 30 min in oxidation cell).

Fig. 11. Oxide films formed in the oxidation cell under a cover gas of 0.5%SF6/CO2, and their SEM-EDS element maps (using Philips JEOL7000). They were held at 700 °C for (a) 5 min; (b) 30 min. The red points in (b) are the location references, denoting the boundary between the top and bottom layers in the oxide film.

4. Discussion

4.1. Evolution of entrainment defects formed in SF6/air

HSC software from Outokumpu HSC Chemistry for Windows (http://www.hsc-chemistry.net/) was used to carry out thermodynamic calculations needed to explore the reactions which might occur between the trapped gases and liquid AZ91 alloy. The solutions to the calculations suggest which products are most likely to form in the reaction process between a small amount of cover gas (i.e., the amount within a trapped bubble) and the AZ91-alloy melt.

In the trials, the pressure was set to 1 atm, and the temperature set to 700 °C. The amount of the cover gas was assumed to be 7 × 10−7 kg, with a volume of approximately 0.57 cm3 (3.14 × 10−8 kmol) for 0.5%SF6/air, and 0.35 cm3 (3.12 × 10−8 kmol) for 0.5%SF6/CO2. The amount of the AZ91 alloy melt in contact with the trapped gas was assumed to be sufficient to complete all reactions. The decomposition products of SF6 were SF5, SF4, SF3, SF2, F2, S(g), S2(g) and F(g) [57][58][59][60].

Fig. 12 shows the equilibrium diagram of the thermodynamic calculation of the reaction between the AZ91 alloy and 0.5%SF6/air. In the diagram, the reactants and products with less than 10−15 kmol have not been shown, as this was 5 orders of magnitude less than the amount of SF6 present (≈ 1.57 × 10−10 kmol) and therefore would not affect the observed process in a practical way.

Fig. 12. An equilibrium diagram for the reaction between 7e-7 kg 0.5%SF6/air and a sufficient amount of AZ91 alloy. The X axis is the amount of AZ91 alloy melt having reacted with the entrained gas, and the vertical Y-axis is the amount of the reactants and products.

This reaction process could be divided into 3 stages.

Stage 1: The formation of fluorides. the AZ91 melt preferentially reacted with SF6 and its decomposition products, producing MgF2, AlF3, and ZnF2. However, the amount of ZnF2 may have been too small to be detected practically (1.25 × 10−12 kmol of ZnF2 compared with 3 × 10−10 kmol of MgF2), which may be the reason why Zn was not detected in any the oxide films shown in Sections 3.13.3. Meanwhile, sulphur accumulated in the residual gas as SO2.

Stage 2: The formation of oxides. After the liquid AZ91 alloy had depleted all the available fluorides in the entrapped gas, the amount of AlF3 and ZnF2 quickly reduced due to a reaction with Mg. O2(g) and SO2 reacted with the AZ91 melt, forming MgO, Al2O3, MgAl2O4, ZnO, ZnSO4 and MgSO4. However, the amount of ZnO and ZnSO4 would have been too small to be found practically by EDS (e.g. 9.5 × 10−12 kmol of ZnO,1.38 × 10−14 kmol of ZnSO4, in contrast to 4.68 × 10−10 kmol of MgF2, when the amount of AZ91 on the X-axis is 2.5 × 10−9 kmol). In the experimental cases, the concentration of F in the cover gas is very low, whole the concentration f O is much higher. Therefore, the stage 1 and 2, i.e, the formation of fluoride and oxide may happen simultaneously at the beginning of the reaction, resulting in the formation of a singer-layered mixture of fluoride and oxide, as shown in Figs. 4 and 10(a). While an inner layer consisted of oxides but fluorides could form after the complete depletion of F element in the cover gas.

Stages 1- 2 theoretically verified the formation process of the multi-layered structure shown in Fig. 10.

The amount of MgAl2O4 and Al2O3 in the oxide film was of a sufficient amount to be detected, which was consistent with the oxide films shown in Fig. 4. However, the existence of aluminium could not be recognized in the oxide films grown in the oxidation cell, as shown in Fig. 10. This absence of Al may be due to the following reactions between the surface film and AZ91 alloy melt:(1)

Al2O3 + 3Mg + = 3MgO + 2Al, △G(700 °C) = -119.82 kJ/mol(2)

Mg + MgAl2O4 = MgO + Al, △G(700 °C) =-106.34 kJ/molwhich could not be simulated by the HSC software since the thermodynamic calculation was carried out under an assumption that the reactants were in full contact with each other. However, in a practical process, the AZ91 melt and the cover gas would not be able to be in contact with each other completely, due to the existence of the protective surface film.

Stage 3: The formation of Sulphide and nitride. After a holding time of 30 min, the gas-phase fluorides and oxides in the oxidation cell had become depleted, allowing the melt reaction with the residual gas, forming an additional sulphur-enriched layer upon the initial F-enriched or (F, O)-enriched surface film, thus resulting in the observed multi-layered structure shown in Fig. 10 (b and c). Besides, nitrogen reacted with the AZ91 melt until all reactions were completed. The oxide film shown in Fig. 6 may correspond to this reaction stage due to its nitride content. However, the results shows that the nitrides were not detected in the polished samples shown in Figs. 4 and 5, but only found on the test bar fracture surfaces. The nitrides may have hydrolysed during the sample preparation process, as follows [54]:(3)

Mg3N2 + 6H2O =3Mg(OH)2 + 2NH3↑(4)

AlN+ 3H2O =Al(OH)3 + NH3

In addition, Schmidt et al. [61] found that Mg3N2 and AlN could react to form ternary nitrides (Mg3AlnNn+2, n= 1, 2, 3…). HSC software did not contain the database of ternary nitrides, and it could not be added into the calculation. The oxide films in this stage may also contain ternary nitrides.

4.2. Evolution of entrainment defects formed in SF6/CO2

Fig. 13 shows the results of the thermodynamic calculation between AZ91 alloy and 0.5%SF6/CO2. This reaction processes can also be divided into three stages.

Fig. 13. An equilibrium diagram for the reaction between 7e-7 kg 0.5%SF6/CO2 and a sufficient amount of AZ91 alloy. The X axis denotes the amount of Mg alloy melt having reacted with the entrained gas, and the vertical Y-axis denotes the amounts of the reactants and products.

Stage 1: The formation of fluorides. SF6 and its decomposition products were consumed by the AZ91 melt, forming MgF2, AlF3, and ZnF2. As in the reaction of AZ91 in 0.5%SF6/air, the amount of ZnF2 was too small to be detected practically (1.51 × 10−13 kmol of ZnF2 compared with 2.67 × 10−10 kmol of MgF2). Sulphur accumulated in the residual trapped gas as S2(g) and a portion of the S2(g) reacted with CO2, to form SO2 and CO. The products in this reaction stage were consistent with the film shown in Fig. 11(a), which had a single layer structure that contained fluorides only.

Stage 2: The formation of oxides. AlF3 and ZnF2 reacted with the Mg in the AZ91 melt, forming MgF2, Al and Zn. The SO2 began to be consumed, producing oxides in the surface film and S2(g) in the cover gas. Meanwhile, the CO2 directly reacted with the AZ91 melt, forming CO, MgO, ZnO, and Al2O3. The oxide films shown in Figs. 9 and 11(b) may correspond to this reaction stage due to their oxygen-enriched layer and multi-layered structure.

The CO in the cover gas could further react with the AZ91 melt, producing C. This carbon may further react with Mg to form Mg carbides, when the temperature reduced (during solidification period) [62]. This may be the reason for the high carbon content in the oxide film shown in Figs. 89. Liang et al. [39] also reported carbon-detection in an AZ91 alloy surface film protected by SO2/CO2. The produced Al2O3 may be further combined with MgO, forming MgAl2O4 [63]. As discussed in Section 4.1, the alumina and spinel can react with Mg, causing an absence of aluminium in the surface films, as shown in Fig. 11.

Stage 3: The formation of Sulphide. the AZ91 melt began to consume S2(g) in the residual entrapped gas, forming ZnS and MgS. These reactions did not occur until the last stage of the reaction process, which could be the reason why the S-content in the defect shown Fig. 7(c) was small.

In summary, thermodynamic calculations indicate that the AZ91 melt will react with the cover gas to form fluorides firstly, then oxides and sulphides in the last. The oxide film in the different reaction stages would have different structures and compositions.

4.3. Effect of the carrier gases on consumption of the entrained gas and the reproducibility of AZ91 castings

The evolution processes of entrainment defects, formed in SF6/air and SF6/CO2, have been suggested in Sections 4.1 and 4.2. The theoretical calculations were verified with respect to the corresponding oxide films found in practical samples. The atmosphere within an entrainment defect could be efficiently consumed due to the reaction with liquid Mg-alloy, in a scenario dissimilar to the Al-alloy system (i.e., nitrogen in an entrained air bubble would not efficiently react with Al-alloy melt [64,65], however, nitrogen would be more readily consumed in liquid Mg alloys, commonly referred to as “nitrogen burning” [66]).

The reaction between the entrained gas and the surrounding liquid Mg-alloy converted the entrained gas into solid compounds (e.g. MgO) within the oxide film, thus reducing the void volume of the entrainment defect and hence probably causing a collapse of the defect (e.g., if an entrained gas of air was depleted by the surrounding liquid Mg-alloy, under an assumption that the melt temperature is 700 °C and the depth of liquid Mg-alloy is 10 cm, the total volume of the final solid products would be 0.044% of the initial volume taken by the entrapped air).

The relationship between the void volume reduction of entrainment defects and the corresponding casting properties has been widely studied in Al-alloy castings. Nyahumwa and Campbell [16] reported that the Hot Isostatic Pressing (HIP) process caused the entrainment defects in Al-alloy castings to collapse and their oxide surfaces forced into contact. The fatigue lives of their castings were improved after HIP. Nyahumwa and Campbell [16] also suggested a potential bonding of the double oxide films that were in contact with each other, but there was no direct evidence to support this. This binding phenomenon was further investigated by Aryafar et.al.[8], who re-melted two Al-alloy bars with oxide skins in a steel tube and then carried out a tensile strength test on the solidified sample. They found that the oxide skins of the Al-alloy bars strongly bonded with each other and became even stronger with an extension of the melt holding time, indicating a potential “healing” phenomenon due to the consumption of the entrained gas within the double oxide film structure. In addition, Raidszadeh and Griffiths [9,19] successfully reduced the negative effect of entrainment defects on the reproducibility of Al-alloy castings, by extending the melt holding time before solidification, which allowed the entrained gas to have a longer time to react with the surrounding melt.

With consideration of the previous work mentioned, the consumption of the entrained gas in Mg-alloy castings may diminish the negative effect of entrainment defects in the following two ways.

(1) Bonding phenomenon of the double oxide films. The sandwich-like structure shown in Fig. 5 and 7 indicated a potential bonding of the double oxide film structure. However, more evidence is required to quantify the increase in strength due to the bonding of the oxide films.

(2) Void volume reduction of entrainment defects. The positive effect of void-volume reduction on the quality of castings has been widely demonstrated by the HIP process [67]. As the evolution processes discussed in Section 4.14.2, the oxide films of entrainment defects can grow together due to an ongoing reaction between the entrained gas and surrounding AZ91 alloy melt. The volume of the final solid products was significant small compared with the entrained gas (i.e., 0.044% as previously mentioned).

Therefore, the consumption rate of the entrained gas (i.e., the growth rate of oxide films) may be a critical parameter for improving the quality of AZ91 alloy castings. The oxide film growth rate in the oxidization cell was accordingly further investigated.

Fig. 14 shows a comparison of the surface film growth rates in different cover gases (i.e., 0.5%SF6/air and 0.5%SF6/CO2). 15 random points on each sample were selected for film thickness measurements. The 95% confidence interval (95%CI) was computed under an assumption that the variation of the film thickness followed a Gaussian distribution. It can be seen that all the surface films formed in 0.5%SF6/air grew faster than those formed in 0.5%SF6/CO2. The different growth rates suggested that the entrained-gas consumption rate of 0.5%SF6/air was higher than that of 0.5%SF6/CO2, which was more beneficial for the consumption of the entrained gas.

Fig. 14. A comparison of the AZ91 alloy oxide film growth rates in 0.5%SF6/air and 0.5%SF6/CO2

It should be noted that, in the oxidation cell, the contact area of liquid AZ91 alloy and cover gas (i.e. the size of the crucible) was relatively small with consideration of the large volume of melt and gas. Consequently, the holding time for the oxide film growth within the oxidation cell was comparatively long (i.e., 5–30 min). However, the entrainment defects contained in a real casting are comparatively very small (i.e., a few microns size as shown in Figs. 36, and [7]), and the entrained gas is fully enclosed by the surrounding melt, creating a relatively large contact area. Hence the reaction time for cover gas and the AZ91 alloy melt may be comparatively short. In addition, the solidification time of real Mg-alloy sand castings can be a few minutes (e.g. Guo [68] reported that a Mg-alloy sand casting with 60 mm diameter required 4 min to be solidified). Therefore, it can be expected that an entrained gas trapped during an Mg-alloy melt pouring process will be readily consumed by the surrounding melt, especially for sand castings and large-size castings, where solidification times are long.

Therefore, the different cover gases (0.5%SF6/air and 0.5%SF6/CO2) associated with different consumption rates of the entrained gases may affect the reproducibility of the final castings. To verify this assumption, the AZ91 castings produced in 0.5%SF6/air and 0.5%SF6/CO2 were machined into test bars for mechanical evaluation. A Weibull analysis was carried out using both linear least square (LLS) method and non-linear least square (non-LLS) method [69].

Fig. 15(a-b) shows a traditional 2-p linearized Weibull plot of the UTS and elongation of the AZ91 alloy castings, obtained by the LLS method. The estimator used is P= (i-0.5)/N, which was suggested to cause the lowest bias among all the popular estimators [69,70]. The casting produced in SF6/air has an UTS Weibull moduli of 16.9, and an elongation Weibull moduli of 5.0. In contrast, the UTS and elongation Weibull modulus of the casting produced in SF6/CO2 are 7.7 and 2.7 respectively, suggesting that the reproducibility of the casting protected by SF6/CO2 were much lower than that produced in SF6/air.

Fig. 15. The Weibull modulus of AZ91 castings produced in different atmospheres, estimated by (a-b) the linear least square method, (c-d) the non-linear least square method, where SSR is the sum of residual squares.

In addition, the author’s previous publication [69] demonstrated a shortcoming of the linearized Weibull plots, which may cause a higher bias and incorrect R2 interruption of the Weibull estimation. A Non-LLS Weibull estimation was therefore carried out, as shown in Fig. 15 (c-d). The UTS Weibull modulus of the SF6/air casting was 20.8, while the casting produced under SF6/CO2 had a lower UTS Weibull modulus of 11.4, showing a clear difference in their reproducibility. In addition, the SF6/air elongation (El%) dataset also had a Weibull modulus (shape = 5.8) higher than the elongation dataset of SF6/CO2 (shape = 3.1). Therefore, both the LLS and Non-LLS estimations suggested that the SF6/air casting has a higher reproducibility than the SF6/CO2 casting. It supports the method that the use of air instead of CO2 contributes to a quicker consumption of the entrained gas, which may reduce the void volume within the defects. Therefore, the use of 0.5%SF6/air instead of 0.5%SF6/CO2 (which increased the consumption rate of the entrained gas) improved the reproducibility of the AZ91 castings.

However, it should be noted that not all the Mg-alloy foundries followed the casting process used in present work. The Mg-alloy melt in present work was degassed, thus reducing the effect of hydrogen on the consumption of the entrained gas (i.e., hydrogen could diffuse into the entrained gas, potentially suppressing the depletion of the entrained gas [7,71,72]). In contrast, in Mg-alloy foundries, the Mg-alloy melt is not normally degassed, since it was widely believed that there is not a ‘gas problem’ when casting magnesium and hence no significant change in tensile properties [73]. Although studies have shown the negative effect of hydrogen on the mechanical properties of Mg-alloy castings [41,42,73], a degassing process is still not very popular in Mg-alloy foundries.

Moreover, in present work, the sand mould cavity was flushed with the SF6 cover gas prior to pouring [22]. However, not all the Mg-alloy foundries flushed the mould cavity in this way. For example, the Stone Foundry Ltd (UK) used sulphur powder instead of the cover-gas flushing. The entrained gas within their castings may be SO2/air, rather than the protective gas.

Therefore, although the results in present work have shown that using air instead of CO2 improved the reproducibility of the final casting, it still requires further investigations to confirm the effect of carrier gases with respect to different industrial Mg-alloy casting processes.

7. Conclusion

Entrainment defects formed in an AZ91 alloy were observed. Their oxide films had two types of structure: single-layered and multi-layered. The multi-layered oxide film can grow together forming a sandwich-like structure in the final casting.2.

Both the experimental results and the theoretical thermodynamic calculations demonstrated that fluorides in the trapped gas were depleted prior to the consumption of sulphur. A three-stage evolution process of the double oxide film defects has been suggested. The oxide films contained different combinations of compounds, depending on the evolution stage. The defects formed in SF6/air had a similar structure to those formed in SF6/CO2, but the compositions of their oxide films were different. The oxide-film formation and evolution process of the entrainment defects were different from that of the Mg-alloy surface films previous reported (i.e., MgO formed prior to MgF2).3.

The growth rate of the oxide film was demonstrated to be greater under SF6/air than SF6/CO2, contributing to a quicker consumption of the damaging entrapped gas. The reproducibility of an AZ91 alloy casting improved when using SF6/air instead of SF6/CO2.

