• Title/Summary/Keyword: spark plasma sintering (SPS)

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방전 플라즈마 소결 공법을 이용한 FSW-Tool 용 $WC-5Mo_2C-5Co$ 소결체 제조와 기계적 특성 평가

  • Yun, Hui-Jun;Park, Hyeon-Guk;Lee, Seung-Min;Bang, Han-Seo;Bang, Hui-Seon;O, Ik-Hyeon
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.10a
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    • pp.40.2-40.2
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    • 2011
  • 초경합금은 경도가 높은 재료를 말하며 일반적으로는 탄화텅스텐(WC)계 재료를 말한다. 국내 현재 초경합금 동향은 반도체 산업, 내마모성 공구, 절삭공구, 금형 등 많은 분야에 사용되어지고 있다. 또한 최근 들어 FSW (Friction Stir Welding, FSW)기술이 발전함에 따라 접합기술개발이 다양화되면서 FSW Tool의 고성능의 초경 재료가 요구되어지며 장수명의 Tool개발이 되어야 한다. 국내에서는 초경 합금 재료로 사용되어지고 있는 텅스텐 카바이드(WC)와 코발트(Co)를 이용하여 많은 연구가 진행되었다. 본 실험에서는 텅스텐 카바이드와 코발트 및 몰르브덴 카바이드를 혼합하여 소결체를 제조하였다. 실험에 사용된 텅스텐 카바이드는 높은 경도를 가지고 강한 취성을 나타내며, 소결에 어려운 단점이 있다. 이러한 단점을 코발트와 몰리브덴 카바이드를 첨가하여 소결온도를 낮춰주는 역할과 액상 소결시 텅스텐카바이드 입자사이에 침투하여 액상소결에 의한 치밀화가 가능하게 해주며 인성이 향상되어 고인성 재료를 만들 수 있었다. 본 실험에서는 합성과 치밀화가 동시에 진행되는 SPS (Spark Plasma Sintering:SPS) 장비를 이용하여 실험을 진행하였다. 이 방법은 방전플라즈마 소결 공법으로, 기존의 연소법과 열간 가압기술(Hot-press, HIP)을 결합한 방식으로 단 시간, 단일공정으로 치밀한 소결체를 얻을 수 있는 장점이 있다. 본 연구에서는 $WC-5Mo_2C$-5wt%Co 소결체 제조를 위해 원소 분말을 Horizontal ball milling 혼합하였다. 균일하게 혼합된 분말을 흑연다이에 충진하여 펄스전류와 기계적 압력을 동시에 가하여 $WC-5Mo_2C-5Co$ 복합재료를 제조하고 소결체의 밀도, 순도, 상변태, 미세조직 등을 분석 및 평가하였다. SPS공정 조건은 고진공하에서 $1,200^{\circ}C$-60MPa, 펄스비 12:1 조건으로 수행하였으며, 얻어진 $WC-5Mo_2C-5Co$ 소결체의 상대 밀도는 98%이상 이였다. 또한, 결정립 크기는 약 400 nm였으며, 경도는 $2,453kg/mm^2$를 나타내었다.

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Synthesis and Properties of Amorphous Matrix Composites using Cu-based/Ni-based Amorphous Powders (Cu계 및 Ni계 비정질 합금 분말을 이용한 비정질기지 복합재의 제조 및 특성)

  • Kim Taek-Soo;Lee Jin-Kyu;Kim Hwi-Jun;Bae Jung-Chan
    • Journal of Powder Materials
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    • v.12 no.6 s.53
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    • pp.406-412
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    • 2005
  • This work is to present a new synthesis of metallic glass (MG)/metallic glass (MG) composites using gas atomization and spark plasma sintering (SPS) processes. The MG powders of $Cu_{54}Ni_6Zr_{22}Ti_{18}$ (CuA) and $Ni_{59}Zr_{15}Ti_{13}Nb_7Si_3Sn_2Al_1$(NiA) as atomized consist of fully amorphous phases and present a different thermal behavior; $T_g$ (glass transition temperature) and $T_x$ (crystallization temperature) are 716K and 765K for the Cu base powder, but 836K and 890K for the Ni base ones, respectively. SPS process was used to consolidate the mixture of each amorphous powder, being $CuA/10\%NiA\;and\;NiA/10\%CuA$ in weight. The resultant phases were Cu crystalline dispersed NiA matrix composites as well as NiA phase dispersed CuA matrix composites, depending on the SPS temperatures. Effect of the second phases embedded in the MG matrix was discussed on the micro-structure and mechanical properties.

