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1 Jurnal f Krean Pwder Metallurg Institute Vl. 16, N. 5, 2009 DI: /KPMI /ekœ w TiC/C w w ¼ *Áw a w œ w œw, a Snthesis f TiC/C Cmpsite Pwder b the Carbthermal Reductin Prcess Gil-Geun Lee* and Gk-Hun Ha a Divisin f Materials Science and Engineering, Cllege f Engineering, Pukng Natinal Universit, San 100, Yngdang-dng, Nam-gu, Busan , Krea a Krea Institute f Materials Science, 531 Changwndaer, Changwn, Kungnam , Krea (Received Jul 10, 2009; Revised Jul 30, 2009; Accepted August 12, 2009) Abstract Ultra-fine TiC/C cmpsite pwder was snthesized b the carbthermal reductin prcess withut wet chemical prcessing. The starting pwder was prepared b milling f titanium diide and cbalt alate pwders fllwed b subsequent calcinatin t have a target cmpsitin f TiC-15 wt.%c. The prepared ide pwder was mied again with carbn black, and this miture was then heat-treated under flwing argn atmsphere. The changes in the phase, mass and particle size f the miture during heat treatment were investigated using XRD, TG-DTA and SEM. The snthesized ide pwder after heat treatment at 700 C has a mied phase f Ti 2 and CTi 3 phases. This cmpsite ide pwder was carbthermall reduced t TiC/C cmpsite pwder b the slid carbn. The snthesized TiC/C cmpsite pwder at 1300 C fr 9 hurs has particle size f under abut 0.4 μm. Kewrds : Carbthermal reductin, Titanium carbide, Cbalt, Cmpsite pwder 1. w (hard metals)» (phase) j w. w w k (WC, TiC, TaC ) j»ƒ š ƒ w» ù kü [1]. w ü ƒ w w» w ƒ w w ³ ww w w. j» w» w ƒ /w [2-5] š, k (WC, TiC ) s³ j»ƒ 200 nm w k k / w ƒ ƒ w [5, 6]. TiC WC-TiC-C œ TiC, TiCN p(cermet) œ Ÿ w š [7, 8]. š TiC pk (Ti 2 ) pk (TiH 2 )» /ek (carbthermal reductin) j œ w š [9-12]. ù œ 1400 C š, w TiC w j» w ƒ. w š w w wš TiC j» w» w, (spra dring) œ /ek(carbthermal reductin) œ w wœ (spra thermal *Crrespnding Authr : [Tel : ; [email protected]] 310

2 cnversin prcess), Ti-C- w w 1400 C w s³ j»ƒ 200 nm w TiC/C w w ƒ w [6, 13, 14]. ù wœ w ( ) w» w» w w,» w. wœ w TiC/ C w w pk (TiCl 4 ) g p (C(N 3 ) 3 6H 2 ) w pk (Ti 2 ) g p (C(N 3 ) 3 6H 2 ) w wš [6, 13, 14]. w wš, TiC/C w w œ w w ƒ. w wš ( )» w wœ œ Ti-C- w w, /ek TiC/C w wš w. /ekœ w TiC/C w w pk g p ³ w Ti-C- w w», pk Ti 2, g p cbalt alate (C 2 4 2H 2 ) w, 1 ƒƒ SEM ùkü., ek z TiC-15 wt.%c Ti 2 cbalt alate w ³ ww. z w»» 800 C¾ w w ü { w. w z w { carbn black(s³ j» : 0.5 μm) 24 ³ ww w w. carbn black w w z carbn w, ek, TiC/C w w v w carbn 130% w. w šƒ» 1400 C¾ /ek w TGA w dw. w TGA k w p Fig. 1. SEM micrgraphs f (a) titanium diide and (b) cbalt alate pwders. w šƒ» (1000~1400 C) (30 ~9 ) /ek w. šƒ 200 cc/min. w w. w /e k z XRD FE-SEM w w /ek (phase) w. 3. š 2 Ti 2 cbalt alate w» w w ùkü. TiC-15 wt.%c w ƒ w ü w { Ti-C- w w.» w Vl. 16, N. 5, 2009