Acknowledgements

The authors acknowledge funding from the EPSRC LiME grant EP/H026177/1, and the help from Dr W.D. Griffiths and Mr. Adrian Carden (University of Birmingham). The casting work was carried out in University of Birmingham.

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Fig. 1. Schematic of lap welding for 6061/5182 aluminum alloys.

알루미늄 합금 겹침 용접 중 용접 형성, 용융 흐름 및 입자 구조에 대한 사인파 발진 레이저 빔의 영향

린 첸 가오 양 미시 옹 장 춘밍 왕
Lin Chen , Gaoyang Mi , Xiong Zhang , Chunming Wang *
중국 우한시 화중과학기술대학 재료공학부, 430074

Effects of sinusoidal oscillating laser beam on weld formation, melt flow and grain structure during aluminum alloys lap welding

Abstract

A numerical model of 1.5 mm 6061/5182 aluminum alloys thin sheets lap joints under laser sinusoidal oscillation (sine) welding and laser welding (SLW) weld was developed to simulate temperature distribution and melt flow. Unlike the common energy distribution of SLW, the sinusoidal oscillation of laser beam greatly homogenized the energy distribution and reduced the energy peak. The energy peaks were located at both sides of the sine weld, resulting in the tooth-shaped sectional formation. This paper illustrated the effect of the temperature gradient (G) and solidification rate (R) on the solidification microstructure by simulation. Results indicated that the center of the sine weld had a wider area with low G/R, promoting the formation of a wider equiaxed grain zone, and the columnar grains were slenderer because of greater GR. The porosity-free and non-penetration welds were obtained by the laser sinusoidal oscillation. The reasons were that the molten pool volume was enlarged, the volume proportion of keyhole was reduced and the turbulence in the molten pool was gentled, which was observed by the high-speed imaging and simulation results of melt flow. The tensile test of both welds showed a tensile fracture form along the fusion line, and the tensile strength of sine weld was significantly better than that of the SLW weld. This was because that the wider equiaxed grain area reduced the tendency of cracks and the finer grain size close to the fracture location. Defect-free and excellent welds are of great significance to the new energy vehicles industry.

온도 분포 및 용융 흐름을 시뮬레이션하기 위해 레이저 사인파 진동 (사인) 용접 및 레이저 용접 (SLW) 용접에서 1.5mm 6061/5182 알루미늄 합금 박판 랩 조인트 의 수치 모델이 개발되었습니다. SLW의 일반적인 에너지 분포와 달리 레이저 빔의 사인파 진동은 에너지 분포를 크게 균질화하고 에너지 피크를 줄였습니다. 에너지 피크는 사인 용접의 양쪽에 위치하여 톱니 모양의 단면이 형성되었습니다. 이 논문은 온도 구배(G)와 응고 속도 의 영향을 설명했습니다.(R) 시뮬레이션에 의한 응고 미세 구조. 결과는 사인 용접의 중심이 낮은 G/R로 더 넓은 영역을 가짐으로써 더 넓은 등축 결정립 영역의 형성을 촉진하고 더 큰 GR로 인해 주상 결정립 이 더 가늘다는 것을 나타냅니다. 다공성 및 비관통 용접은 레이저 사인파 진동에 의해 얻어졌습니다. 그 이유는 용융 풀의 부피가 확대되고 열쇠 구멍의 부피 비율이 감소하며 용융 풀의 난류가 완만해졌기 때문이며, 이는 용융 흐름의 고속 이미징 및 시뮬레이션 결과에서 관찰되었습니다. 두 용접부 의 인장시험 은 융착선을 따라 인장파괴형태를인장강도사인 용접의 경우 SLW 용접보다 훨씬 우수했습니다. 이는 등축 결정립 영역이 넓을수록 균열 경향이 감소하고 파단 위치에 근접한 입자 크기가 미세 하기 때문입니다. 결함이 없고 우수한 용접은 신에너지 자동차 산업에 매우 중요합니다.

Fig. 1. Schematic of lap welding for 6061/5182 aluminum alloys.
Fig. 1. Schematic of lap welding for 6061/5182 aluminum alloys.
Fig. 2. Finite element mesh.
Fig. 2. Finite element mesh.
Fig. 3. Weld morphologies of cross-section and upper surface for the two welds: (a) sine pattern weld; (b) SLW weld.
Fig. 3. Weld morphologies of cross-section and upper surface for the two welds: (a) sine pattern weld; (b) SLW weld.
Fig. 4. Calculation of laser energy distribution: (a)-(c) sine pattern weld; (d)-(f) SLW weld.
Fig. 4. Calculation of laser energy distribution: (a)-(c) sine pattern weld; (d)-(f) SLW weld.
Fig. 5. The partially melted region of zone A.
Fig. 5. The partially melted region of zone A.
Fig. 6. The simulated profiles of melted region for the two welds: (a) SLW weld; (b) sine pattern weld.
Fig. 6. The simulated profiles of melted region for the two welds: (a) SLW weld; (b) sine pattern weld.
Fig. 7. The temperature field simulation results of cross section for sine pattern weld.
Fig. 7. The temperature field simulation results of cross section for sine pattern weld.
Fig. 8. Dynamic behavior of the molten pool at the same time interval of 0.004 s within one oscillating period: (a) SLW weld; (b) sine pattern weld.
Fig. 8. Dynamic behavior of the molten pool at the same time interval of 0.004 s within one oscillating period: (a) SLW weld; (b) sine pattern weld.
Fig. 9. The temperature field and flow field of the molten pool for the SLW weld: (a)~(f) t = 80 ms~100 ms.
Fig. 9. The temperature field and flow field of the molten pool for the SLW weld: (a)~(f) t = 80 ms~100 ms.
Fig. 10. The temperature field and flow field of the molten pool for the sine pattern weld: (a)~(f) t = 151 ms~171 ms.
Fig. 10. The temperature field and flow field of the molten pool for the sine pattern weld: (a)~(f) t = 151 ms~171 ms.
Fig. 11. The evolution of the molten pool volume and keyhole depth within one period.
Fig. 11. The evolution of the molten pool volume and keyhole depth within one period.
Fig. 12. The X-ray inspection results for the two welds: (a) SLW weld, (b) sine pattern weld.
Fig. 12. The X-ray inspection results for the two welds: (a) SLW weld, (b) sine pattern weld.
Fig. 13. Comparison of the solidification parameters for sine and SLW patterns: (a) the temperature field simulated results of the molten pool upper surfaces; (b) temperature gradient G and solidification rate R along the molten pool boundary isotherm from weld centerline to the fusion boundary; (c) G/R; (d) GR.
Fig. 13. Comparison of the solidification parameters for sine and SLW patterns: (a) the temperature field simulated results of the molten pool upper surfaces; (b) temperature gradient G and solidification rate R along the molten pool boundary isotherm from weld centerline to the fusion boundary; (c) G/R; (d) GR.
Fig. 14. The EBSD results of equiaxed grain zone in the weld center of: (a) sine pattern weld; (b) SLW weld; (c) grain size.
Fig. 14. The EBSD results of equiaxed grain zone in the weld center of: (a) sine pattern weld; (b) SLW weld; (c) grain size.
Fig. 15. (a) EBSD results of horizontal sections of SLW weld and sine pattern weld; (b) The columnar crystal widths of SLW weld and sine pattern weld.
Fig. 15. (a) EBSD results of horizontal sections of SLW weld and sine pattern weld; (b) The columnar crystal widths of SLW weld and sine pattern weld.
Fig. 16. (a) The tensile test results of the two welds; (b) Fracture location of SLW weld; (b) Fracture location of sine pattern weld.
Fig. 16. (a) The tensile test results of the two welds; (b) Fracture location of SLW weld; (b) Fracture location of sine pattern weld.

Keywords

Laser welding, Sinusoidal oscillating, Energy distribution, Numerical simulation, Molten pool flow, Grain structure

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Fig 3. Front view of the ejected powder particles due to the plume movement. Powder particles are colored by their respective temperature while trajectory colors show their magnitude at 0.007 seconds.

316-L 스테인리스강의 레이저 분말 베드 융합 중 콜드 스패터 형성의 충실도 높은 수치 모델링

316-L 스테인리스강의 레이저 분말 베드 융합 중 콜드 스패터 형성의 충실도 높은 수치 모델링

M. BAYAT1,* , AND J. H. HATTEL1

  • Corresponding author
    1 Technical University of Denmark (DTU), Building 425, Kgs. 2800 Lyngby, Denmark

ABSTRACT

Spatter and denudation are two very well-known phenomena occurring mainly during the laser powder bed fusion process and are defined as ejection and displacement of powder particles, respectively. The main driver of this phenomenon is the formation of a vapor plume jet that is caused by the vaporization of the melt pool which is subjected to the laser beam. In this work, a 3-dimensional transient turbulent computational fluid dynamics model coupled with a discrete element model is developed in the finite volume-based commercial software package Flow-3D AM to simulate the spatter phenomenon. The numerical results show that a localized low-pressure zone forms at the bottom side of the plume jet and this leads to a pseudo-Bernoulli effect that drags nearby powder particles into the area of influence of the vapor plume jet. As a result, the vapor plume acts like a momentum sink and therefore all nearby particles point are dragged towards this region. Furthermore, it is noted that due to the jet’s attenuation, powder particles start diverging from the central core region of the vapor plume as they move vertically upwards. It is moreover observed that only particles which are in the very central core region of the plume jet get sufficiently accelerated to depart the computational domain, while the rest of the dragged particles, especially those which undergo an early divergence from the jet axis, get stalled pretty fast as they come in contact with the resting fluid. In the last part of the work, two simulations with two different scanning speeds are carried out, where it is clearly observed that the angle between the departing powder particles and the vertical axis of the plume jet increases with increasing scanning speed.

스패터와 denudation은 주로 레이저 분말 베드 융합 과정에서 발생하는 매우 잘 알려진 두 가지 현상으로 각각 분말 입자의 배출 및 변위로 정의됩니다.

이 현상의 주요 동인은 레이저 빔을 받는 용융 풀의 기화로 인해 발생하는 증기 기둥 제트의 형성입니다. 이 작업에서 이산 요소 모델과 결합된 3차원 과도 난류 ​​전산 유체 역학 모델은 스패터 현상을 시뮬레이션하기 위해 유한 체적 기반 상용 소프트웨어 패키지 Flow-3D AM에서 개발되었습니다.

수치적 결과는 플룸 제트의 바닥면에 국부적인 저압 영역이 형성되고, 이는 근처의 분말 입자를 증기 플룸 제트의 영향 영역으로 끌어들이는 의사-베르누이 효과로 이어진다는 것을 보여줍니다.

결과적으로 증기 기둥은 운동량 흡수원처럼 작용하므로 근처의 모든 입자 지점이 이 영역으로 끌립니다. 또한 제트의 감쇠로 인해 분말 입자가 수직으로 위쪽으로 이동할 때 증기 기둥의 중심 코어 영역에서 발산하기 시작합니다.

더욱이 플룸 제트의 가장 중심 코어 영역에 있는 입자만 계산 영역을 벗어날 만큼 충분히 가속되는 반면, 드래그된 나머지 입자, 특히 제트 축에서 초기 발산을 겪는 입자는 정체되는 것으로 관찰됩니다. 그들은 휴식 유체와 접촉하기 때문에 꽤 빠릅니다.

작업의 마지막 부분에서 두 가지 다른 스캔 속도를 가진 두 가지 시뮬레이션이 수행되었으며, 여기서 출발하는 분말 입자와 연기 제트의 수직 축 사이의 각도가 스캔 속도가 증가함에 따라 증가하는 것이 명확하게 관찰되었습니다.

Fig 1. Two different views of the computational domain for the fluid domain. The vapor plume is simulated by a moving momentum source with a prescribed temperature of 3000 K.
Fig 1. Two different views of the computational domain for the fluid domain. The vapor plume is simulated by a moving momentum source with a prescribed temperature of 3000 K.
Fig 2. (a) and (b) are two snapshots taken at an x-y plane parallel to the powder layer plane before and 0.008 seconds after the start of the scanning process. (c) Shows a magnified view of (b) where detailed powder particles' movement along with their velocity magnitude and directions are shown.
Fig 2. (a) and (b) are two snapshots taken at an x-y plane parallel to the powder layer plane before and 0.008 seconds after the start of the scanning process. (c) Shows a magnified view of (b) where detailed powder particles’ movement along with their velocity magnitude and directions are shown.
Fig 3. Front view of the ejected powder particles due to the plume movement. Powder particles are colored by their respective temperature while trajectory colors show their magnitude at 0.007 seconds.
Fig 3. Front view of the ejected powder particles due to the plume movement. Powder particles are colored by their respective temperature while trajectory colors show their magnitude at 0.007 seconds.

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Fig. 1. Schematic figure showing the PREP with additional gas flowing on the end face of electrode.

플라즈마 회전 전극 공정 중 분말 형성에 대한 공정 매개변수 및 냉각 가스의 영향

Effects of process parameters and cooling gas on powder formation during the plasma rotating electrode process

Yujie Cuia Yufan Zhaoa1 Haruko Numatab Kenta Yamanakaa Huakang Biana Kenta Aoyagia AkihikoChibaa
aInstitute for Materials Research, Tohoku University, Sendai 980-8577, JapanbDepartment of Materials Processing, Graduate School of Engineering, Tohoku University, Sendai 980-8577, Japan

Highlights

•The limitation of increasing the rotational speed in decreasing powder size was clarified.

•Cooling and disturbance effects varied with the gas flowing rate.

•Inclined angle of the residual electrode end face affected powder formation.

•Additional cooling gas flowing could be applied to control powder size.

Abstract

The plasma rotating electrode process (PREP) is rapidly becoming an important powder fabrication method in additive manufacturing. However, the low production rate of fine PREP powder limits the development of PREP. Herein, we investigated different factors affecting powder formation during PREP by combining experimental methods and numerical simulations. The limitation of increasing the rotation electrode speed in decreasing powder size is attributed to the increased probability of adjacent droplets recombining and the decreased tendency of granulation. The effects of additional Ar/He gas flowing on the rotational electrode on powder formation is determined through the cooling effect, the disturbance effect, and the inclined effect of the residual electrode end face simultaneously. A smaller-sized powder was obtained in the He atmosphere owing to the larger inclined angle of the residual electrode end face compared to the Ar atmosphere. Our research highlights the route for the fabrication of smaller-sized powders using PREP.

플라즈마 회전 전극 공정(PREP)은 적층 제조 에서 중요한 분말 제조 방법으로 빠르게 자리잡고 있습니다. 그러나 미세한 PREP 분말의 낮은 생산율은 PREP의 개발을 제한합니다. 여기에서 우리는 실험 방법과 수치 시뮬레이션을 결합하여 PREP 동안 분말 형성에 영향을 미치는 다양한 요인을 조사했습니다. 분말 크기 감소에서 회전 전극 속도 증가의 한계는 인접한 액적 재결합 확률 증가 및 과립화 경향 감소에 기인합니다.. 회전 전극에 흐르는 추가 Ar/He 가스가 분말 형성에 미치는 영향은 냉각 효과, 외란 효과 및 잔류 전극 단면의 경사 효과를 통해 동시에 결정됩니다. He 분위기에서는 Ar 분위기에 비해 잔류 전극 단면의 경사각이 크기 때문에 더 작은 크기의 분말이 얻어졌다. 우리의 연구는 PREP를 사용하여 더 작은 크기의 분말을 제조하는 경로를 강조합니다.

Keywords

Plasma rotating electrode process

Ti-6Al-4 V alloy, Rotating speed, Numerical simulation, Gas flowing, Powder size

Introduction

With the development of additive manufacturing, there has been a significant increase in high-quality powder production demand [1,2]. The initial powder characteristics are closely related to the uniform powder spreading [3,4], packing density [5], and layer thickness observed during additive manufacturing [6], thus determining the mechanical properties of the additive manufactured parts [7,8]. Gas atomization (GA) [9–11], centrifugal atomization (CA) [12–15], and the plasma rotating electrode process (PREP) are three important powder fabrication methods.

Currently, GA is the dominant powder fabrication method used in additive manufacturing [16] for the fabrication of a wide range of alloys [11]. GA produces powders by impinging a liquid metal stream to droplets through a high-speed gas flow of nitrogen, argon, or helium. With relatively low energy consumption and a high fraction of fine powders, GA has become the most popular powder manufacturing technology for AM.

The entrapped gas pores are generally formed in the powder after solidification during GA, in which the molten metal is impacted by a high-speed atomization gas jet. In addition, satellites are formed in GA powder when fine particles adhere to partially molten particles.

The gas pores of GA powder result in porosity generation in the additive manufactured parts, which in turn deteriorates its mechanical properties because pores can become crack initiation sites [17]. In CA, a molten metal stream is poured directly onto an atomizer disc spinning at a high rotational speed. A thin film is formed on the surface of the disc, which breaks into small droplets due to the centrifugal force. Metal powder is obtained when these droplets solidify.

Compared with GA powder, CA powder exhibits higher sphericity, lower impurity content, fewer satellites, and narrower particle size distribution [12]. However, very high speed is required to obtain fine powder by CA. In PREP, the molten metal, melted using the plasma arc, is ejected from the rotating rod through centrifugal force. Compared with GA powder, PREP-produced powders also have higher sphericity and fewer pores and satellites [18].

