• Title/Summary/Keyword: Spark Plasma Sintering

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방전플라즈마 소결법으로 제조한 Mo-Cu 합금 소결체의 물성 및 전기적 특성에 관한 연구

  • Lee, Han-Chan;Mun, Gyeong-Il;Lee, Bung-Ju;Sin, Baek-Gyun
    • 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.

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Effect of Space Holder Content on Pore Size and Distribution in HA/β-TCP Composites Consolidated by SPS (SPS로 제조된 HA/β-TCP 복합재의 기공의 크기와 분포에 미치는 지지체 량의 영향)

  • Lee, Tack;Woo, Kee-Do;Kang, Dong-Soo;Lee, Hae-Cheol;Jang, Jun-Ho
    • Korean Journal of Materials Research
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    • v.25 no.4
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    • pp.165-170
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    • 2015
  • Ceramics biomaterials are useful as implant materials in orthopedic surgery. In this study, porous HA(hydroxyapatite)/${\beta}$-TCP(tricalcium phosphate) composite biomaterials were successfully fabricated using HA/${\beta}$-TCP powders with 10-30 wt% $NH_4HCO_3$ as a space holder(SH) and $TiH_2$ as a foaming agent, and MgO powder as a binder. The HA/${\beta}$-TCP powders were consolidated by spark plasma sintering(SPS) process at $1000^{\circ}C$ under 20 MPa conditions. The effect of SH content on the pore size and distribution of the HA/${\beta}$-TCP composite was observed by scanning electron microscopy(SEM) and a microfocus X-ray computer tomography system(SMX-225CT). These microstructure observations revealed that the volume fraction of the pores increased with increasing SH content. The pore size of the HA/${\beta}$-TCP composites is about $400-500{\mu}m$. The relative density of the porous HA/${\beta}$-TCP composite increased with decreasing SH content. The porous HA/${\beta}$-TCP composite fabricated with 30%SH exhibited an elastic modulus similar to that of cortical bone; however, the compression strength of this composite is higher than that of cortical bone.

Investigation on the Thermoelectric Properties of Bismuth Telluride Matrix Composites by Addition of Graphene Oxide Powders (그래핀 산화물 분말 첨가에 의한 비스무스 텔루라이드 기지 복합재료의 열전에너지변환 특성 고찰)

  • Kim, Kyung Tae;Min, Taesik;Kim, Dong Won
    • Journal of Powder Materials
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    • v.23 no.4
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    • pp.263-269
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    • 2016
  • Graphene oxide (GO) powder processed by Hummer's method is mixed with p-type $Bi_2Te_3$ based thermoelectric materials by a high-energy ball milling process. The synthesized GO-dispersed p-type $Bi_2Te_3$ composite powder has a composition of $Bi_{0.5}Sb_{1.5}Te_3$ (BSbT), and the powder is consolidated into composites with different contents of GO powder by using the spark plasma sintering (SPS) process. It is found that the addition of GO powder significantly decreases the thermal conductivity of the pure BSbT material through active phonon scattering at the newly formed interfaces. In addition, the electrical properties of the GO/BSbT composites are degraded by the addition of GO powder except in the case of the 0.1 wt% GO/BSbT composite. It is found that defects on the surface of GO powder hinder the electrical transport properties. As a result, the maximum thermoelectric performance (ZT value of 0.91) is achieved from the 0.1% GO/BSbT composite at 398 K. These results indicate that introducing GO powder into thermoelectric materials is a promising method to achieve enhanced thermoelectric performance due to the reduction in thermal conductivity.

Stretch-Flangeability of Harmonic Structure Material Manufactured by Powder Metallurgy Method (분말야금법으로 제조한 하모닉 구조재료의 신장플랜지 가공성)

  • Yoon, Jae Ik;Lee, Hak Hyeon;Park, Hyung Keun;Ameyama, Kei;Kim, Hyoung Seop
    • Journal of Powder Materials
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    • v.24 no.2
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    • pp.128-132
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    • 2017
  • Harmonic structure materials are materials with a core-shell structure having a shell with a small grain size and a core with a relatively large grain size. They are in the spotlight because their mechanical properties reportedly feature strength similar to that of a sintered powder with a fine grain size and elongation similar to that of a sintered powder with a coarse grain size at the same time. In this study, the tensile properties, microstructure, and stretch-flangeability of harmonic structure SUS304L made using powder metallurgy are investigated to check its suitability for automotive applications. The harmonic powders are made by mechanical milling and sintered using a spark plasma sintering method at 1173 K and a pressure of 50 MPa in a cylindrical die. The sintered powders of SUS304L having harmonic structure (harmonic SUS304L) exhibit excellent tensile properties compared with sintered powders of SUS304L having homogeneous microstructure. In addition, the harmonic SUS304L has excellent stretch-flangeability compared with commercial advanced high-strength steels (AHSSs) at a similar strength grade. Thus, the harmonic SUS304L is more suitable for automotive applications than conventional AHSSs because it exhibits both excellent tensile properties and stretch-flangeability.

