• 한국분말재료학회지
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• 제18권4호
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• pp.378-384
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• 2011

In this research, the indium dissolution properties of the waste LCD panel powders were investigated as a function of milling time fabricated by high-energy ball milling (HEBM) process. The particle morphology of waste LCD panel powders changed from sharp and irregular shape of initial cullet to spherical shape with an increase in milling time. The particle size quickly decreased to 15 ${\mu}m$ until the first minute, then decreased gradually about 6 ${\mu}m$ with presence of agglomerated particles after 5 minutes, which increased gradually reaching a uniform size of 13 ${\mu}m$ consist of agglomerated particles after 30 minutes. The glass recovery, after dissolution, was over 99% at initial cullet, which decreased to 90.1 and 78.6% with increasing milling time of 1 and 30 minute respectively, due to a loss in remaining powder of the surface ball and jar, as well as the filter paper. The dissolution amount of indium out of the initial cullet was 208 ppm before milling, turning into 223 ppm for the mechanically milled powder after 1 minute, and nearly 146~125 ppm with further increase in milling time because of the reaction surface decrease of powders due to agglomeration. With this process, maximum dissolving indium amount (223 ppm) could be achieved at a particle size of 15 ${\mu}m$ with 1 minute of milling.

• 한국분말재료학회지
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• 제29권1호
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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℃.

• Progress in Superconductivity
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• 제10권1호
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• pp.17-22
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• 2008

We have examined the effect of ball-milling on the superconducting properties of $MgB_2$ doped with C. The ball-milling of pre-reacted $MgB_2$ powder was carried out in dry or wet state using C or diethylenetriamine ($C_{4}H_{13}N_3$) as additives. The diethylenetriamine, whose chemical formula contains no oxygen, was chosen to avoid an excess oxidation during doping. The superconducting transition temperature (Tc) of the ball-milled or doped $MgB_2$ powders was only slightly smaller than that of undoped $MgB_2$. The critical current density (Jc) of the highly ball-milled $MgB_2$ was higher than that of C-doped $MgB_2$. The addition of diethylenetriamine was detrimental to Jc, although Tc was almost unchanged.

• 한국전기전자재료학회논문지
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• 제17권1호
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• pp.39-45
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• 2004

Fine LaAlO$_3$ powders wore successfully synthesized from La$_2$O$_3$ and ${\gamma}$ $Al_2$O$_3$ powders milling for 10∼50 hours via the high energy milling technique (mechanochemical method) in room temperature and air. The particle size of LaAlO$_3$ powder were estimated from XRD patterns and SEM images to be 160∼180 nm. The LaAlO$_3$ ceramics arc derived for the synthesized powders (milling for 10, 30 and 50 hours) by sintering at 140$0^{\circ}C$ and 150$0^{\circ}C$. The micrographs of grains showed an agglomeration and the degree of agglomeration increased with the milling time. The LaAlO$_3$ made from synthesized powders milling for 50 hours can be sintered to 99.5％ of theoretical density at 150$0^{\circ}C$ for 1 hour. These ceramics exhibits a dielectric constant of 20, a dielectric loss of 0.0003 and a temperature coefficient of capacitance of 15 ppm/$^{\circ}C$ at 1 MHz.

• 한국재료학회지
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• 제31권12호
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• pp.677-681
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• 2021

The Mn-Zn ferrite powders were prepared by high energy ball milling, then compacted and sintered at various temperatures to assess their sintering behavior and magnetic properties. The initial ferrite powders were spherical in shape with the size of approximately 70 ㎛. After 3 h of ball milling at 300 rpm, aggregated powders ~230 nm in size and composed of ~15 nm nanoparticles were formed. The milled powders had a density of ~70 % when compacted at 490 MPa for 3 min. In the samples subsequently sintered at 1,273 K ~ 1,673 K for 3 h, the MnZnFe₂O₄ phase was detected. The density of the sintered samples had a tendency to increase with increasing sintering temperature up to 1,473 K, which produced the highest density of 98 %. On the other hand, the sample sintered at 1,373 K had the highest micro-hardness of approximately 610 Hv, which is due to much finer grains.