For instance, PREP-fabricated Ti6Al-4 V alloy powder with a powder size below 150 μm exhibits lower porosity than gas-atomized powder [19], which decreases the porosity of additive manufactured parts. Furthermore, the process window during electron beam melting was broadened using PREP powder compared to GA powder in Inconel 718 alloy [20] owing to the higher sphericity of the PREP powder.

In summary, PREP powder exhibits many advantages and is highly recommended for powder-based additive manufacturing and direct energy deposition-type additive manufacturing. However, the low production rate of fine PREP powder limits the widespread application of PREP powder in additive manufacturing.

Although increasing the rotating speed is an effective method to decrease the powder size [21,22], the reduction in powder size becomes smaller with the increased rotating speed [23]. The occurrence of limiting effects has not been fully clarified yet.

Moreover, the powder size can be decreased by increasing the rotating electrode diameter [24]. However, these methods are quite demanding for the PREP equipment. For instance, it is costly to revise the PREP equipment to meet the demand of further increasing the rotating speed or electrode diameter.

Accordingly, more feasible methods should be developed to further decrease the PREP powder size. Another factor that influences powder formation is the melting rate [25]. It has been reported that increasing the melting rate decreases the powder size of Inconel 718 alloy [26].

In contrast, the powder size of SUS316 alloy was decreased by decreasing the plasma current within certain ranges. This was ascribed to the formation of larger-sized droplets from fluid strips with increased thickness and spatial density at higher plasma currents [27]. The powder size of NiTi alloy also decreases at lower melting rates [28]. Consequently, altering the melting rate, varied with the plasma current, is expected to regulate the PREP powder size.

Furthermore, gas flowing has a significant influence on powder formation [27,29–31]. On one hand, the disturbance effect of gas flowing promotes fluid granulation, which in turn contributes to the formation of smaller-sized powder [27]. On the other hand, the cooling effect of gas flowing facilitates the formation of large-sized powder due to increased viscosity and surface tension. However, there is a lack of systematic research on the effect of different gas flowing on powder formation during PREP.

Herein, the authors systematically studied the effects of rotating speed, electrode diameter, plasma current, and gas flowing on the formation of Ti-6Al-4 V alloy powder during PREP as additive manufactured Ti-6Al-4 V alloy exhibits great application potential [32]. Numerical simulations were conducted to explain why increasing the rotating speed is not effective in decreasing powder size when the rotation speed reaches a certain level. In addition, the different factors incited by the Ar/He gas flowing on powder formation were clarified.

Fig. 1. Schematic figure showing the PREP with additional gas flowing on the end face of electrode.
Fig. 1. Schematic figure showing the PREP with additional gas flowing on the end face of electrode.

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Gating System Design Based on Numerical Simulation and Production Experiment Verification of Aluminum Alloy Bracket Fabricated by Semi-solid Rheo-Die Casting Process

Gating System Design Based on Numerical Simulation and Production Experiment Verification of Aluminum Alloy Bracket Fabricated by Semi-solid Rheo-Die Casting Process

반고체 레오 다이 캐스팅 공정으로 제작된 알루미늄 합금 브래킷의 수치 시뮬레이션 및 생산 실험 검증을 기반으로 한 게이팅 시스템 설계

International Journal of Metalcasting volume 16, pages878–893 (2022)Cite this article

Abstract

In this study a gating system including sprue, runner and overflows for semi-solid rheocasting of aluminum alloy was designed by means of numerical simulations with a commercial software. The effects of pouring temperature, mold temperature and injection speed on the filling process performance of semi-solid die casting were studied. Based on orthogonal test analysis, the optimal die casting process parameters were selected, which were metal pouring temperature 590 °C, mold temperature 260 °C and injection velocity 0.5 m/s. Semi-solid slurry preparation process of Swirled Enthalpy Equilibration Device (SEED) was used for die casting production experiment. Aluminum alloy semi-solid bracket components were successfully produced with the key die casting process parameters selected, which was consistent with the simulation result. The design of semi-solid gating system was further verified by observing and analyzing the microstructure of different zones of the casting. The characteristic parameters, particle size and shape factor of microstructure of the produced semi-solid casting showed that the semi-solid aluminum alloy components are of good quality.

이 연구에서 알루미늄 합금의 반고체 레오캐스팅을 위한 스프루, 러너 및 오버플로를 포함하는 게이팅 시스템은 상용 소프트웨어를 사용한 수치 시뮬레이션을 통해 설계되었습니다. 주입 온도, 금형 온도 및 사출 속도가 반고체 다이캐스팅의 충전 공정 성능에 미치는 영향을 연구했습니다. 직교 테스트 분석을 기반으로 금속 주입 온도 590°C, 금형 온도 260°C 및 사출 속도 0.5m/s인 최적의 다이 캐스팅 공정 매개변수가 선택되었습니다. Swirled Enthalpy Equilibration Device(SEED)의 반고체 슬러리 제조 공정을 다이캐스팅 생산 실험에 사용하였다. 알루미늄 합금 반고체 브래킷 구성 요소는 시뮬레이션 결과와 일치하는 주요 다이 캐스팅 공정 매개변수를 선택하여 성공적으로 생산되었습니다. 반고체 게이팅 시스템의 설계는 주조의 다른 영역의 미세 구조를 관찰하고 분석하여 추가로 검증되었습니다. 생산된 반고체 주조물의 특성 매개변수, 입자 크기 및 미세 구조의 형상 계수는 반고체 알루미늄 합금 부품의 품질이 양호함을 보여주었습니다.

Gating System Design Based on Numerical Simulation and Production Experiment Verification of Aluminum Alloy Bracket Fabricated by Semi-solid Rheo-Die Casting Process
Gating System Design Based on Numerical Simulation and Production Experiment Verification of Aluminum Alloy Bracket Fabricated by Semi-solid Rheo-Die Casting Process

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Keywords

  • semi-solid rheo-die casting
  • gating system
  • process parameters
  • numerical simulation
  • microstructure
Fig. 1. Modified Timelli mold design.

Characterization of properties of Vanadium, Boron and Strontium addition on HPDC of A360 alloy

A360 합금의 HPDC에 대한 바나듐, 붕소 및 스트론튬 첨가 특성 특성

OzenGursoya
MuratColakb
KazimTurc
DeryaDispinarde

aUniversity of Padova, Department of Management and Engineering, Vicenza, Italy
bUniversity of Bayburt, Mechanical Engineering, Bayburt, Turkey
cAtilim University, Metallurgical and Materials Engineering, Ankara, Turkey
dIstanbul Technical University, Metallurgical and Materials Engineering, Istanbul, Turkey
eCenter for Critical and Functional Materials, ITU, Istanbul, Turkey

ABSTRACT

The demand for lighter weight decreased thickness and higher strength has become the focal point in the
automotive industry. In order to meet such requirements, the addition of several alloying elements has been started to be investigated. In this work, the additions of V, B, and Sr on feedability and tensile properties of A360 has been studied. A mold design that consisted of test bars has been produced. Initially, a simulation was carried out to optimize the runners, filling, and solidification parameters. Following the tests, it was found that V addition revealed the highest UTS but low elongation at fracture, while B addition exhibited visa verse. On the other hand, impact energy was higher with B additions.

더 가벼운 무게의 감소된 두께와 더 높은 강도에 대한 요구는 자동차 산업의 초점이 되었습니다. 이러한 요구 사항을 충족하기 위해 여러 합금 원소의 추가가 조사되기 시작했습니다. 이 연구에서는 A360의 이송성 및 인장 특성에 대한 V, B 및 Sr의 첨가가 연구되었습니다. 시험봉으로 구성된 금형 설계가 제작되었습니다. 처음에는 러너, 충전 및 응고 매개변수를 최적화하기 위해 시뮬레이션이 수행되었습니다. 시험 결과, V 첨가는 UTS가 가장 높지만 파단 연신율은 낮았고, B 첨가는 visa verse를 나타냈다. 반면에 충격 에너지는 B 첨가에서 더 높았다.

Fig. 1. Modified Timelli mold design.
Fig. 1. Modified Timelli mold design.
Fig. 2. Microstructural images (a) unmodified alloy, (b) Sr modified, (c) V added, (d) B added.
Fig. 2. Microstructural images (a) unmodified alloy, (b) Sr modified, (c) V added, (d) B added.
Fig. 3. Effect of Sr and V addition on the tensile properties of A360
Fig. 3. Effect of Sr and V addition on the tensile properties of A360
Fig. 4. Effect of Sr and B addition on the tensile properties of A360.
Fig. 4. Effect of Sr and B addition on the tensile properties of A360.
Fig. 5. Bubbles chart of tensile properties values obtained from Weibull statistics. | Fig. 6. Effect of Sr, V and B addition on the impact properties of A360.
Fig. 5. Bubbles chart of tensile properties values obtained from Weibull statistics.
Fig. 6. Effect of Sr, V and B addition on the impact properties of A360.
Fig. 7. SEM images on the fracture surfaces (a) V added, (b) B added.
Fig. 7. SEM images on the fracture surfaces (a) V added, (b) B added.

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Figure 3: 3D temperature contours and 2D melt pool cross-sections where the melt pool is stabilized at x=500 µm from the start of the laser initial location for cases where (a) absorptivity = 0.1, Recoil pressure coefficient B = 1 and laser beam radius = 12 µm, (b) absorptivity = 0.1, Recoil pressure coefficient B = 20 and laser beam radius = 12 µm, (c) absorptivity = 0.1, Recoil pressure coefficient B = 1 and laser beam radius = 18 µm, (d) absorptivity = 0.45, Recoil pressure coefficient B = 1 and laser beam radius = 18 µm, (e) absorptivity = 0.45, Recoil pressure coefficient B = 20 and laser beam radius = 12 µm, (f) absorptivity = 0.45, Recoil pressure coefficient B = 20 and laser beam radius = 18 µm.

MULTI-PHYSICS NUMERICAL MODELLING OF 316L AUSTENITIC STAINLESS STEEL IN LASER POWDER BED FUSION PROCESS AT MESO-SCALE

W.E. Alphonso1, M.Bayat1,*, M. Baier 2, S. Carmignato2, J.H. Hattel1
1Department of Mechanical Engineering, Technical University of Denmark (DTU), Lyngby, Denmark
2Department of Management and Engineering – University of Padova, Padova, Italy

ABSTRACT

L-PBF(Laser Powder Bed Fusion)는 레이저 열원을 사용하여 선택적으로 통합되는 분말 층으로 복잡한 3D 금속 부품을 만드는 금속 적층 제조(MAM) 기술입니다. 처리 영역은 수십 마이크로미터 정도이므로 L-PBF를 다중 규모 제조 공정으로 만듭니다.

기체 기공의 형성 및 성장 및 용융되지 않은 분말 영역의 생성은 다중물리 모델에 의해 예측할 수 있습니다. 또한 이러한 모델을 사용하여 용융 풀 모양 및 크기, 온도 분포, 용융 풀 유체 흐름 및 입자 크기 및 형태와 같은 미세 구조 특성을 계산할 수 있습니다.

이 작업에서는 용융, 응고, 유체 흐름, 표면 장력, 열 모세관, 증발 및 광선 추적을 통한 다중 반사를 포함하는 스테인리스 스틸 316-L에 대한 충실도 다중 물리학 중간 규모 수치 모델이 개발되었습니다. 완전한 실험 설계(DoE) 방법을 사용하는 통계 연구가 수행되었으며, 여기서 불확실한 재료 특성 및 공정 매개변수, 즉 흡수율, 반동 압력(기화) 및 레이저 빔 크기가 용융수지 모양 및 크기에 미치는 영향을 분석했습니다.

또한 용융 풀 역학에 대한 위에서 언급한 불확실한 입력 매개변수의 중요성을 강조하기 위해 흡수율이 가장 큰 영향을 미치고 레이저 빔 크기가 그 뒤를 잇는 주요 효과 플롯이 생성되었습니다. 용융 풀 크기에 대한 반동 압력의 중요성은 흡수율에 따라 달라지는 용융 풀 부피와 함께 증가합니다.

모델의 예측 정확도는 유사한 공정 매개변수로 생성된 단일 트랙 실험과 시뮬레이션의 용융 풀 모양 및 크기를 비교하여 검증됩니다.

더욱이, 열 렌즈 효과는 레이저 빔 크기를 증가시켜 수치 모델에서 고려되었으며 나중에 결과적인 용융 풀 프로파일은 모델의 견고성을 보여주기 위한 실험과 비교되었습니다.

Laser Powder Bed Fusion (L-PBF) is a Metal Additive Manufacturing (MAM) technology where a complex 3D metal part is built from powder layers, which are selectively consolidated using a laser heat source. The processing zone is in the order of a few tenths of micrometer, making L-PBF a multi-scale manufacturing process. The formation and growth of gas pores and the creation of un-melted powder zones can be predicted by multiphysics models. Also, with these models, the melt pool shape and size, temperature distribution, melt pool fluid flow and its microstructural features like grain size and morphology can be calculated. In this work, a high fidelity multi-physics meso-scale numerical model is developed for stainless steel 316-L which includes melting, solidification, fluid flow, surface tension, thermo-capillarity, evaporation and multiple reflection with ray-tracing. A statistical study using a full Design of Experiments (DoE) method was conducted, wherein the impact of uncertain material properties and process parameters namely absorptivity, recoil pressure (vaporization) and laser beam size on the melt pool shape and size was analysed. Furthermore, to emphasize on the significance of the above mentioned uncertain input parameters on the melt pool dynamics, a main effects plot was created which showed that absorptivity had the highest impact followed by laser beam size. The significance of recoil pressure on the melt pool size increases with melt pool volume which is dependent on absorptivity. The prediction accuracy of the model is validated by comparing the melt pool shape and size from the simulation with single track experiments that were produced with similar process parameters. Moreover, the effect of thermal lensing was considered in the numerical model by increasing the laser beam size and later on the resultant melt pool profile was compared with experiments to show the robustness of the model.

Figure 1: a) Computational domain for single track L-PBF which includes a 200 μm thick substrate and 45 μm powder layer thickness b) 3D temperature contour plot after scanning a single track with melt pool contours at two locations along the scanning direction where the green region indicates the melted regions.
Figure 1: a) Computational domain for single track L-PBF which includes a 200 μm thick substrate and 45 μm powder layer thickness b) 3D temperature contour plot after scanning a single track with melt pool contours at two locations along the scanning direction where the green region indicates the melted regions.
Figure 2: Main effects plot of uncertain parameters: absorptivity, recoil pressure coefficient and laser beam radius on the melt pool dimensions (width and depth)
Figure 2: Main effects plot of uncertain parameters: absorptivity, recoil pressure coefficient and laser beam radius on the melt pool dimensions (width and depth)
Figure 3: 3D temperature contours and 2D melt pool cross-sections where the melt pool is stabilized at x=500 µm from the start of the laser initial location for cases where (a) absorptivity = 0.1, Recoil pressure coefficient B = 1 and laser beam radius = 12 µm, (b) absorptivity = 0.1, Recoil pressure coefficient B = 20 and laser beam radius = 12 µm, (c) absorptivity = 0.1, Recoil pressure coefficient B = 1 and laser beam radius = 18 µm, (d) absorptivity = 0.45, Recoil pressure coefficient B = 1 and laser beam radius = 18 µm, (e) absorptivity = 0.45, Recoil pressure coefficient B = 20 and laser beam radius = 12 µm, (f) absorptivity = 0.45, Recoil pressure coefficient B = 20 and laser beam radius = 18 µm.
Figure 3: 3D temperature contours and 2D melt pool cross-sections where the melt pool is stabilized at x=500 µm from the start of the laser initial location for cases where (a) absorptivity = 0.1, Recoil pressure coefficient B = 1 and laser beam radius = 12 µm, (b) absorptivity = 0.1, Recoil pressure coefficient B = 20 and laser beam radius = 12 µm, (c) absorptivity = 0.1, Recoil pressure coefficient B = 1 and laser beam radius = 18 µm, (d) absorptivity = 0.45, Recoil pressure coefficient B = 1 and laser beam radius = 18 µm, (e) absorptivity = 0.45, Recoil pressure coefficient B = 20 and laser beam radius = 12 µm, (f) absorptivity = 0.45, Recoil pressure coefficient B = 20 and laser beam radius = 18 µm.
Figure 4: Validation of Numerical model with Recoil pressure coefficient B= 20, absorptivity = 0.45 and a) laser beam radius = 15 µm b) laser beam radius = 20 µm
Figure 4: Validation of Numerical model with Recoil pressure coefficient B= 20, absorptivity = 0.45 and a) laser beam radius = 15 µm b) laser beam radius = 20 µm

CONCLUSION

In this work, a high-fidelity multi-physics numerical model was developed for L-PBF using the FVM method in Flow-3D. The impact of uncertainty in the input parameters including absorptivity, recoil pressure and laser beam size on the melt pool is addressed using a DoE method. The DoE analysis shows that absorptivity has the highest impact on the melt pool. The recoil pressure and laser beam size only become significant once absorptivity is 0.45. Furthermore, the numerical model is validated by comparing the predicted melt pool shape and size with experiments conducted with similar process parameters wherein a high prediction accuracy is achieved by the model. In addition, the impact of thermal lensing on the melt pool dimensions by increasing the laser beam spot size is considered in the validated numerical model and the resultant melt pool is compared with experiments.

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Figure 2: Temperature contours and melt pool border lines at different times for the 50 % duty cycle case: (a) - (c) Δtcycle = 400 μs, (d) – (f) Δtcycle = 1000 μs and (g) – (i) Δtcycle = 3000 μs.

