The effects of annealing on the microstructure and mechanical properties of Al–Zn–Mg–Cu–Si alloys fabricated by high-energy ball milling (HEBM) and spark plasma sintering (SPS) were investigated. The HEBM-free sintered alloy primarily contained Mg₂Si, Q-AlCuMgSi, and Si phases. Meanwhile, the HEBM-sintered alloy contains Mg-free Si and θ-Al₂Cu phases due to the formation of MgO, which causes Mg depletion in the Al matrix. Annealing without and with HEBM at 500°C causes partial dissolution and coarsening of the Q-AlCuMgSi and Mg₂Si phases in the alloy and dissolution of the θ-Al₂Cu phase in the alloy, respectively. In both alloys, a thermally stable α-AlFeSi phase was formed after long-term heat treatment. The grain size of the sintered alloys with and without HEBM increased from 0.5 to 1.0 μm and from 2.9 to 6.3 μm, respectively. The hardness of the sintered alloy increases after annealing for 1 h but decreases significantly after 24 h of annealing. Extending the annealing time to 168 h improved the hardness of the alloy without HEBM but had little effect on the alloy with HEBM. The relationship between the microstructural factors and the hardness of the sintered and annealed alloys is discussed.

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• Microstructural evolution and thermal stability of Al–Zn–Mg–Cu–Si–Zr alloy fabricated via spark plasma sintering
  Junho Lee, Seonghyun Park, Sang-Hwa Lee, Seung Bae Son, Hanjung Kwon, Seok-Jae Lee, Jae-Gil Jung
  Journal of Materials Research and Technology.2024; 31: 205.     CrossRef

In this study, machine learning models are proposed to predict the Vickers hardness of AlSi10Mg alloys fabricated by laser powder bed fusion (LPBF). A total of 113 utilizable datasets were collected from the literature. The hyperparameters of the machine-learning models were adjusted to select an accurate predictive model. The random forest regression (RFR) model showed the best performance compared to support vector regression, artificial neural networks, and k-nearest neighbors. The variable importance and prediction mechanisms of the RFR were discussed by Shapley additive explanation (SHAP). Aging time had the greatest influence on the Vickers hardness, followed by solution time, solution temperature, layer thickness, scan speed, power, aging temperature, average particle size, and hatching distance. Detailed prediction mechanisms for RFR are analyzed using SHAP dependence plots.

We investigate the austenite stability in nanocrystalline Fe-7%Mn-X%Mo (X = 0, 1, and 2) alloys fabricated by spark plasma sintering. Mo is known as a ferrite stabilizing element, whereas Mn is an austenite stabilizing element, and many studies have focused on the effect of Mn addition on austenite stability. Herein, the volume fraction of austenite in nanocrystalline Fe-7%Mn alloys with different Mo contents is measured using X-ray diffraction. Using a disk compressive test, austenite in Fe–Mn–Mo alloys is confirmed to transform into strain-induced martensite during plastic deformation by a disk d. The variation in austenite stability in response to the addition of Mo is quantitatively evaluated by comparing the k-parameters of the kinetic equation for the strain-induced martensite transformation.

Soft magnetic powder materials are used throughout industries such as motors and power converters. When manufacturing Fe-based soft magnetic composites, the size and shape of the soft magnetic powder and the microstructure in the powder are closely related to the magnetic properties. In this study, Fe-Si-Al-P alloy powders were manufactured using various manufacturing process parameter sets, and the process parameters of the vacuum induction melt gas atomization process were set as melt temperature, atomization gas pressure, and gas flow rate. Process variable data that records are converted into 6 types of data for each powder recovery section. Process variable data that recorded minute changes were converted into 6 types of data and used as input variables. As output variables, a total of 6 types were designated by measuring the particle size, flowability, apparent density, and sphericity of the manufactured powders according to the process variable conditions. The sensitivity of the input and output variables was analyzed through the Pearson correlation coefficient, and a total of 6 powder characteristics were analyzed by artificial neural network model. The prediction results were compared with the results through linear regression analysis and response surface methodology, respectively.

