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1 Jurnal f the Krean Ceramic Sciety Vl. 46, N. 5, pp. 58~533, 009. DOI: /KCERS Effects f β-sic Particle Seeds n Mrphlgy and Size f High Purity β-sic Pwder Synthesized using Sl-Gel Prcess Gyu-Mi Kim*, **, Gyung-Sun Ch*, and Sang-Whan Park* *Material Science & Technlgy Research Divisin, Krea Institute f Science and Technlgy, Seul , Krea **Department Materials Science and Engineering, Krea University, Seul , Krea (Received August 3, 009; Revised September 14, 009; Accepted September 16, 009) β-sic Seedsƒ Sl-gel œ w š β-sic x j» e w ½³ *, **Á *Á y* *w w»» **š w œw ( ; ; ) ABSTRACT High purity β-sic pwders were synthesized using sl-gel prcessing. TEOS and phenl resin were used as the starting material fr the silicn surce and carbn surce, respectively. The prcess turned ut t be capable f prducing high purity SiC pwder purity degree with %. Hwever, it was difficult t cntrl the shape and size f β-sic pwders synthesized by sl-gel prcess. In this study, β-sic pwder with size f 1~5 um an 30 nm were used as the seeds fr β-sic t cntrl the β-sic pwder mrphlgy. It was fund that β-sic pwder seeds was effective t increase the pwder average size f synthesized β-sic using sl-gel prcess by acting as the preferred grwing sites fr β-sic. Key wrds : Sl-gel prcess, Synthesis f SiC, ß-SiC, Pwder, High purity, Seeds 1. ky³ (SiC) ü, š š, š ƒ ü ƒ» s š. 1-4) Si wafer yƒ w» š id w š œ š üyw p w ky³ ƒ š. š œ š ky³ š ky³, CVD ky³ ky³ ƒ š œ t y y p, p, ep r. š œ ky³ p š w» w š ƒ š ù Crrespnding authr : Sang-Whan Park spark@kist.re.kr Tel : Fax : š ky³ p œ t w š» š œ ky³ š CVD gq w t š. 5) ky³ ³ Achesn prcess ³ k yww» š carbthermal reductin q SiC š ù, α-sic ƒ û š œ t w» w ƒ š y œ. Carbthermal reductin š k k ³ yww š ky³ w w œ û β-sic w w ù k ³ ³ w yw» w z SiO carbn w š ky³ ww, w ky³ j» x ƒ š š. 6,7) 58

2 59 ½³ Á Á y š ky³ w œ š y w š ky³ w w yw» (chemical vapr depsitin prcess, CVD prcess) sl-gel prcess. 8-1) CVD w ky³ w w j» s sub micrmeter j» š β-sic w ù, β-sic j»ƒ 1µm w» w š œ ky³ ww. w, CVD w ky³ w ww š ƒ» w š. š ky³ w wù sl-gel œ ³ k ³ w yww hybrid gel w z š š ky³ w w œ ) Kurachi 17-0) phenl resin ethylsilicate w ³ w yww z ƒ w œ hybrid gel w z š š β-sic w. w, ³ tetraethyl rthsilicate (TEOS) tetramethyl rthsilicate(tmos) wš k phenl resin w sl-gel œ hybrid gel w z 1700~1800 C š β-sic w w, w β-sic j» hybrid gel œ, w ùkû ù micrmeter w. 1,) Sl-gel œ w š ky³ œ wš ¾ yw œ» ³ š œ ƒ û w β-sic x j»» ¾ y ƒ š š. k Phenl resin ³ TEOS w sl-gel hybrid gel w z š œ š β-sic w w. Sl-gel œ w ky³ w œ w β-sic x j» w» w ky³ w w seeds w j» β-sic particle hybrid gel SiC precursr ƒw sl-gel w β-sic j» x e w w.. x Table 1 Sl-gel š SiC w w x ³ Table 1. Starting Materials used in This Study Materials Supplier Remark Purity/Size Tetraethyl Orthsilicate Aldrich TEOS 98% Tluene sulfnic acid Aldrich P-TSA >98.5% Nvlac type Phenl Resin Klng SPR Carbn cntents>55% purity>90% Nan SiC particle