MULTIPHYSICS SIMULATION OF THEMRAL AND FLUID DYNAMICS PHENOMENA DURING THE PULSED LASER POWDER BED FUSION PROCESS OF 316-L STEEL

M. Bayat* , V. K. Nadimpalli, J. H. Hattel
1Department of Mechanical Engineering, Technical University of Denmark (DTU), Produktionstorvet
425, Kgs. 2800, Lyngby, Denmark

ABSTRACT

L-PBF(Laser Powder Bed Fusion)는 다양한 산업 분야에서 많은 관심을 받았으며, 주로 기존 제조 기술을 사용하여 만들 수 없었던 복잡한 토폴로지 최적화 구성 요소를 구현하는 잘 알려진 능력 덕분입니다. . 펄스 L-PBF(PL-PBF)에서 레이저의 시간적 프로파일은 주기 지속 시간과 듀티 주기 중 하나 또는 둘 다를 수정하여 변조할 수 있습니다. 따라서 레이저의 시간적 프로파일은 향후 적용을 위해 이 프로세스를 더 잘 제어할 수 있는 길을 열어주는 새로운 프로세스 매개변수로 간주될 수 있습니다. 따라서 이 작업에서 우리는 레이저의 시간적 프로파일을 변경하는 것이 PL-PBF 공정에서 용융 풀 조건과 트랙의 최종 모양 및 형상에 어떻게 영향을 미칠 수 있는지 조사하는 것을 목표로 합니다. 이와 관련하여 본 논문에서는 CFD(Computational Fluid Dynamics) 소프트웨어 패키지인 Flow-3D를 기반으로 하는 316-L 스테인리스강 PL-PBF 공정의 다중물리 수치 모델을 개발하고 이 모델을 사용하여 열과 유체를 시뮬레이션합니다. 다양한 펄스 모드에서 공정 과정 중 용융 풀 내부에서 발생하는 유동 조건. 따라서 고정된 레이저 듀티 사이클(50%)이 있는 레이저 주기 지속 시간이 용융 풀의 모양과 크기 및 최종 트랙 형태에 미치는 영향을 연구하기 위해 매개변수 연구가 수행됩니다. 더 긴 주기 기간에서 더 많은 재료가 더 큰 용융 풀 내에서 변위됨에 따라 용융 풀의 후류에 더 눈에 띄는 혹이 형성되며, 동시에 더 심각한 반동 압력을 받습니다. 또한 시뮬레이션에서 50% 듀티 사이클에서 1000μs에서 형성된 보다 대칭적인 용융 풀과 비교하여 400μs 사이클 주기에서 더 긴 용융 풀이 형성된다는 것이 관찰되었습니다. 풀 볼륨은 1000μs의 경우 더 큽니다. 매개변수 연구는 연속 트랙과 파손된 트랙 PL-PBF 사이의 경계를 설명하며, 여기서 연속 트랙은 항상 소량의 용융 재료를 유지함으로써 유지됩니다.

English Abstract

Laser Powder Bed Fusion (L-PBF) has attracted a lot of attention from various industrial sectors and mainly thanks to its well-proven well-known capacity of realizing complex topology-optimized components that have so far been impossible to make using conventional manufacturing techniques. In Pulsed L-PBF (PL-PBF), the laser’s temporal profile can be modulated via modifying either or both the cycle duration and the duty cycle. Thus, the laser’s temporal profile could be considered as a new process parameter that paves the way for a better control of this process for future applications. Therefore, in this work we aim to investigate how changing the laser’s temporal profile can affect the melt pool conditions and the final shape and geometry of a track in the PL-PBF process. In this respect, in this paper a multiphysics numerical model of the PL-PBF process of 316-L stainless steel is developed based on the computational fluid dynamics (CFD) software package Flow-3D and the model is used to simulate the heat and fluid flow conditions occurring inside the melt pool during the course of the process at different pulsing modes. Thus, a parametric study is carried out to study the influence of the laser’s cycle duration with a fixed laser duty cycle (50 %) on the shape and size of the melt pool and the final track morphology. It is noticed that at longer cycle periods, more noticeable humps form at the wake of the melt pool as more material is displaced within bigger melt pools, which are at the same time subjected to more significant recoil pressures. It is also observed in the simulations that at 50 % duty cycle, longer melt pools form at 400 μs cycle period compared to the more symmetrical melt pools formed at 1000 μs, primarily because of shorter laser off-times in the former, even though melt pool volume is bigger for the 1000 μs case. The parameteric study illustrates the boundary between a continuous track and a broken track PL-PBF wherein the continuous track is retained by always maintaining a small volume of molten material.

Figure 1: Front and side views of the computational domain. Note that the region along z and from -100 μm to +50 μm is void.
Figure 1: Front and side views of the computational domain. Note that the region along z and from -100 μm to +50 μm is void.
Figure 2: Temperature contours and melt pool border lines at different times for the 50 % duty cycle case: (a) - (c) Δtcycle = 400 μs, (d) – (f) Δtcycle = 1000 μs and (g) – (i) Δtcycle = 3000 μs.
Figure 2: Temperature contours and melt pool border lines at different times for the 50 % duty cycle case: (a) – (c) Δtcycle = 400 μs, (d) – (f) Δtcycle = 1000 μs and (g) – (i) Δtcycle = 3000 μs.
Figure 3: Plot of melt pool volume versus time for four cases including continuous wave laser as well as 50 % duty cycle at 400 μs, 1000 μs and 3000 μs.
Figure 3: Plot of melt pool volume versus time for four cases including continuous wave laser as well as 50 % duty cycle at 400 μs, 1000 μs and 3000 μs.

CONCLUSIONS

In this work a CFD model of the modulated PL-PBF process of stainless steel 316-L is developed in the commercial software package Flow-3D. The model involves physics such as solidification, melting, evaporation, convection, laser-material interaction, capillarity, Marangoni effect and the recoil pressure effect. In the current study, a parametric study is carried out to understand how the change in the cycle period duration affects the melt pool’s thermo-fluid conditions during the modulated PL-PBF process. It is observed that at the pulse mode with 50 % duty cycle and 400 μs cycle period, an overlapped chain of humps form at the wake of the melt pool and at a spatial frequency of occurrence of about 78 μm. Furthermore and as expected, it is noted that the melt pool volume, the size of the hump as well as the crater size at the end of the track, increase with increase in the cycle period duration, as more material is re-deposited at the back of the melt pool and that itself is caused by more pronounced recoil pressures. Moreover, it is noticed that due to the short off-time period of the laser in the 400 μs cycle period case, there is always an amount of liquid metal left from the previous cycle, at the time the new cycle starts. This is found to be the main reason why longer and elongated melt pools form at 400 μs cycle period, compared to the bigger, shorter and more symmetrical-like melt pools forming at the 1000 μs case. In this study PL-PBF single tracks including the broken track and the continuous track examples were studied to illustrate the boundary of this transition at a given laser scan parameter setting. At higher scan speeds, it is expected that the Plateau–Rayleigh instability will compete with the pulsing behavior to change the transition boundary between a broken and continuous track, which is suggested as future work from this study.

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Fluid Thermodynamic Simulation of Ti-6Al-4V Alloy in Laser Wire Deposition

Fluid Thermodynamic Simulation of Ti-6Al-4V Alloy in Laser Wire Deposition

Xiang WangLin-Jie ZhangJie Ning, and Suck-Joo Na
Published Online:8 Apr 2022https://doi.org/10.1089/3dp.2021.0159

Abstract

A 3D numerical model of heat transfer and fluid flow of molten pool in the process of laser wire deposition was presented by computational fluid dynamics technique. The simulation results of the deposition morphology were also compared with the experimental results under the condition of liquid bridge transfer mode. Moreover, they showed a good agreement. Considering the effect of recoil pressure, the morphology of the deposit metal obtained by the simulation was similar to the experiment result. Molten metal at the wire tip was peeled off and flowed into the molten pool, and then spread to both sides of the deposition layer under the recoil pressure. In addition, the results of simulation and high-speed charge-coupled device presented that a wedge transition zone, with a length of ∼6 mm, was formed behind the keyhole in the liquid bridge transfer process, where the height of deposited metal decreased gradually. After solidification, metal in the transition zone retained the original melt morphology, resulting in a decrease in the height of the tail of the deposition layer.

Keywords

LWD, CFD, liquid bridge transfer, fluid dynamics, wedge transition zone

Fluid Thermodynamic Simulation of Ti-6Al-4V Alloy in Laser Wire Deposition
Fluid Thermodynamic Simulation of Ti-6Al-4V Alloy in Laser Wire Deposition
Fluid Thermodynamic Simulation of Ti-6Al-4V Alloy in Laser Wire Deposition
Fluid Thermodynamic Simulation of Ti-6Al-4V Alloy in Laser Wire Deposition

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Figure 3.10: Snapshots of Temperature Profile for Single Track in Keyhole Regime (P = 250W and V = 0.5m/s) at the Preheating Temperature of 100 °C

Multiscale Process Modeling of Residual Deformation and Defect Formation for Laser Powder Bed Fusion Additive Manufacturing

Qian Chen, PhD
University of Pittsburgh, 2021

레이저 분말 베드 퓨전(L-PBF) 적층 제조(AM)는 우수한 기계적 특성으로 그물 모양에 가까운 복잡한 부품을 생산할 수 있습니다. 그러나 빌드 실패 및 다공성과 같은 결함으로 이어지는 원치 않는 잔류 응력 및 왜곡이 L-PBF의 광범위한 적용을 방해하고 있습니다.

L-PBF의 잠재력을 최대한 실현하기 위해 잔류 변형, 용융 풀 및 다공성 형성을 예측하는 다중 규모 모델링 방법론이 개발되었습니다. L-PBF의 잔류 변형 및 응력을 부품 규모에서 예측하기 위해 고유 변형 ​​방법을 기반으로 하는 다중 규모 프로세스 모델링 프레임워크가 제안됩니다.

고유한 변형 벡터는 마이크로 스케일에서 충실도가 높은 상세한 다층 프로세스 시뮬레이션에서 추출됩니다. 균일하지만 이방성인 변형은 잔류 왜곡 및 응력을 예측하기 위해 준 정적 평형 유한 요소 분석(FEA)에서 레이어별로 L-PBF 부품에 적용됩니다.

부품 규모에서의 잔류 변형 및 응력 예측 외에도 분말 규모의 다중물리 모델링을 수행하여 공정 매개변수, 예열 온도 및 스패터링 입자에 의해 유도된 용융 풀 변동 및 결함 형성을 연구합니다. 이러한 요인과 관련된 용융 풀 역학 및 다공성 형성 메커니즘은 시뮬레이션 및 실험을 통해 밝혀졌습니다.

제안된 부품 규모 잔류 응력 및 왜곡 모델을 기반으로 경로 계획 방법은 큰 잔류 변형 및 건물 파손을 방지하기 위해 주어진 형상에 대한 레이저 스캐닝 경로를 조정하기 위해 개발되었습니다.

연속 및 아일랜드 스캐닝 전략을 위한 기울기 기반 경로 계획이 공식화되고 공식화된 컴플라이언스 및 스트레스 최소화 문제에 대한 전체 감도 분석이 수행됩니다. 이 제안된 경로 계획 방법의 타당성과 효율성은 AconityONE L-PBF 시스템을 사용하여 실험적으로 입증되었습니다.

또한 기계 학습을 활용한 데이터 기반 프레임워크를 개발하여 L-PBF에 대한 부품 규모의 열 이력을 예측합니다. 본 연구에서는 실시간 열 이력 예측을 위해 CNN(Convolutional Neural Network)과 RNN(Recurrent Neural Network)을 포함하는 순차적 기계 학습 모델을 제안합니다.

유한 요소 해석과 비교하여 100배의 예측 속도 향상이 달성되어 실제 제작 프로세스보다 빠른 예측이 가능하고 실시간 온도 프로파일을 사용할 수 있습니다.

Laser powder bed fusion (L-PBF) additive manufacturing (AM) is capable of producing complex parts near net shape with good mechanical properties. However, undesired residual stress and distortion that lead to build failure and defects such as porosity are preventing broader applications of L-PBF. To realize the full potential of L-PBF, a multiscale modeling methodology is developed to predict residual deformation, melt pool, and porosity formation. To predict the residual deformation and stress in L-PBF at part-scale, a multiscale process modeling framework based on inherent strain method is proposed.

Inherent strain vectors are extracted from detailed multi-layer process simulation with high fidelity at micro-scale. Uniform but anisotropic strains are then applied to L-PBF part in a layer-by-layer fashion in a quasi-static equilibrium finite element analysis (FEA) to predict residual distortion and stress. Besides residual distortion and stress prediction at part scale, multiphysics modeling at powder scale is performed to study the melt pool variation and defect formation induced by process parameters, preheating temperature and spattering particles. Melt pool dynamics and porosity formation mechanisms associated with these factors are revealed through simulation and experiments.

Based on the proposed part-scale residual stress and distortion model, path planning method is developed to tailor the laser scanning path for a given geometry to prevent large residual deformation and building failures. Gradient based path planning for continuous and island scanning strategy is formulated and full sensitivity analysis for the formulated compliance- and stress-minimization problem is performed.

The feasibility and effectiveness of this proposed path planning method is demonstrated experimentally using the AconityONE L-PBF system. In addition, a data-driven framework utilizing machine learning is developed to predict the thermal history at part-scale for L-PBF.

In this work, a sequential machine learning model including convolutional neural network (CNN) and recurrent neural network (RNN), long shortterm memory unit, is proposed for real-time thermal history prediction. A 100x prediction speed improvement is achieved compared to the finite element analysis which makes the prediction faster than real fabrication process and real-time temperature profile available.

Figure 1.1: Schematic Overview of Metal Laser Powder Bed Fusion Process [2]
Figure 1.1: Schematic Overview of Metal Laser Powder Bed Fusion Process [2]
Figure 1.2: Commercial Powder Bed Fusion Systems
Figure 1.2: Commercial Powder Bed Fusion Systems
Figure 1.3: Commercial Metal Components Fabricated by Powder Bed Fusion Additive Manufacturing: (a) GE Fuel Nozzle; (b) Stryker Hip Biomedical Implant.
Figure 1.3: Commercial Metal Components Fabricated by Powder Bed Fusion Additive Manufacturing: (a) GE Fuel Nozzle; (b) Stryker Hip Biomedical Implant.
Figure 2.1: Proposed Multiscale Process Simulation Framework
Figure 2.1: Proposed Multiscale Process Simulation Framework
Figure 2.2: (a) Experimental Setup for In-situ Thermocouple Measurement in the EOS M290 Build Chamber; (b) Themocouple Locations on the Bottom Side of the Substrate.
Figure 2.2: (a) Experimental Setup for In-situ Thermocouple Measurement in the EOS M290 Build Chamber; (b) Themocouple Locations on the Bottom Side of the Substrate.
Figure 2.3: (a) Finite Element Model for Single Layer Thermal Analysis; (b) Deposition Layer
Figure 2.3: (a) Finite Element Model for Single Layer Thermal Analysis; (b) Deposition Layer
Figure 2.4: Core-skin layer: (a) Surface Morphology; (b) Scanning Strategy; (c) Transient Temperature Distribution and Temperature History at (d) Point 1; (e) Point 2 and (f) Point 3
Figure 2.4: Core-skin layer: (a) Surface Morphology; (b) Scanning Strategy; (c) Transient Temperature Distribution and Temperature History at (d) Point 1; (e) Point 2 and (f) Point 3
Figure 2.5: (a) Scanning Orientation of Each Layer; (b) Finite Element Model for Micro-scale Representative Volume
Figure 2.5: (a) Scanning Orientation of Each Layer; (b) Finite Element Model for Micro-scale Representative Volume
Figure 2.6: Bottom Layer (a) Thermal History; (b) Plastic Strain and (c) Elastic Strain Evolution History
Figure 2.6: Bottom Layer (a) Thermal History; (b) Plastic Strain and (c) Elastic Strain Evolution History
Figure 2.7: Bottom Layer Inherent Strain under Default Process Parameters along Horizontal Scanning Path
Figure 2.7: Bottom Layer Inherent Strain under Default Process Parameters along Horizontal Scanning Path
Figure 2.8: Snapshots of the Element Activation Process
Figure 2.8: Snapshots of the Element Activation Process
Figure 2.9: Double Cantilever Beam Structure Built by the EOS M290 DMLM Process (a) Before and (b) After Cutting off; (c) Faro Laser ScanArm V3 for Distortion Measurement
Figure 2.9: Double Cantilever Beam Structure Built by the EOS M290 DMLM Process (a) Before and (b) After Cutting off; (c) Faro Laser ScanArm V3 for Distortion Measurement
Figure 2.10: Square Canonical Structure Built by the EOS M290 DMLM Process
Figure 2.10: Square Canonical Structure Built by the EOS M290 DMLM Process
Figure 2.11: Finite Element Mesh for the Square Canonical and Snapshots of Element Activation Process
Figure 2.11: Finite Element Mesh for the Square Canonical and Snapshots of Element Activation Process
Figure 2.12: Simulated Distortion Field for the Double Cantilever Beam before Cutting off the Supports: (a) Inherent Strain Method; (b) Simufact Additive 3.1
Figure 2.12: Simulated Distortion Field for the Double Cantilever Beam before Cutting off the Supports: (a) Inherent Strain Method; (b) Simufact Additive 3.1
Figure 3.10: Snapshots of Temperature Profile for Single Track in Keyhole Regime (P = 250W and V = 0.5m/s) at the Preheating Temperature of 100 °C
Figure 3.10: Snapshots of Temperature Profile for Single Track in Keyhole Regime (P = 250W and V = 0.5m/s) at the Preheating Temperature of 100 °C
s) at the Preheating Temperature of 500 °C
s) at the Preheating Temperature of 500 °C
Figure 3.15: Melt Pool Cross Section Comparison Between Simulation and Experiment for Single Track
Figure 3.15: Melt Pool Cross Section Comparison Between Simulation and Experiment for Single Track

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Figure 2. (a) Scanning electron microscopy images of Ti6Al4V powder particles and (b) simulated powder bed using discrete element modelling

Laser Powder Bed에서 Laser Drilling에 의한 Keyhole 형성 Ti6Al4V 생체 의학 합금의 융합: 메조스코픽 전산유체역학 시뮬레이션 대 경험적 검증을 사용한 수학적 모델링

Keyhole Formation by Laser Drilling in Laser Powder Bed Fusion of Ti6Al4V Biomedical Alloy: Mesoscopic Computational Fluid Dynamics Simulation versus Mathematical Modelling Using Empirical Validation

Asif Ur Rehman 1,2,3,*
,† , Muhammad Arif Mahmood 4,*
,† , Fatih Pitir 1
, Metin Uymaz Salamci 2,3
,
Andrei C. Popescu 4 and Ion N. Mihailescu 4

Abstract

LPBF(Laser Powder Bed fusion) 공정에서 작동 조건은 열 분포를 기반으로 레이저 유도 키홀 영역을 결정하는 데 필수적입니다. 얕은 구멍과 깊은 구멍으로 분류되는 이러한 영역은 LPBF 프로세스에서 확률과 결함 형성 강도를 제어합니다.

