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• Preparation and Microstructural Characteristics of Ti Nanopowder by Ball Milling and Dehydrogenation of TiH2 Powder
  Ji Young Kim, Eui Seon Lee, Ji Won Choi, Youngmin Kim, Sung-Tag Oh
  Journal of Powder Materials.2024; 31(4): 324.     CrossRef

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

This study investigates the melting point and brazing properties of the aluminum (Al)-copper (Cu)-silicon (Si)-tin (Sn) alloy fabricated for low-temperature brazing based on the alloy design. Specifically, the Al-20Cu-10Si-Sn alloy is examined and confirmed to possess a melting point of approximately 520°C. Analysis of the melting point of the alloy based on composition reveals that the melting temperature tends to decrease with increasing Cu and Si content, along with a corresponding decrease as the Sn content rises. This study verifies that the Al-20Cu-10Si-5Sn alloy exhibits high liquidity and favorable mechanical properties for brazing through the joint gap filling test and Vickers hardness measurements. Additionally, a powder fabricated using the Al-20Cu-10Si-5Sn alloy demonstrates a melting point of around 515°C following melting point analysis. Consequently, it is deemed highly suitable for use as a low-temperature Al brazing material.

Thermite welding is an exceptional process that does not require additional energy supplies, resulting in welded joints that exhibit mechanical properties and conductivity equivalent to those of the parent materials. The global adoption of thermite welding is growing across various industries. However, in Korea, limited research is being conducted on the core technology of thermite welding. Currently, domestic production of thermite powder in Korea involves recycling copper oxide (CuO). Unfortunately, controlling the particle size of waste CuO poses challenges, leading to the unwanted formation of pores and cracks during thermite welding. In this study, we investigate the influence of powder particle size on thermite welding in the production of Cu-thermite powder using waste CuO. We conduct the ball milling process for 0.5–24 h using recycled CuO. The evolution of the powder shape and size is analyzed using particle size analysis and scanning electron microscopy (SEM). Furthermore, we examine the thermal reaction characteristics through differential scanning calorimetry. Additionally, the microstructures of the welded samples are observed using optical microscopy and SEM to evaluate the impact of powder particle size on weldability. Lastly, hardness measurements are performed to assess the strengths of the welded materials.

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• Friction Welding of Casted SCM440 and Sintered F-05-140 Dissimilar Steels and Their Joint Properties under Various Welding Conditions
  Jisung Lee, Hansung Lee, Eunhyo Song, Byungmin Ahn
  Journal of Powder Materials.2024; 31(5): 414.     CrossRef

Tungsten disulfide (WS₂) nanosheets have attracted considerable attention because of their unique optical and electrical properties. Several methods for fabrication of WS₂ nanosheets have been developed. However, methods for mass production of high-quality WS₂ nanosheets remain challenging. In this study, WS₂ nanosheets were fabricated using mechano-chemical ball milling based on the synergetic effects of chemical intercalation and mechanical exfoliation. The ball-milling time was set as a variable for the optimized fabricating process of WS₂ nanosheets. Under the optimized conditions, the WS₂ nanosheets had lateral sizes of 500–600 nm with either a monolayer or bilayer. They also exhibited high crystallinity in the 2H semiconducting phase. Thus, the proposed method can be applied to the exfoliation of other transition metal dichalcogenides using suitable chemical intercalants. It can also be used with highperformance WS₂-based photodiodes and transistors used in practical semiconductor applications.

Recently, high-entropy carbides have attracted considerable attention owing to their excellent physical and chemical properties such as high hardness, fracture toughness, and conductivity. However, as an emerging class of novel materials, the synthesis methods, performance, and applications of high-entropy carbides have ample scope for further development. In this study, equiatomic (Hf-Ti-Ta-Zr-Nb)C high-entropy carbide powders have been prepared by an ultrahigh- energy ball-milling (UHEBM) process with different milling times (1, 5, 15, 30, and 60 min). Further, their refinement behavior and high-entropy synthesis potential have been investigated. With an increase in the milling time, the particle size rapidly reduces (under sub-micrometer size) and homogeneous mixing of the prepared powder is observed. The distortions in the crystal lattice, which occur as a result of the refinement process and the multicomponent effect, are found to improve the sintering, thereby notably enhancing the formation of a single-phase solid solution (high-entropy). Herein, we present a procedure for the bulk synthesis of highly pure, dense, and uniform FCC single-phase (Fm3m crystal structure) (Hf-Ti-Ta-Zr-Nb)C high-entropy carbide using a milling time of 60 min and a sintering temperature of 1,600°C.