• 한국재료학회지
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• 제15권3호
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• pp.166-171
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• 2005

Fe-6Al-9Si(N) alloy powders were synthesized by hybrid process of chemical nitrification and mechanical milling. The nitriding treatment on Fe-6Al-9Si alloy powders formed $\gamma'-Fe_4N$ phase on the powders surface. The nitriding-treated powders were pulverized by horizontal high-energy ball milling machine. The longer ball milling time tended to reduce the size of alloy powders. In ball milling for 36h, extremely fine powders with about $7\~9wt\%$ nitrogen were obtained. Through X-ray diffraction analysis on the powders, it was found out that the longer milling time caused a disappearance of the crystallinity of $\alpha-Fe$ in the powders. TEM study confirmed that the powders is comprised of a few tens nano-meter sized crystals, including $\alpha-Fe$ phase with partially $\gamma'-Fe_4N$ phase. Hysteresis curves of the synthesized powders measured by VSM revealed lower saturation magnetization and higher coercivity, which seemed to be attributed to nitrogen-impregnation and severe residual stress developed during the high energy milling. Microstructure observation on the powder annealed at 873 K for 1 h showed 10 to 20 nm sized $\alpha-Fe$ crystal. Such a enhanced crystallinity significantly increased the magnetization and decreased the coercivity, which was attributed to not only the crystallinity but also residual stress relaxation.

• 한국분말재료학회지
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• 제5권4호
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• pp.250-257
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• 1998

The synthesis of titanium silicides ($Ti_3Si$, $TiSi_2$, $Ti_5Si_4$, $Ti_5Si_3$ and TiSi) by mechanical alloying has been investigated. Rapid, self-propagating high-temperature synthesis (SHS) reactions were observed to produce the last three phases during room-temperature high-energy ball milling of elemental powders. Such reactions appeared to be ignited by mechanical impact in an intimate, fine powder mixture formed after a critical milling period. During the high-energy ball milling, the repeated impact at contact points leads to a local concentration of energy which may ignite a self-propagating reaction. From in-situ thermal analysis, each critical milling period for the formation of $Ti_5Si_4$, $Ti_5Si_3$ and TiSi was observed to be 22, 35.5 and 53.5 min, respectively. $Ti_3Si$ and $TiSi_2$, however, have not been produced even till the milling period of 360 min due to lack of the homogeneity of the powder mixtures. The formation of titanium silicides by mechanical alloying and the relevant reaction rates appeared to depend upon the critical milling period, the homogeneity of the powder mixtures, and the heat of formation of the products involved.

• Transactions on Electrical and Electronic Materials
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• 제16권2호
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• pp.53-61
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• 2015

High-energy ball milling was tested as a method for producing Ultra High Molecular Weight Polyethylene (UHMWPE)- based nanodielectrics containing 1 wt% and 5 wt% OctaIsoButylPOSS (OibPOSS). Qualitative and quantitative evaluations were used to explore the compatibility between OibPOSS and PE. Several ball milling variables were optimized in a bid to achieve UHMWPE/OibPOSS nanodielectrics. The morphology, as well as the thermal and the dielectric properties of the samples, were characterized by scanning electron microscopy, thermogravimetric analysis, broadband dielectric spectroscopy, and progressive-stress breakdown tests. The results showed that (i) ball milling was an effective method for producing UHMWPE/OibPOSS dielectric composites, but appeared ineffective in dispersing OibPOSS at the nanoscale, and (ii) the resulting UHMWPE/OibPOSS dielectric composites presented thermal and dielectric properties similar to those of neat UHMWPE.

• 한국수소및신에너지학회논문집
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• 제17권3호
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• pp.309-316
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• 2006

Co-ferrite was synthesized by HEBM (High Energy Ball Milling) with a stoichiometric (Co/Fe=0.5/2.5) mixture of CoO and $Fe_2O_3$ powders. The effect of milling time on the phase transformation of the mixture was investigated by XRD. Mono-phase solid solution of Co-ferrite, which was milled for 4 h and then calcined at $900^{\circ}C$ in the Ar atmosphere, was confirmed by XRD analysis. The composition and thermal reduction behavior of Co-ferrite were analyzed by TGA and XRF. As a result, oxygen deficient Co-ferrite was synthesized by HEBM and the weight decrease of the Co-ferrite, which was oxidized at $600^{\circ}C$ for 10h by $H_2O$ vapor, was 2.41 wt% during thermal reduction at $1300^{\circ}C$.

• 한국분말재료학회지
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• 제17권4호
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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.