LPBF 프로세스의 핵심 구멍을 연구하고 제어하기 위해 수학적 및 CFD(전산 유체 역학) 모델이 제공됩니다. CFD의 경우 이산 요소 모델링 기법을 사용한 유체 체적 방법이 사용되었으며, 분말 베드 보이드 및 표면에 의한 레이저 빔 흡수를 포함하여 수학적 모델이 개발되었습니다.

동적 용융 풀 거동을 자세히 살펴봅니다. 실험적, CFD 시뮬레이션 및 분석적 컴퓨팅 결과 간에 정량적 비교가 수행되어 좋은 일치를 얻습니다.

LPBF에서 레이저 조사 영역 주변의 온도는 높은 내열성과 분말 입자 사이의 공기로 인해 분말층 주변에 비해 급격히 상승하여 레이저 횡방향 열파의 이동이 느려집니다. LPBF에서 키홀은 에너지 밀도에 의해 제어되는 얕고 깊은 키홀 모드로 분류될 수 있습니다. 에너지 밀도를 높이면 얕은 키홀 구멍 모드가 깊은 키홀 구멍 모드로 바뀝니다.

깊은 키홀 구멍의 에너지 밀도는 다중 반사와 키홀 구멍 내의 2차 반사 빔의 집중으로 인해 더 높아져 재료가 빠르게 기화됩니다.

깊은 키홀 구멍 모드에서는 온도 분포가 높기 때문에 액체 재료가 기화 온도에 가까우므로 얕은 키홀 구멍보다 구멍이 형성될 확률이 훨씬 높습니다. 온도가 급격히 상승하면 재료 밀도가 급격히 떨어지므로 비열과 융해 잠열로 인해 유체 부피가 증가합니다.

그 대가로 표면 장력을 낮추고 용융 풀 균일성에 영향을 미칩니다.

In the laser powder bed fusion (LPBF) process, the operating conditions are essential in determining laser-induced keyhole regimes based on the thermal distribution. These regimes, classified into shallow and deep keyholes, control the probability and defects formation intensity in the LPBF process. To study and control the keyhole in the LPBF process, mathematical and computational fluid dynamics (CFD) models are presented. For CFD, the volume of fluid method with the discrete element modeling technique was used, while a mathematical model was developed by including the laser beam absorption by the powder bed voids and surface. The dynamic melt pool behavior is explored in detail. Quantitative comparisons are made among experimental, CFD simulation and analytical computing results leading to a good correspondence. In LPBF, the temperature around the laser irradiation zone rises rapidly compared to the surroundings in the powder layer due to the high thermal resistance and the air between the powder particles, resulting in a slow travel of laser transverse heat waves. In LPBF, the keyhole can be classified into shallow and deep keyhole mode, controlled by the energy density. Increasing the energy density, the shallow keyhole mode transforms into the deep keyhole mode. The energy density in a deep keyhole is higher due to the multiple reflections and concentrations of secondary reflected beams within the keyhole, causing the material to vaporize quickly. Due to an elevated temperature distribution in deep keyhole mode, the probability of pores forming is much higher than in a shallow keyhole as the liquid material is close to the vaporization temperature. When the temperature increases rapidly, the material density drops quickly, thus, raising the fluid volume due to the specific heat and fusion latent heat. In return, this lowers the surface tension and affects the melt pool uniformity.

Keywords: laser powder bed fusion; computational fluid dynamics; analytical modelling; shallow
and deep keyhole modes; experimental correlation

Figure 1. Powder bed schematic with voids.
Figure 1. Powder bed schematic with voids.
Figure 2. (a) Scanning electron microscopy images of Ti6Al4V powder particles and (b) simulated powder bed using discrete element modelling
Figure 2. (a) Scanning electron microscopy images of Ti6Al4V powder particles and (b) simulated powder bed using discrete element modelling
Figure 3. Temperature field contour formation at various time intervals (a) 0.695 ms, (b) 0.795 ms, (c) 0.995 ms and (d) 1.3 ms.
Figure 3. Temperature field contour formation at various time intervals (a) 0.695 ms, (b) 0.795 ms, (c) 0.995 ms and (d) 1.3 ms.
Figure 4. Detailed view of shallow depth melt mode with temperature field at 0.695 ms
Figure 4. Detailed view of shallow depth melt mode with temperature field at 0.695 ms
Figure 5. Melt flow stream traces formation at various time intervals (a) 0.695 ms, (b) 0.795 ms, (c) 0.995 ms and (d) 1.3 ms
Figure 5. Melt flow stream traces formation at various time intervals (a) 0.695 ms, (b) 0.795 ms, (c) 0.995 ms and (d) 1.3 ms
Figure 6. Density evolution of the melt pool at various time intervals (a) 0.695 ms, (b) 0.795 ms, (c) 0.995 ms and (d) 1.3 ms.
Figure 6. Density evolution of the melt pool at various time intervals (a) 0.695 ms, (b) 0.795 ms, (c) 0.995 ms and (d) 1.3 ms.
Figure 7. Un-melted and melted regions at different time intervals (a) 0.695 ms, (b) 0.795 ms, (c) 0.995 ms and (d) 1.3 ms
Figure 7. Un-melted and melted regions at different time intervals (a) 0.695 ms, (b) 0.795 ms, (c) 0.995 ms and (d) 1.3 ms
Figure 8. Transformation from shallow depth melt flow to deep keyhole formation when laser power increased from (a) 170 W to (b) 200 W
Figure 8. Transformation from shallow depth melt flow to deep keyhole formation when laser power increased from (a) 170 W to (b) 200 W
Figure 9. Stream traces and laser beam multiple reflections in deep keyhole melt flow mode
Figure 9. Stream traces and laser beam multiple reflections in deep keyhole melt flow mode
Figure 10. A comparison between analytical and CFD simulation results for peak thermal distribution value in the deep keyhole formation
Figure 10. A comparison between analytical and CFD simulation results for peak thermal distribution value in the deep keyhole formation
Figure 11. A comparison among experiments [49], CFD and analytical simulations for deep keyhole top width and bottom width
Figure 11. A comparison among experiments [49], CFD and analytical simulations for deep keyhole top width and bottom width

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Fig. 1. (a) Dimensions of the casting with runners (unit: mm), (b) a melt flow simulation using Flow-3D software together with Reilly's model[44], predicted that a large amount of bifilms (denoted by the black particles) would be contained in the final casting. (c) A solidification simulation using Pro-cast software showed that no shrinkage defect was contained in the final casting.

AZ91 합금 주물 내 연행 결함에 대한 캐리어 가스의 영향

Effect of carrier gases on the entrainment defects within AZ91 alloy castings

Tian Liab J.M.T.Daviesa Xiangzhen Zhuc
aUniversity of Birmingham, Birmingham B15 2TT, United Kingdom
bGrainger and Worrall Ltd, Bridgnorth WV15 5HP, United Kingdom
cBrunel Centre for Advanced Solidification Technology, Brunel University London, Kingston Ln, London, Uxbridge UB8 3PH, United Kingdom

Abstract

An entrainment defect (also known as a double oxide film defect or bifilm) acts a void containing an entrapped gas when submerged into a light-alloy melt, thus reducing the quality and reproducibility of the final castings. Previous publications, carried out with Al-alloy castings, reported that this trapped gas could be subsequently consumed by the reaction with the surrounding melt, thus reducing the void volume and negative effect of entrainment defects. Compared with Al-alloys, the entrapped gas within Mg-alloy might be more efficiently consumed due to the relatively high reactivity of magnesium. However, research into the entrainment defects within Mg alloys has been significantly limited. In the present work, AZ91 alloy castings were produced under different carrier gas atmospheres (i.e., SF6/CO2, SF6/air). The evolution processes of the entrainment defects contained in AZ91 alloy were suggested according to the microstructure inspections and thermodynamic calculations. The defects formed in the different atmospheres have a similar sandwich-like structure, but their oxide films contained different combinations of compounds. The use of carrier gases, which were associated with different entrained-gas consumption rates, affected the reproducibility of AZ91 castings.

Keywords

Magnesium alloyCastingOxide film, Bifilm, Entrainment defect, Reproducibility

연행 결함(이중 산화막 결함 또는 이중막 결함이라고도 함)은 경합금 용융물에 잠길 때 갇힌 가스를 포함하는 공극으로 작용하여 최종 주물의 품질과 재현성을 저하시킵니다. Al-합금 주조로 수행된 이전 간행물에서는 이 갇힌 가스가 주변 용융물과의 반응에 의해 후속적으로 소모되어 공극 부피와 연행 결함의 부정적인 영향을 줄일 수 있다고 보고했습니다. Al-합금에 비해 마그네슘의 상대적으로 높은 반응성으로 인해 Mg-합금 내에 포집된 가스가 더 효율적으로 소모될 수 있습니다. 그러나 Mg 합금 내 연행 결함에 대한 연구는 상당히 제한적이었습니다. 현재 작업에서 AZ91 합금 주물은 다양한 캐리어 가스 분위기(즉, SF 6 /CO2 , SF 6 / 공기). AZ91 합금에 포함된 엔트레인먼트 결함의 진화 과정은 미세조직 검사 및 열역학적 계산에 따라 제안되었습니다. 서로 다른 분위기에서 형성된 결함은 유사한 샌드위치 구조를 갖지만 산화막에는 서로 다른 화합물 조합이 포함되어 있습니다. 다른 동반 가스 소비율과 관련된 운반 가스의 사용은 AZ91 주물의 재현성에 영향을 미쳤습니다.

키워드

마그네슘 합금주조Oxide film, Bifilm, Entrainment 불량, 재현성

1 . 소개

지구상에서 가장 가벼운 구조용 금속인 마그네슘은 지난 수십 년 동안 가장 매력적인 경금속 중 하나가 되었습니다. 결과적으로 마그네슘 산업은 지난 20년 동안 급속한 발전을 경험했으며 [1 , 2] , 이는 전 세계적으로 Mg 합금에 대한 수요가 크게 증가했음을 나타냅니다. 오늘날 Mg 합금의 사용은 자동차, 항공 우주, 전자 등의 분야에서 볼 수 있습니다. [3 , 4] . Mg 금속의 전 세계 소비는 특히 자동차 산업에서 앞으로 더욱 증가할 것으로 예측되었습니다. 기존 자동차와 전기 자동차 모두의 에너지 효율성 요구 사항이 설계를 경량화하도록 더욱 밀어붙이기 때문입니다 [3 , 56] .

Mg 합금에 대한 수요의 지속적인 성장은 Mg 합금 주조의 품질 및 기계적 특성 개선에 대한 광범위한 관심을 불러일으켰습니다. Mg 합금 주조 공정 동안 용융물의 표면 난류는 소량의 주변 대기를 포함하는 이중 표면 필름의 포획으로 이어질 수 있으므로 동반 결함(이중 산화막 결함 또는 이중막 결함이라고도 함)을 형성합니다. ) [7] , [8] , [9] , [10] . 무작위 크기, 수량, 방향 및 연행 결함의 배치는 주조 특성의 변화와 관련된 중요한 요인으로 널리 받아들여지고 있습니다 [7] . 또한 Peng et al. [11]AZ91 합금 용융물에 동반된 산화물 필름이 Al 8 Mn 5 입자에 대한 필터 역할을 하여 침전될 때 가두는 것을 발견했습니다 . Mackie et al. [12]는 또한 동반된 산화막이 금속간 입자를 트롤(trawl)하는 작용을 하여 입자가 클러스터링되어 매우 큰 결함을 형성할 수 있다고 제안했습니다. 금속간 화합물의 클러스터링은 비말동반 결함을 주조 특성에 더 해롭게 만들었습니다.

연행 결함에 관한 이전 연구의 대부분은 Al-합금에 대해 수행되었으며 [7 , [13] , [14] , [15] , [16] , [17] , [18] 몇 가지 잠재적인 방법이 제안되었습니다. 알루미늄 합금 주물의 품질에 대한 부정적인 영향을 줄이기 위해. Nyahumwa et al., [16] 은 연행 결함 내의 공극 체적이 열간 등방압 압축(HIP) 공정에 의해 감소될 수 있음을 보여줍니다. Campbell [7] 은 결함 내부의 동반된 가스가 주변 용융물과의 반응으로 인해 소모될 수 있다고 제안했으며, 이는 Raiszedeh와 Griffiths [19]에 의해 추가로 확인되었습니다 ..혼입 가스 소비가 Al-합금 주물의 기계적 특성에 미치는 영향은 [8 , 9]에 의해 조사되었으며 , 이는 혼입 가스의 소비가 주조 재현성의 개선을 촉진함을 시사합니다.

Al-합금 내 결함에 대한 조사와 비교하여 Mg-합금 내 연행 결함에 대한 연구는 상당히 제한적입니다. 연행 결함의 존재는 Mg 합금 주물 [20 , 21] 에서 입증 되었지만 그 거동, 진화 및 연행 가스 소비는 여전히 명확하지 않습니다.

Mg 합금 주조 공정에서 용융물은 일반적으로 마그네슘 점화를 피하기 위해 커버 가스로 보호됩니다. 따라서 모래 또는 매몰 몰드의 공동은 용융물을 붓기 전에 커버 가스로 세척해야 합니다 [22] . 따라서, Mg 합금 주물 내의 연행 가스는 공기만이 아니라 주조 공정에 사용되는 커버 가스를 포함해야 하며, 이는 구조 및 해당 연행 결함의 전개를 복잡하게 만들 수 있습니다.

SF 6 은 Mg 합금 주조 공정에 널리 사용되는 대표적인 커버 가스입니다 [23] , [24] , [25] . 이 커버 가스는 유럽의 마그네슘 합금 주조 공장에서 사용하도록 제한되었지만 상업 보고서에 따르면 이 커버는 전 세계 마그네슘 합금 산업, 특히 다음과 같은 글로벌 마그네슘 합금 생산을 지배한 국가에서 여전히 인기가 있습니다. 중국, 브라질, 인도 등 [26] . 또한, 최근 학술지 조사에서도 이 커버가스가 최근 마그네슘 합금 연구에서 널리 사용된 것으로 나타났다 [27] . SF 6 커버 가스 의 보호 메커니즘 (즉, 액체 Mg 합금과 SF 6 사이의 반응Cover gas)에 대한 연구는 여러 선행연구자들에 의해 이루어졌으나 표면 산화막의 형성과정이 아직 명확하게 밝혀지지 않았으며, 일부 발표된 결과들도 상충되고 있다. 1970년대 초 Fruehling [28] 은 SF 6 아래에 형성된 표면 피막이 주로 미량의 불화물과 함께 MgO 임을 발견 하고 SF 6 이 Mg 합금 표면 피막에 흡수 된다고 제안했습니다 . Couling [29] 은 흡수된 SF 6 이 Mg 합금 용융물과 반응하여 MgF 2 를 형성함을 추가로 확인했습니다 . 지난 20년 동안 아래에 자세히 설명된 것처럼 Mg 합금 표면 필름의 다양한 구조가 보고되었습니다.(1)

단층 필름 . Cashion [30 , 31] 은 X선 광전자 분광법(XPS)과 오제 분광법(AES)을 사용하여 표면 필름을 MgO 및 MgF 2 로 식별했습니다 . 그는 또한 필름의 구성이 두께와 전체 실험 유지 시간에 걸쳐 일정하다는 것을 발견했습니다. Cashion이 관찰한 필름은 10분에서 100분의 유지 시간으로 생성된 단층 구조를 가졌다.(2)

이중층 필름 . Aarstad et. al [32] 은 2003년에 이중층 표면 산화막을 보고했습니다. 그들은 예비 MgO 막에 부착된 잘 분포된 여러 MgF 2 입자를 관찰 하고 전체 표면적의 25-50%를 덮을 때까지 성장했습니다. 외부 MgO 필름을 통한 F의 내부 확산은 진화 과정의 원동력이었습니다. 이 이중층 구조는 Xiong의 그룹 [25 , 33] 과 Shih et al. 도 지지했습니다 . [34] .(삼)

트리플 레이어 필름 . 3층 필름과 그 진화 과정은 Pettersen [35]에 의해 2002년에 보고되었습니다 . Pettersen은 초기 표면 필름이 MgO 상이었고 F의 내부 확산에 의해 점차적으로 안정적인 MgF 2 상 으로 진화한다는 것을 발견했습니다 . 두꺼운 상부 및 하부 MgF 2 층.(4)

산화물 필름은 개별 입자로 구성 됩니다. Wang et al [36] 은 Mg-alloy 표면 필름을 SF 6 커버 가스 하에서 용융물에 교반 한 다음 응고 후 동반된 표면 필름을 검사했습니다. 그들은 동반된 표면 필름이 다른 연구자들이 보고한 보호 표면 필름처럼 계속되지 않고 개별 입자로 구성된다는 것을 발견했습니다. 젊은 산화막은 MgO 나노 크기의 산화물 입자로 구성되어 있는 반면, 오래된 산화막은 한쪽 면에 불화물과 질화물이 포함된 거친 입자(평균 크기 약 1μm)로 구성되어 있습니다.