MIT Ave. size=30 nm Micr SiC particle KIST Ave. size=1~5 µm Fig. 1. Experimental prcedure fr synthesis f β-sic pwder using sl-gel prcess. lp p f p (tetraethyl rthsilicate (Si(OCH 3 ) 4, TEOS, 98%, Sigma Aldrich) w š, p-tsa(98.5%, Sigma Aldrich), k k r (Klng C.) w. r e w d w» w r y» carbnizatiny y d w e w w. phenl resin ü e l hybride gel ü C/Si 1.6. Fig. 1 sl-gel š β-sic w» w xœ. Slgel š β-sic w w r TEOS ³ w yw w r k ww TEOS yww, TEOS ƒ w w tluene sulfnic acid (p-tsa, 30 wt% ) ƒw 40 C 400 rpm 36 w. hybrid gel 100 C 4, 900 C(5 C/min) 30» w SiC precursr w. β-sic x j» w Table 1 30 nm j» SiC 1~5 µm j» β-sic 1, 5, 10 wt% y g hybrid gel yww z, 1800 C 3 Ar w wz

3 β-sic Seedsƒ Sl-gel œ w š β-sic x j» e w 530 Fig.. The thermal behavir f phenlic resin in N atmsphere.» w w š β-sic w w. 1~5 µm j» β-sic x w. phenl resin, hybrid gel SiC precursr š w β-sic FT-IR(Furier transfrm infrared spectrscpy)» w n w, X- z e w. w SEM(scanning electrn micrscpy) w w β-sic w. 3. š TEOS 4ml (p-tsa) w ƒ wƒ, wì yw r w w gel k. β-sic w C/Si ml rati š β-sic w w ƒ w r x w. Fig. r TG(therm gravimetric analysis) DSC(differential scanning calrimetry) 400 C l 800 C¾ w yƒ w š 800 C 1100 C ¾ yƒ y w. r carbnizatin 800 C q 1100 C e w 5%. l hybrid gel w N»w 900 C w SiC precursr w. Fig. 3 r, C/Si ml rati hybrid gel, SiC precursr w β-sic FT-IR rp. r hybrid gel O-H bnding (3600~3100 cm 1 ), benzene ring (1605, 1587, 1493 cm 1 ), Si-O-Si (150~1050, 480 cm 1 ) š C-O bnding (100 cm 1 ) š, hybrid gel 900 C w w SiC precursr hybrid gel Fig. 3. Furier transfrm infrared spectra f (a) phenl resin, (b) dried hybrid gel, (c) SiC precursr after heat treatment f hybrid gel, and (d) synthesized β-sic pwder. vj O-H, benzene ring, Si-O-Si bnding. SiC precursr 1800 C w w β-sic 796 cm 1 Si-C bnding. w r TG 400 C l 800 C ¾ w y w O-H bnding, benzene ring { 800 C. Si-O-Si bnding š carbn y ky Si-C bnding x š SiO 1800 C 3 r ƒ. Fig. 4 C/Si ml rati hybrid gel, SiC precursr, 1350 C 1800 C w β-sic 1~5 um j» β-sic seeds 1wt% ƒ g w β-sic XRD z pattern. Fig. 4 hybrid gel SiC precursr brad w ùkù carbn peak C w SiC 0 y e w brad diffractin pattern ùkû û w û β-sic w. sl-gel prcess w ³ k yww hybrid gel ³ SiO k Cƒ ³ w yw» 1350 C β-sic e XRD peak yw ùkù SiO wì w ƒ C w SiC XRD 0 y e w ùkù brad diffractin pattern β-sic 46«5y(009)

4 김규미 조경선 박상환 531 Fig. 6. Fig. 4. XRD patterns f (a) dried hybrid gel, (b) SiC precursr, (c) SiC pwders synthesized at 1350C fr 1 h, (d) SiC pwders synthesized at 1800C fr 3 h, and (e) SiC pwders synthesized at 1800C with β-sic seeds fr 3 h. SEM f synthesized β-sic pwder using dried hybrid gel with the additin f 1~5 µm sized β-sic pwder seeds; (a) 0 wt%, (b) 1 wt%, (c) 5 wt%, and (d) 10 wt%. 