• Journal of Powder Materials
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• v.20 no.1
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• pp.53-59
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• 2013

Fe-TiC composite powder was fabricated via two steps. The first step was a high-energy milling of FeO and carbon powders followed by heat treatment for reduction to obtain a (Fe+C) powder mixture. The optimal condition for high-energy milling was 500 rpm for 1h, which had been determined by a series of preliminary experiment. Reduction heat-treatment was carried out at $900^{\circ}C$ for 1h in flowing argon gas atmosphere. Reduced powder mixture was investigated by X-ray Diffraction (XRD), Field Emission-Scanning Electron Microscopy (FE-SEM) and Laser Particle Size Analyser (LPSA). The second step was a high-energy milling of (Fe+C) powder mixture and additional $TiH_2$ powder, and subsequent in-situ synthesis of TiC particulate in Fe matrix through a reaction of carbon and Ti. High-energy milling was carried out at 500 rpm for 1 h. Heat treatment for reaction synthesis was carried out at $1000{\sim}1200^{\circ}C$ for 1 h in flowing argon gas atmosphere. X-ray diffraction (XRD) results of the fabricated Fe-TiC composite powder showed that only TiC and Fe phases exist. Results from FE-SEM observation and Energy-Dispersive X-ray Spectros-copy (EDS) revealed that TiC phase exists uniformly dispersed in the Fe matrix in a form of particulate with a size of submicron.

• Journal of Powder Materials
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• v.17 no.4
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• pp.302-311
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• 2010

In this research, the refinement behavior of the coarse magnesium powders fabricated by gas atomization was investigated as a function of milling time using a short duration high-energy ball milling equipment, which produces fine powders by means of an ultra high-energy within a short duration. The microstructure, hardness, and formability of the powders were investigated as a function of milling time using X-ray diffraction, scanning electron microscopy, Vickers micro-hardness tester and magnetic pulsed compaction. The particle morphology of Mg powders changed from spherical particles of feed metals to irregular oval particles, then platetype particles, with increasing milling time. Due to having HCP structure, deformation occurs due to the existence of the easily breakable C-axis perpendicular to the base, resulting in producing plate-type powders. With increasing milling time, the particle size increased until 5 minutes, then decreased gradually reaching a uniform size of about 50 micrometer after 20 minutes. The relative density of the initial power was 98% before milling, and mechanically milled powder was 92~94% with increase milling time (1~5 min) then it increased to 99% after milling for 20 minutes because of the change in particle shapes.

• Journal of Powder Materials
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• v.24 no.5
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• pp.406-413
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• 2017

A Nanosized $WO_3$ 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 $WO_3-CuO$ powder mixtures is investigated. The results show that the ball-milled $WO_3-CuO$ 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 $37m^2/g$, and powder mean particle size ($D_{50}$) of $0.57{\mu}m$. The $WO_3-CuO$ powder mixtures milled for 10 h are heat-treated at different temperatures in $H_2$ atmosphere to produce W-Cu powder. The XRD results shows that both the $WO_3$ and CuO phases can be reduced to W and Cu phases at temperatures over $700^{\circ}C$. 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.

• Journal of the Korean Ceramic Society
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• v.45 no.6
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• pp.363-367
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• 2008

Lead-free $(K_{0.44}Na_{0.52})(Nb_{0.86}Ta_{0.10})-0.04LiSbO_3$ piezoelectric ceramics have been synthesized by conventional sintering process and then investigated on the sintering and piezoelectric properties by high energy ball milling (HEBM) treatment. The powders milled for different time are characterized by XRD, FE-SEM. The powders are pressed into a pellet and sintered. It is found that the piezoelectric properties of sintered specimens are strongly dependent on the milling time. The piezoelectric properties are enhanced by high energy ball milling treatment. The planer electromechanical coupling factor ($k_p$) and piezoelectric constant ($d_{33}$) of a specimen sintered at $1050^{\circ}C$ are 0.44 and 267 pC/N, respectively.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.28 no.12
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• pp.852-856
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• 2015

In this study, we investigate the effect of high-energy ball milling on thermoelectric transport properties in double-filled $CoSb_3$ skutterudite ($In_{0.2}Yb_{0.1}Co_4Sb_{12}$). $In_{0.2}Yb_{0.1}Co_4Sb_{12}$ powders are milled using high-energy ball milling for different periods of time (0, 5, 10, and 20 min), and the milled powders are consolidated into bulk samples by spark plasma sintering. Microstructure analysis shows that the high-energy ball milled bulk samples are composed of nano- and micro-grains. Because the filling fractions are reduced in the bulk samples due to the kinetic energy of the high-energy ball milling, the carrier concentration of the bulk samples decreases with the ball milling time. Furthermore, the mobility of the bulk samples also decreases with the ball milling time due to enhanced grain boundary scattering of electrons. Reduction of electrical conductivity by ball milling has a decisive effect on thermoelectric transport in the bulk samples, power factor decreases with the ball milling time.

• Korean Journal of Materials Research
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• v.25 no.8
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• pp.386-390
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• 2015

Fe-base superalloy powders with $Y_2O_3$ dispersion were prepared by high energy ball milling, followed by spark plasma sintering for consolidation. High-purity elemental powders with different Fe powder sizes of 24 and 50 mm were used for the preparation of $Fe-20Cr-4.5Al-0.5Ti-O.5Y_2O_3$ powder mixtures (wt%). The milling process of the powders was carried out in a horizontal rotary ball mill using a stainless steel vial and balls. The milling times of 1 to 5 h by constant operation (350 rpm, ball-to-powder ratio of 30:1 in weight) or cycle operation (1300 rpm for 4 min and 900 rpm for 1 min, 15:1) were applied. Microstructural observation revealed that the crystalline size of Fe decreased with an increase in milling time by cyclic operation and was about 15 nm after 3 h, forming a FeCr alloy phase. The cyclic operation had an advantage over constant milling in that a smaller-agglomerated structure was obtained. The milled powders were sintered at $1100^{\circ}C$ for 30 min in vacuum. With an increase in milling time, the sintered specimen showed a more homogeneous microstructure. In addition, a homogenous distribution of Y-compound particles in the grain boundary was confirmed by EDX analysis.

• 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 the Korean Ceramic Society
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• v.48 no.5
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• pp.418-425
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• 2011

In this study, a high energy ball milling process was introduced in order to improve the densification of direct nitrided AlN powder. The sintering behavior and thermal conductivity of the AlN milled powder was investigated. The mixture of AlN powder and 5 wt% $Y_2O_3$ as a sintering additive was pulverized and dispersed by a bead mill with very small $ZrO_2$ bead media. The milled powders were sintered at $1700^{\circ}C-1800^{\circ}C$ for 4 h under $N_2$ atmosphere. The results showed that the sintered density was enhanced with increasing milling time due to the particle refinement as well as the increase in oxygen contents. Appropriate milling time was effective for the improvement of thermal conductivity, but the extensive millied powder formed more fractions of secondary phase during sintering, resulted in the decrease in thermal conductivity. The AlN powder milled for 10min after sintering at $1800^{\circ}C$ revealed the highest thermal conductivity, of 164W/$m{\cdot}K$ in tne densified AlN sintered at $1800^{\circ}C$.

• 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.

• 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.