• Journal of the Korean Ceramic Society
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• v.49 no.6
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• pp.648-653
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• 2012

Hybridization of dense ceramic membranes for hydrogen separation with an electronically conductive metallic phase is normally utilized to enhance the hydrogen permeation flux and thereby to increase the production efficiency of hydrogen. In this study, we developed a nickel and proton conducting oxide ($BaCe_{0.9}Y_{0.1}O_{3-{\delta}}$: BCY) based cermet (ceramic-metal composites) membrane. Focused on the general criteria in that the hydrogen permeation properties of a cermet membrane depend on its microstructural features, such as the grain size and the homogeneity of the mix, we tried to optimize the microstructure of Ni-BCY cermets by controlling the fabrication condition. The Ni-BCY composite powder was synthesized via a solid-state reaction using $2NiCO_3{\cdot}3Ni(OH)_2{\cdot}4H_2O$, $BaCeO_3$, $CeO_2$ and $Y_2O_3$ as a starting material. To optimize the mixing scale and homogeneity of the composite powder, we employed a high-energy milling process. With this high-energy milled composite powder, we could fabricate a fine-grained dense membrane with an excellent level of mixing homogeneity. This controlled Ni-BCY cermet membrane showed higher hydrogen permeability compared to uncontrolled Ni-BCY cermets created with a conventionally ball-milled composite powder.

• Journal of Powder Materials
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• v.19 no.1
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• pp.25-31
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• 2012

In this study, a high energy ball milling process was employed in order to improve the densification of direct nitrided AlN powder. The densification behavior and the sintered microstructure of the milled AlN powder were investigated. Mixture of AlN powder doped with 5 wt.% $Y_2O_3$ as a sintering additive was pulverized and dispersed up to 50 min in a bead mill with very small $ZrO_2$ beads. Ultrafine AlN powder with a particle size of 600 nm and a specific surface area of 9.54 $m^2/g$ was prepared after milling for 50 min. The milled powders were pressureless-sintered at $1700^{\circ}C-1800^{\circ}C$ for 4 h under $N_2$ atmosphere. This powder showed excellent sinterability leading to full densification after sintering at $1700^{\circ}C$ for 4 h. However, the sintered microstructure revealed that the fraction of yitttium aluminate increased with milling time and sintering temperature and the newly-secondary phase of ZrN was observed due to the reaction of AlN with the $ZrO_2$ impurity.

• Journal of Powder Materials
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• v.19 no.1
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• pp.32-39
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• 2012

This study investigated refinement behaviors of TiC powders produced under different impact energy conditions using a mechanical milling process. The initial coarse TiC powders with an average diameter of 9.3 ${\mu}m$ were milled for 5, 20, 60 and 120 mins through the conventional low energy mechanical milling (LEMM, 22G) and specially designed high energy mechanical milling (HEMM, 65G). TiC powders with angular shape became spherical one and their sizes decreased as the milling time increased, irrespective of milling energy. Based upon the FE-SEM and BET results of milled powders, it was found initial coarse TiC powders readily became much finer near 100 nm within 60 min under HEMM, while their sizes were over 200 nm under LEMM, despite the long milling time of up to 120 min. Particularly, ultra-fine TiC powders with an average diameter of 77 nm were fabricated within 60 min in the presence of toluene under HEMM.

• Korean Journal of Materials Research
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• v.10 no.10
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• pp.715-720
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• 2000

By the mechanical alloying method. Ni-WC composite materials were prepared to improve the deformation-resistance for creep and sintering of Ni-anode at the operating temperature of $650^{\circ}C$. Mechanically alloyed powder w was initially fabricated by ball milling for 80hr, and then amorphization was occurred by the destruction of ordered crystals based on XRD analysis. In order to investigate the electrochemical performance and sheet characteristics of Ni-WC anode, tape casting process was adopted. Finally, the obtained sheet thickness of Ni- we after sintering at $1180^{\circ}C$ for 60 minutes in $H_2$ atmosphere was O.9mm and the average pore size was $3~5{\mu\textrm{m}}$ with porosities of 55%. The second phase was not observed in Ni- W matrix while W particles were finely and uniformly distributed in Ni matrix. This fine and uniform distributed W particles in Ni matrix are expected to enhance the mechanical properties of Ni anode through the dispersion and solid solution hardening mechanisms.

