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1 Jurnal f the Krean Ceramic Sciety Vl. 6, N. 5, pp. 515~519, 009. DOI:10.191/KCERS Estimatin f Triblgical Prperties n Surface Mdified SiC by Chlrine Gas Reactin at Varius Temperatures Heung-Taek Bae, Ji-Hn Jeng, Hyun-Ju ChiS and Dae-Sn Lim Department f Materials Science and Engineering, Krea University, Seul , Krea (Received July 0, 009; Revised August 6, 009; Accepted August 7, 009) w ƒ w t SiC p p sƒ ká zá x Á š w œw ( ; ; ) ABSTRACT Carbn layers were fabricated n silicn carbide by chlrinatin reactin at temperatures between 1000 C and 1500 C with Cl /H gas mixtures. The effect f reactin temperature n the micr-structures and triblgical behavir f SiC derived carbn layer was investigated. Triblgical tests were carried ut ball-n-disk type wear tester. Carbn layers were characterized by X-ray diffractmeter, Raman spectrscpy and surface prfilmeter. Bth frictin cefficients and wear rates were maintained lw values at reactin temperature up t 1300 C but increased suddenly abve this temperature. Variatin f surface rughness as a functin f reactin temperature was dminant factr affecting triblgical transitin behavir f carbn layer derived frm silicn carbide at high temperature. Key wrds : Triblgy, Silicn carbide, CDC (Carbide derived carbn), Carbn layer, Surface rughness 1. ky³ ky ü,, ü ü p w ƒyw y f f z š. 1-3) ù k y³ y k w ùkü w ƒw w. w w» w k y³ DLC(Diamnd Like Carbn)ù gq w p w t p w jš j wš. -6) p DLC gq sp sp 3 k w y š û ùkü» rv w» w ƒ y w š. 7) ù DLC gq»q gq w µm gq Ì w š, 300 C w š. ky³ ky t š Crrespnding authr : dslim@krea.ac.kr Tel : Fax : w k d y j» t. ky l CDC(Carbide Derived Carbn) d Ì w ƒ š p w f f z t ƒ š. ky³ CDC gq 1000 C š ƒ g t ³ k wš k k k d x k. x k w y k p ü p ùküš š š 8). p k Ì µm~ µm¾ w, ³ z k w x x û p ƒ š. 9) CDC ƒ ƒ y k d Ì w. 10-1) ù yw k d triblgy p w w š ƒ C~1500 C y g CDC gq p y w. w k w y 515

2 배흥택 정지훈 최현주 임대순 516 화 등을 측정하여 반응온도에 따라 변화하는 triblgy 특 성 변화에 미치는 주된 영향을 알아보고자 하였다.. 실험 방법 탄소막의 형성 탄소막 형성에 사용된 시편은 탄화규소 분말에 0.5 at% 붕소와 0.5 at% 탄소를 첨가하여 00 C에서 시간 동안 반응 소결한 직경 5 mm 두께 mm의 고밀도의 탄화규 소 디스크를 사용했다. 준비된 시편은 아세톤 용액 속에 서 3분 동안 초음파 세척을 하여 표면에 흡착된 이물질 을 제거한 후 알루미나 보트위에 고정 시키고, 튜브로의 중앙에 위치하도록 하였다. 반응로의 상세도는 기존 발표 논문을 참고할 수 있다. 아르곤가스 분위기로 상온에서 반응 온도인 1000 C~1500 C까지 5 C/min으로 승온 시킨 후 각각의 반응 온도에서 시간 동안 Ar-H -Cl 혼합가스 에 노출시켰다. 탄화규소시편을 시간 동안 Ar-H -Cl 혼합가스에 반응 시킨 후 생성된 탄소막에 잔여한 염소가스의 제거를 위 해 각각의 반응 온도에서 시간 동안 Ar-H 가스에 노출 시킨 후 온도를 상온까지 하강시켰다. 특성평가 앞의 공정에 의해 탄화규소 디스크 표면에 형성된 탄 소막의 마모 및 마찰 특성은 회전식 ball-n-disk 장비를 사용하여 측정됐다. 상대재로는 직경 6.35 mm인 Si N ball을 사용하였고, 마찰계수는 상온 공기 중에서 3 N의 하중과 0.63 m/s의 속 도로 30분 동안 측정됐다. 이때 마모원의 직경은 6 mm를 나타냈다. 마찰계수는 마모시험 장치에 설치된 lad cell 에서 0.5초 간격으로 마찰력을 실시간으로 측정한 후 가 해준 하중으로부터 계산되었다. 마모율은 a-step을 사용하 여 마모원의 상하좌우 네 지점에서의 마모 깊이를 측정 하여 실제 마모량을 계산하였고, 각각의 평균값을 취했다. 탄소막의 두께 변화 및 구조 분석 반응온도의 변화에 따라 시편 표면에 형성된 CDC층의 표면 조도 변화량은 a-step을 사용하여 각각 3 mm 구간을 5회씩 측정하여 평균값을 구했다. 전자주사 현미경 (SEM, S-3000H Hitachi High technlgies America, Inc.)을 사용하여 시편의 단면을 촬영 탄소막의 두께 측정 하였고, XRD (X-Ray Diffractmeter)를 사용하 여 탄소막 내에 형성된 결정상을 확인 했다. 또한 Raman 분 광기 (LabRam HR mdel, Jbin-Yvn, France)를 사용하여 탄소층의 결합 구조를 분석했다. 이때 조사된 Raman 분광 광원은 Ar 레이저에서 방출되는 51.5 nm 대역의 가시광 파 장을 이용하여 각각의 시편에 대하여 파수 00 ~1800 cm.1. 13).. Triblgy 13) 3 Crss-sectinal SEM images f a specimen reacted varius temperature; (a) 1000C, (b) 1100C, (c) 100C, (d) 1300C, (e) 100C, and (f) 1500C. 영역을 분석했다. 측정된 분광분석은 D-band, disrupted Gband 그리고 G-band로 분류하여 D-band와 G-band에서의 강도비를 구하였다 한국세라믹학회지 Fig 결과 및 고찰 반응 온도에 따른 탄소막의 두께 변화 탄화규소는 800 C 이상의 온도에서 규소 성분이 염소 가스와 반응하여 SiCl 의 기상으로 추출됨에 따라 탄화규 소의 표면에는 탄소 성분만 남게 된다. 잔류한 탄소원자 들이 재결합 하여 탄소막이 생성되는 것으로 알려져 있 다. Fig. 1은 1000 C~1500 C의 반응 온도에 따라 생성된 반응 층의 단면 SEM 사진이다. 탄화규소 표면에 형성된 탄소막은 비교적 균일한 두께로 형성됨을 보여준다. 또한 반응온도에 따라 탄소막의 두께가 크게 변화하는 것을 알 수 있다. 반응 온도에 따라 변화하는 탄소막의 두께변화를 Fig. 에 나타냈다. 탄소막의 두께는 반응 온도 1300 C에서 최 대를 보이며 증가하다 감소하는 경향을 보인다. 이러한 경향은 타 연구자도 관찰한바 있다. 반응 온도가 증가 함에 따라 SiCl 상이 안정화됨으로 반응 온도의 상승에 따라 형성되는 탄소막의 두께가 증가한다. 높은 온도에서 탄소막의 두께가 감소하는 것은 반응에 참여한 수소가스 가 염소가스와 반응하여 규소의 추출에 직접적으로 관여 )

