• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2006.09b
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• pp.1264-1265
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• 2006

Study about the feasibility and effect of high-energy ball milling on a specific Mg alloy under protection medium of alcohol was presented via comparing with conventional vacuum milling. More fine particles with wider powder size distribution but more irregular shape were shown of the powder milled under alcohol. No obvious oxide was revealed from the two kinds of Mg alloy powders with limited milling time. And since slip induced in a preferential direction, the (002) texture was formed in the Mg alloy powders at the initial stage of alcohol milling. More O and Fe contaminants were introduced into the powders milled under alcohol according to the EDS analysis.

• Journal of Powder Materials
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• v.9 no.6
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• pp.416-421
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• 2002

Elemental powders are used in high energy milling processes for the synthesis of new compounds. The low temperature solid state reactions during milling in inert gas atmosphere may result in intermetallic phases, carbides, nitrides or silicides with a nanocrystalline structure. To obtain dense materials from the powders a pressure assisted densification is necessary. On the other side the defect-rich microstructure can be used for activated sintering of elemental powder mixtures to obtain dense bodies by pressureless sintering. Results are discussed for nanocrystalline cermet systems and for the sintering of aluminides and silicides.

• Journal of Powder Materials
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• v.5 no.4
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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.

• Journal of Powder Materials
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• v.20 no.5
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• pp.338-344
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• 2013

Fe-TiC composite was fabricated from Fe and TiC powders by high-energy milling and subsequent spark-plasma sintering. The microstructure, particle size and phase of Fe-TiC composite powders were investigated by field emission scanning electron microscopy and X-ray diffraction to evaluate the effect of milling conditions on the size and distribution of TiC particles in Fe matrix. TiC particle size decreased with milling time. The average TiC particle size of 38 nm was obtained after 60 minutes of milling at 1000 rpm. Prepared Fe-TiC powder mixture was densified by spark-plasma sintering. Sintered Fe-TiC compacts showed a relative density of 91.7~96.2%. The average TiC particle size of 150 nm was observed from the FE-SEM image. The microstructure, densification behavior, Vickers hardness, and fracture toughness of Fe-TiC sintered compact were investigated.

• Journal of Powder Materials
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• v.18 no.4
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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.

• 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℃.

• Corrosion Science and Technology
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• v.21 no.6
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• pp.445-453
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• 2022

SiO_x was prepared from a mixture of Si and SiO₂ via high-energy ball milling as a negative electrode material for Li-ion batteries. The molar ratio of Si to SiO₂ as precursors and the milling time were varied to identify the synthetic condition that could exhibit desirable anode performances. With an appropriate milling time, the material showed a unique microstructure in which amorphous Si nanoparticles were intimately embedded within the SiO₂ matrix. The interface between the Si and SiO₂ was composed of silicon suboxides with Si oxidation states from 0 to +4 as proven by X-ray photoelectron spectroscopy and electrochemical analysis. With the addition of a conductive carbon (Super P carbon black) as a coating material, the SiO_x/C manifested superior specific capacity to a commercial SiO_x/C composite without compromising its cycle-life performance. The simple mechanochemical method described in this study will shed light on cost-effective synthesis of high-capacity silicon oxides as promising anode materials.

• Proceedings of the Korean Magnestics Society Conference
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• 2002.12a
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• pp.116-117
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• 2002

High energy mi]ling은 mechanical alloying을 일컫는 분말 제조 공정으로서 금속 뿐 아니라 세라믹스 분말 합성에도 많이 응용되고 있으며, 입자크기의 나노화와 일반적인 세라믹 분말의 특성을 개질할 수 있다는 특징을 갖고 있어서 다양한 연구 결과가 보고되고 있다[1-2]. Ba 및 Sr 페라이트와 같은 육방정 페라이트는 보자력(high coercivity)이 높은 특성을 가지므로 영구자석용, 기록재료용 등으로 광범위하게 사용되어온 재료이다. 이와 같은 높은 보자력을 유지하기 위해서는 입자크기가 단자구 입경(<1 $\mu\textrm{m}$) 보다 작아야 하기 때문에, 초미립자 합성에 관한 많은 연구가 진행되어 왔다[3-4]. (중략)

• 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 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.