• 한국분말재료학회지
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• 제15권5호
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• pp.371-377
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• 2008

This paper deals with the phase analysis of $MgB_2$ bulk using spark plasma sintering process after ball milling. Mg and amorphous B powders were used as raw materials, and milled by planetary-mill for 9 hours at argon atmosphere. In order to confirm formation of $MgB_2$ phase, DTA and XRD were used. The milled powders were fabricated to $MgB_2$ bulk at the various temperatures by Spark Plasma Sintering. The fabricated $MgB_2$ bulk was evaluated with XRD, EDS, FE-SEM and PPMS. In the DTA result, reaction on formation of $MgB_2$ phase started at $340^{\circ}C$. This means that ball milling process improves reactivity on formation of $MgB_2$ phase. The $MgB_2$ MgO and FeB phases were characterized from XRD result. MgO and FeB were undesirable phases which affect formation of $MgB_2$ phase, and it's distribution could be confirmed from EDS mapping result. Spark Plasma Sintered sample for 5 min at $700^{\circ}C$ was relatively densified and it's density and transition temperature showing super conducting property were $1.87\;g/cm^3$ and 21K.

• 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.

• Applied Microscopy
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• 제32권4호
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• pp.311-317
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• 2002

입자 크기에 따라 상전이 경로가 달라지며 매우 큰 응집체로 존재하는 gibbsite 분말과 같은 재료의 정량적인 전이 구조 분석의 전제로서 입자 크기가 선택적인 TEM 시편의 준비가 절실히 요구된다. 입자 크기 선택성을 실현한 TEM 시편 준비의 방법론을 확립하기 위한 방안으로서 본 실험이 전개되었다. 약 1 wt%의 gibbsite 원료 분말을 에탄올 용매에 혼합 한 뒤, ball-milling에 의해 조분쇄 처리를 하고 증류수에 1 : 19의 비로 희석된 분산 조제, Darvan C, 0.25 vol%의 첨가와 함께 ultrasonic 처리를 하여 gibbsite suspension을 만들었다. 제조된 gibbsite suspension의 누적 농도 변화 관찰에 의한 침강 시간의 조정 후 정적 침강 분리에 의해 nm 크기별로 분리된 TEM 시편을 만들 수가 있었다. 시편의 전체적인 양상은 SEM으로 관찰하였고 개개 입자들의 morphology 는 TEM으로 분석하였다. 또한, 공정 과정 중의 상변화 가능성을 검토하기 위해 XRD 분석을 실시하였다.

• 한국분말재료학회지
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• 제23권4호
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• pp.282-286
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• 2016

A sintered body of $TiB_2$-reinforced iron matrix composite ($Fe-TiB_2$) is fabricated by pressureless-sintering of a mixture of titanium hydride ($TiH_2$) and iron boride (FeB) powders. The powder mixture is prepared in a planetary ball-mill at 700 rpm for 3 h and then pressurelessly sintered at 1300, 1350 and $1400^{\circ}C$ for 0-2 h. The optimal sintering temperature for high densities (above 95% relative density) is between 1350 and $1400^{\circ}C$, where the holding time can be varied from 0.25 to 2 h. A maximum relative density of 96.0% is obtained from the ($FeB+TiH_2$) powder compacts sintered at $1400^{\circ}C$ for 2 h. Sintered compacts have two main phases of Fe and $TiB_2$ along with traces of TiB, which seems to be formed through the reaction of TiB2 formed at lower temperatures during the heating stage with the excess Ti that is intentionally added to complete the reaction for $TiB_2$ formation. Nearly fully densified sintered compacts show a homogeneous microstructure composed of fine $TiB_2$ particulates with submicron sizes and an Fe-matrix. A maximum hardness of 71.2 HRC is obtained from the specimen sintered at $1400^{\circ}C$ for 0.5 h, which is nearly equivalent to the HRC of conventional WC-Co hardmetals containing 20 wt% Co.

• 센서학회지
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• 제17권6호
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• pp.418-424
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• 2008

The PZT based piezoelectric thick films prepared by screen printing method have been mainly used as a functional material for MEMS applications due to their compatibility of MEMS process. However the screen printed thick films generally reveal poor electrical and mechanical properties because of their porous microstructure. To improve microstructure we mixed attrition milled powder with ball milled powder of 0.01Pb$(Mg_{1/2}W_{1/2})O_3$-0.41Pb$(Ni_{1/3}Nb_{2/3})O_3$-$0.35PbTiO_3$-$0.23PbZrO_3$+0.1 wt% ${Y_2}{O_3}$+1.5 wt% ZnO composition. By mixing 25 % of attrition milled powder and 75 % of ball milled powder, the broadest particle size distribution was obtained, leading to a dense thick film with crack-free microstructure and improved dielectric properties. The X-ray diffraction analysis revealed that the film was in wellcrystallized perovskite phase. The remanent polarization was increased from $13.7{\mu}C/cm^2$ to $23.3{\mu}C/cm^2$ at the addition of 25 % attrition milled powder.