3 w ƒ w t SiC p p sƒ 517 Fig.. Thickness f carbn as a functin f reactin temperature. Fig.. Frictin cefficient f reacted SiC in Cl /H mixture gas. The reactin temperature was varied frm 1000 C t 1500 C. Fig. 3. Wear rate f reacted SiC in Cl /H mixture gas. The reactin temperature was varied frm 1000 C t 1500 C. w HCl ƒ ƒ ƒw ³ v w ƒ w» 9). 3.. Fig. 3 y j x k k y ùkü C¾ ƒ g ƒ 100 C, 1500 C ƒ k w ƒw w C¾ w w ùkü z 100 C, 1500 C w r w ƒ w š (Fig. ). Fig. 3 Fig. y 1300 C¾ x k. Fig. 5. XRD patterns f SiC derived carbn layer, which is reacted by Cl /H mixture gas y k y Fig. 5 ky³ Cl /H ywƒ y XRD C 1300 C¾ ƒ k rhmbhedral graphite (00) vj ƒw w ùkü. ƒ ƒw graphite ƒw ƒ» w SiC vj w wù k d Ì y w vj w w ƒ w. XRD l rhmbhedral graphiteƒ k d sw. k d Raman vj y Fig. 6 ùkþ cm cm vjƒ 1. disrdered k D G vj. w 15) Raman Ÿ I D /I G w 1300 C¾ 6«5y(009)

4 518 ká zá x Á Fig. 6. Raman spectra f each reactin temperature and its I D /I G rati inserted. Fig. 7. Mdified surface images which were reacted at (a) 1000 C, (b) 1300 C and (c) 1500 C. y w w ƒ z ƒw w. û k d š ƒ ƒw ƒ w. ù 9) 100 C ƒ g»œx w.»œ ƒ ü ƒ k w ƒ jš, w. ƒ t»œ ƒw w SEM y w (Fig. 7). 16,17) Fig. 7(a) û» ky³»œ x. Fig. 7(b) ƒ j y w k w w»œ x ƒ¾ y. ƒ j»œ j» f y w (Fig. 7 (c)). ƒƒ x k d t Fig. 8 ùkþ. t 1000 C ~1300 C j yƒ ù 1300 C ƒ ƒw w ƒw. t y w» œ j» y» w. y p p y 1000 C l 1300 C¾ ƒ 0.15 ü û Fig. 8. The influence f reactin temperature n the surface rughness (Ra) f SiC derived carbn. w 1300 C l 1500 C¾ ƒ C 1300 C¾ ƒ ƒw rhmbhedral graphite ƒw I D /I G w w ùkþ. I D /I G graphite ƒ w. 1) Graphite ƒƒ» w. Graphite ƒw graphite yp ƒ w. 18) 100 C z I D /I G ƒw w ù 1000 C I D /I G w. 100 C j ƒ w graphite w ƒ t w ƒ j. Fig. 8 t 100 C z w ƒ ƒ w ew. t w ƒ ƒ gš, w ƒw.. SiC Cl /H ƒ 1000 C l 1500 C¾ y g x k p yƒ p p e w w C~1300 C¾ x k û. 100 C x k ùkþ ƒw w. û w graphite disrder ƒ w e. 100 C ƒ k w wz