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• Controlling Particle Size of Recycled Copper Oxide Powder for Copper Thermite Welding Characteristics
  Hansung Lee, Minsu Kim, Byungmin Ahn
  journal of Korean Powder Metallurgy Institute.2023; 30(4): 332.     CrossRef

Tin/graphite composites are prepared as anode materials for Li-ion batteries using a dry ball-milling process. The main experimental variables in this work are the ball milling time (0–8 h) and composition ratio (tin:graphite=5:95, 15:85, and 30:70 w/w) of graphite and tin powder. For comparison, a tin/graphite composite is prepared using wet ball milling. The morphology and structure of the different tin/graphite composites are investigated using X-ray diffraction, Raman spectroscopy, energy-dispersive X-ray spectroscopy, and scanning and transmission electron microscopy. The electrochemical properties of the samples are also examined. The optimal dry ball milling time for the uniform mixing of graphite and tin is 6 h in a graphite-30wt.%Sn sample. The electrode prepared from the composite that is dry-ballmilled for 6 h exhibits the best cycle performance (discharge capacity after 50^th cycle: 308 mAh/g and capacity retention: 46%). The discharge capacity after the 50^th cycle is approximately 112 mAh/g, higher than that when the electrode is composed of only graphite (196 mAh/g after 50^th cycle). This result indicates that it is possible to manufacture a tin/graphite composite anode material that can effectively buffer the volume change that occurs during cycling, even using a simple dry ball-milling process.

In this study, Ti-Mo-EB composites are prepared by ball milling and spark plasma sintering (SPS) to obtain a low elastic modulus and high strength and to evaluate the microstructure and mechanical properties as a function of the process conditions. As the milling time and sintering temperature increased, Mo, as a β-Ti stabilizing element, diffused, and the microstructure of β-Ti increased. In addition, the size of the observed phase was small, so the modulus and hardness of α-Ti and β-Ti were measured using nanoindentation equipment. In both phases, as the milling time and sintering temperature increased, the modulus of elasticity decreased, and the hardness increased. After 12 h of milling, the specimen sintered at 1000°C showed the lowest values of modulus of elasticity of 117.52 and 101.46 GPa for α-Ti and β-Ti, respectively, confirming that the values are lower compared to the that in previously reported studies.

Oxide dispersion-strengthened (ODS) steel has excellent high-temperature properties, corrosion resistance, and oxidation resistance, and is expected to be applicable in various fields. Recently, various studies on mechanical alloying (MA) have been conducted for the dispersion of oxide particles in ODS steel with a high number density. In this study, ODS steel is manufactured by introducing a complex milling process in which planetary ball milling, cryogenic ball milling, and drum ball milling are sequentially performed, and the microstructure and high-temperature mechanical properties of the ODS steel are investigated. The microstructure observation revealed that the structure is stretched in the extrusion direction, even after the heat treatment. In addition, transmission electron microscopy (TEM) analysis confirmed the presence of oxide particles in the range of 5 to 10 nm. As a result of the room-temperature and high-temperature compression tests, the yield strengths were measured as 1430, 1388, 418, and 163 MPa at 25, 500, 700, and 900°C, respectively. Based on these results, the correlation between the microstructure and mechanical properties of ODS steel manufactured using the composite milling process is also discussed.

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.

