• Journal of Powder Materials
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• v.9 no.4
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• pp.235-244
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• 2002

The effects of residual impurities on solid state sintering of the powder injection molded (PIMed) W-15wt%Cu nanocomposite powder were investigated. The W-Cu nanocomposite powder was produced by the mech-ano-chemical process consisting of high energy ball-milling and hydrogen reduction of W blue powder-cuO mixture. Solid state sintering of the powder compacts was conducted at $1050^{\circ}C$ for 2~10 h in hydrogen atmosphere. The den-sification of PIM specimen was slightly larger than that of PM(conventional PM specimen), being due to fast coalescence of aggregate in the PIM. The only difference between PIM and PM specimens was the amount of residual impurities. The carbon as a strong reduction agent effectively reduced residual W oxide in the PIM specimen. The $H_2O$ formed by $H_2$ reduction of oxide disintegrated W-Cu aggregates during removal process, on the contrary to this, micropore volume rapidly decreased due to coalescence of the disintegrated W-Cu aggregates during evolution of CO.It can be concluded that the higher densification was due to the earlier occurred Cu phase spreading that was induced by effective removal of residual oxides by carbon.

• KIEE International Transactions on Electrophysics and Applications
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• v.5C no.3
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• pp.119-123
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• 2005

Lithium titanium oxide as anode material for energy storage prepared by novel synthesis method. Li$_{4}$Ti$_{5}$O$_{12}$ based spinel-framework structures are of great interest material for lithium-ion batteries. We describe here Li$_{4}$Ti$_{5}$O$_{12}$ a zero-strain insertion material was prepared by novel sol-gel method and by high energy ball milling (HEBM) of precursor to from nanocrystalline phases. According to the X-ray diffraction and scanning electron microscopy analysis, uniformly distributed Li$_{4}$ Ti$_{5}$O$_{12}$ particles with grain sizes of 100nm were synthesized. Lithium cells, consisting of Li$_{4}$ Ti$_{5}$O$_{12}$ anode and lithium cathode showed the 173 mAh/g in the range of 1.0 $\~$ 3.0 V. Furthermore, the crystalline structure of Li$_{4}$ Ti$_{5}$O$_{12}$ didn't transform during the lithium intercalation and deintercalation process.

• Journal of the Korean Ceramic Society
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• v.44 no.5 s.300
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• pp.148-150
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• 2007

A process to synthesize $La_{0.8}Sr_{0.2}CrO_3$ (LSC), which is a promising material for use as a separator in a soild oxide fuel cell, is investigated in this study. LSC powders without secondary Phases could be synthesized with ultrasonic spray pyrolysis and a heat treatment at $1200^{\circ}C$ for 20 h; however, it showed an average diameter of $0.6{\mu}m$ with a wide particle size distribution. On the other hand, LSC powders synthesized with spray pyrolysis at $800^{\circ}C$, heat-treated at $900^{\circ}C$ for 5 h, ball-milled and finally heat-treated again at $1200^{\circ}C$ for 20 h showed a smaller average diameter of $0.3{\mu}m$ and narrower size distribution. Very few particles above $0.5{\mu}m$ were found. Thus, a proper combination of the heat treatment and milling process after spray pyrolysis it determined to be very important in synthesizing fine and uniform LSC perovskite powders.

• Korean Journal of Materials Research
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• v.9 no.6
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• pp.615-621
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• 1999

The new process in order to fabricate of Ni catalyst with high activity by the mechanochemical(MC) method which was combined the mechanical alloying(MA) and the chemical treatment process. The microstructure and characterization of mechanically alloyed Ni-5-wt% Al powder and Ni catalyst gained by alkali leaching were investigated byt he various analysis such as XRD, SEM-EDS, HRTEM and laser particle analyzer. The steady state powder with 1~2$\mu\textrm{m}$ mean particle size was obtained after 30hr milling with the PCA of 2 wt% stearic acid under the condition of grinding stainless steel ball to powder ratio of 60:1 and rotating speed fo 300rpm. According to result of HRTEM diffraction pattern, MA powder of the steady state was nanocrystalline $Al_3$$Ni_2$ intermetallic compound. Ni catalyst was obtained after KOH leaching of the steady state powder was about 20nm nanocrystalline which contained about 8 wt % Al.

• 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 Crystal Growth and Crystal Technology
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• v.14 no.4
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• pp.129-134
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• 2004

In this study, we investigated the effect of a nitrogen atom on the amorphization of V-Fe alloy through solid-gas reaction during mechanical alloying (MA). MA by planetary ball mill of $V_{70}Fe_{30}$ elemental powders was carried out under the nitrogen gas atmosphere. Amorphization has been observed after 160 hours of ball milling in this case. The DSC spectrum for the mechanically alloyed ($V_{70}Fe$_{30}$)_{0.89}N_{0.11}$ powders exhibits a sharp exothermic peak due to crystallization at about $600^{\circ}C$. Structural transformation from the bcc crystalline to amorphous states was also observed through X-ray and neutron diffractions. We take a full advantage of a negligibly small scattering length of the V atom in the neutron diffraction measurement. During amorphization process the octahedral unit, which is typical of a polyhedron formed in any crystal structures, was preferentially destroyed and transformed into the tetrahedral unit. Futhermore, neutron diffraction measurements revealed that a nitrogen atom is selectively situated at a center of the polyhedron formed by V atoms.

