• Transactions of the Korean hydrogen and new energy society
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• v.16 no.3
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• pp.238-243
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• 2005

Mg and Mg-based alloys are most important hydrogen storage materials. It is a lightweight and low-cost materials with high hydrogen storage capacity. However, the formation of hydride at high temperature, the deterioration effect, the hydriding and dehydriding kinetics are bad factor for application. In this study, Mg and Ni have been produced by hydrogen induced mechanical alloying(HIMA) process. The raw materials, Mg(purity 99.9%) chip and Ni(purity 99.95%) chip was prepared by using a planetary ball mill apparatus(FRITSCH pulverisette 5). The balls to chips mass ratio(BCR) are 30:1. The hydrogen pressure induced 2.0MPa and milling times were 12, 24, 48, 72, 96 hours with a rotating speed of 200rpm. X-ray diffraction(XRD) analysis was made to characterize the crystallite size and misfit strain. The crystallite size measured by laser particle size analysis(PSA). Microstructure changes were investigated by scanning electron microscopy(SEM) and the transmission electron microscopy(TEM). The hydrogen storage properties were evaluated by using an Sivert's type automatic pressure-composition-therm(PCT) apparatus.

• 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 the Korean Crystal Growth and Crystal Technology
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• v.21 no.6
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• pp.246-252
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• 2011

The semiconducting $MnSi_{1.73}$ compound has been recognized as a thermoelectric material with excellent oxidation resistance and stable characteristics at elevated temperature. In the present work, we applied mechanical alloying (MA) technique to produce $MnSi_{1.73}$ compound using a mixture of elemental manganese and silicon powders. The mechanical alloying was carried out using a Fritsch P-5 planetary mill under Ar gas atmosphere. The MA powders were characterized by the X-ray diffraction with Cu-$K{\alpha}$ radiation, thermal analysis and scanning electron microscopy. Due to the observed larger loss of Si relative to Mn during mechanical alloying of $MnSi_{1.73}$, the starting composition of a mixture Mn-Si was modified to $MnSi_{1.83}$ and then $MnSi_{1.88}$. The single $MnSi_{1.73}$ phase has been obtained by mechanical alloying of $MnSi_{1.88}$ mixture powders for 200 hours. It is also found that the grain size of $MnSi_{1.73}$ compound powders analyzed by Hall plot method is reduced to 40 nm after 200 hours of milling.

• Progress in Superconductivity
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• v.8 no.1
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• pp.108-112
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• 2006

We fabricated Bi-2212/$SrSO_4$ bulk superconductors by the casting process and evaluated the effects of the powder mixing method and annealing temperature on the texture, microstructure, and critical current. In the process, the Bi-2212 powders were mixed with $SrSO_4$ by hand-mixing(HM) and planetary ball milling(PBM) method and then the powder mixtures were melted at $1100^{\circ}C{\sim}1200^{\circ}C$, solidified, and annealed. We observed that the rod made by the PBM had a more homogeneous microstructure and smaller $SrSO_4$ and second phases than that of the rod made by the HM, resulting in increased $I_c$. The $I_c$ of the rod also depended on the annealing temperature and the highest $I_c$ was obtained to be 200 A when prepared by HM at $1200^{\circ}C$ and annealed at $810^{\circ}C$ which is probably due to the moderate density and 2212 texture and the smaller and less second phase compared to that at higher temperature. The possible causes of the variations of $I_c$ with the powder mixing method and annealing temperature were related to the microstructural evolution based on the SEM, EPMA, and DTA analyses.