Piezoelectric Properties in ZnO Dopped (Na,K)NbO3 Ceramics (ZnO가 첨가된 (Na,K)NbO3계 세라믹스의 압전 특성)

  • Ryu Sung-Lim;Kweon Soon-Yong;Ur Soon-Chul;Kim Si-Chul;Yoo Ju-Hyun
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.19 no.8
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    • pp.707-711
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    • 2006
  • ZnO was doped up to 0.3 wt% for improving the electrical properties of lead-free $[Li_{0.04}(Na_{0.44}Ko_{0.52})-(Nb_{0.86}\;Ta_{0.10}\;Sb_{0.04})]O_3$ piezoelectric ceramics. The ceramics were fabricated with the conventional sintering processes. Crystal structure of the samples was tetragonal phase regardless of ZnO amount. However, the piezoelectric properties were varied with the ZnO amount. The electro-mechanical coupling factor $(k_p)$ was with the ZnO amount up to 0.2 wt% but decreased with the further addition. the maximum value of $k_p$ was 0.475. Density, piezoelectric charge constant and relative dielectric constant was also showed maximum value at 0.2 wt%. The maximum values are $4.75g/cm^3$, 275 pC/N, 1403, respectively. In contrast, the mechanical quality factor $(Q_m)$ was not varied with increasing the ZnO addition up to 0.2 wt% but rapidly increased at 0.3 wt%.

The Development of an Electroconductive SiC-ZrB2 Composite through Spark Plasma Sintering under Argon Atmosphere

  • Lee, Jung-Hoon;Ju, Jin-Young;Kim, Cheol-Ho;Park, Jin-Hyoung;Lee, Hee-Seung;Shin, Yong-Deok
    • Journal of Electrical Engineering and Technology
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    • v.5 no.2
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    • pp.342-351
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    • 2010
  • The SiC-$ZrB_2$ composites were fabricated by combining 30, 35, 40, 45 and 50 vol. % of zirconium diboride ($ZrB_2$) powders with silicon carbide (SiC) matrix. The SiC-$ZrB_2$ composites and the sintered compacts were produced through spark plasma sintering (SPS) under argon atmosphere, and its physical, electrical, and mechanical properties were examined. Also, the thermal image analysis of the SiC-$ZrB_2$ composites was examined. Reactions between $\beta$-SiC and $ZrB_2$ were not observed via x-ray diffraction (XRD) analysis. The apparent porosity of the SiC+30vol.%$ZrB_2$, SiC+35vol.%$ZrB_2$, SiC+40vol.%$ZrB_2$, SiC+45vol.%$ZrB_2$ and SiC+50vol.%$ZrB_2$ composites were 7.2546, 0.8920, 0.6038, 1.0981, and 10.0108%, respectively. The XRD phase analysis of the sintered compacts demonstrated a high phase of SiC and $ZrB_2$. Among the $SiC+ZrB_2$ composites, the SiC+50vol.%$ZrB_2$ composite had the lowest flexural strength, 290.54MPa, the other composites had more than 980MPa flexural strength except the SiC+30vol.%$ZrB_2$ composite; the SiC+40vol.%$ZrB_2$ composite had the highest flexural strength, 1011.34MPa, at room temperature. The electrical properties of the SiC-$ZrB_2$ composites had positive temperature coefficient resistance (PTCR). The V-I characteristics of the SiC-$ZrB_2$ composites had a linear shape in the temperature range from room to $500^{\circ}C$. The electrical resistivities of the SiC+30vol.%$ZrB_2$, SiC+35vol.%$ZrB_2$, SiC+40vol.%$ZrB_2$ SiC+45vol.%$ZrB_2$ and SiC+50vol.%$ZrB_2$ composites were $4.573\times10^{-3}$, $1.554\times10^{-3}$, $9.365\times10^{-4}$, $6.999\times10^{-4}$, and $6.069\times10^{-4}\Omega{\cdot}cm$, respectively, at room temperature, and their resistance temperature coefficients were $1.896\times10^{-3}$, $3.064\times10^{-3}$, $3.169\times10^{-3}$, $3.097\times10^{-3}$, and $3.418\times10^{-3}/^{\circ}C$ in the temperature range from room to $500^{\circ}C$, respectively. Therefore, it is considered that among the sintered compacts the SiC+35vol.%$ZrB_2$, SiC+40vol.%$ZrB_2$ and SiC+45vol.%$ZrB_2$ composites containing the most outstanding mechanical properties as well as PTCR and V-I characteristics can be used as an energy friendly ceramic heater or ohmic-contact electrode material through SPS.

Development of Electroconductive SiC-$ZrB_2$ Ceramic Heater and Electrod by Spark Plasma Sintering (SPS에 의한 SiC-$ZrB_2$계 전도성 세라믹 발열체 및 전극 개발)

