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1 Journal of the Korean Ceramic Society Vol. 48, No. 1, pp. 1~5, 011. DOI: /KCERS Synthesis of SiC Nano-powder from TEOS by RF Induction Thermal Plasma Sang-Min Ko*, **, Sang-Man Koo**, Jin-Ho Kim*, Ji-Ho Kim*, Myeong-Seob Byeon*, and Kwang-Taek Hwang* *Korea Institute of Ceramic Engineering and Technology, Icheon , Korea **Department of Chemical Engineering, Hanyang University, Seoul , Korea (Received May 1, 010; Revised September 15, 010; Accepted September 17, 010) RF v w TEOS l SiC ù w š *, **Á **Á½ y*á½ y*á *ÁyŸk* *w» **w w ywœw ( ; ; ) ABSTRACT Silicon carbide (SiC) has recently drawn an enormous industrial interest because of its useful mechanical properties such as thermal resistance, abrasion resistance and thermal conductivity at high temperature. RF Thermal plasma (PL-35 Induction Plasma, Tekna CO., Canada) has been utilized for synthesis of high purity SiC powder from cheap inorganic solution (Tetraethyl Orthosilicate, TEOS). It is found that the powders by thermal plasma consist of SiC with free carbon and amorphous silica (SiO ) and, by thermal treatment and HF treatment, the impurities are driven off resulting high purity SiC nano-powder. The synthesized SiC powder lies below 30 nm and its properties such microstructure, phase composition, specific surface area and free carbon content have been characterized by X-ay diffraction (XRD), field emission scanning electron microscopy (FE-SEM), thermogravimetric (TG) and Brunauer-Emmett- Teller (BET). Key words : RF thermal plasma, Silicon carbide (SiC), TEOS, Nano powder 1. g e (Silicon carbide, SiC) t y y w ƒ š» š. š š, š,, w y w ü p SiC üy,, y š ù š. SiC e(sio ) k yww k y (Carbothermal reduction) w Acheson process w š. ù k y w SiC w œ š SiC x ƒ š š. š 1) SiC w œ š w (Self-propagation high-temperature synthesis, SHS), - (sol-gel) v w š. š w w SiC w g(si) Corresponding author : Hwang Kwang-Taek Tel : Fax : e (C) w SiC w w, w ƒ y w w ƒ š ù x šƒ. - Si C ) ³ w yww hybrid gel w z š š SiC w w. ù 3) - x yƒ š š. v w w š ( 4-6) 10 4 K), šy þ (>10 K/s) p 6 w, y, y, ky w xk ù w ƒ y w š š. v w 7,8) ƒ œ š v»y(vaporization) š,»y w, š v þ(quenching) ù. w v w ƒ š w» š,,» k w w š, 10 ms w. v w, œ, þƒƒ (Quenching gas), œ 1

2 š Á Á½ yá½ yá ÁyŸk Table 1. Plasma and Precursor Feeding Condition Plasma power 18 kw Central gas 0 slpm Dispersion gas 5 slpm Sheath gas 60 slpm Quenching gas 150 slpm Reactor pressure 15 psi Feed rate 19.5 ml/min Fig. 1. Schematic diagram of thermal plasma system for preparation of SiC nano powder. w, xk, j» w w. Tetraethyl orthosilicate(teos) v w w SiC ù w wš w. TEOS ƒ š, Si, O, C š H swwš SiO ù, 9,10) 1800 o C TEOS w SiC w š š. 11) SiC w w z free carbon e y w, z mw (free carbon, e) w š SiC ù š w. š v w SiC ù x, t š j»» q š SiC ù (T1, SUMITOMO, Japan) w.. x.1. e w v e (PL-35 Induction Plasma, Tekna CO., Canada) Fig. 1. v w e v me(torch), (Reactor), j (Cyclone) š s (Collector). ù w v j me š, w (Reactor bottom), j w (Cyclone bottom) š s w (Collector bottom) (Fig. 1). Fig. 1 Central gas me g š v w. Dispersion gas probe wì š v w, š v» y (vaporization). v ü» y v w, v w. Sheath gas m e ü me ü ywš v w. Quenching gas v ó v m w þ j, ù j w e. j e ³ wš j»ƒ ù s w SiC w. Central gas Dispersion gas š š ƒ (Ar, %) w, Sheath gas Quenching gas ƒ (N, %) w. v w x Table 1 ùkü... SiC ù w v w ù w» y(vaporization), w (nucleation), (growth) þ(quenching) mw. Tetraethyl orthosilicate (TEOS, Si(OC H 5 ) 4, >98.0%, SAMCHUN) rv mw š v m g» y z, w mw SiC ù w w. w SiC ü w free carbon e 850 C 1 o (Hydrofluoric acid) mw w..3. ù p w SiC ù y T1 X-ray Diffraction (XRD, D/MAX500VL/PC, Rigaku, Japan) ql x (FE-SEM, JSM-7001F, JEOL, Japan) m w ƒƒ ww. Thermo- w wz