Mg 합금 용융 표면의 산화막 또는 동반 가스는 모두 액체 Mg 합금과 커버 가스 사이의 반응으로 인해 형성되므로 Mg 합금 표면막에 대한 위에서 언급한 연구는 진화에 대한 귀중한 통찰력을 제공합니다. 연행 결함. 따라서 SF 6 커버 가스 의 보호 메커니즘 (즉, Mg-합금 표면 필름의 형성)은 해당 동반 결함의 잠재적인 복잡한 진화 과정을 나타냅니다.

그러나 Mg 합금 용융물에 표면 필름을 형성하는 것은 용융물에 잠긴 동반된 가스의 소비와 다른 상황에 있다는 점에 유의해야 합니다. 예를 들어, 앞서 언급한 연구에서 표면 성막 동안 충분한 양의 커버 가스가 담지되어 커버 가스의 고갈을 억제했습니다. 대조적으로, Mg 합금 용융물 내의 동반된 가스의 양은 유한하며, 동반된 가스는 완전히 고갈될 수 있습니다. Mirak [37] 은 3.5% SF 6 /기포를 특별히 설계된 영구 금형에서 응고되는 순수한 Mg 합금 용융물에 도입했습니다. 기포가 완전히 소모되었으며, 해당 산화막은 MgO와 MgF 2 의 혼합물임을 알 수 있었다.. 그러나 Aarstad [32] 및 Xiong [25 , 33]에 의해 관찰된 MgF 2 스팟 과 같은 핵 생성 사이트 는 관찰되지 않았습니다. Mirak은 또한 조성 분석을 기반으로 산화막에서 MgO 이전에 MgF 2 가 형성 되었다고 추측했는데 , 이는 이전 문헌에서 보고된 표면 필름 형성 과정(즉, MgF 2 이전에 형성된 MgO)과 반대 입니다. Mirak의 연구는 동반된 가스의 산화막 형성이 표면막의 산화막 형성과 상당히 다를 수 있음을 나타내었지만 산화막의 구조와 진화에 대해서는 밝히지 않았습니다.

또한 커버 가스에 캐리어 가스를 사용하는 것도 커버 가스와 액체 Mg 합금 사이의 반응에 영향을 미쳤습니다. SF 6 /air 는 용융 마그네슘의 점화를 피하기 위해 SF 6 /CO 2 운반 가스 [38] 보다 더 높은 함량의 SF 6을 필요로 하여 다른 가스 소비율을 나타냅니다. Liang et.al [39] 은 CO 2 가 캐리어 가스로 사용될 때 표면 필름에 탄소가 형성된다고 제안했는데 , 이는 SF 6 /air 에서 형성된 필름과 다릅니다 . Mg 연소 [40]에 대한 조사 에서 Mg 2 C 3 검출이 보고되었습니다.CO 2 연소 후 Mg 합금 샘플 에서 이는 Liang의 결과를 뒷받침할 뿐만 아니라 이중 산화막 결함에서 Mg 탄화물의 잠재적 형성을 나타냅니다.

여기에 보고된 작업은 다양한 커버 가스(즉, SF 6 /air 및 SF 6 /CO 2 )로 보호되는 AZ91 Mg 합금 주물에서 형성된 연행 결함의 거동과 진화에 대한 조사 입니다. 이러한 캐리어 가스는 액체 Mg 합금에 대해 다른 보호성을 가지며, 따라서 상응하는 동반 가스의 다른 소비율 및 발생 프로세스와 관련될 수 있습니다. AZ91 주물의 재현성에 대한 동반 가스 소비의 영향도 연구되었습니다.

2 . 실험

2.1 . 용융 및 주조

3kg의 AZ91 합금을 700 ± 5 °C의 연강 도가니에서 녹였습니다. AZ91 합금의 조성은 표 1 에 나타내었다 . 가열하기 전에 잉곳 표면의 모든 산화물 스케일을 기계가공으로 제거했습니다. 사용 된 커버 가스는 0.5 %이었다 SF 6 / 공기 또는 0.5 % SF 6 / CO 2 (부피. %) 다른 주물 6L / 분의 유량. 용융물은 15분 동안 0.3L/min의 유속으로 아르곤으로 가스를 제거한 다음 [41 , 42] , 모래 주형에 부었습니다. 붓기 전에 샌드 몰드 캐비티를 20분 동안 커버 가스로 플러싱했습니다 [22] . 잔류 용융물(약 1kg)이 도가니에서 응고되었습니다.

표 1 . 본 연구에 사용된 AZ91 합금의 조성(wt%).

아연미네소타마그네슘
9.40.610.150.020.0050.0017잔여

그림 1 (a)는 러너가 있는 주물의 치수를 보여줍니다. 탑 필링 시스템은 최종 주물에서 연행 결함을 생성하기 위해 의도적으로 사용되었습니다. Green과 Campbell [7 , 43] 은 탑 필링 시스템이 바텀 필링 시스템에 비해 주조 과정에서 더 많은 연행 현상(즉, 이중 필름)을 유발한다고 제안했습니다. 이 금형의 용융 흐름 시뮬레이션(Flow-3D 소프트웨어)은 연행 현상에 관한 Reilly의 모델 [44] 을 사용하여 최종 주조에 많은 양의 이중막이 포함될 것이라고 예측했습니다( 그림 1 에서 검은색 입자로 표시됨) . NS).

그림 1

수축 결함은 또한 주물의 기계적 특성과 재현성에 영향을 미칩니다. 이 연구는 주조 품질에 대한 이중 필름의 영향에 초점을 맞추었기 때문에 수축 결함이 발생하지 않도록 금형을 의도적으로 설계했습니다. ProCAST 소프트웨어를 사용한 응고 시뮬레이션은 그림 1c 와 같이 최종 주조에 수축 결함이 포함되지 않음을 보여주었습니다 . 캐스팅 건전함도 테스트바 가공 전 실시간 X-ray를 통해 확인했다.

모래 주형은 1wt를 함유한 수지 결합된 규사로 만들어졌습니다. % PEPSET 5230 수지 및 1wt. % PEPSET 5112 촉매. 모래는 또한 억제제로 작용하기 위해 2중량%의 Na 2 SiF 6 을 함유했습니다 .. 주입 온도는 700 ± 5 °C였습니다. 응고 후 러너바의 단면을 Sci-Lab Analytical Ltd로 보내 H 함량 분석(LECO 분석)을 하였고, 모든 H 함량 측정은 주조 공정 후 5일째에 실시하였다. 각각의 주물은 인장 강도 시험을 위해 클립 신장계가 있는 Zwick 1484 인장 시험기를 사용하여 40개의 시험 막대로 가공되었습니다. 파손된 시험봉의 파단면을 주사전자현미경(SEM, Philips JEOL7000)을 이용하여 가속전압 5~15kV로 조사하였다. 파손된 시험 막대, 도가니에서 응고된 잔류 Mg 합금 및 주조 러너를 동일한 SEM을 사용하여 단면화하고 연마하고 검사했습니다. CFEI Quanta 3D FEG FIB-SEM을 사용하여 FIB(집속 이온 빔 밀링 기술)에 의해 테스트 막대 파괴 표면에서 발견된 산화막의 단면을 노출했습니다. 분석에 필요한 산화막은 백금층으로 코팅하였다. 그런 다음 30kV로 가속된 갈륨 이온 빔이 산화막의 단면을 노출시키기 위해 백금 코팅 영역을 둘러싼 재료 기판을 밀링했습니다. 산화막 단면의 EDS 분석은 30kV의 가속 전압에서 FIB 장비를 사용하여 수행되었습니다.

2.2 . 산화 세포

전술 한 바와 같이, 몇몇 최근 연구자들은 마그네슘 합금의 용탕 표면에 형성된 보호막 조사 [38 , 39 , [46] , [47] , [48] , [49] , [50] , [51] , [52 ] . 이 실험 동안 사용된 커버 가스의 양이 충분하여 커버 가스에서 불화물의 고갈을 억제했습니다. 이 섹션에서 설명하는 실험은 엔트레인먼트 결함의 산화막의 진화를 연구하기 위해 커버 가스의 공급을 제한하는 밀봉된 산화 셀을 사용했습니다. 산화 셀에 포함된 커버 가스는 큰 크기의 “동반된 기포”로 간주되었습니다.

도 2에 도시된 바와 같이 , 산화셀의 본체는 내부 길이가 400mm, 내경이 32mm인 폐쇄형 연강관이었다. 수냉식 동관을 전지의 상부에 감았습니다. 튜브가 가열될 때 냉각 시스템은 상부와 하부 사이에 온도 차이를 만들어 내부 가스가 튜브 내에서 대류하도록 했습니다. 온도는 도가니 상단에 위치한 K형 열전대로 모니터링했습니다. Nieet al. [53] 은 Mg 합금 용융물의 표면 피막을 조사할 때 SF 6 커버 가스가 유지로의 강철 벽과 반응할 것이라고 제안했습니다 . 이 반응을 피하기 위해 강철 산화 전지의 내부 표면(그림 2 참조)) 및 열전대의 상반부는 질화붕소로 코팅되었습니다(Mg 합금은 질화붕소와 ​​접촉하지 않았습니다).

그림 2

실험 중에 고체 AZ91 합금 블록을 산화 셀 바닥에 위치한 마그네시아 도가니에 넣었습니다. 전지는 1L/min의 가스 유속으로 전기 저항로에서 100℃로 가열되었다. 원래의 갇힌 대기(즉, 공기)를 대체하기 위해 셀을 이 온도에서 20분 동안 유지했습니다. 그런 다음, 산화 셀을 700°C로 더 가열하여 AZ91 샘플을 녹였습니다. 그런 다음 가스 입구 및 출구 밸브가 닫혀 제한된 커버 가스 공급 하에서 산화를 위한 밀폐된 환경이 생성되었습니다. 그런 다음 산화 전지를 5분 간격으로 5분에서 30분 동안 700 ± 10°C에서 유지했습니다. 각 유지 시간이 끝날 때 세포를 물로 켄칭했습니다. 실온으로 냉각한 후 산화된 샘플을 절단하고 연마한 다음 SEM으로 검사했습니다.

3 . 결과

3.1 . SF 6 /air 에서 형성된 엔트레인먼트 결함의 구조 및 구성

0.5 % SF의 커버 가스 하에서 AZ91 주물에 형성된 유입 결함의 구조 및 조성 6 / 공기는 SEM 및 EDS에 의해 관찰되었다. 결과는 그림 3에 스케치된 엔트레인먼트 결함의 두 가지 유형이 있음을 나타냅니다 . (1) 산화막이 전통적인 단층 구조를 갖는 유형 A 결함 및 (2) 산화막이 2개 층을 갖는 유형 B 결함. 이러한 결함의 세부 사항은 다음에 소개되었습니다. 여기에서 비말동반 결함은 생물막 또는 이중 산화막으로도 알려져 있기 때문에 B형 결함의 산화막은 본 연구에서 “다층 산화막” 또는 “다층 구조”로 언급되었습니다. “이중 산화막 결함의 이중층 산화막”과 같은 혼란스러운 설명을 피하기 위해.

그림 3

그림 4 (ab)는 약 0.4μm 두께의 조밀한 단일층 산화막을 갖는 Type A 결함을 보여줍니다. 이 필름에서 산소, 불소, 마그네슘 및 알루미늄이 검출되었습니다( 그림 4c). 산화막은 마그네슘과 알루미늄의 산화물과 불화물의 혼합물로 추측됩니다. 불소의 검출은 동반된 커버 가스가 이 결함의 형성에 포함되어 있음을 보여주었습니다. 즉, Fig. 4 (a)에 나타난 기공 은 수축결함이나 수소기공도가 아니라 연행결함이었다. 알루미늄의 검출은 Xiong과 Wang의 이전 연구 [47 , 48] 와 다르며 , SF 6으로 보호된 AZ91 용융물의 표면 필름에 알루미늄이 포함되어 있지 않음을 보여주었습니다.커버 가스. 유황은 원소 맵에서 명확하게 인식할 수 없었지만 해당 ESD 스펙트럼에서 S-피크가 있었습니다.

그림 4

도 5 (ab)는 다층 산화막을 갖는 Type B 엔트레인먼트 결함을 나타낸다. 산화막의 조밀한 외부 층은 불소와 산소가 풍부하지만( 그림 5c) 상대적으로 다공성인 내부 층은 산소만 풍부하고(즉, 불소가 부족) 부분적으로 함께 성장하여 샌드위치 모양을 형성합니다. 구조. 따라서 외층은 불화물과 산화물의 혼합물이며 내층은 주로 산화물로 추정된다. 황은 EDX 스펙트럼에서만 인식될 수 있었고 요소 맵에서 명확하게 식별할 수 없었습니다. 이는 커버 가스의 작은 S 함량(즉, SF 6 의 0.5% 부피 함량 때문일 수 있음)커버 가스). 이 산화막에서는 이 산화막의 외층에 알루미늄이 포함되어 있지만 내층에서는 명확하게 검출할 수 없었다. 또한 Al의 분포가 고르지 않은 것으로 보입니다. 결함의 우측에는 필름에 알루미늄이 존재하지만 그 농도는 매트릭스보다 높은 것으로 식별할 수 없음을 알 수 있다. 그러나 결함의 왼쪽에는 알루미늄 농도가 훨씬 높은 작은 영역이 있습니다. 이러한 알루미늄의 불균일한 분포는 다른 결함(아래 참조)에서도 관찰되었으며, 이는 필름 내부 또는 아래에 일부 산화물 입자가 형성된 결과입니다.

그림 5

무화과 도 4 및 5 는 SF 6 /air 의 커버 가스 하에 주조된 AZ91 합금 샘플에서 형성된 연행 결함의 횡단면 관찰을 나타낸다 . 2차원 단면에서 관찰된 수치만으로 연행 결함을 특성화하는 것만으로는 충분하지 않습니다. 더 많은 이해를 돕기 위해 테스트 바의 파단면을 관찰하여 엔트레인먼트 결함(즉, 산화막)의 표면을 더 연구했습니다.

Fig. 6 (a)는 SF 6 /air 에서 생산된 AZ91 합금 인장시험봉의 파단면을 보여준다 . 파단면의 양쪽에서 대칭적인 어두운 영역을 볼 수 있습니다. 그림 6 (b)는 어두운 영역과 밝은 영역 사이의 경계를 보여줍니다. 밝은 영역은 들쭉날쭉하고 부서진 특징으로 구성되어 있는 반면, 어두운 영역의 표면은 비교적 매끄럽고 평평했습니다. 또한 EDS 결과( Fig. 6 c-d 및 Table 2) 불소, 산소, 황 및 질소는 어두운 영역에서만 검출되었으며, 이는 어두운 영역이 용융물에 동반된 표면 보호 필름임을 나타냅니다. 따라서 어두운 영역은 대칭적인 특성을 고려할 때 연행 결함이라고 제안할 수 있습니다. Al-합금 주조물의 파단면에서 유사한 결함이 이전에 보고되었습니다 [7] . 질화물은 테스트 바 파단면의 산화막에서만 발견되었지만 그림 1과 그림 4에 표시된 단면 샘플에서는 검출되지 않았습니다 4 및 5 . 근본적인 이유는 이러한 샘플에 포함된 질화물이 샘플 연마 과정에서 가수분해되었을 수 있기 때문입니다 [54] .

그림 6

표 2 . EDS 결과(wt.%)는 그림 6에 표시된 영역에 해당합니다 (커버 가스: SF 6 /공기).

영형마그네슘NS아연NSNS
그림 6 (b)의 어두운 영역3.481.3279.130.4713.630.570.080.73
그림 6 (b)의 밝은 영역3.5884.4811.250.68

도 1 및 도 2에 도시된 결함의 단면 관찰과 함께 도 4 및 도 5 를 참조하면, 인장 시험봉에 포함된 연행 결함의 구조를 도 6 (e) 와 같이 스케치하였다 . 결함에는 산화막으로 둘러싸인 동반된 가스가 포함되어 있어 테스트 바 내부에 보이드 섹션이 생성되었습니다. 파괴 과정에서 결함에 인장력이 가해지면 균열이 가장 약한 경로를 따라 전파되기 때문에 보이드 섹션에서 균열이 시작되어 연행 결함을 따라 전파됩니다 [55] . 따라서 최종적으로 시험봉이 파단되었을 때 Fig. 6 (a) 와 같이 시험봉의 양 파단면에 연행결함의 산화피막이 나타났다 .