  • Shin, Yong-Deok;Ju, Jin-Young;Kim, Jae-Jin;Lee, Jung-Hoon;Kim, Cheol-Ho;Choi, Won-Seok
    • Proceedings of the KIEE Conference
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    • 2009.07a
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    • pp.1254_1255
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    • 2009
  • The composites were fabricated by adding 30, 35, 40, 45[vol.%] Zirconium Diboride(hereafter, $ZrB_2$) powders as a second phase to Silicon Carbide(hereafter, SiC) matrix. The physical, mechanical and electrical properties of electroconductive SiC ceramic composites by Spark Plasma Sintering(hereafter, SPS) were examined. Reactions between $\beta$-SiC and $ZrB_2$ were not observed in the XRD analysis. The relative density of SiC+30[vol.%]$ZrB_2$, SiC+35[vol.%]$ZrB_2$, SiC+40[vol.%]$ZrB_2$ and SiC+45[vol.%]$ZrB_2$ composites are 88.64[%], 76.80[%], 79.09[%] and 88.12[%], respectively. The XRD phase analysis of the electroconductive SiC ceramic composites reveals high of SiC and $ZrB_2$ and low of $ZrO_2$ phase. The electrical resistivity of SiC+30[vol.%]$ZrB_2$, SiC+35[vol.%]$ZrB_2$, SiC+40[vol.%]$ZrB_2$ and SiC+45[vol.%]$ZrB_2$ composites are $6.74{\times}10^{-4}$, $4.56{\times}10^{-3}$, $1.92{\times}10^{-3}$ and $4.95{\times}10^{-3}[{\Omega}{\cdot}cm]$ at room temperature, respectively. The electrical resistivity of SiC+30[vol.%]$ZrB_2$, SiC+35[vol.%]$ZrB_2$, SiC+40[vol.%]$ZrB_2$ and SiC+45[vol.%]$ZrB_2$ are Positive Temperature Coefficient Resistance(hereafter, PTCR) in temperature ranges from 25[$^{\circ}C$] to 500[$^{\circ}C$]. It is convinced that SiC+40[vol.%]$ZrB_2$ composite by SPS can be applied for heater or electrode.

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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.

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.

Microstructure and Electric Contact Properties of Spark Plasma Sintered Ta-Cu Composite (방전플라즈마 소결법으로 제조된 Ta-Cu의 미세조직 및 전기접점 특성)

  • Ju, Won;Kim, Young Do;Sim, Jae Jin;Choi, Sang-Hoon;Hyun, Soong Keun;Lim, Kyoung Mook;Park, Kyoung-Tae
    • Journal of Powder Materials
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    • v.24 no.5
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    • pp.377-383
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    • 2017
  • Microstructure, electric, and thermal properties of the Ta-Cu composite is evaluated for the application in electric contact materials. This material has the potential to be used in a medium for a high current range of current conditions, replacing Ag-MO, W, and WC containing materials. The optimized SPS process conditions are a temperature of $900^{\circ}C$ for a 5 min holding time under a 30 MPa mechanical pressure. Comparative research is carried out for the calculated and actual values of the thermal and electric properties. The range of actual thermal and electric properties of the Ta-Cu composite are 50~300 W/mk and 10~90 %IACS, respectively, according to the compositional change of the 90 to 10 wt% Ta-Cu system. The results related to the electric contact properties, suggest that less than 50 wt% of Ta compositions are possible in applications of electric contact materials.

Mechanical Properties and Bio-Compatibility of Ti-Nb-Zr-HA Biomaterial Fabricated by Rapid Sintering Using HEMM Powders (고에너지 밀링분말과 급속소결을 이용한 Ti-Nb-Zr-HA 생체복합재의 기계적 성질 및 생체적합성)

  • Park, Sang-Hoon;Woo, Kee-Do;Kim, Sang-Hyuk;Lee, Seung-Min;Kim, Ji-Young;Ko, Hye-Rim;Kim, Sang-Mi
    • Korean Journal of Materials Research
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    • v.21 no.7
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    • pp.384-390
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    • 2011
  • Ti-6Al-4V ELI (Extra Low Interstitial) alloy has been widely used as an alternative to bone due to its excellent biocompatibility. However, it still has many problems, including a high elastic modulus and toxicity. Therefore, nontoxic biomaterials with a low elastic modulus should be developed. However, the fabrication of a uniform coating is challenging. Moreover, the coating layer on Ti and Ti alloy substrates can be peeled off after implantation. To overcome these problems, it is necessary to produce bulk Ti and Ti alloy with hydroxyapatite (HA) composites. In this study, Ti, Nb, and Zr powders, which are biocompatible elements, were milled in a mixing machine (24h) and by planetary mechanical ball milling (1h, 4h, and 6h), respectively. Ti-35%Nb-7%Zr and Ti-35%Nb-7%Zr-10%HA composites were fabricated by spark plasma sintering (SPS) at $1000^{\circ}C$ under 70MPa using mixed and milled powders. The effects of HA addition and milling time on the biocompatibility and physical and mechanical properties of the Ti-35%Nb-7%Zr-(10%HA) alloys have been investigated. $Ti_2O$, CaO, $CaTiO_3$, and $Ti_xP_y$ phases were formed by chemical reaction during sintering. Vickers hardness of the sintered composites increases with increased milling time and by the addition of HA. The biocompatibilty of the HA added Ti-Nb-Zr alloys was improved, but the sintering ability was decreased.