• Journal of Powder Materials
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• v.22 no.5
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• pp.356-361
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• 2015

Fe-30 wt% TiC composite powders are fabricated by in situ reaction synthesis after planetary ball milling of (Fe, $TiH_2$, Carbon) powder mixture. Two sintering methods of a pressureless sintering and a spark-plasma sintering are tested to densify the Fe-30 wt% TiC composite powder compacts. Pressureless sintering is performed at 1100, 1200 and $1300^{\circ}C$ for 1-3 hours in a tube furnace under flowing argon gas atmosphere. Spark-plasma sintering is carried out under the following condition: sintering temperature of $1050^{\circ}C$, soaking time of 10 min, sintering pressure of 50 MPa, heating rate of $50^{\circ}C/min$, and in a vacuum of 0.1 Pa. The curves of shrinkage and its derivative (shrinkage rate) are obtained from the data stored automatically during sintering process. The densification behaviors are investigated from the observation of fracture surface and cross-section of the sintered compacts. The pressureless-sintered powder compacts are not densified even after sintering at $1300^{\circ}C$ for 3 h, which shows a relative denstiy of 66.9%. Spark-plasma sintering at $1050^{\circ}C$ for 10 min exhibits nearly full densification of 99.6% relative density under the sintering pressure of 50 MPa.

• Korean Journal of Materials Research
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• v.12 no.8
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• pp.600-607
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• 2002

The Ni-Zn synthetic ferrite were acquired from thermally decomposing the metal nitrates Fe(NO$_3$)$_3$.$9H_2$O, Zn($NO_3$)$_2$.$6H_2$O, Ni($NO_3$)$_2$. $6H_2$O, and Cu($NO_3$)$_2$. $3H_2$O at $150^{\circ}C$ for 24 hours and was calcined at $500^{\circ}C$. Each of those was pulverized for 3, 6, 9, and 12 hours in a steel ball mill and was sintered between $700^{\circ}C$ and $1,000^{\circ}C$ for 1 hour, and then their microstructures and electromagnetic properties were examined. We could make the initial specimens chemically bonded in liquid at the temperature as low as $150^{\circ}C$, by using the melting points less than $200^{\circ}C$ of the metal nitrates instead of the mechanical ball milling, then narrowed a distance between the particles into a molecular level, and thus lowed sintering temperature by at least $200^{\circ}C$ to$ 300^{\circ}C$. Their initial permeability was 50 to 400 and their saturation magnetic induction density and coercive force 2,400 G and 0.3 Oe to 0.5 Oe each, which were similar to those of Ni- Zn ferrite synthesized in the conventional process. In the graph of initial permeability vs frequencies, we could observe a $180^{\circ}C$rotation of the magnetic domain, which appears in a broad band of microwave near the resonance frequency.

• Proceedings of the IEEK Conference
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• 2001.10a
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• pp.315-324
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• 2001

Mechanochemical effects that occurred in the fine grinding process of quartz particles using planetary ball mill was investigated. Quartz particles have been frequently utilized for optical materials, semiconductor molding materials. We determined that grinding for a long time can be create amorphous structures from the crystalline quartz by Mechanochemical effects. But, to be produced nano-composite particles that the critical grinding time reached for composite materials in a short time. Henceforth, a qualitative estimation must be conducted on the filler for EMC(Epoxy molding compound) materials. It can be produced mechanochemically treated composite materials and also an integrated grinding efficiency considering of the nano-composite amorphous structured particles. The mechanochemical characteristics were evaluated based on particle morphology, size distribution, specific surface area, density and the amount of amorphous phase materials into the particle surface. The grinding operation in the planetary ball mill can be classified into three stages. During the first stage, initial particle size was reduced for the increase of specific surface area. In the second stage, the specific surface areas increased in spite of the increase in particle size. The final stage as a critical grinding stage, the ground quartz was considered mechanochemically treated particles as a nano- composite amorphous structured particles. The development of amorphous phase on the particle surface was evaluated by X-ray diffractometry, thermal gravity analysis and IR spectrometer. The amount of amorphous phase of particles ground for 2048 minutes was 85.3% and 88.2% by X-ray analysis and thermal gravity analysis, respectively.

• Journal of the Korean Society for Heat Treatment
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• v.9 no.1
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• pp.1-11
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• 1996

Mechanical alloying is an effective process to finely distribute inert dispersoids in an Al-TM(TM is a transition metal) system. It has been considered that high melting point aluminides are formed by precipitation from supersaturated Al(Ti) powder. This analysis is based on the fact that much higher content of TM than the solubioity can be dissolved in alpha aluminum during the high energy ball milling. Thus, decomposition behavior of Ti in the Al(Ti) was considered very important. But it is confirmed that the higher portion of Ti than Al(Ti) solid solution is existed as nano-sized Ti particles in the MA powders by high energy ball nilling from the XRD spectrum and TEM analysis in this study. Therefore, the role of undissolved TM particles affect the formation of aluminides should be suitably considered. In this study, we present experimental observation on the formation of $Al_3Ti$ fron mechanical alloyed Al-Ti alloys in the hyperperitectic region. This study showed that, in the mechanically alloyed Al-20wt%Ti specimen, intermediate phase of cubic $Al_3Ti$ and tetragonal $Al_{24}Ti_8$ formed at $300{\sim}400^{\circ}C$ and $400{\sim}500^{\circ}C$, respectively, before the MA state reaches to equilibrium at higher temperatures. The formation behavior of $Ll_2-Al_3Ti$ is interpreted by interdiffusion of Al and Ti in solid state based on the fact that large amount of nano-sized Ti particles exist in the milled powder. Present analysis indicated undissolved Ti particles of nanosize should have played an important role initiation the formation of $Al_3Ti$ phase during annealing.