3.2 . SF 6 /CO 2 에 형성된 연행 결함의 구조 및 조성

SF 6 /air 에서 형성된 엔트레인먼트 결함과 유사하게, 0.5% SF 6 /CO 2 의 커버 가스 아래에서 형성된 결함 도 두 가지 유형의 산화막(즉, 단층 및 다층 유형)을 가졌다. 도 7 (a)는 다층 산화막을 포함하는 엔트레인먼트 결함의 예를 도시한다. 결함에 대한 확대 관찰( 그림 7b )은 산화막의 내부 층이 함께 성장하여 SF 6 /air 의 분위기에서 형성된 결함과 유사한 샌드위치 같은 구조를 나타냄을 보여줍니다 ( 그림 7b). 5 나 ). EDS 스펙트럼( 그림 7c) 이 샌드위치형 구조의 접합부(내층)는 주로 산화마그네슘을 함유하고 있음을 보여주었다. 이 EDS 스펙트럼에서는 불소, 황, 알루미늄의 피크가 확인되었으나 그 양은 상대적으로 적었다. 대조적으로, 산화막의 외부 층은 조밀하고 불화물과 산화물의 혼합물로 구성되어 있습니다( 그림 7d-e).

그림 7

Fig. 8 (a)는 0.5%SF 6 /CO 2 분위기에서 제작된 AZ91 합금 인장시험봉의 파단면의 연행결함을 보여준다 . 상응하는 EDS 결과(표 3)는 산화막이 불화물과 산화물을 함유함을 보여주었다. 황과 질소는 검출되지 않았습니다. 게다가, 확대 관찰(  8b)은 산화막 표면에 반점을 나타내었다. 반점의 직경은 수백 나노미터에서 수 마이크론 미터까지 다양했습니다.

그림 8

산화막의 구조와 조성을 보다 명확하게 나타내기 위해 테스트 바 파단면의 산화막 단면을 FIB 기법을 사용하여 현장에서 노출시켰다( 그림 9 ). 도 9a에 도시된 바와 같이 , 백금 코팅층과 Mg-Al 합금 기재 사이에 연속적인 산화피막이 발견되었다. 그림 9 (bc)는 다층 구조( 그림 9c 에서 빨간색 상자로 표시)를 나타내는 산화막에 대한 확대 관찰을 보여줍니다 . 바닥층은 불소와 산소가 풍부하고 불소와 산화물의 혼합물이어야 합니다 . 5 와 7, 유일한 산소가 풍부한 최상층은 도 1 및 도 2에 도시 된 “내층”과 유사하였다 5 및 7 .

그림 9

연속 필름을 제외하고 도 9 에 도시된 바와 같이 연속 필름 내부 또는 하부에서도 일부 개별 입자가 관찰되었다 . 그림 9( b) 의 산화막 좌측에서 Al이 풍부한 입자가 검출되었으며, 마그네슘과 산소 원소도 풍부하게 함유하고 있어 스피넬 Mg 2 AlO 4 로 추측할 수 있다 . 이러한 Mg 2 AlO 4 입자의 존재는 Fig. 5 와 같이 관찰된 필름의 작은 영역에 높은 알루미늄 농도와 알루미늄의 불균일한 분포의 원인이 된다 .(씨). 여기서 강조되어야 할 것은 연속 산화막의 바닥층의 다른 부분이 이 Al이 풍부한 입자보다 적은 양의 알루미늄을 함유하고 있지만, 그림 9c는 이 바닥층의 알루미늄 양이 여전히 무시할 수 없는 수준임을 나타냅니다 . , 특히 필름의 외층과 비교할 때. 도 9b에 도시된 산화막의 우측 아래에서 입자가 검출되어 Mg와 O가 풍부하여 MgO인 것으로 추측되었다. Wang의 결과에 따르면 [56], Mg 용융물과 Mg 증기의 산화에 의해 Mg 용융물의 표면에 많은 이산 MgO 입자가 형성될 수 있다. 우리의 현재 연구에서 관찰된 MgO 입자는 같은 이유로 인해 형성될 수 있습니다. 실험 조건의 차이로 인해 더 적은 Mg 용융물이 기화되거나 O2와 반응할 수 있으므로 우리 작업에서 형성되는 MgO 입자는 소수에 불과합니다. 또한 필름에서 풍부한 탄소가 발견되어 CO 2 가 용융물과 반응하여 탄소 또는 탄화물을 형성할 수 있음을 보여줍니다 . 이 탄소 농도는 표 3에 나타낸 산화막의 상대적으로 높은 탄소 함량 (즉, 어두운 영역) 과 일치하였다 . 산화막 옆 영역.

표 3 . 도 8에 도시된 영역에 상응하는 EDS 결과(wt.%) (커버 가스: SF 6 / CO 2 ).

영형마그네슘NS아연NSNS
그림 8 (a)의 어두운 영역7.253.6469.823.827.030.86
그림 8 (a)의 밝은 영역2.100.4482.8313.261.36

테스트 바 파단면( 도 9 ) 에서 산화막의 이 단면 관찰은 도 6 (e)에 도시된 엔트레인먼트 결함의 개략도를 추가로 확인했다 . SF 6 /CO 2 와 SF 6 /air 의 서로 다른 분위기에서 형성된 엔트레인먼트 결함 은 유사한 구조를 가졌지만 그 조성은 달랐다.

3.3 . 산화 전지에서 산화막의 진화

섹션 3.1 및 3.2 의 결과 는 SF 6 /air 및 SF 6 /CO 2 의 커버 가스 아래에서 AZ91 주조에서 형성된 연행 결함의 구조 및 구성을 보여줍니다 . 산화 반응의 다른 단계는 연행 결함의 다른 구조와 조성으로 이어질 수 있습니다. Campbell은 동반된 가스가 주변 용융물과 반응할 수 있다고 추측했지만 Mg 합금 용융물과 포획된 커버 가스 사이에 반응이 발생했다는 보고는 거의 없습니다. 이전 연구자들은 일반적으로 개방된 환경에서 Mg 합금 용융물과 커버 가스 사이의 반응에 초점을 맞췄습니다 [38 , 39 , [46] , [47][48] , [49] , [50] , [51] , [52] , 이는 용융물에 갇힌 커버 가스의 상황과 다릅니다. AZ91 합금에서 엔트레인먼트 결함의 형성을 더 이해하기 위해 엔트레인먼트 결함의 산화막의 진화 과정을 산화 셀을 사용하여 추가로 연구했습니다.

.도 10 (a 및 d) 0.5 % 방송 SF 보호 산화 셀에서 5 분 동안 유지 된 표면 막 (6) / 공기. 불화물과 산화물(MgF 2 와 MgO) 로 이루어진 단 하나의 층이 있었습니다 . 이 표면 필름에서. 황은 EDS 스펙트럼에서 검출되었지만 그 양이 너무 적어 원소 맵에서 인식되지 않았습니다. 이 산화막의 구조 및 조성은 도 4 에 나타낸 엔트레인먼트 결함의 단층막과 유사하였다 .

그림 10

10분의 유지 시간 후, 얇은 (O,S)가 풍부한 상부층(약 700nm)이 예비 F-농축 필름에 나타나 그림 10 (b 및 e) 에서와 같이 다층 구조를 형성했습니다 . ). (O, S)가 풍부한 최상층의 두께는 유지 시간이 증가함에 따라 증가했습니다. Fig. 10 (c, f) 에서 보는 바와 같이 30분간 유지한 산화막도 다층구조를 가지고 있으나 (O,S)가 풍부한 최상층(약 2.5μm)의 두께가 10분 산화막의 그것. 도 10 (bc) 에 도시 된 다층 산화막 은 도 5에 도시된 샌드위치형 결함의 막과 유사한 외관을 나타냈다 .

도 10에 도시된 산화막의 상이한 구조는 커버 가스의 불화물이 AZ91 합금 용융물과의 반응으로 인해 우선적으로 소모될 것임을 나타내었다. 불화물이 고갈된 후, 잔류 커버 가스는 액체 AZ91 합금과 추가로 반응하여 산화막에 상부 (O, S)가 풍부한 층을 형성했습니다. 따라서 도 1 및 도 3에 도시된 연행 결함의 상이한 구조 및 조성 4 와 5 는 용융물과 갇힌 커버 가스 사이의 진행 중인 산화 반응 때문일 수 있습니다.

이 다층 구조는 Mg 합금 용융물에 형성된 보호 표면 필름에 관한 이전 간행물 [38 , [46] , [47] , [48] , [49] , [50] , [51] 에서 보고되지 않았습니다 . . 이는 이전 연구원들이 무제한의 커버 가스로 실험을 수행했기 때문에 커버 가스의 불화물이 고갈되지 않는 상황을 만들었기 때문일 수 있습니다. 따라서 엔트레인먼트 결함의 산화피막은 도 10에 도시된 산화피막과 유사한 거동특성을 가지나 [38 ,[46] , [47] , [48] , [49] , [50] , [51] .

SF 유지 산화막와 마찬가지로 6 / 공기, SF에 형성된 산화물 막 (6) / CO 2는 또한 세포 산화 다른 유지 시간과 다른 구조를 가지고 있었다. .도 11 (a)는 AZ91 개최 산화막, 0.5 %의 커버 가스 하에서 SF 표면 용융 도시 6 / CO 2, 5 분. 이 필름은 MgF 2 로 이루어진 단층 구조를 가졌다 . 이 영화에서는 MgO의 존재를 확인할 수 없었다. 30분의 유지 시간 후, 필름은 다층 구조를 가졌다; 내부 층은 조밀하고 균일한 외관을 가지며 MgF 2 로 구성 되고 외부 층은 MgF 2 혼합물및 MgO. 0.5%SF 6 /air 에서 형성된 표면막과 다른 이 막에서는 황이 검출되지 않았다 . 따라서, 0.5%SF 6 /CO 2 의 커버 가스 내의 불화물 도 막 성장 과정의 초기 단계에서 우선적으로 소모되었다. SF 6 /air 에서 형성된 막과 비교하여 SF 6 /CO 2 에서 형성된 막에서 MgO 는 나중에 나타났고 황화물은 30분 이내에 나타나지 않았다. 이는 SF 6 /air 에서 필름의 형성과 진화 가 SF 6 /CO 2 보다 빠르다 는 것을 의미할 수 있습니다 . CO 2 후속적으로 용융물과 반응하여 MgO를 형성하는 반면, 황 함유 화합물은 커버 가스에 축적되어 반응하여 매우 늦은 단계에서 황화물을 형성할 수 있습니다(산화 셀에서 30분 후).

그림 11

4 . 논의

4.1 . SF 6 /air 에서 형성된 연행 결함의 진화

Outokumpu HSC Chemistry for Windows( http://www.hsc-chemistry.net/ )의 HSC 소프트웨어를 사용하여 갇힌 기체와 액체 AZ91 합금 사이에서 발생할 수 있는 반응을 탐색하는 데 필요한 열역학 계산을 수행했습니다. 계산에 대한 솔루션은 소량의 커버 가스(즉, 갇힌 기포 내의 양)와 AZ91 합금 용융물 사이의 반응 과정에서 어떤 생성물이 가장 형성될 가능성이 있는지 제안합니다.

실험에서 압력은 1기압으로, 온도는 700°C로 설정했습니다. 커버 가스의 사용량은 7 × 10으로 가정 하였다 -7  약 0.57 cm의 양으로 kg 3 (3.14 × 10 -6  0.5 % SF위한 kmol) 6 / 공기, 0.35 cm (3) (3.12 × 10 – 8  kmol) 0.5%SF 6 /CO 2 . 포획된 가스와 접촉하는 AZ91 합금 용융물의 양은 모든 반응을 완료하기에 충분한 것으로 가정되었습니다. SF 6 의 분해 생성물 은 SF 5 , SF 4 , SF 3 , SF 2 , F 2 , S(g), S 2(g) 및 F(g) [57] , [58] , [59] , [60] .

그림 12 는 AZ91 합금과 0.5%SF 6 /air 사이의 반응에 대한 열역학적 계산의 평형 다이어그램을 보여줍니다 . 다이어그램에서 10 -15  kmol 미만의 반응물 및 생성물은 표시되지 않았습니다. 이는 존재 하는 SF 6 의 양 (≈ 1.57 × 10 -10  kmol) 보다 5배 적 으므로 영향을 미치지 않습니다. 실제적인 방법으로 과정을 관찰했습니다.

그림 12

이 반응 과정은 3단계로 나눌 수 있다.

1단계 : 불화물의 형성. AZ91 용융물은 SF 6 및 그 분해 생성물과 우선적으로 반응하여 MgF 2 , AlF 3 및 ZnF 2 를 생성 합니다. 그러나 ZnF 2 의 양 이 너무 적어서 실제적으로 검출되지  않았을 수 있습니다(  MgF 2 의 3 × 10 -10 kmol에 비해 ZnF 2 1.25 × 10 -12 kmol ). 섹션 3.1 – 3.3에 표시된 모든 산화막 . 한편, 잔류 가스에 황이 SO 2 로 축적되었다 .

2단계 : 산화물의 형성. 액체 AZ91 합금이 포획된 가스에서 사용 가능한 모든 불화물을 고갈시킨 후, Mg와의 반응으로 인해 AlF 3 및 ZnF 2 의 양이 빠르게 감소했습니다. O 2 (g) 및 SO 2 는 AZ91 용융물과 반응하여 MgO, Al 2 O 3 , MgAl 2 O 4 , ZnO, ZnSO 4 및 MgSO 4 를 형성 합니다. 그러나 ZnO 및 ZnSO 4 의 양은 EDS에 의해 실제로 발견되기에는 너무 적었을 것입니다(예: 9.5 × 10 -12  kmol의 ZnO, 1.38 × 10 -14  kmol의 ZnSO 4 , 대조적으로 4.68 × 10−10  kmol의 MgF 2 , X 축의 AZ91 양 이 2.5 × 10 -9  kmol일 때). 실험 사례에서 커버 가스의 F 농도는 매우 낮고 전체 농도 f O는 훨씬 높습니다. 따라서 1단계와 2단계, 즉 불화물과 산화물의 형성은 반응 초기에 동시에 일어나 그림 1과 2와 같이 불화물과 산화물의 가수층 혼합물이 형성될 수 있다 . 4 및 10 (a). 내부 층은 산화물로 구성되어 있지만 불화물은 커버 가스에서 F 원소가 완전히 고갈된 후에 형성될 수 있습니다.

단계 1-2는 도 10 에 도시 된 다층 구조의 형성 과정을 이론적으로 검증하였다 .

산화막 내의 MgAl 2 O 4 및 Al 2 O 3 의 양은 도 4에 도시된 산화막과 일치하는 검출하기에 충분한 양이었다 . 그러나, 도 10 에 도시된 바와 같이, 산화셀에서 성장된 산화막에서는 알루미늄의 존재를 인식할 수 없었다 . 이러한 Al의 부재는 표면 필름과 AZ91 합금 용융물 사이의 다음 반응으로 인한 것일 수 있습니다.(1)

Al 2 O 3  + 3Mg + = 3MgO + 2Al, △G(700°C) = -119.82 kJ/mol(2)

Mg + MgAl 2 O 4  = MgO + Al, △G(700°C) = -106.34 kJ/mol이는 반응물이 서로 완전히 접촉한다는 가정 하에 열역학적 계산이 수행되었기 때문에 HSC 소프트웨어로 시뮬레이션할 수 없었습니다. 그러나 실제 공정에서 AZ91 용융물과 커버 가스는 보호 표면 필름의 존재로 인해 서로 완전히 접촉할 수 없습니다.

3단계 : 황화물과 질화물의 형성. 30분의 유지 시간 후, 산화 셀의 기상 불화물 및 산화물이 고갈되어 잔류 가스와 용융 반응을 허용하여 초기 F-농축 또는 (F, O )이 풍부한 표면 필름, 따라서 그림 10 (b 및 c)에 표시된 관찰된 다층 구조를 생성합니다 . 게다가, 질소는 모든 반응이 완료될 때까지 AZ91 용융물과 반응했습니다. 도 6 에 도시 된 산화막 은 질화물 함량으로 인해 이 반응 단계에 해당할 수 있다. 그러나, 그 결과는 도 1 및 도 5에 도시 된 연마된 샘플에서 질화물이 검출되지 않음을 보여준다. 4 와 5, 그러나 테스트 바 파단면에서만 발견됩니다. 질화물은 다음과 같이 샘플 준비 과정에서 가수분해될 수 있습니다 [54] .(삼)

Mg 3 N 2  + 6H 2 O = 3Mg(OH) 2  + 2NH 3 ↑(4)

AlN+ 3H 2 O = Al(OH) 3  + NH 3 ↑

또한 Schmidt et al. [61] 은 Mg 3 N 2 와 AlN이 반응하여 3원 질화물(Mg 3 Al n N n+2, n=1, 2, 3…) 을 형성할 수 있음을 발견했습니다 . HSC 소프트웨어에는 삼원 질화물 데이터베이스가 포함되어 있지 않아 계산에 추가할 수 없습니다. 이 단계의 산화막은 또한 삼원 질화물을 포함할 수 있습니다.

4.2 . SF 6 /CO 2 에서 형성된 연행 결함의 진화

도 13 은 AZ91 합금과 0.5%SF 6 /CO 2 사이의 열역학적 계산 결과를 보여준다 . 이 반응 과정도 세 단계로 나눌 수 있습니다.

