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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

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, acoustic and viscosity data are collected in real time during the ball milling process and analyzed for correlation. After fast Fourier transformation (FFT) of the acoustic data, changes in the signals are observed as a function of the milling time. To analyze this quantitatively, the frequency band is divided into 1 kHz ranges to obtain an integral value. The integrated values in the 2–3 kHz range of the frequency band decrease linearly, confirming that they have a high correlation with changes in viscosity. The experiment is repeated four times to ensure the reproducibility of the data. The results of this study show that it is possible to estimate changes in slurry properties, such as viscosity and particle size, during the ball milling process using an acoustic signal.

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.

Ni-based oxide dispersion strengthened (ODS) alloys have a higher usable temperature and better hightemperature mechanical properties than conventional superalloys. They are therefore being explored for applications in various fields such as those of aerospace and gas turbines. In general, ODS alloys are manufactured from alloy powders by mechanical alloying of element powders. However, our research team produces alloy powders in which the Ni₅Y intermetallic phase is formed by an atomizing process. In this study, mechanical alloying was performed using a planetary mill to analyze the milling behavior of Ni-based oxide dispersions strengthened alloy powder in which the Ni₅Y is the intermetallic phase. As the milling time increased, the Ni₅Y intermetallic phase was refined. These results are confirmed by SEM and EPMA analysis on microstructure. In addition, it is confirmed that as the milling increased, the mechanical properties of Ni-based ODS alloy powder improve due to grain refinement by plastic deformation.

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• Efficient prediction of corrosion behavior in ternary Ni-based alloy systems: Theoretical calculations and experimental verification
  Xuelian Xiao, Keke Chang, Kai Xu, Ming Lou, Liping Wang, Qunji Xue
  Journal of Materials Science & Technology.2023; 167: 94.     CrossRef
• Effect of high-energy ball milling on the microstructure and mechanical properties of Ni-based ODS alloys fabricated using gas-atomized powder
  Chun Woong Park, Won June Choi, Jongmin Byun, Young Do Kim
  Journal of Materials Science.2022; 57(38): 18195.     CrossRef

In the present study, we develop a conductive copper/carbon nanomaterial additive and investigate the effects of the morphologies of the carbon nanomaterials on the conductivities of composites containing the additive. The conductive additive is prepared by mechanically milling copper powder with carbon nanomaterials, namely, multi-walled carbon nanotubes (MWCNTs) and/or few-layer graphene (FLG). During the milling process, the carbon nanomaterials are partially embedded in the surfaces of the copper powder, such that electrically conductive pathways are formed when the powder is used in an epoxy-based composite. The conductivities of the composites increase with the volume of the carbon nanomaterial. For a constant volume of carbon nanomaterial, the FLG is observed to provide more conducting pathways than the MWCNTs, although the optimum conductivity is obtained when a mixture of FLG and MWCNTs is used.

A conductive additive is prepared by dispersing multi-walled carbon nanotubes (MWCNTs) on Cu powder by mechanical milling and is distributed in epoxy to enhance its electrical conductivity. During milling, the MWCNTs are dispersed and partially embedded on the surface of the Cu powder to provide electrically conductive pathways within the epoxy-based composite. The degree of dispersion of the MWCNTs is controlled by varying the milling medium and the milling time. The MWCNTs are found to be more homogeneously dispersed when solvents (particularly, non-polar solvent, i.e., NMP) are used. MWCNTs gradually disperse on the surface of Cu powder because of the plastic deformation of the ductile Cu powder. However, long-time milling is found to destroy the molecular structure of MWCNTs, instead of effectively dispersing the MWCNTs more uniformly. Thus, the epoxy composite film fabricated in this study exhibits a higher electrical conductivity than 1.1 S/cm.