• 한국세라믹학회지
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• 제16권1호
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• pp.13-20
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• 1979

High purity alumina has been extracted form low grade Korean alunite. Alunite ore was treated by 15% $NH_4OH$ solution, followed by 10% $H_2SO_4$ leaching and metallic impurities such as Fe and Ti were removed by solvent extraction method. Alumina prepared by the extraction process was 99.9% in purity. Hot Petroleum Drying Method has been employed for the preparation of uniformly fine alumina powder, using chemical reagent aluminum sulfate and ammonium aluminum sulfate extrated from Korea alunite. The sinterability of alumina powder prepared by Hot Petroleum Drying Method was shown to be improved in comparison with the one treated by other methods such as ball milling method, but dry pressing was difficult due to the agglomeration of calcined powder. The best slip of alumina powder prepared by Hot Petroleum Drying Method contained a lower soild content than the one treated by other methods. The alumina body formed by soild and drain casting with the former alumina powder showed a higher sintered density.

• 한국분말재료학회지
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• 제8권2호
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• pp.110-116
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• 2001

Abstract To investigate the effect of mechanical alloying process to thermoelectric properties of PbTe sintered body, Pb-Te mixed powder with Pb : Te : 1 : 1 composition was mechanically alloyed using tumbler-ball mill. Thermoelectric properties of the sintered body were evaluated by measuring of the Seebeck coefficient and specific electric resistivity from the room temperature to 50$0^{\circ}C$. Sintered body of only mechanically alloyed PbTe powder showed p-type behavior at the room temperature, and occurred type transition from p-type to n-type at about 30$0^{\circ}C$. PbTe sintered body which was fabricated using heat treated powder in $H_2$ atmosphere after mechanical alloying showed stable n-type behavior under 50$0^{\circ}C$. N-type PbTe sintered body fabricated by mechanical alloying process had 4 times higher power factor than that fabricated by the melt-crushing process. Application of a mechanical alloying process to fabricate of n-type PbTe thermoelectric material seemed to be useful to increase the power factor of PbTe sintered body.

• 한국분말재료학회지
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• 제7권1호
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• pp.19-26
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• 2000

Al-Cr-Zr metal powders were prepared by cryo-milling(-75$^{\circ}C$),ambi-milling(25$^{\circ}C$) and warm-milling(200$^{\circ}C$) to investige the effect of milling temperature. The morphogical changes and microstructural evolution of Al-6wt.%Cr-3wt.%Zr metal powder ball milling were investigated by SEM, OM and XRD. The cryo-milling at -75$^{\circ}C$ caused the more refinement of powder particle size than ambi-milling and warm-milling. The partic morpholgy of Al-Cr-Zr metal powders changed changes into spheroidal particles at 25$^{\circ}C$and spherical particles at 200$^{\circ}C$The spherical particles were formed by agglomertion and contiuous wrapping of the spheroidal particles. The calculated Al crystallite size in Al-Cr-Zr metal powders by the Scherer equation were refined rapidly for short milling time -75$^{\circ}C$compared with milling at 25$^{\circ}C$ and 200$^{\circ}C$.

• 한국분말재료학회지
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• 제4권3호
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• pp.188-195
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• 1997

In most of sintered metal powder compacts, the sintered density distribution is controlled to be as high and uniform as possible to ensure the required mechanical properties. In general, the density distribution in the compacts is not uniform and not easy to measure. In the present study, a method for measuring the density distribution was developed, based on the indentation force equation by which the hardness and the relative density were related. The indentation force equation, expressed as a function of strength constant, workhardening coefficient and relative density, was obtained by finite element analysis of rigid-ball indentation on sintered powder metal compacts. The present method was verified by comparing the predicted density distribution in the sintered Fe-0.5%C-2%Cu compacts with that obtained by experiments, in which the density distribution was directly measured by machining the compacts from the outer surface progressively.

• 한국분말야금학회:학술대회논문집
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• 한국분말야금학회 2006년도 Extended Abstracts of 2006 POWDER METALLURGY World Congress Part2
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• pp.1331-1332
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• 2006

The present investigation has attemped to optimize hydrogen reduction process for the mass production of Fe-8wt%Ni nanoalloy powder from ball milled $Fe_2O_3-NiO$ powder. In-situ hygrometry study was performed to monitor the reduction behavior in real time through measurement of water vapor outflowing rate. It was found that the reduction process can be optimized by taking into account the apparent influence of water vapor trap in the reactor on reduction kinetics which strongly depends on gas flow rate, reactor volume and reduction.