Changes in the mechanical properties and microstructure of an IN 939 W alloy according to the sintering heating rate were evaluated. IN 939 W alloy samples were fabricated by spark plasma sintering. The phase fraction, number density, and mean radius of the IN 939W alloy were calculated using a thermodynamic calculation. A universal testing machine and micro-Vickers hardness tester were employed to confirm the mechanical properties of the IN 939W alloy. X-ray diffraction, optical microscopy, field-emission scanning electron microscopy, Cs-corrected-field emission transmission electron microscopy, and energy dispersive X-ray spectrometry were used to evaluate the microstructure of the alloy. The rapid sintering heating rate resulted in a slightly dispersed γ' phase and chromium oxide. It also suppressed the precipitation of the η phase. These helped to reinforce the mechanical properties.

A typical trade-off relationship exists between strength and elongation in face-centered cubic metals. Studies have recently been conducted to enhance strength without ductility reduction through surface-treatment-based ultrasonic nanocrystalline surface modification (UNSM), which creates a gradient microstructure in which grains become smaller from the inside to the surface. The transformation-induced plasticity effect in Fe-Mn alloys results in excellent strength and ductility due to their high work-hardening rate. This rate is achieved through strain-induced martensitic transformation when an alloy is plastically deformed. In this study, Fe-6%Mn powders with different sizes were prepared by high-energy ball milling and sintered through spark plasma sintering to produce Fe-6%Mn samples. A gradient microstructure was obtained by stacking the different-sized powders to achieve similar effects as those derived from UNSM. A compressive test was performed to investigate the mechanical properties, including the yielding behavior. The deformed microstructure was observed through electron backscatter diffraction to determine the effects of gradient plastic deformation.

Novel Ni- and Fe-based alloys are developed to impart improved mechanical properties and corrosion resistance. The designed alloys are manufactured as a powder and deposited on a steel substrate using a high-velocity oxygen-fuel process. The coating layer demonstrates good corrosion resistance, and the thus-formed passive film is beneficial because of the Cr contained in the alloy system. Furthermore, during low-temperature heat treatment, factors that deteriorate the properties and which may arise during high-temperature heat treatment, are avoided. For the heattreated coating layers, the hardness increases by up to 32% and the corrosion resistance improves. The influence of the heat treatment is investigated through various methods and is considered to enhance the mechanical properties and corrosion resistance of the coating layer.

An alternative fabrication method for carburizing steel using spark plasma sintering (SPS) is investigated. The sintered carburized sample, which exhibits surface modification effects such as carburizing, sintered Fe, and sintered Fe–0.8 wt.%C alloys, is fabricated using SPS. X-ray diffraction and micro Vickers tests are employed to confirm the phase and properties. Finite element analysis is performed to evaluate the change in hardness and analyze the carbon content and residual stress of the carburized sample. The change in the hardness of the carburized sample has the same tendency to predict hardness. The difference in hardness between the carburized sample and the predicted value is also discussed. The carburized sample exhibits a compressive residual stress at the surface. These results indicate that the carburized sample experiences a surface modification effect without carburization. Field emission scanning electron microscopy is employed to verify the change in phase. A novel fabrication method for altering the carburization is successfully proposed. We expect this fabrication method to solve the problems associated with carburization.

A new Fe-Cr-Mo-B-C amorphous alloy is designed, which offers high mechanical strength, corrosion resistance as well as high glass-forming ability and its gas-atomized amorphous powder is deposited on an ASTM A213-T91 steel substrate using the high-velocity oxygen fuel (HVOF) process. The hybrid coating layer, consisting of nanocrystalline and amorphous phases, exhibits strong bonding features with the substrate, without revealing significant pore formation. By the coating process, it is possible to obtain a dense structure in which pores are hardly observed not only inside the coating layer but also at the interface between the coating layer and the substrate. The coating layer exhibits good adhesive strength as well as good wear resistance, making it suitable for coating layers for biomass applications.

The effect of the process conditions of high-velocity oxygen fuel (HVOF) thermal spray coating on the porosity of the coating layer is investigated. HVOF coating layers are formed by depositing amorphous FeMoCrBC powder. Oxygen pressure varies from 126 to 146 psi and kerosene pressure from 110 to 130 psi. The Microstructural analysis confirms its porosity. Data analysis is performed using experimental data. The oxygen pressure-kerosene pressure ratio is found to be a key contributor to the porosity. An empirical model is proposed using linear regression analysis. The proposed model is then validated using additional test data. We confirm that the oxygen pressure-kerosene pressure ratio exponentially increases porosity. We present a porosity prediction model relationship for the oxygen pressure-kerosene pressure ratio.