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• Effects of Morphologies of Carbon Nanomaterials on Conductivity of Composites Containing Copper/Carbon Nanomaterial Hybrid Fillers
  Yeonjoo Lee, Sung-uk Hong, Hyunjoo Choi
  Journal of Korean Powder Metallurgy Institute.2018; 25(5): 435.     CrossRef

Aluminum nitride (AlN) powder specimens are treated by high-energy bead milling and then sintered at various temperatures. Depending on the solvent and milling time, the oxygen content in the AlN powder varies significantly. When isopropyl alcohol is used, the oxygen content increases with the milling time. In contrast, hexane is very effective at suppressing the oxygen content increase in the AlN powder, although severe particle sedimentation after the milling process is observed in the AlN slurry. With an increase in the milling time, the primary particle size remains nearly constant, but the particle agglomeration is reduced. After spark plasma sintering at 1400°C, the second crystalline phase changes to compounds containing more Al₂O₃ when the AlN raw material with an increased milling time is used. When the sintering temperature is decreased from 1750°C to 1400°C, the DC resistivity increases by approximately two orders of magnitude, which implies that controlling the sintering temperature is a very effective way to improve the DC resistivity of AlN ceramics.

A Nanosized WO₃ and CuO powder mixture is prepared using novel high-energy ball milling in a bead mill to obtain a W-Cu nanocomposite powder, and the effect of milling time on the structural characteristics of WO₃-CuO powder mixtures is investigated. The results show that the ball-milled WO₃-CuO powder mixture reaches at steady state after 10 h milling, characterized by the uniform and narrow particle size distribution with primary crystalline sizes below 50 nm, a specific surface area of 37 m²/g, and powder mean particle size (D₅₀) of 0.57 μm. The WO₃-CuO powder mixtures milled for 10 h are heat-treated at different temperatures in H₂ atmosphere to produce W-Cu powder. The XRD results shows that both the WO₃ and CuO phases can be reduced to W and Cu phases at temperatures over 700°C. The reduced W-Cu nanocomposite powder exhibits excellent sinterability, and the ultrafine W-Cu composite can be obtained by the Cu liquid phase sintering process.

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• Morphological Characteristics of W/Cu Composite Nanoparticles with Complex Phase Structure Synthesized via Reactive Radio Frequency (RF) Thermal Plasma
  Chulwoong Han, Song-Yi Kim, Soobin Kim, Ji-Woon Lee
  Metals.2024; 14(9): 1070.     CrossRef

The effect of the mixing method on the characteristics of hybrid-structure W powder with nano and micro sizes is investigated. Fine WO₃ powders with sizes of ~0.6 μm, prepared by ball milling for 10 h, are mixed with pure W powder with sizes of 12 μm by various mixing process. In the case of simple mixing with ball-milled WO₃ and micro sized W powders, WO₃ particles are locally present in the form of agglomerates in the surface of large W powders, but in the case of ball milling, a relatively uniform distribution of WO₃ particles is exhibited. The microstructural observation reveals that the ball milled WO₃ powder, heat-treated at 750°C for 1 h in a hydrogen atmosphere, is fine W particles of ~200 nm or less. The powder mixture prepared by simple mixing and hydrogen reduction exhibits the formation of coarse W particles with agglomeration of the micro sized W powder on the surface. Conversely, in the powder mixture fabricated by ball milling and hydrogen reduction, a uniform distribution of fine W particles forming nano-micro sized hybrid structure is observed.

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• The Efficiency of Radiation Shielding Sheet to Reduce Radiation Exposure during C-arm Fluoroscopy
  Hosang Jeon, Won Chul Shin, Hee Yun Seol, Yongkan Ki, Kyeong Baek Kim, Ki Seok Choo, Sang Don Lee, Suk-Woong Kang
  Journal of the Korean Fracture Society.2023; 36(4): 111.     CrossRef
• Facile phosphorus-embedding into SnS2 using a high-energy ball mill to improve the surface kinetics of P-SnS2 anodes for a Li-ion battery
  Hongsuk Choi, Seungmin Lee, KwangSup Eom
  Applied Surface Science.2019; 466: 578.     CrossRef
• Hydrogen reduction behavior and microstructural characteristics of WO3 and WO3-NiO powders
  Hyunji Kang, Young-Keun Jeong, Sung-Tag Oh
  International Journal of Refractory Metals and Hard Materials.2019; 80: 69.     CrossRef
• Fabrication of Densified W-Ti by Reaction Treatment and Spark Plasma Sintering of WO3-TiH2 Powder Mixtures
  Hyunji Kang, Heun Joo Kim, Ju-Yeon Han, Yunju Lee, Young-Keun Jeong, Sung-Tag Oh
  Korean Journal of Materials Research.2018; 28(9): 511.     CrossRef