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1 Journal of Korean Powder Metallurgy Institute DOI: /KPMI š / g e w p» p a,b Á y b Áy x a, * a KAIST œw, b ( )» Interfacial Characteristics and Mechanical Properties of HPHT Sintered Diamond/SiC Composites Hee Sub Park a, b, Min Ho Ryoo b G and Soon Hyung Hong a, * a Department of Materials Science and Engineering, KAIST, Yuseong-Gu, Daejeon, , Korea b Institute of Industrial Technology, ILJIN Diamond Co, Ltd, Eumsung-Kun, Chucheongbuk-Do, , Korea (Received October 21, 2009; Revised November 13, 2009; Accepted November 20, 2009) Abstract Diamond/SiC composites are appropriate candidate materials for heat conduction as well as high temperature abrasive materials because they do not form liquid phase at high temperature Diamond/SiC composite consists of diamond particles embedded in a SiC binding matrix SiC is a hard material with strong covalent bonds having similar structure and thermal expansion with diamond Interfacial reaction plays an important role in diamond/sic composites Diamond/SiC composites were fabricated by high temperature and high pressure (HPHT) sintering with different diamond content, single diamond particle size and bi-modal diamond particle size, and also the effects of composition of diamond and silicon on microstructure, mechanical properties and thermal properties of diamond/sic composite were investigated The critical factors influencing the dynamics of reaction between diamond and silicon, such as graphitization process and phase composition, were characterized Key factor to enhance mechanical and thermal properties of diamond/sic composites is to keep strong interfacial bonding at diamond/sic composites and homogeneous dispersion of diamond particles in SiC matrix Keywords : Diamond/SiC composite, Diamond, SiC, HPHT sintering, Interface 1 ƒ ƒ š, w w ü š w w 6GPa, 2400 K š š œ (High Temperature and High Pressure Sintering, HPHT sintering) w Hall w [1] z w HPHT œ w j l j» w ƒ [2-4] w œ j l j» x g p, f, w we w w w w (Polycrystalline Diamond, PCD) ƒ œ š *Corresponding Author : [Tel : ; 416

2 š / g e w p» p 417 w ü š, û w š y š p g p 700 o C PCD wš k ƒ y k ƒ w [5] ƒœ ƒ ƒ y ƒœ ù w š p ƒ ƒ» w û w j w w w» w w w l œ mw w ƒ ù, w w w t»œ w w ü y š» ƒ, p š g p g y j w w w ƒ š g w g e x w e y g p w PCD / g e w» w PCD ƒ w š g p g pƒ we e g p w (dissolution and precipitation) w w, / g e w, e y g w x g e w ƒ w, HPHT œ z g e w w w v w g e w ƒ wš w» p, y j w w š û q š» w» w w w» ww [6-9] g yw w g w wš g e s³ w» w s³ j»ƒ ƒ bi-modal w j» / g e w š š œ w w y p wš» p p sƒwš w w 2 x j»ƒ 4-6 µm, µm œ w ( ( )) s³ 35 µm g (HC Starck) 10~50 wt% g sp 24 k ƒ k œ mw ³ w yw y yw w ywz 100 mesh m k z 800 o C 2» w œ w w p k š e w 6 GPa ƒw k 1500 o C ƒ w 30 ƒ w k ww xt { w t wš, w p sƒ ww g yw y w» w (Differential scanning calorimetry(dsc), Netzsch 404 C) Ar» 10 o C/ min ww / g e w»œ j w d w š, Ÿwx (Leica, DC-200), x (Philips XL30SFEG) w š, Ÿ (LabRAM HR) XRD(Rigaku D/Max IIIC(3 kw)) mw w wš w