5 w ƒ w t SiC p p sƒ 519 ƒƒ ( 10 6 mm 3 /Nm) w ƒ w. w ƒ»œj» t y. mw š ƒ k ky³ t x k d p w j» w š k w»œ ƒ w. Acknwledgment» w. REFERENCES 1. B S Nau, Mechanical Seal Face Materials, Prc. Instn. Mech. Engrs., 11 Part J (1997).. M. Pppp, R. Sternagel -CEROBEAR GmbH, and Herzgenrath, Hybrid- and Ceramic Rlling Bearings with mdified Surface and Lw Frictin Rlling Cntact, Vl., pp. 1-6, EUROMAT 99, Micrstructural Investigatin and Analysis, Wiley Eurpe, P. A. Cnner and M. T. Thew, Trends at Three Prcess Plants in the Oil Industry, Industrial Lubricatin and Triblgy, 7 [] -11 (1995).. C. S. Abrue, M. S. Amaral, F. J. Oliveira, A. Tallaire, and F. Benedic, Triblgical Testing f Self-mated Nancrystalline Diamnd Catings n Si 3 N Ceramics, Surface & Catings Technlgy, (006). 5. A. Erdemir, Frictin and Wear f Diamnd and Diamndlike Carbn Films, Prc. Instn. Mech. Engrs., Part J: J. Engineering Triblgy, (00). 6. J. Fntaine, Twards the use f Diamnd-like Carbn Slid Lubricant Catings in Vacuum and Space Envirnments, Prc. IMechE Part J: J. Engineering Triblgy, (008). 7. G. A. jnes, On the Triblgical Behaviur f Mechanical Seal Face Materials in Dry Line Cntact: Part II. Bulk Ceramics, Diamnd and Diamnd-like Carbn Films, Wear, (00). 8. H.-J. Chi, H.-T. Bae, B. C. Na, J.-K. Lee, and D.-S. Lim, Triblgical Prperties f Carbn Layers Prduced by High Temperature Chlrinatin Cmparisn with DLC Cating, J. Kr. Ceram. Sc., [7] (007). 9. H.-J. Chi, H.-T. Bae, J.-K. Lee, B.-C. Na. M. J. McNallan, and D.-S. Lim, Sliding Wear f Silicn Carbide Mdified by Etching with Chlrine at Varius Temperatures, Wear, (009). 10. Y. G. Ggtsi, I.-D. Jen, and M. J. McNallan, Carbn Catings n Silicn Carbide by Reactin with Chlrine-cntaining Gases, J. Mater. Chem., 7 [9] (1997). 11. Yury Ggtsi, Sascha Welz, Daniel A, Ersy, and Michael J. McNallan, Cnversin f Silicn Carbide t Crystalline Diamnd-structured Carbn at Ambient Pressure, Nature, (001). 1. A. Erdemir, A. Kvalchenk, M. J. McNallan, S. Welz, A. Lee, Y. Ggtsi, and B. Carrll, Effect f High-temperature Hydrgenatin Treatment n Sliding Frictin and Wear Behavir f Carbide-derived Carbn Films, Surface and Catings Technlgy, (00). 13. H.-T. Bae, J.-H. Jeng, D.-S. Lim, and B.-C. Na, Dependence f Cl Gas Reactin Time n Triblgical Prperties f TiC Derived carbn Layer, J. KSTLE, 5 [1] 0- (009). 1. M. Krmann, H. Gerhard, and N. Ppvska, Cmparative Study f Carbide-derived Carbns Obtained frm Bimrphic TiC and SiC Structures, Carbn, 7-50 (009). 15. S. Reich and C. Thmsen, Raman Spectrscpy f Graphite, Phil. Trans. R. Sc. Lnd. A, (00). 16. G. Yushin, R. Dash, J. Jagiell, J. E. Fischer, and Y. ggtsi, Carbide-Derived Carbns: Effect f Pre Size n Hydrgen Uptake and Heat f Adsrptin, Adv. Funct. Mater., (006). 17. G. Yushin, E. N. Hffman, M. W. Barsum, and Y. Ggtsi, Mesprus Carbide-derived Carbn with Prsity Tuned fr Efficient Adsrptin f Cytkines, Bimaterials, (006). 18. J. Kvacik, S. Emmer, J. Bielek, and L. Kelesi, Effect f Cmpsitin n Fricti Cefficient f Cu-graphite Cmpsites, Wear, (008). 6«5y(009)

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