• Journal of the Korean Society for Heat Treatment
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• v.31 no.4
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• pp.171-179
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• 2018

Copper powder dispersed with 4 vol.% of $Cr_2O_3$ was successfully produced by a simple milling at 210 K with a mixture of $Cu_2O$, Cu and Cr elemental powders, followed by Hot Pressing (HP) at 1123 K and 50 MPa for 2h to consolidate the milled powder. The microstructure of the HPed material was characterized by standard metallographic techniques such as XRD (X-ray Diffraction), TEM and STEM-EDS. The results of STEMEDS analysis showed that the HPed materials comprised a mixture of nanocrystalline Cu matrix and $Cr_2O_3$ dispersoid with a homogeneous bimodal size distribution. The mechanical properties of the HPed materials were characterized by micro Vickers hardness test at room temperature. The thermodynamic considerations on the heat of formation, the incubation time to ignite MSR (Mechanically induced Self-sustaining Reaction), and the adiabatic temperature for the heat of displacement reaction between the oxide-metal are made for the delayed formation of $Cr_2O_3$ dispersoid in terms of MSR suppression. The results of TEM observation and hardness test indicated that the relatively large dispersoids in the HPed materials are attributed to the significant coarsening for the high temperature consolidation; this leads to the low Vickers hardness value. Based on the thermodynamic calculation for the operating processes with a limited number of parameters, the formation kinetics and coarsening of the $Cr_2O_3$ dispersoid are discussed.

• Journal of Powder Materials
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• v.26 no.5
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• pp.410-414
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• 2019

The hydrogen reduction behavior of the $CuO-SCo_3O_4$ powder mixture for the synthesis of the homogeneous Cu-15at%Co composite powder has been investigated. The composite powder is prepared by ball milling the oxide powders, followed by a hydrogen reduction process. The reduction behavior of the ball-milled powder mixture is analyzed by X-ray diffraction (XRD) and temperature-programmed reduction at different heating rates in an Ar-10%H2 atmosphere. The scanning electron microscopy and XRD results reveal that the hydrogen-reduced powder mixture is composed of fine agglomerates of nanosized Cu and Co particles. The hydrogen reduction kinetics is studied by determining the degree of peak shift as a function of the heating rate. The activation energies for the reduction of the oxide powders estimated from the slopes of the Kissinger plots are 58.1 kJ/mol and 65.8 kJ/mol, depending on the reduction reaction: CuO to Cu and $SCo_3O_4$ to Co, respectively. The measured temperature and activation energy for the reduction of $SCo_3O_4$ are explained on the basis of the effect of pre-reduced Cu particles.

• Journal of Powder Materials
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• v.28 no.2
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• pp.103-109
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• 2021

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-to-powder 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.

• Journal of Powder Materials
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• v.28 no.5
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• pp.389-395
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• 2021

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℃, 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.

• Korean Journal of Metals and Materials
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• v.49 no.2
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• pp.161-166
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• 2011

The aim of this study was to determine the effect of high-energy mechanical milling (HEMM) time and sintering temperature on microstructure and mechanical properties of the TiAl composite fabricated by pulse current activated sintering. TiAl intermetallic powders were milled by HEMM for 1h, 4h, and 8h respectively. Thermal analysis was used to observe the phase transformation of the milled TiAl powders. The sintering time decreased with increase of milling time. The hardness and fracture toughness of the sintered specimens also was improved with increasing milling time. The grain size of the sintered specimens which was milled for 4h was in the range of 50~100 nm.

• Journal of Powder Materials
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• v.29 no.1
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• pp.34-40
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• 2022

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℃.