Effect of High-Energy Ball Milling on Thermoelectric Transport Properties in CoSb3 Skutterudite (고에너지 볼 밀링이 Skutterudite계 CoSb3의 열전 및 전하 전송 특성에 미치는 영향)

  • Nam, Woo Hyun;Meang, Eun-Ji;Lim, Young Soo;Lee, Soonil;Seo, Won-Seon;Lee, Jeong Yong
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.28 no.12
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    • pp.852-856
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    • 2015
  • In this study, we investigate the effect of high-energy ball milling on thermoelectric transport properties in double-filled $CoSb_3$ skutterudite ($In_{0.2}Yb_{0.1}Co_4Sb_{12}$). $In_{0.2}Yb_{0.1}Co_4Sb_{12}$ powders are milled using high-energy ball milling for different periods of time (0, 5, 10, and 20 min), and the milled powders are consolidated into bulk samples by spark plasma sintering. Microstructure analysis shows that the high-energy ball milled bulk samples are composed of nano- and micro-grains. Because the filling fractions are reduced in the bulk samples due to the kinetic energy of the high-energy ball milling, the carrier concentration of the bulk samples decreases with the ball milling time. Furthermore, the mobility of the bulk samples also decreases with the ball milling time due to enhanced grain boundary scattering of electrons. Reduction of electrical conductivity by ball milling has a decisive effect on thermoelectric transport in the bulk samples, power factor decreases with the ball milling time.

Thermoelectric Properties of Bi2Te2.7Se0.3 Powder Synthesized by an Oxide-Reduction Process (산화물 환원공정에 의해 제조된 Bi2Te2.7Se0.3 분말의 열전특성)

  • Park, Bae-Gun;Lee, Gil-Geun;Kim, Woo-Yeol;Ha, Gook-Hyun
    • Journal of Powder Materials
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    • v.18 no.5
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    • pp.437-442
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    • 2011
  • The present study focused on the synthesis of Bi-Te-Se-based powder by an oxide-reduction process, and analysis of the thermoelectric properties of the synthesized powder. The phase structure, chemical composition, and morphology of the synthesized powder were analyzed by XRD, EPMA and SEM. The synthesized powder was sintered by spark plasma sintering. The thermoelectric properties of the sintered body were evaluated by measuring its Seebeck coefficient, electrical resistivity, and thermal conductivity. $Bi_2Te_{2.7}Se_{0.3}$ powder was synthesized from a mixture of $Bi_2O_3$, $TeO_2$, and $SeO_2$ powders by mechanical milling, calcination, and reduction. The sintered body of the synthesized powder exhibited n-type thermoelectric characteristics. The thermoelectric properties of the sintered bodies depend on the reduction temperature. The Seebeck coefficient and electrical resistivity of the sintered body were increased with increasing reduction temperature. The sintered body of the $Bi_2Te_{2.7}Se_{0.3}$ powder synthesized at $360^{\circ}C$ showed about 0.5 of the figure of merit (ZT) at room temperature.

단일 타겟을 이용한 반응성 마그네트론 스퍼터링 공정에 의한 나노 복합구조의 MoN-Cu 코팅층 형성 기술 개발

  • Jeong, Deok-Hyeong;Lee, Han-Chan;Sin, Seung-Yong;Mun, Gyeong-Il
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.237-237
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    • 2010
  • 에너지소비와 엔진 부품의 마모문제를 해결하기 위해, soft-phase를 doping한 hard상의 coating에 대한 실험이 최근 중요한 연구 테마로서 진행 중이다. 특히 MoN-Cu coating은 미국 Argon 연구소의 Erdemer박사 등에 의해, 고온 및 상온 윤활성이 우수한 코팅층으로 보고된 이후 많은 연구가 진행되고 있다. 그러나 기존 연구는 Mo와 Cu의 원소타겟을 이용한 연구가 주력이 되었다. 높은 경도와 저온 고온에서의 낮은 나노 혼합물 코팅 종류는 일반적으로 Mo와 Cu와 같은 원소 합금을 이용한 다수 타겟을 이용한 공정에 의해 진행되어왔다. 이러한 복수의 타겟에 의해 증착 동안에는, 정확한 조성, 큰 크기의 시편들의 균일 증착을 조절하기가 쉽지 않다. 또한, 코팅층에 3번째 성분을 추가하기가 어렵다는 문제점이 있다. 본 연구에서는, 최상의 마찰계수와 표면경도를 보이는 MoN-Cu층을 형성시키기 위하여 합금으로 단일 타겟을 제조하였다. 이를 위한 최적 조성을 결정하기 위하여 Mo, Cu 단일 타겟을 이용한 Unbalanced Magnetron sputtering 법으로 다양한 Cu 함량의 MoN+Cu 합금을 제조하였으며, 이에 대한 경도 및 마찰계수 측정을 통해 최적의 Cu 함량을 결정하였다. 이러한 최적 조성의 Cu 타겟제조를 기계적 합금화와 Spark plasma sintering 기술을 이용하여 제작하였으며, 복수의 합금 타겟과 단일 합금 타겟으로 제조된 코팅층의 물성 비교를 통해 합금 타겟의 우수성 여부를 확인하고자 하였다. 증착된 두 조건의 물성을 비교 단일 타겟은 두가지 타겟으로 증착한 것보다 비슷한 조성에서 경도가 높았으며 경도가 비슷한 조성에서는 마찰계수가 낮았다. 또 입자는 10 at.% Cu 조성에 대해 단일타겟이 50nm 결정립을 갖는 반해 단일타겟은 측정이 불가능할 정도의 미세한 결정립을 가졌다. Erdemir의 연구 결과에 의하면, Cu 함량이 증가함에 따라 columnar 형태의 코팅층구조가 나노 구조로 변한다고 하였는데, 본 연구에서 복수의 원소 타겟에서는 확인이 안되었으며, 단일 합금 타겟에서 완벽한 featurless 형태의 코팅층 구조와 우수한 조도의 박막층을 얻을 수 있었다. 이렇게 제조된 다양한 코팅층에 대한 마찰계수 측정이 진행중이다.