• Proceedings of the Korean Vacuum Society Conference
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• 2011.02a
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• pp.277-277
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• 2011

Mo-Cu 합금은 고강도이고 우수한 열전도성 및 전기전도성를 가지는 특성이 있어 현재 방열소재, 반도체 부품, 자동차 부품 등 여러 응용분야에서 연구가 활발히 진행되고 있다. 본 연구에서는 서로 고용성이 없는 Mo-Cu 합금을 제조하기 위해서 Mo, Cu 분말을 PBM (Planetary Ball Milling) 방법을 이용하여 제조 하였으며, 제조된 분말은 SPS (Spark Plasma Sintering) 공정을 이용하여 소결체를 제조하였다. Mo-Cu의 조성 변화는 Cu의 함유량을 각각 5at%Cu, 10at%Cu, 20at%Cu로 조절하여 수행하였으며, PBM 의 공정 변수로 회전수(RPM), 볼과 분말의 비율, 분산제의 양, 볼밀 시간, 분위기 변화를 주어 최적조건을 얻기 위한 실험을 진행하였다. PBM 방법을 이용하여 제조한 분말은 PSA (Particle Size Analysis)에 의해 분말의 크기를 측정하고 EDS(Energy Disperse X-ray Spectrometer) 분석에 의해 조성을 확인하였으며, XRD (X-Ray Diffraction) 분석에 의해 Cu peak이 사라지는 조건을 PBM의 최적조건으로 잡고 실험을 진행하였다. 소결체를 고밀도화하기 위해 소결공정을 SPS 방식으로 하였으며 소결체의 경도, 내마모성, 마찰계수 일함수 등을 분석하기 위해 소결체의 크기를 직경 30 mm 및 두께 5 mm로 설계하였고, 소결 공정 변수로 소결온도를 각각 $900^{\circ}C$, $1000^{\circ}C$, $1100^{\circ}C$, 소결압력을 50MPa, 60MPa, 70MPa, 유지시간을 0분, 10분, 20분으로 차이를 주어, 소결체의 밀도차이와 물성차이를 분석하였다. 그 결과 PBM의 최적조건으로는 5at%Cu 에서는 10h, 10at%Cu, 20at%Cu 에서는 20h의 최적의 밀링 시간을 확인하였고, 다른 공정 변수의 최적조건으로는 회전수 300RPM, 10:1의 볼과 분말 비, 분산제 4wt%, Ar 분위기라는 조건을 얻을 수 있었다. 각각의 공정변수 변화에 따른 소결체 최적밀도 달성조건, 소결체 물성 및 전기적 특성 등의 상관관계에 관하여 보고한다.

• Korean Journal of Materials Research
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• v.25 no.6
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• pp.274-278
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• 2015

The possibility of using the chemical precipitation method of up-cycled ammonium paratungstate (APT) was studied and compared with the thermal decomposition method. $WO_3$ particles were synthesized by chemical precipitation method using a 1:2 weight ratio of APT: Di-water. For thermal decomposition, APT powder was heated for 4h at $600^{\circ}C$ in air atmosphere. The reaction products were characterized by X-ray diffraction (XRD), X-ray fluorescence spectrometer (XRF), particle size analyzer (PSA), and field emission-scanning electron microscopy (FE-SEM). Thermogravimetric analysis (TGA) of the up-cycled APT allowed for the identification of the sequence of decomposition and reduction reactions that occurred during the heat treatment. TGA data indicated a total weight loss of 10.78% with the reactions completed in $658^{\circ}C$. The XRD results showed that APT completely decomposed to $WO_3$ by thermal decomposition and chemical precipitation. The particle size of the synthesized $WO_3$ powders by thermal decomposition with 2 h of planetary milling was around $2{\mu}m$ During the chemical precipitation process, the particle size of the synthesized $WO_3$ powders showed a round-shape with ${\sim}0.6{\mu}m$ size.

• Journal of Powder Materials
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• v.20 no.3
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• pp.215-220
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• 2013

In the present work, 6061 Al-$B_4C$ sintered composites containing different $B_4C$ contents were fabricated and their characteristic were investigated as a function of sintering temperature. For this, composite powders and their compacts with $B_4C$ various contents from 0 to 40 wt.% were fabricated using a planetary ball milling equipment and cold isostatic pressing, respectively, and then they were sintered in the temperature ranges of 580 to $660^{\circ}C$. Above sintering temperature of $640^{\circ}C$, real density was decreased due to the occurrence of sweat phenomena. In addition, it was realized that sinterability of 6061Al-$B_4C$ composite material was lowered with increasing $B_4C$ content, resulting in the decrease in its real density and at the same time in the increment of porosity.