3 RF v w TEOS l SiC ù w 3 Fig.. TG curve of synthesized SiC powder. gravimetric (TG, DTG-60H, SHIMADZU) mw free carbon w w y w, free carbon w (850 o C, 1 ) ww. BET (BelsorpII mini, BEL, Japan) mw SiC ù t d w, w j» w. d p =6/(ρ p S BET ) (1) d p s³, ρ p SiC (3.1 g/cm 3 ), š S BET BET d t. w j» ƒ w. 3. š v w w w SiC TG Fig. ùkü. y w 400 o C 750 o C¾ w yƒ ùš, 750 o C 900 o C¾ ƒ ù. w free carbon w, w SiC ü free carbon 750 o C. w SiC ü free carbon w 850 o C w, 1 ww. TEOS l v w g š, z g w ü free carbon w 8 wt% y. w free carbon w TG mw 30 wt% ew y w. Fig. 3 v w w w SiC XRD. Fig. 3(a) w SiC XRD. β-sic vj α-sic vjƒ y, 5 free carbon y. w 0~30 Fig. 3. X-ray diffraction patterns of the synthesized powder (a) as synthesized (b) after heat treatment at 850 o C/1 h (c) after HF treatment. e(sio ) q. Lee 11) TEOS w 1800 o C š SiC w šw. TEOS w v w K š w» SiCƒ x q w. ù TEOSƒ v m w š, v m ƒƒ», v ü w w 48«1y(011)

4 고상민 구상만 김진호 김지호 변명섭 황광택 4 기 때문에 TEOS 구성성분인 O, C 성분 등에 의한 free carbon 및 실리카가 일부 형성되는 것으로 확인되었다. 따 라서 앞서 언급한 바와 같이 free carbon 제거를 위한 열 처리 공정 및 비정질 실리카 제거를 위한 불산처리 공정 을 통하여 고순도의 SiC 나노분말을 제조하였다. Fig. 3(b) 는 합성된 분말을 850 C에서 1시간 열처리를 수행한 후 XRD 분석 결과이다. 결과에서 확인할 수 있듯이 주 성 분인 β-sic 피크, α-sic 피크 그리고 비정질의 실리카는 여전히 관찰되는 반면에, Fig. 3(a)에서 관찰되었던 비정 질 상의 free carbon 상은 확인되지 않았다. 이러한 결과 는 합성된 분말 내 free carbon이 열처리 과정을 통하여 기체상의 CO 로 제거된 것으로 판단된다. 그리고 Fig. 3(c) 는 free carbon이 제거된 합성분말에 대하여 불산처리를 수행한 SiC 분말의 XRD 분석 결과이다. 결과에서 알 수 있는 것처럼, 불산처리를 통하여 5도 근처에서 관찰되던 비정질 실리카 피크는 제거되고, SiC 피크만이 남아있는 것을 확인하였다. 따라서 열플라즈마 합성을 통하여 제조 된 합성 분말에 대하여 후처리 공정으로 불순물 (free carbon, 비정질 실리카)을 제거함으로써 고순도의 SiC 분 말을 얻을 수 있었다. Fig. 4는 열플라즈마 합성된 SiC 분말과 기존 상용화 SiC 분말 (T1)의 FE-SEM 분석 결과이다. Fig. 4(a)는 열 플라즈마 합성된 후처리 (열처리, 불산처리) 이전 SiC 분 말의 FE-SEM 이미지이다. 후처리 전의 SiC 분말은 수십 nm 크기의 입자들이 서로 뭉쳐있는 것을 확인할 수 있다. 반면에 Fig. 4(b)는 후처리를 통해 free carbon과 Silica를 제거한 SiC 분말의 FE-SEM 결과이며, SiC 분말 입자의 크기는 약 0~30 nm 인 것을 확인할 수 있다. 이러한 결 과는 입자크기 상대적으로 큰 불순물 (free carbon, 비정 질 실리카)이 후처리 공정으로 제거됨으로써 SiC 나노분 말이 유일하게 존재하는 것을 의미한다. Fig. 4(c)는 기존 의 시판중인 T1 분말의 FE-SEM 결과이며, 결과에서 알 수 있는 것처럼 T1 분말은 입자들의 크기가 약 70~80 nm 의 비교적 큰 입자들로 구성되어 있는 것을 확인 할 수 있다. 또한 FE-SEM 관찰 결과에서 열플라즈마 합성 SiC 분말(Fig. 4(b))은 비교적 입자 크기가 균일하며 구형을 보 이는 것에 비하여 T1 분말(Fig. 4(c))은 입자크기와 형상 이 균일하지 못한 것을 확인 할 수 있다. Table 는 BET 분석을 통한 SiC 합성분말의 비표면적 과 입자 크기를 계산한 결과이다. 후처리를 통하여 free carbon 과 실리카가 제거된 SiC 분말의 비표면적은 10.6 m /g으로 상용 T1 분말(4.5 m /g)의 약 3배에 이르는 것으로 확인 되었다. 위의 식 (1)을 이용하여 비표면적을 통한 입자들 의 평균 입경을 계산한 결과, 열플라즈마 SiC 분말의 평 균입경은 15.5 nm이고, T1 분말은 43.9 nm로 나타내었다. 이러한 계산 결과는 앞서의 FE-SEM 관찰 결과와도 일치 하는 것으로, 열플라즈마 합성을 통하여 제조된 SiC 분말 o Fig. 4. FE-SEM images of the synthesized particles (a) as synthesized (b) after heat and HF treatment, and (c) commercialized SiC powder(t1). 한국세라믹학회지 BET Surface Areas and Mean Particle Sizes of Synthesized Powder Sample BET (m/g) Particle size (nm) Synthesized powder T1 powder Table.