를 보여준다 C에서 합성된 분말은 SEM 미세구조 및 XRD pattern에서 보여주는 것과 같이 10 nm 이하 크기 의 β-sic 입자 및 미반응 카본입자 및 SiO 입자로 이루어 져 있다. Hybrid gel을 열처리하여 제조된 SiC precursr는 1350 C에서 환원 및 탄화반응이 진행됨에 따라 crss link 된 SiC precursr 내 카본 과 SiO 가 반응하여 초기단계에 는 나노 크기의 β-sic 입자가 합성되며, 합성 시간의 증 가 및 합성온도의 증가에 따라 미반응 SiO 및 카본과의 사이에서 반응이 진행되어 새롭게 합성되는 β-sic의 증 착 및 10 nm 이하 크기의 β-sic 입자 사이에서의 입자 성 장으로 β-sic 입자의 성장이 일어나는 것으로 생각된다. Fig. 6은 건조된 hybrid gel 분말과 1~5 µm 크기의 β-sic 분말 seeds를 0 wt%, 1 wt%, 5 wt% 및 10 wt% 혼합하여 1800 C에서 3시간 동안 합성한 β-sic 분말의 SEM 미세구 조를 보여준다. β-sic 분말 seeds를 첨가하지 않고 합성된 β-sic 분말의 미세구조는 Fig. 6(a)에서 보여주는 것과 같 이 합성된 β-sic 분말의 입자 크기 분포는 넓게 관찰되었 으며 합성된 β-sic 분말의 크기는 대체적으로 약 5 µm 이 하이었다 C에서 합성된 β-sic 분말의 미세구조와 비 교하여 β-sic 분말의 입자 크기는 크게 증가하였으며 합 성된 입자의 형태로부터 β-sic 입자의 결정도도 증가된 것 으로 나타났다. 본 연구에서 합성된 β-sic 분말의 순도는 99.98% 이상이었다. β-sic 입자 seeds를 1 wt% 첨가하여 합성된 β-sic 분말의 SEM 미세구조는 β-sic 분말의 seeds 를 첨가하지 않고 합성된 β-sic 분말보다 입자크기는 증 가되었고 입자 크기 분포가 좁아지는 것으로 나타났다. Fig. 6(b)에서 보여주는 것과 같이 합성된 β-sic 입자의 최 대 크기는 15 µm 정도이었다. 따라서 첨가된 SiC seeds 입 자 표면은 합성 원료 내 카본 과 SiO 가 반응하여 초기단 계에서 형성되는 β-sic의 우선적인 합성 위치로 작용하여 Fig. 5. SEM f synthesized β-sic pwders at 1350C. 되었다 C에서 나타나는 결정도가 낮은 β-sic 결정 상은 합성온도가 1800 C로 증가됨에 따라 높은 결정도를 갖는 β-sic 결정상으로 나타났으며 미반응 카본 및 미반 응 SiO 사이에서 환원 및 탄화반응이 진행되어 β-sic로 합성되면서 순도가 높은 β-sic가 합성되는 것으로 생각 된다. β-sic 분말의 seeds를 1 wt% 첨가시켜 합성된 SiC 의 XRD 회절 pattern은 β-sic 분말의 seeds가 첨가되지 않고 합성된 SiC의 XRD 회절 pattern과 동일하게 관찰되 었으며, β-sic seeds의 첨가는 합성된 SiC의 결정상에 영 향을 미치지 않는 것으로 생각된다. Fig. 5는 C/Si ml rati로 제조된 hybrid gel을 사용하 여 1350 C에서 1시간 동안 합성된 분말의 SEM 미세구조 한국세라믹학회지

5 β-sic Seedsƒ Sl-gel œ w š β-sic x j» e w 53 Fig. 7. SEM f synthesized β-sic pwder using dried hybrid gel with the additin f 10 nm sized β-sic pwder seeds; (a) 1 wt% and (b) 10 wt%. ù š β-sic ù 15 µm j» j β-sic w ƒ. hybrid gel ü ƒ β-sic seeds ƒ Fig. 6(c) (d) w β-sic j» w w β- SiC j» s ƒ ùkû. hybrid gel ü ƒ β-sic seeds ƒ β-sic w e ƒ ƒ š β-sic w w SiO e» w β-sic j»ƒ β-sic j» sƒ f ƒ. ù β-sic seeds 5 10 wt% ƒw w β-sic j» β-sic seeds ƒw š w β-sic j» ƒ ùkû. Fig. 7 hybrid gel 30 nm j» β-sic seeds 1wt% 10 wt% yww 1800 C 3 w w β-sic SEM. 30 nm j» β-sic seeds 1wt% ƒw w β-sic SEM Fig. 7(a) β-sic seeds ƒw š w β-sic j» ƒ w β-sic j» 18 µm j» sƒ w. 30 nm j» SiC seeds ƒ 1~5 µm j» β-sic seeds ƒ w β- SiC s z w ùkû. hybrid gel ü ƒ β-sic seeds 10 wt% ƒ 1~5 µm j» β- SiC seeds ƒw w β-sic w β-sic j» w w w β-sic j» s ƒw. hybrid gel ü ƒ 30 nm j» β-sic seeds t 1~5 µm j» β-sic seeds t j ƒ e SiO w β-sic eƒ j ƒ w» l 30 nm j» β-sic seeds y y š ù j» ƒ w j ƒ j j» β-sic w ƒ w yw» w ƒ ƒ. 4. TEOS r w sl-gel hybrid gel 900 C 30 N»w w SiC precursr w z 1800 C 3 Ar»w w g ƒ 99.98% β-sic w w. 1~5 µm j» β-sic 30 nm j» β-sic seed hybrid gel 1wt%, 5wt%, 10wt% ƒƒ w SiC j» x e w w. 5 µm j» β-sic seeds 1wt% ƒ j»ƒ 15 µm¾ û, j» sƒ w. 5 µm j» β-sic seeds 5 wt%, 10 wt% ƒ w β-sic j» š j» s w ƒ ùkû, 5 µm j» β-sic seeds 5 wt%, 10 wt% ƒ w 1~5 µm j» β-sic seeds ƒw š w β-sic j» ƒ š j» s w. 30 nm j» β-sic seeds ƒw β-sic w w, j»ƒ 18 µm 1~5 µm j» β-sic ƒ w β-sic s z ƒ w. Acknwledgment» w. REFERENCES 1. N. Kageyama, Silicn Carbide Prducts fr Silicn Semicnductr Manufacturing, Ceramics, Jpn., 30 [5] 44-7 (1995).. J. A. Tmanvich, LPCVD Cmpnents Trend Tward SiC, Slid State Tech., 40 [6] (1997). 3. K. Segawara, Intrductry Remarks n Ceramics fr Silicn Semicnductr Manufacturing VLSI Fabricatin and its Related, Ceramics, Jpn., 30 [5] (1995). 4. K. Fhiraishi, Silica Glass fr Semicnductr Prcess, Ceramics, Jpn., 30 [5] (1995) Wei GC, Kennedy CR, and Harris LA, Synthesis f Sin- 46«5y(009)