The automotive industry has focused on the development of metallic materials with high specific strength, which can meet both fuel economy and safety goals. Here, a new class of ultrafine-grained high-Mn steels containing nano-scale oxides is developed using powder metallurgy. First, high-energy mechanical milling is performed to dissolve alloying elements in Fe and reduce the grain size to the nanometer regime. Second, the ball-milled powder is consolidated using spark plasma sintering. During spark plasma sintering, nanoscale manganese oxides are generated in Fe-15Mn steels, while other nanoscale oxides (e.g., aluminum, silicon, titanium) are produced in Fe-15Mn-3Al-3Si and Fe-15Mn-3Ti steels. Finally, the phases and resulting hardness of a variety of high-Mn steels are compared. As a result, the sintered pallets exhibit superior hardness when elements with higher oxygen affinity are added; these elements attract oxygen from Mn and form nanoscale oxides that can greatly improve the strength of high-Mn steels.

In this study, we report the microstructure and characterization of Ta₂₀Nb₂₀V₂₀W₂₀Ti₂₀ high-entropy alloy powders and sintered samples. The effects of milling time on the microstructure and mechanical properties were investigated in detail. Microstructure and structural characterization were performed by scanning electron microscopy and X-ray diffraction. The mechanical properties of the sintered samples were analyzed through a compressive test at room temperature with a strain rate of 1 × 10⁻⁴ s⁻¹. The microstructure of sintered Ta₂₀Nb₂₀V₂₀W₂₀Ti₂₀ high-entropy alloy is composed of a BCC phase and a TiO phase. A better combination of compressive strength and strain was achieved by using prealloyed Ta₂₀Nb₂₀V₂₀W₂₀Ti₂₀ powder with low oxygen content. The results suggest that the oxide formed during the sintering process affects the mechanical properties of Ta₂₀Nb₂₀V₂₀W₂₀Ti₂₀ high-entropy alloys, which are related to the interfacial stability between the BCC matrix and TiO phase.

Tungsten heavy alloys (W–Ni–Fe) play an important role in various industries because of their excellent mechanical properties, such as the excellent hardness of tungsten, low thermal expansion, corrosion resistance of nickel, and ductility of iron. In tungsten heavy alloys, tungsten nanoparticles allow the relatively low-temperature molding of high-melting-point tungsten and can improve densification. In this study, to improve the densification of tungsten heavy alloy, nanoparticles are manufactured by ultrasonic milling of metal oxide. The physical properties of the metal oxide and the solvent viscosity are selected as the main parameters. When the density is low and the Mohs hardness is high, the particle size distribution is relatively high. When the density is high and the Mohs hardness is low, the particle size distribution is relatively low. Additionally, the average particle size tends to decrease with increasing viscosity. Metal oxides prepared by ultrasonic milling in high-viscosity solvent show an average particle size of less than 300 nm based on the dynamic light scattering and scanning electron microscopy analysis. The effects of the physical properties of the metal oxide and the solvent viscosity on the pulverization are analyzed experimentally.

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• Manufacture of high sensitive Ag-Fe3O4-PDMS nanocomposite pressure sensor through morphology control of conductive filler
  Keunhyuk Ryu, Namhun Kwon, Kun-Jae Lee
  Advanced Powder Technology.2021; 32(7): 2441.     CrossRef
• Grinding behavior of WO3, NiO, Fe2O3 by ultrasonic milling parameters control and preparation of nanocomposite powder
  Keunhyuk Ryu, Kun-Jae Lee
  Advanced Powder Technology.2020; 31(9): 3867.     CrossRef

The activation energy to create a phase transformation or for the reaction to move to the next stage in the milling process can be calculated from the slop of the DSC plot, obtained at the various heating rates for mechanically activated Al-Ni alloy systems by using Kissinger’s equation. The mechanically activated material has been called “the driven material” as it creates new phases or intermetallic compounds of AlNi in Al-Ni alloy systems. The reaction time for phase transformation by milling can be calculated using the activation energy obtained from the above mentioned method and from the real required energy. The real required energy (activation energy) could be calculated by subtracting the loss energy from the total input energy (calculated input energy from electric motor). The loss energy and real required energy divided by the reaction time are considered the “metabolic energy” and “the effective input energy”, respectively. The milling time for phase transformation at other Al-Co alloy systems from the calculated data of Al-Ni systems can be predicted accordingly.