3 312 ¼ Áw Fig. 2. Change in the weight fractin f the miture f titanium diide and cbalt alate pwders versus temperature. Fig. 3. X-ra diffractin patterns f the milled and calcined pwders. ùkü.» w 150 C 290 C w ƒ ùš 320 C j ùkü. w ü sw { { w w ƒ sww ƒ s ùkü w s k ƒ w w k w. { w z /ekœ, ek» w e q, ƒ s k ƒ w š q 500 C w kw C, 700 C, 800 C ƒƒ 2 w w XRD z ql ùkü.» anatase Ti 2 z vj š, 500 C w anatase-ti 2 C 3 4 z vjƒ, 700 C w anatase-ti 2, rutile-ti 2, CTi 3 z vjƒ š. 800 C w 700 C w z vj (phase) z vjƒ ù, 700 C w anatase-ti 2 z vj ƒ wš rutile-ti 2 CTi 3 z vj ƒ ƒw. pk cbalt alate w» w w Ti-C- w. cbalt alate» 300~800 C w w XRD w C 3 4 z vj. 500 C w w cbalt alate ü { z g p anatase-ti 2 C 3 4 ƒ q. 700 C w w cbalt alate ü { { g p Ti 2 ƒ C w CTi 3 w. w 700 C w w» anatase-ti 2 ƒ rutile-ti 2 z vjƒ, w Ti 2 kƒ û. wr Lee [13, 15] wœ w TiC/C w Ti-C- w w g p kƒ CTi 3 ƒ C 3 4 w pk w g TiC/C w /ek š š. w pk (Ti 2 ) ƒ anatase ƒ rutile w (pen Jurnal f Krean Pwder Metallurg Institute

4 /ekœ w TiC/C w w 313 Fig. 4. SEM micrgraph f cmpsite ide pwder calcined at 700 C. structure) ƒ š /ek ù š š [16]. w w Ti-C- w /ek w» w, g p ƒ CTi 3 wš, pk anatase w 700 C w w C w w SEM ùkü. w 0.2 μm w j» ƒ. w» w cbalt alate ( 1 ) { j» ƒ, pk cbalt alateƒ ³ w w» w kw» œ w μm ¼ ƒ e cbalt alate ƒ š, cbalt alate ƒ w œ w» q. pk cbalt alate w œ» w w w j»ƒ 0.2 μm w Ti-C- w w. Ti-C- w Lee [6, 13, 15] TiC/C w w w w œ e w w (phase) ƒ š. 5 w Ti-C- w carbn black ww w š ƒ» w Fig. 5. Change in the weight fractin f the miture f the calcined cmpsite ide pwder and carbn black versus temperature. ùkü. Ti-C- w carbn black w (1) w carbn 130% w w.» (Ti, C) w w z XRD l Ti 2 CTi 3 w carbn black w w. Ti 2 (s)+cti 3 (s)+7c=2tic(s)+c(s)+5c(g) (1) w 850 C¾ j ƒ ù, 850 C l ƒ wì w ù kùš, 1300 C w š. w Ti-C- w, ek» w, š k w /ek w TiC/C w w ƒ» w w p w šƒ» w. 6 Ti-C- w carbn black ww w 1200 C 1300 C w XRD z ql ùkü C 1300 C w, Ti-C- w 1300 C w /ek g ( 5 ), wœ Ti-C- w [13] š k w TiC/C /ek 1200 C 9 Vl. 16, N. 5, 2009