In this study, a nanocrystalline FeNiCrMoMnSiC alloy was fabricated, and its austenite stability, microstructure, and mechanical properties were investigated. A sintered FeNiCrMoMnSiC alloy sample with nanosized crystal was obtained by high-energy ball milling and spark plasma sintering. The sintering behavior was investigated by measuring the displacement according to the temperature of the sintered body. Through microstructural analysis, it was confirmed that a compact sintered body with few pores was produced, and cementite was formed. The stability of the austenite phase in the sintered samples was evaluated by X-ray diffraction analysis and electron backscatter diffraction. Results revealed a measured value of 51.6% and that the alloy had seven times more austenite stability than AISI 4340 wrought steel. The hardness of the sintered alloy was 60.4 HRC, which was up to 2.4 times higher than that of wrought steel.

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• Microstructure and mechanical behavior of AISI 4340 steel fabricated via spark plasma sintering and post-heat treatment
  Jungbin Park, Junhyub Jeon, Namhyuk Seo, Singon Kang, Seung Bae Son, Seok-Jae Lee, Jae-Gil Jung
  Materials Science and Engineering: A.2023; 862: 144433.     CrossRef

The effect of sintering conditions on the austenite stability and strain-induced martensitic transformation of nanocrystalline FeCrC alloy is investigated. Nanocrystalline FeCrC alloys are successfully fabricated by spark plasma sintering with an extremely short densification time to obtain the theoretical density value and prevent grain growth. The nanocrystallite size in the sintered alloys contributes to increased austenite stability. The phase fraction of the FeCrC sintered alloy before and after deformation according to the sintering holding time is measured using X-ray diffraction and electron backscatter diffraction analysis. During compressive deformation, the volume fraction of strain-induced martensite resulting from austenite decomposition is increased. The transformation kinetics of the strain-induced martensite is evaluated using an empirical equation considering the austenite stability factor. The hardness of the S0W and S10W samples increase to 62.4-67.5 and 58.9-63.4 HRC before and after deformation. The hardness results confirmed that the mechanical properties are improved owing to the effects of grain refinement and strain-induced martensitic transformation in the nanocrystalline FeCrC alloy.

We fabricate the non-equiatomic high-entropy alloy (NE-HEA) Fe_49.5Mn₃₀Co₁₀Cr₁₀C_0.5 (at.%) using spark plasma sintering under various sintering conditions. Each elemental pure powder is milled by high-energy ball milling to prepare NE-HEA powder. The microstructure and mechanical properties of the sintered samples are investigated using various methods. We use the X-ray diffraction (XRD) method to investigate the microstructural characteristics. Quantitative phase analysis is performed by direct comparison of the XRD results. A tensile test is used to compare the mechanical properties of small samples. Next, electron backscatter diffraction analysis is performed to analyze the phase fraction, and the results are compared to those of XRD analysis. By combining different sintering durations and temperature conditions, we attempt to identify suitable spark plasma sintering conditions that yield mechanical properties comparable with previously reported values. The samples sintered at 900 and 1000°C with no holding time have a tensile strength of over 1000 MPa.

High-entropy alloys have excellent mechanical properties under extreme environments, rendering them promising candidates for next-generation structural materials. It is desirable to develop non-equiatomic high-entropy alloys that do not require many expensive or heavy elements, contrary to the requirements of typical high-entropy alloys. In this study, a non-equiatomic high-entropy alloy powder Fe_49.5Mn₃₀Co₁₀Cr₁₀C_0.5 (at.%) is prepared by high energy ball milling and fabricated by spark plasma sintering. By combining different ball milling times and ball-topowder ratios, we attempt to find a proper mechanical alloying condition to achieve improved mechanical properties. The milled powder and sintered specimens are examined using X-ray diffraction to investigate the progress of mechanical alloying and microstructural changes. A miniature tensile specimen after sintering is used to investigate the mechanical properties. Furthermore, quantitative analysis of the microstructure is performed using electron backscatter diffraction.