• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.17 no.1
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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.

• Journal of Powder Materials
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• v.17 no.2
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• pp.130-135
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• 2010

Sm-16.7wt%Co alloy powders were prepared by high energy ball milling under the conditions of various milling time and the content of process control agent (PCA), and their microstructure and magnetic properties were investigated to establish optimum processing conditions. The initial powders employed showed irregular shape and had a size ranging from 5 to $110\;{\mu}m$. After milling for 5 h, the shape of powders changed to round shape and their mean powder size was approximately $5\;{\mu}m$, which consisted of the agglomerated nano-sized particles with 15 nm in diameter. The coercivity was reduced with increasing the milling time, whereas the saturation magnetization increased. As the content of PCA increased, the powder size minutely decreased to approximately $7\;{\mu}m$ at the PCA content of 10 wt%. The XRD patterns showed that the main diffraction peaks disappeared apparently after milling, indicating the formation of amorphous structure. The measured values of coercivity were almost unchanged with increasing the content of PCA.

• Advances in materials Research
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• v.6 no.3
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• pp.245-255
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• 2017

High energy ball milling is employed to produce iron matrix- multiwall carbon nanotube (MWCNT) reinforced composite. The damage caused to MWCNT due to harsh ball milling condition and its influence on interfacial bonding is studied. Different amount of MWCNT is used to find the optimal percentage of MWCNT for avoidance of the formation of chemical reaction product at the matrix - reinforcement interface. Effect of process control agent is assessed by the use of different materials for the purpose. It is observed that ethanol as a process control agent (PCA) causes degradation of MWCNT reinforcements after milling for two hours whereas solid stearic acid used as process control agent, allows satisfactory conservation of MWCNT structure. It is further noted that at a high MWCNT content (~ 2wt.%), high energy ball milling leads to reaction of iron and carbon and forms iron carbide (cementite) at the iron-MWCNT interface. At low percentage of MWCNT, dissolution of carbon in iron takes place and the amount of reinforcement in iron matrix composite becomes negligibly small. However, under the present ball milling condition (ball to metal ratio~ 6:1 and 200 rpm vial speed) iron-1wt.% MWCNT composite of good interfacial bonding can retain the tubular structure of reinforcing MWCNT.

• 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.