5 RF v w TEOS l SiC ù w 5 T1 w ³ wš, p y. 4. RF v w w š SiC ù w w. ƒ TEOS» w, w SiC free carbon e swwš. w w mw free carbon w (850 o C, 1 ) w, free carbon w 8% ( ) d. v w w z œ ww, š SiC ù. z e š SiC FE-SEM d 15.5 nm s³, BET 10.6 m /g t d š. y SiC (T1) 43.9 nm s³ 4.5 m /g t p š. mw ƒ l v w mw š SiC w w ƒ y w. wz y v w œ (œ, Quenching gas, œ ) y w mw w w z œ wš w w ƒ ww. Acknowledgment» y (008-C-CD11-P ) w. REFERENCES 1. A. Chrysanthou and P. Grieveson, Formation of Silicon Carbide Whiskers and Their Microstructure, J. Mat. Sct., (1991).. D.K. Kim, S. Park, K. Cho, and H.B. Lee, Synthesis of SiC by Self-Propagating High Temperature Synthesis Chemical Furnace(in Korean), J. Kor. Ceram. Soc., 31 [11] (1994). 3. I.N. Kholmanov, A. Kharlamov, E. Barborini, C. Lenardi, A. Li Bassi, C.E. Bottani, C. Ducati, S. Maffi, N.V. Kirillova, P. Milani, and J. Nanosci, A Simple Method for the Synthesis of Silicon Carbide Nanorods, J. Nanosci Nanotech, [5] (00). 4. T. Ishigaki, S.M. Oh, J.G. Li, and D.W. Park, Controlling the Synthesis of TaC Nanopowders by Injecting Liquid Precursor Into RF Induction Plasma, Science and Technology of Advanced Materials, (005). 5. R. Ye, J.G. Li, and Ishigaki, Controlled Synthesis of Alumina Nanoparticles Using Inductively Coupled Thermal Plasma with Enhanced Quenching, Thin Solid Films, (007). 6. Z. Karoly, J. Szepvolgyi, and Z. Farkas, Simultaneous Calcination and Spheroidization of Gibbsite Powders in an RF Thermal Plasma, Powder Technology, (000). 7. S. M. Oh and D. W. Park, Preparation of AlN Fine Powder by Thermal Plasma Processing, Thin Solid Films, (1998). 8. I. S. Han, S. M. Oh, W. P. Tai, W. S. Ahn, C. M. Lee, J. H. Oh, and D. W. park, Synthesis of Titanium Carbide Nanopowder using Thermal Plasma(in Korean), J. Kor. Ind. Eng. Chem., 14 [8] (003). 9. J. H. Lee, W. J. Kim, and J. Lee, Porous Silica Ceramics Prepared by Sol-gel Process-Effect of H O/TEOS Molar Ratio(in Korean), J. Kor. Ceram. Soc., 34 [] 16-4 (1997). 10. S. C. Lee and C. M. Lee, Studies on the Properties of the Plasma TEOS SiO Film(in Korean), J. Kor. Ceram. Soc., 31 [] 06-1 (1994). 11. S. Y. Lee, Synthesis of SiC-C Compound Using Oranic Precursor(in Korean), Ceramist Kor. Ceram. Soc., 1 [] 116- (1997). 1. Y. C. Yang and Y. N. Chun, Hydrogen Production for PEMFC Application in Plasma Reforming System(in Korean), Kor. Chem. Eng. Res., 46 [5] (008). 48«1y(011)

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