3 418 Á yáy x w, g e w» w FIB(FEI Nova 200) w TEM (FEI TecnaiTM F2 F30) mw w» p sƒ 98 N v d wš s ƒw, ü p sƒw» w µm SiC ƒ 20% w g e» w (Al-20%SiC p MMC, Duralcan F3S20S) v w x ww 3 š 31 / g e w g w» w g yw w ww 1 g yw w Ar» 1450 o C¾ DSC g 1414 o C, 1430 o C k g yw w peak w, SiC ùkü š œ ƒ ƒw Si û Si» w, k w t t w SiC» w w C diamond (s) + Si(l) β-sic (1) 2 a) / g e w š b) w XRD d, β-sic, Si w w peakƒ ù, w w disordered D band 1310 cm 1 graphic G band 1590 cm peak 1 XRD, β-sic, Si peakƒ ù α-sic w w peak š œ mw g w β-sicƒ x š w Si w ùk ü w ƒw SiC Si peak wš peak ƒw Fig 1 DSC curves of diamond and Si powder mixture up to 1450 o C in Ar atmosphere Fig 2 Phase analysis results by XRD and Raman spectra a) Raman spectra of diamond/sic composite with 70 wt% diamond content and b) XRD diffraction patterns of diamond/sic composites with 50 to 90 wt% diamond content Journal of Korean Powder Metallurgy Institute

4 초고압 소결된 다이아몬드/실리콘 카바이드 복합재료의 계면특성 및 기계적 특성 419 Fig 3 SEM micrographs of diamond/sic composite fabricated with different diamond content and bi-modal particle size a) 90 wt% diamond content, b) 90 wt% diamond content and bi-modal structure, c) 70 wt% diamond content and d) 70 wt% diamond content and bi-modal structure Table 1 A summary of quantitative analysis of diamond/sic composite containing different amounts of diamond, SiC and Si Diamond (wt%) 90 wt% 80 wt% 70 wt% 60 wt% 50 wt% Bulk Density (g/cm3) Diamond (vol%) 8466 ± ± ± ± ± 487 SiC (vol%) 1432 ± ± ± ± ± 594 그림 은 초고압 소결공정에 의해 제조된 다양한 조성과 다양한 다이아몬드 입자 크기를 갖는 다이아 몬드 실리콘 카바이드 복합재료의 사진이다 다 이아몬드입자가 실리콘 카바이드 기지 내에 균일하 게 분산되어 있는 미세구조를 나타내고 있으며 흑연 이나 다른 추가 상들은 관찰되지 않고 다만 일부 반 응하지 않고 남은 실리콘이 존재하는 것을 알 수 있다 소결체의 밀도 측정 결과와 다이아몬드 β 상에 대한 미세조직의 이미지 분석을 통한 정량분석 3 / SEM,,, -SiC, Si Si Theoretical Density Relative Density (vol%) (g/cm3) (%) 102 ± ± ± ± ± 결과를 표 에 나타내었다 이론 밀도는 출발원료인 금속 실리콘이 완전히 다이아몬드와 반응했을 때를 기준으로 계산되었다 초고압 소결공정에 의해 소결 된 다이아몬드 실리콘 카바이드 복합재료가 다이아몬 드의 함유량에 따라서 이상의 상대밀도를 나타내 었다 그림 는 다이아몬드의 함유량에 따라서 복합 재료를 구성하고 있는 다이아몬드 의 정량분 석 결과와 각 상의 회절강도와의 비교를 나타 내고 있으며 다이아몬드의 함유량이 증가함에 따라 1 / 98% 4, SiC, Si XRD,

5 420 Á yáy x Fig 4 Quantitative relationship between Diamond, SiC and Si from image analysis and XRD relative intensity a) SiC content as a function of diamond content and b) remained Si content as a function of diamond content SiC Si z ƒ w w ùkü š XRD z w ewš 32 / g e w» p sƒ 5a) / g e w w v d w v 26~46 GPa d, w ƒw w ƒ ƒw ƒ j» bi-modal w w wƒ j» w w 70 wt% 80 wt% û ùkü š, 90 wt% w Fig 5 Mechanical properties of diamond/sic composites a) Knoop hardness of diamond/sic composites with different diamond content, b) bending strength of diamond/ SiC composites with different diamond content and c) compressive strength of diamond/sic composites with different diamond content after heat-treated at room temp at 800 o C, 1000 o C and 1200 o C in air w w w û Journal of Korean Powder Metallurgy Institute