6 533 ½³ Á Á y terable SiC Pwders by Carbthermic Reductin f Gelderived Precursrs and Pyrlysis f Plycarbsilane, Am Ceram. Sc. Bull., (1984). 7. A. Chrysanthu and P. Grievesn, Frmatin f Silicn Carbide Whiskers and Their Micrstructure, J. Mat. Sct., (1991). 8. H. Rbert Baumgartner and B. R. Rssin, Pressureless Sintering and Prperties f Plasma Synthesized SiC pwder, Ceramic Transactins, 3-16 (1987). 9. K. M. Rigtrup and R. A. Cutler, Synthesis f Submicrn Carbide pwder, Ceramic Transactins, (1987). 10. D. A. White, S. M. Oleff, R. D. Byer, P. A. Budinger, and J. R. Fx, Preparatin f Silicn Carbide frm Organsilicn Gels: I, Synthesis and Characterizatin f Precursr Gels, Adv. Ceram. Mat., [1] 45-5 (1987). 11. White, D. A., Oleff, S. M., and Fx, J. R. Preparatin f Silicn Carbide frm Organsilicn Gels: II, Gel Pyrlysis and SiC Characterizatin, Adv. Ceram. Mater., [1] 53-9 (1987). 1. M. Narisawa, K. Yamane, Y. Okabe, and K. OKamura, Carbn-Silica Ally Material as Silicn Carbide Precursr Prepared frm Phenl Resin and Ethyl Silicate, J. Mater. Res., 14 [1] (1999). 13. J. Y. Gu, F. Gitzhfer, and M. I. Buls, Inductin Plasma Synthesis f Ultrafine SiC Pwders, J. Mater. Sci., (1995). 14. Y. Li, Y. Liang, F. Zheng, and Z. Hu, Carbn Dixide laser Synthesis f Ultrafine Silicn Carbide Pwders frm Diethxydimethylsilane, J. Am. Ceram. Sc., (1994). 15. I.N. Khlmanv, A. Kharlamv, E. Barbrini, C. Lenardi, A. Li Bassi, C.E. Bttani, C. Ducati, S. Maffi, N.V. Kirillva, P. Milani, and J. Nansci, A Simple Methd fr the Synthesis f Silicn Carbide Nanrds, J. Nansci Nantech, [5] (00). 16. P.J. Guichelaar, in: A.W. Weimer (Ed.), pp Carbide, Nitride and Bride Materials Synthesis and Prcessing, Chapman and Hall, New Yrk, S. Ishihara, H. Tanaka, and T. Nishimura Synthesis f Silicn Carbide Pwders frm Fumed Silica Pwder and Phenlic Resin, J. Mater. Res., 1 [5] (006). 18. J. Li, J. Tian, and L, Dng Synthesis f SiC Precursrs by Tw-step Sl-gel Prcess and Their Cnversin t SiC Pwders, J. Eur. Ceram. Sc., (000). 19. H. Tanaka and Y. Kurachi, Synthesis f β-sic Pwder frm Organic Precursr and its Sinterability, Ceram. Inter., (1988). 0. L. Shi, H. Zha, Y. Yan, Z. Li, and C. Tang, Synthesis and Characterizatin f Submicrn Silicn Carbide Pwders with Silicn and Phenlic Resin, Pwder Technlgy, (006). 1. H.P. Martin, R. Ecke, and E. Müller, Synthesis f Nancrystalline Silicn Carbide Pwder by Carbthermal Reductin, J. Eur. Ceram. Sc., (1998).. K.D. Vladimir and Kastic, Prductin f Fine High-purity Beta Silicn Carbide Pwder, J. Am. Ceram. Sc., 75 [1] (199). w wz

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