5 314 ¼ Áw Fig. 6. X-ra diffractin patterns f the miture f the calcined cmpsite ide pwder and carbn black heat treated in the tube furnace under a flwing stream f argn at a specified temperature fr a specified time. Fig. 7. Change in the lattice parameter f TiC versus heat treatment time.». Ti-C- w 1200 C 9 /ek wš Ti 3 5, Ti 2 3, TiC, C z v jƒ, pk w. /ek ƒw pk z vjƒ w, 1300 C 6 w TiC C z vj. wr 6 XRD z vj TiC [11, 17, 18] TiC Ti š, TiC ƒ w ùkù XRD z q l TiC TiC w». TiC TiC /ek» w XRD z ql l TiC w, /ek mw. 7 XRD z vj l TiC /ek ùkü. XRD z ql TiC vj w w 41.8 z v j l w. /ek ƒw ƒw w ùk ü. TiC ~ nm ƒ š, Ti nm ƒ [12]. TiC Ti š TiC, TiC Ti Fig. 8. SEM micrgraph f snthesized TiC/C cmpsite pwder at 1300 C fr 9 hurs b the carbthermal reductin using titanium-cbalt-gen-based cmpsite ide pwder. w w ƒ. w TiC ƒ /ek TiC j, TiC ƒw. 7 ùk ü TiC ƒ /ek ƒw ƒw w ù kü, /ek ƒw TiC ƒ TiC /ek. w 1200 C 9 w 1300 C 2 w ƒ ùkü, pk /ek j w. p 1300 C 9 w ƒ TiC w ùkü, Ti-C- w Jurnal f Krean Pwder Metallurg Institute

6 1300 C 9 š k w /ek w TiC/C /ek C 9 /ek g w TiC/C w SEM ùkü. w 0.4 μm w j» ƒ w.» pk cbalt alate w wœ œ 0.4 μm w j» ƒ TiC/C w w. TiC/ C w w œ Lee [6, 13, 15] w wœ š, /ek w w j» j w ùkü. ù w œ wœ w (Cl) (N), q. 4. wœ œ TiC/C w w» w, pk cbalt alate» w TiC/C w w ƒ mw. 1. Ti 2 cbalt alate» w w w w 0.2 μm w j» ƒ Ti-C- w w C w w Ti-C- w Ti 2 C 3 4, 700 C w w Ti-C- w Ti 2 CTi Ti 2 CTi 3 Ti-C- w š k w 1300 C 9 /ekœ w TiC/C w w 315 /ek w j»ƒ 0.4 μm w TiC/C w w w. š [1] K.J.A. Brkes: Wrd Directr and Handbk f Hardmetals and Hard Materials, 6th ed., K.J.A. Brkes (Ed.) Internatinal Carbide Data, Marsh Bartn (1996) 9. [2] G.G. Lee, G.H. Ha and B.K. Kim: Pwder Metallurg, 43 (2000) 79. [3] G.G. Lee and W.Y. Kim: Metals and Materials Internatinal, 11 (2005) 177. [4] K.E. Gnsalves, S.P. Rangarajan and J. Wang: Handbk f Nanstructured Materials and Nantechnlg, H.S.Nalwa (Ed.) Academic Press, Lndn (2000) 1. [5] B.K. Kim, G.H. Ha, D.W. Lee and G.G. Lee: Advanced Perfrmance Materials, 5 (1998) 341. [6] G.G. Lee, C.M. Mn and B.K. Kim: J. Krean Pwder Metallurg Institute, 10 (2003) 228 (Krean). [7] M. Sherif El-Eskandaran: J. f Alls Cmpund, 305 (2000) 225. [8] H. Preiss, L.M. Beger and D. Schultze: J. f Eurpean Ceramic Sciet, 19 (1999) 195. [9] N.A. Hassine, J.G.P. Binner and T.E. Crss: Refractr Metals & Hard Materials, 13 (1995) 353. [10] R. Kc: J. f Eurpean Ceramic Sciet, 17 (1997) [11] R. Kc: J. Mater. Sci., 33 (1998) [12] R. Kc and J.S. Flmer: J. Mater. Sci., 32 (1997) [13] G.G. Lee and G.H. Ha: Materials Transactins, 47 (2006) [14] G.H. Ha, G.G. Lee, M.C. Yang and B.K. Kim: Prceeding f EUR PM 2006 Vl. 1 Hard Materials, Eurpean Pwder Metallurg Assciatin, Shrewsbur (2006) 97. [15] G.G. Lee and C.Y. Kim: J. f Krean Pwder Metall. Inst., 12 (2005) 336 (Krean). [16] G.G. Lee and B. Kim: Materials Transactins, 44 (2003) [17] R. Shaviv: Mater. Sci. Eng., A209 (1996) 345. [18] L.M. Berger, W. Gruner, E. Langhlf and S. Stlle: Int. J. Refract. Met. Hard Mater., 17 (1999) 235. Vl. 16, N. 5, 2009