6 š / g e w p» p 421 Fig 6 SEM micrographs of the typical fracture surface of diamond/sic composite ƒ j w ûš, 90 wt% bimodal ƒ ƒ» wƒ w w ùkü ƒ g e ƒ ƒ ƒ 70 GPa, 25 GPa š w rule of mixture w 90% 55 GPa ùkü w, 84% ùkü w w Si w SiC w ƒ û» w 5b) / g e w w d w ƒ w ƒ ƒw ƒ 70 wt% w w ƒ ƒ ùkü, w bi-modal w ƒ 35% bi-modal g e s³ g e s³ Ì w j w» ƒ 70 wt% w w w ƒ ùkü û g û»œ» w ƒ 5c) sƒ w, 60 wt% w w 1000 o C¾ w ƒ ü w 1000 o C w w g y š g y ƒ ƒ ƒw g y l w t j w w w j w 6 / g e q SEM w q x q ùkü cleavage xk q š, j wš qw y j q ƒ k g e w w ù, / g e w q w g e w w 7a) / g e ü sƒw, w v 180 mm, ¼ 300 mm» x 7b) v w Al-20%SiC p MMC w w z w œ v j (flank wear) d w w 8 ùkü w ƒw v j w w w bi-modal w ƒ w p ùkü bi-modal w g e

7 422 박희섭 류민호 홍순형 Fig 9 TEM image of diamond-sic interface in diamond/ SiC composite fabricated by HPHT process wear)와 함께 절삭 과정중 에 발생하는 열에 의한 Al의 절삭공구 인선 부위로의 접착에 의한 흡착마모 (adhesive wear)가 발생함으로써 다이아몬드/실리콘 Fig 7 Wear tests of diamond/sic composites in high speed turning of MMC a) Machining of MMC and b) Microstructure of work pieces Fig 8 Wear behavior of diamond/sic composites with different diamond content 이드의 계면과 실리콘 카바이드의 평균 자유경로가 작기 때문으로 판단된다 Al MMC의 절삭가공에서 경 도가 높은 SiC에 의해서 강한 기계적인 마모(abrasive Journal of Korean Powder Metallurgy Institute 카바이드 복합재료로 제조된 절삭공구에 마모가 발 생함을 알 수 있었다 다이아몬드/실리콘 카바이드 복합재료의 계면분석 그림 9는 다이아몬드와 실리콘 카바이드의 계면부 위를 촬영한 TEM 사진이다 다이아몬드와 실리콘 카바이드의 계면 부위에 dislocation, stacking fault 와 microtwin의 많은 미세 결함이 존재하는 것이 관 찰되었다 이러한 계면 부위에서의 고밀도 결함은 다 이아몬드와 실리콘 카바이드의 결정학적 차이를 보 상하기 위해서 존재하며, 이로 인해 다이아몬드/실리 콘 카바이드 복합재료의 높은 열저항성과 계면 결합 특성을 보이는 것으로 사료된다 실리콘 카바이드 결 정립이 다이아몬드보다 심하게 변형되어 있는 것을 알 수 있으며, 이것은 초고압 고온 소결중에 상대적 으로 낮은 강도를 갖는 실리콘 카바이드에서 상대적 으로 많은 소성변형 거동을 나타낸 것으로 생각된다 33 4 결 론 다이아몬드/실리콘 카바이드 복합재료를 다이아몬

8 š / g e w p» p 423 w j» y g w š e w / g e w 98% ùkü, w y w w ƒw g e g w, g e w w» w ƒ w y w w j w, w ƒw ƒw ƒ 70 wt% ƒ ùkü, w bi-modal w w ü p w» p k g w x g e w» w y w 2007» l (ATC ) 2005 ( ) w w w (KRF J00901), š x [1] H T Hall: Science, 169 (1970) 868 [2] H D Stromberg and D R Stephens: Am Ceram Soc Bull, 49 (1970) 1030 [3] H Katzman and W F Libby: Science, 172 (1971) 1132 [4] P A Bex and W I Wilson: Ind Diamond Rev, 37 (1977) 10 [5] Y S Ko, T Tsurumi, O Fukunaga and T Yano: J Mater Sci, 36 (2001) 469 [6] J Qian, G Voronin, TW Zerda, D He and Y Zhao: J Mater Res, 17(8) (2002) 2153 [7] G A Voronin, T W Zerda, J Qian, Y Zhao, D He and S N Dub: Dia Rela Mater, 12 (2003) 1477 [8] Y Zhao, J Qian, L L Daemen, C Pantea, J Zhang, G A Voronin and T W Zerda: Appl Phy Lett, 84(8) (2004) 1356 [9] E A Ekimov, S Gierlotka, E L Gromnitskaya, J A Kozubowski, B Palosz, W Lojkowski and A M Naletov: Inorganic Materials, 38(11) (2002) 1117

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