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Study on material properties of $Cu-TiB_2$ nanocomposite ($Cu-TiB_2$ 나노 금속복합재의 물성치에 대한 연구)

  • Kim Ji-Soon;Chang Myung-Gyu;Yum Young-Jin
    • Composites Research
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    • v.19 no.2
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    • pp.28-34
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    • 2006
  • [ $Cu-TiB_2$ ] metal matrix composites with various weight fractions of $TiB_2$ were fabricated by combination of manufacturing process, SPS (self-propagating high-temperature synthesis) and SPS (spark plasma sintering). The feasibility of $Cu-TiB_2$ composites for welding electrodes and sliding contact material was investigated through experiments on the tensile properties, hardness and wear resistance. To obtain desired properties of composites, composites are designed according to reinforcement's shape, size and volume fraction. Thus proper modeling is essential to predict the effective material properties. The elastic moduli of composites obtained by FEM and tensile test were compared with effective properties from the original Eshelby model, Eshelby model with Mori-Tanaka theory and rule-of-mixture. FEM result showed almost the same value as the experimental modulus and it was found that Eshelby model with Mori-Tanaka theory predicted effective modulus the best among the models.

Reduction of Thermal Conductivity Through Complex Microstructure by Dispersion of Carbon Nanofiber in p-Type Bi0.5Sb1.5Te3 Alloys

  • P. Sharief;B. Madavali;Y. Sohn;J.H. Han;G. Song;S.H. Song;S.J. Hong
    • Archives of Metallurgy and Materials
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    • v.66 no.3
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    • pp.803-808
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    • 2021
  • The influence of nano dispersion on the thermoelectric properties of Bi2Te3 was actively investigating to wide-spread thermoelectric applications. Herein this report, we have systematically controlled the microstructure of Bi0.5Sb1.5Te3 (BST) alloys through the incorporation of carbon nanofiber (CNF), and studied their effect on thermoelectric properties, and mechanical properties. The BST/x-CNF (x-0, 0.05, 0.1, 0.2 wt.%) composites powder was fabricated using high energy ball milling, and subsequently consolidated the powder using spark plasma sintering. The identification of CNF in bulk composites was analyzed in Raman spectroscopy and corresponding CNF peaks were recognized. The BST matrix grain size was greatly reduced with CNF dispersion and consistently decreased along CNF percentage. The electrical conductivity was reduced and Seebeck coefficient varied in small-scale by embedding CNF. The thermal conductivity was progressively diminished, obtained lattice thermal conductivity was lowest compared to bare sample due to induced phonon scattering at interfaces of secondary phases as well as highly dense fine grain boundaries. The peak ZT of 0.95 achieved for 0.1 wt.% dispersed BST/CNF composites. The Vickers hardness value of 101.8 Hv was obtained for the BST/CNF composites.

Fabrication and densification of Heusler Fe2VAl alloy powders by mechanical alloying (MA법에 의한 Heusler Fe2VAl 합금분말의 제조 및 치밀화)

  • Kim, Kwang-Duk;Lee, Chung-Hyo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.23 no.1
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    • pp.51-57
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    • 2013
  • We have applied mechanical alloying (MA) to produce Heusler $Fe_2VAl$ thermoelectric alloy using a mixture of elemental $Fe_{50}V_{25}Al_{25}$ powders. An optimal milling and heat treatment conditions to obtain the single phase of Fe2VAl compound with fine microstructure were investigated by X-ray diffraction and differential scanning calorimetry (DSC) measurement. The $Fe_{50}V_{25}Al_{25}$ MA sample ball-milled for 60 hours exhibits a bcc ${\alpha}$-(Fe,V,Al) solid solution. Single phase of Heusler $Fe_2VAl$ compound can be obtained by MA of $Fe_{50}V_{25}Al_{25}$ mixture for 60 hours and subsequently heated up to $700^{\circ}C$. Sintering of the MA powders was performed in a spark plasma sintering (SPS) machine using graphite dies at $900{\sim}1000^{\circ}C$ under 60 MPa. The Vickers hardness of bulk sample sintered at $1000^{\circ}C$ was high value of Hv 870. All compact bodies have a high relative density above 90 % with metallic glare on the surface.