그림 13

1단계 : 불화물의 형성. SF 6 및 그 분해 생성물은 AZ91 용융물에 의해 소비되어 MgF 2 , AlF 3 및 ZnF 2 를 형성했습니다 . 0.5% SF 6 /air 에서 AZ91의 반응에서와 같이 ZnF 2 의 양 이 너무 작아서 실제적으로 감지되지  않았습니다( 2.67 x 10 -10  kmol의 MgF 2 에 비해 ZnF 2 1.51 x 10 -13 kmol ). S와 같은 잔류 가스 트랩에 축적 유황 2 (g) 및 (S)의 일부분 (2) (g)가 CO와 반응하여 2 SO 형성하는 2및 CO. 이 반응 단계의 생성물은 도 11 (a)에 도시된 필름과 일치하며 , 이는 불화물만을 함유하는 단일 층 구조를 갖는다.

2단계 : 산화물의 형성. ALF 3 및 ZnF 2 MgF로 형성 용융 AZ91 마그네슘의 반응 2 , Al 및 Zn으로한다. SO 2 는 소모되기 시작하여 표면 필름에 산화물을 생성 하고 커버 가스에 S 2 (g)를 생성했습니다. 한편, CO 2 는 AZ91 용융물과 직접 반응하여 CO, MgO, ZnO 및 Al 2 O 3 를 형성 합니다. 도 1에 도시 된 산화막 9 및 11 (b)는 산소가 풍부한 층과 다층 구조로 인해 이 반응 단계에 해당할 수 있습니다.

커버 가스의 CO는 AZ91 용융물과 추가로 반응하여 C를 생성할 수 있습니다. 이 탄소는 온도가 감소할 때(응고 기간 동안) Mg와 추가로 반응하여 Mg 탄화물을 형성할 수 있습니다 [62] . 이것은 도 4에 도시된 산화막의 탄소 함량이 높은 이유일 수 있다 8 – 9 . Liang et al. [39] 또한 SO 2 /CO 2 로 보호된 AZ91 합금 표면 필름에서 탄소 검출을 보고했습니다 . 생성된 Al 2 O 3 는 MgO와 더 결합하여 MgAl 2 O [63]를 형성할 수 있습니다 . 섹션 4.1 에서 논의된 바와 같이, 알루미나 및 스피넬은 도 11 에 도시된 바와 같이 표면 필름에 알루미늄 부재를 야기하는 Mg와 반응할 수 있다 .

3단계 : 황화물의 형성. AZ91은 용융물 S 소비하기 시작 2 인 ZnS와 MGS 형성 갇힌 잔류 가스 (g)를. 이러한 반응은 반응 과정의 마지막 단계까지 일어나지 않았으며, 이는 Fig. 7 (c)에 나타난 결함의 S-함량 이 적은 이유일 수 있다 .

요약하면, 열역학적 계산은 AZ91 용융물이 커버 가스와 반응하여 먼저 불화물을 형성한 다음 마지막에 산화물과 황화물을 형성할 것임을 나타냅니다. 다른 반응 단계에서 산화막은 다른 구조와 조성을 가질 것입니다.

4.3 . 운반 가스가 동반 가스 소비 및 AZ91 주물의 재현성에 미치는 영향

SF 6 /air 및 SF 6 /CO 2 에서 형성된 연행 결함의 진화 과정은 4.1절 과 4.2  에서 제안되었습니다 . 이론적인 계산은 실제 샘플에서 발견되는 해당 산화막과 관련하여 검증되었습니다. 연행 결함 내의 대기는 Al-합금 시스템과 다른 시나리오에서 액체 Mg-합금과의 반응으로 인해 효율적으로 소모될 수 있습니다(즉, 연행된 기포의 질소가 Al-합금 용융물과 효율적으로 반응하지 않을 것입니다 [64 , 65] 그러나 일반적으로 “질소 연소”라고 하는 액체 Mg 합금에서 질소가 더 쉽게 소모될 것입니다 [66] ).

동반된 가스와 주변 액체 Mg-합금 사이의 반응은 동반된 가스를 산화막 내에서 고체 화합물(예: MgO)로 전환하여 동반 결함의 공극 부피를 감소시켜 결함(예: 공기의 동반된 가스가 주변의 액체 Mg 합금에 의해 고갈되면 용융 온도가 700 °C이고 액체 Mg 합금의 깊이가 10 cm라고 가정할 때 최종 고체 제품의 총 부피는 0.044가 됩니다. 갇힌 공기가 취한 초기 부피의 %).

연행 결함의 보이드 부피 감소와 해당 주조 특성 사이의 관계는 알루미늄 합금 주조에서 널리 연구되었습니다. Nyahumwa와 Campbell [16] 은 HIP(Hot Isostatic Pressing) 공정이 Al-합금 주물의 연행 결함이 붕괴되고 산화물 표면이 접촉하게 되었다고 보고했습니다. 주물의 피로 수명은 HIP 이후 개선되었습니다. Nyahumwa와 Campbell [16] 도 서로 접촉하고 있는 이중 산화막의 잠재적인 결합을 제안했지만 이를 뒷받침하는 직접적인 증거는 없었습니다. 이 결합 현상은 Aryafar et.al에 의해 추가로 조사되었습니다. [8], 그는 강철 튜브에서 산화물 스킨이 있는 두 개의 Al-합금 막대를 다시 녹인 다음 응고된 샘플에 대해 인장 강도 테스트를 수행했습니다. 그들은 Al-합금 봉의 산화물 스킨이 서로 강하게 결합되어 용융 유지 시간이 연장됨에 따라 더욱 강해짐을 발견했으며, 이는 이중 산화막 내 동반된 가스의 소비로 인한 잠재적인 “치유” 현상을 나타냅니다. 구조. 또한 Raidszadeh와 Griffiths [9 , 19] 는 연행 가스가 반응하는 데 더 긴 시간을 갖도록 함으로써 응고 전 용융 유지 시간을 연장함으로써 Al-합금 주물의 재현성에 대한 연행 결함의 부정적인 영향을 성공적으로 줄였습니다. 주변이 녹습니다.

앞서 언급한 연구를 고려할 때, Mg 합금 주물에서 혼입 가스의 소비는 다음 두 가지 방식으로 혼입 결함의 부정적인 영향을 감소시킬 수 있습니다.

(1) 이중 산화막의 결합 현상 . 도 5 및 도 7 에 도시 된 샌드위치형 구조 는 이중 산화막 구조의 잠재적인 결합을 나타내었다. 그러나 산화막의 결합으로 인한 강도 증가를 정량화하기 위해서는 더 많은 증거가 필요합니다.

(2) 연행 결함의 보이드 체적 감소 . 주조품의 품질에 대한 보이드 부피 감소의 긍정적인 효과는 HIP 프로세스 [67]에 의해 널리 입증되었습니다 . 섹션 4.1 – 4.2 에서 논의된 진화 과정과 같이 , 동반된 가스와 주변 AZ91 합금 용융물 사이의 지속적인 반응으로 인해 동반 결함의 산화막이 함께 성장할 수 있습니다. 최종 고체 생성물의 부피는 동반된 기체에 비해 상당히 작았다(즉, 이전에 언급된 바와 같이 0.044%).

따라서, 혼입 가스의 소모율(즉, 산화막의 성장 속도)은 AZ91 합금 주물의 품질을 향상시키는 중요한 매개변수가 될 수 있습니다. 이에 따라 산화 셀의 산화막 성장 속도를 추가로 조사했습니다.

도 14 는 상이한 커버 가스(즉, 0.5%SF 6 /air 및 0.5%SF 6 /CO 2 ) 에서의 표면 필름 성장 속도의 비교를 보여준다 . 필름 두께 측정을 위해 각 샘플의 15개의 임의 지점을 선택했습니다. 95% 신뢰구간(95%CI)은 막두께의 변화가 가우시안 분포를 따른다는 가정하에 계산하였다. 0.5%SF 6 /air 에서 형성된 모든 표면막이 0.5%SF 6 /CO 2 에서 형성된 것보다 빠르게 성장함을 알 수 있다 . 다른 성장률은 0.5%SF 6 /air 의 연행 가스 소비율 이 0.5%SF 6 /CO 2 보다 더 높음 을 시사했습니다., 이는 동반된 가스의 소비에 더 유리했습니다.

그림 14

산화 셀에서 액체 AZ91 합금과 커버 가스의 접촉 면적(즉, 도가니의 크기)은 많은 양의 용융물과 가스를 고려할 때 상대적으로 작았다는 점에 유의해야 합니다. 결과적으로, 산화 셀 내에서 산화막 성장을 위한 유지 시간은 비교적 길었다(즉, 5-30분). 하지만, 실제 주조에 함유 된 혼입 결함은 (상대적으로 매우 적은, 즉, 수 미크론의 크기에 도시 된 바와 같이 ,도 3. – 6 및 [7]), 동반된 가스는 주변 용융물로 완전히 둘러싸여 상대적으로 큰 접촉 영역을 생성합니다. 따라서 커버 가스와 AZ91 합금 용융물의 반응 시간은 비교적 짧을 수 있습니다. 또한 실제 Mg 합금 모래 주조의 응고 시간은 몇 분일 수 있습니다(예: Guo [68] 은 직경 60mm의 Mg 합금 모래 주조가 응고되는 데 4분이 필요하다고 보고했습니다). 따라서 Mg-합금 용융주조 과정에서 포획된 동반된 가스는 특히 응고 시간이 긴 모래 주물 및 대형 주물의 경우 주변 용융물에 의해 쉽게 소모될 것으로 예상할 수 있습니다.

따라서, 동반 가스의 다른 소비율과 관련된 다른 커버 가스(0.5%SF 6 /air 및 0.5%SF 6 /CO 2 )가 최종 주물의 재현성에 영향을 미칠 수 있습니다. 이 가정을 검증하기 위해 0.5%SF 6 /air 및 0.5%SF 6 /CO 2 에서 생산된 AZ91 주물 을 기계적 평가를 위해 테스트 막대로 가공했습니다. Weibull 분석은 선형 최소 자승(LLS) 방법과 비선형 최소 자승(비 LLS) 방법을 모두 사용하여 수행되었습니다 [69] .

그림 15 (ab)는 LLS 방법으로 얻은 UTS 및 AZ91 합금 주물의 연신율의 전통적인 2-p 선형 Weibull 플롯을 보여줍니다. 사용된 추정기는 P= (i-0.5)/N이며, 이는 모든 인기 있는 추정기 중 가장 낮은 편향을 유발하는 것으로 제안되었습니다 [69 , 70] . SF 6 /air 에서 생산된 주물 은 UTS Weibull 계수가 16.9이고 연신율 Weibull 계수가 5.0입니다. 대조적으로, SF 6 /CO 2 에서 생산된 주물의 UTS 및 연신 Weibull 계수는 각각 7.7과 2.7로, SF 6 /CO 2 에 의해 보호된 주물의 재현성이 SF 6 /air 에서 생산된 것보다 훨씬 낮음을 시사합니다. .

그림 15

또한 저자의 이전 출판물 [69] 은 선형화된 Weibull 플롯의 단점을 보여주었으며, 이는 Weibull 추정 의 더 높은 편향과 잘못된 2 중단을 유발할 수 있습니다 . 따라서 그림 15 (cd) 와 같이 Non-LLS Weibull 추정이 수행되었습니다 . SF 6 /공기주조물 의 UTS Weibull 계수 는 20.8인 반면, SF 6 /CO 2 하에서 생산된 주조물의 UTS Weibull 계수는 11.4로 낮아 재현성에서 분명한 차이를 보였다. 또한 SF 6 /air elongation(El%) 데이터 세트는 SF 6 /CO 2 의 elongation 데이터 세트보다 더 높은 Weibull 계수(모양 = 5.8)를 가졌습니다.(모양 = 3.1). 따라서 LLS 및 Non-LLS 추정 모두 SF 6 /공기 주조가 SF 6 /CO 2 주조 보다 더 높은 재현성을 갖는다고 제안했습니다 . CO 2 대신 공기를 사용 하면 혼입된 가스의 더 빠른 소비에 기여하여 결함 내의 공극 부피를 줄일 수 있다는 방법을 지원합니다 . 따라서 0.5%SF 6 /CO 2 대신 0.5%SF 6 /air를 사용 하면(동반된 가스의 소비율이 증가함) AZ91 주물의 재현성이 향상되었습니다.

그러나 모든 Mg 합금 주조 공장이 현재 작업에서 사용되는 주조 공정을 따랐던 것은 아니라는 점에 유의해야 합니다. Mg의 합금 용탕 본 작업은 탈기에 따라서, 동반 가스의 소비에 수소의 영향을 감소 (즉, 수소 잠재적 동반 가스의 고갈 억제, 동반 된 기체로 확산 될 수있다 [7 , 71 , 72] ). 대조적으로, 마그네슘 합금 주조 공장에서는 마그네슘을 주조할 때 ‘가스 문제’가 없고 따라서 인장 특성에 큰 변화가 없다고 널리 믿어지기 때문에 마그네슘 합금 용융물은 일반적으로 탈기되지 않습니다 [73] . 연구에 따르면 Mg 합금 주물의 기계적 특성에 대한 수소의 부정적인 영향 [41 ,42 , 73] , 탈기 공정은 마그네슘 합금 주조 공장에서 여전히 인기가 없습니다.

또한 현재 작업에서 모래 주형 공동은 붓기 전에 SF 6 커버 가스 로 플러싱되었습니다 [22] . 그러나 모든 Mg 합금 주조 공장이 이러한 방식으로 금형 캐비티를 플러싱한 것은 아닙니다. 예를 들어, Stone Foundry Ltd(영국)는 커버 가스 플러싱 대신 유황 분말을 사용했습니다. 그들의 주물 내의 동반된 가스 는 보호 가스라기 보다는 SO 2 /공기일 수 있습니다 .

따라서 본 연구의 결과는 CO 2 대신 공기를 사용 하는 것이 최종 주조의 재현성을 향상시키는 것으로 나타났지만 다른 산업용 Mg 합금 주조 공정과 관련하여 캐리어 가스의 영향을 확인하기 위해서는 여전히 추가 조사가 필요합니다.

7 . 결론

1.

AZ91 합금에 형성된 연행 결함이 관찰되었습니다. 그들의 산화막은 단층과 다층의 두 가지 유형의 구조를 가지고 있습니다. 다층 산화막은 함께 성장하여 최종 주조에서 샌드위치 같은 구조를 형성할 수 있습니다.2.

실험 결과와 이론적인 열역학적 계산은 모두 갇힌 가스의 불화물이 황을 소비하기 전에 고갈되었음을 보여주었습니다. 이중 산화막 결함의 3단계 진화 과정이 제안되었습니다. 산화막은 진화 단계에 따라 다양한 화합물 조합을 포함했습니다. SF 6 /air 에서 형성된 결함 은 SF 6 /CO 2 에서 형성된 것과 유사한 구조를 갖지만 산화막의 조성은 달랐다. 엔트레인먼트 결함의 산화막 형성 및 진화 과정은 이전에 보고된 Mg 합금 표면막(즉, MgF 2 이전에 형성된 MgO)의 것과 달랐다 .삼.

산화막의 성장 속도는 SF하에 큰 것으로 입증되었다 (6) / SF보다 공기 6 / CO 2 손상 봉입 가스의 빠른 소비에 기여한다. AZ91 합금 주물의 재현성은 SF 6 /CO 2 대신 SF 6 /air를 사용할 때 향상되었습니다 .

감사의 말

저자는 EPSRC LiME 보조금 EP/H026177/1의 자금 지원 과 WD Griffiths 박사와 Adrian Carden(버밍엄 대학교)의 도움을 인정합니다. 주조 작업은 University of Birmingham에서 수행되었습니다.

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Figures-Effects of sinusoidal oscillating laser beam on weld formation, melt flow and grain structure during aluminum alloys lap welding

알루미늄 합금 겹침 용접 중 용접 형성, 용융 흐름 및 입자 구조에 대한 사인파 발진 레이저 빔의 영향

Effects of sinusoidal oscillating laser beam on weld formation, melt flow and grain structure during aluminum alloys lap welding

Lin Chen, Gaoyang Mi, Xiong Zhang, Chunming Wang
School of Materials Science and Engineering, Huazhong University of Science and Technology, Wuhan, 430074, China

Abstract

레이저 사인파 진동(사인) 용접 및 레이저 용접(SLW)에서 1.5mm 6061/5182 알루미늄 합금 박판 랩 조인트의 수치 모델이 온도 분포와 용융 흐름을 시뮬레이션하기 위해 개발되었습니다.

SLW의 일반적인 에너지 분포와 달리 레이저 빔의 사인파 진동은 에너지 분포를 크게 균질화하고 에너지 피크를 줄였습니다. 에너지 피크는 사인 용접의 양쪽에 위치하여 톱니 모양의 단면이 형성되었습니다. 이 논문은 시뮬레이션을 통해 응고 미세구조에 대한 온도 구배(G)와 응고 속도(R)의 영향을 설명했습니다.

결과는 사인 용접의 중심이 낮은 G/R로 더 넓은 영역을 가짐으로써 더 넓은 등축 결정립 영역의 형성을 촉진하고 더 큰 GR로 인해 주상 결정립이 더 가늘다는 것을 나타냅니다. 다공성 및 비관통 용접은 레이저 사인파 진동에 의해 얻어졌습니다.

그 이유는 용융 풀의 부피가 확대되고 열쇠 구멍의 부피 비율이 감소하며 용융 풀의 난류가 완만해졌기 때문이며, 이는 용융 흐름의 고속 이미징 및 시뮬레이션 결과에서 관찰되었습니다. 두 용접부의