• Korean Journal of Metals and Materials
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• v.50 no.12
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• pp.949-953
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• 2012

$MgH_2$ was employed as a starting material instead of Mg in this work. A sample with a composition of 94 wt% $MgH_2-6$ wt% Ni (called $MgH_2-6Ni$) was prepared by reactive mechanical grinding. The hydriding and dehydriding properties were then examined. An $MgH_2-Ni$ hydrogen storage alloy that does not require an activation process was developed. The alloy was prepared in a planetary ball mill by grinding for 4 h at a ball disc revolution speed of 250 rpm under a hydrogen pressure of about 12 bar. The sample absorbed 3.74 wt% H for 5 min, 4.07 wt% H for 10 min, and 4.41 wt% H for 60 min at 573 K under 12 bar $H_2$, and desorbed 0.93 wt% H for 10 min, 1.99 wt% H for 30 min, and 3.16 wt% H for 60 min at 573 K under 1.0 bar $H_2$. $MgH_2-6Ni$ after reactive mechanical grinding contained ${\beta}-MgH_2$ (a room temperature form of $MgH_2$), Ni, ${\gamma}-MgH_2$ (a high pressure form of $MgH_2$), and a very small amount of MgO. Reactive mechanical grinding of Mg with Ni is considered to facilitate nucleation, and to reduce the particle size of Mg. $Mg_2Ni$ formed during reactive mechanical grinding also increases the hydriding and dehydriding rates of the sample.

• Progress in Superconductivity
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• v.10 no.2
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• pp.79-86
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• 2009

We successfully fabricated C-doped ex-situ $MgB_2$ wires using two different methods such as mechanical alloying(MA) and combined process(CP) of in-situ and ex-situ. In the MA, the precursor powder was prepared with a mixture of $MgB_2$ and 1 at% C powders by planetary ball milling for 0-100 h. In the CP, on the other hand, C-doped $MgB_2$ powder was prepared with Mg, B, and C powders by in-situ process via compaction, sintering, and crushing. The powders prepared by two methods were loaded into Fe tube and then the assemblages were drawn by a conventional powder-in-tube technique. The MA treatment of C-added $MgB_2$ decreased the particles/grains size and resulted in C-doping into $MgB_2$ after sintering, improving the critical current density($J_c$) in high external magnetic field. For the C-doped $MgB_2$ wire by MA for 25 h, the $J_c$ was $4.1{\times}10^3A/cm^2$ at 5 K and 6.4 T, which was 5.9 times higher than that of pure and untreated $MgB_2$ wire. The CP also provided C-doping into $MgB_2$ and improved the $J_c$ in high magnetic field; the C-doped $MgB_2$ wire fabricated by CP exhibited a $J_c$ being 2.3 times higher than that of the ex-situ wire used commercial $MgB_2$ powder at 5 K and 6.0 T($2.7{\times}10^3A/cm^2\;vs.\;1.2{\times}10^3A/cm^2$).

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.10 no.4
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• pp.292-296
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• 2000

Mechenochemical reaction by planetary type ball mill is applied to prepare $Sm_2$$Fe_{17}$$N_{x}$ permanent magnet powders. Starting from pure samarium and iron powders, the formation process of hard magnetic $Sm_2$$Fe_{17}$$N_{x}$ phase by ball milling and a subsequent solid state reaction were studied. At as-milled stage powders were found to consist of amorphous Sm-Fe and $\alpha$-Fe phases in all composition of $Sm_2$$Fe_{100-x}$(x = 11, 13, 15). The dependence of starting composition of elemental powder on the formation of Sm-Fe intermetallic compound was investigated by heat treatment of as-milled powders. When Sm concentration was 15 at%, heat-treated powder consists of mostly $Sm_2$$Fe_{17}$$N_{x}$single phase. For synthesizing of hard magnetic $Sm_2$$Fe_{17}$$N_{x}$ compound, additional nitriding treatment was carried out under $N_2$gas atmosphere at $450^{\circ}C$. The increase in the coercivity and remanence was parallel to the nitrogen content which increased drastically at first and then gradually as the nitriding time was extended. The ball-milled Sm-Fe-N powders were expected to be prospective materials for synthesizing of permanent magnet with high performance.