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1 Jurnal f the Krean Ceramic Sciety Vl. 46, N. 6, pp. 643~647, DOI: /KCERS Densificatin Behavir f C/C Cmpsite Derived frm Cal Tar Pitch with Small Amunt f Idine Additin Kwang Yun Ch, Dh Hyung Riu, Dng Geun Shin, Heyk Jng J*, Hyung Hi K**, and In Se Park** Divisin f Nan Materials Applicatin, KICET, Seul , Krea *Department f Plymer Science and Engineering, Chungnam University, Daejen , Krea **Agency fr Defense Develpment, Daejen , Krea (Received September 16, 2009; Revised Octber 16, 2009; Accepted Octber 22, 2009) k ve ƒw w k w e y Ÿ Á xá Á x *Á xz**á ** w» w * û w š œw ** w 4» ( ; ; ) ABSTRACT We investigated the viscsity behavir and the carbn yield f cal tar pitch (CTP) treated with idine. The viscsity f idine treated pitch shwed that the fluidity f idine treated CTP did nt increase within the idine additin f 1.4%. DTG analysis shwed that crss linking was accelerated at the temperature range frm 400 t 500 C with idine treatment, which is due t the accelerated dehydrgenative reactin by idine. The idine treatment was mainly effective fr β-resin cntent increase f CTP. The carbn yield f CTP increased frm 40 t 60% by the idine nn-treated CTP. Key wrds : C/C cmpsite, Viscsity, Carbn yield, Idine, Pitch 1. k y w (C/C) û,, w,, û q ùkü ƒ w š. k r, u š ve y» š mw. ve y. k /k 1) w we veƒ k (bundle) ù» œ(pre) e w wew œ. k /k w we ve y» š k y w yw w w kyƒ š y. ve k yw { w ve ky 30~40% Crrespnding authr : Kwang Yun Ch kych@kicet.re.kr Tel : Fax : ), 1z weœ mw e w k /k w ƒ x, 5z we, ky, yœ. we ve m w y ve ü w yw CH yw w w š x r w. ƒ w 2) w w k ƒ. ve weœ mw k /k w p we k y w. ve ky ww w. 3) ve ky y k /k w p w e Fernandez we ve œ» mw ky w w. ve aliphatic side chain œ w CH yw wš ƒ yw w w. ve ƒ w y ƒ ƒ ƒw. š 4,5) Kajiura š 643

2 644 Ÿ Á xá Á x Á xzá y mw ky ƒ y š šw. ù veƒ w ƒ 1) ù y, ky y ve y w e w š. š w ve ky y w w š. k /k w j» w w ƒ w ƒ û we z ky ve w š w. k ve g w yww z w ³ w yw yw w, û g w w w ve. ve w w w w. (1) y ve y w š, (2) ve ky w, ve g d w yƒ w. (3) š ve»»(functinal Grup) y ky y z y d w š y y w. 2. x w ve yw w k ve w š p Table 1 ùkü. š ve w» w w e g w 4.93 g/cm 3 š w š p Table 2 ùkü. ve j» 1mm w w z k w Ì» š w. w ve v 1:1 w v ƒw š k ve y w ¼ w. 150~200 rpm 12 w. 12 ve ve 1, Table 1. Prperties f Cal Tar Pitch Slubility(%) S. P. Cking Value Density Items BI TI ( C) (%) (g/cm 3 ) Cntents 10~15 30~35 100~ Table 2. Prperties f Idine Items Phase Density (g/cm 3 ) Melting pint ( C) Biling pint ( C) Cntents Slid 4.93 >113.7 >184.3 Radical -HIO, -HI, -IO, -IO - 3 2, 5, 10 wt% w w ƒw. ƒ ƒ yw 12 w ƒ ve š yww ve w yw w w. ve g, ƒ yw k yw wš» š 80 C» š 12 w g { w w w. w ƒ y w» w ASTM D (glass filter(05 µm), 75 C ƒ w, 1 g) w n, i g d w n i w β-resin w w. 6) ve FT-IR(Midac, M2000) w IR r p w ve»»(functinal Grup) y y w. w ve y y w» w ASTM D w Brkfield d» w spindle number 34, rpm 30, 2 C/min, 200~550 C d w. ve ky w» w 100 mg ve 1000 C¾ 5 C/min, 500 ml/min š» w. ve ky š», 2C/min 1000 C 1 w w. ky xr y š» 15 C/min 2300 C 1 w w. w y xr Cuk XRD» mw w š7,8) t k v Jbin-Yvn LAMAN HR (High Reslutin) w D-peak (diamnd peak) cm vj G-peak (graphite peak) 1590 cm w. š xr ky y xr y w» w Mettler tled TGA851 Thermal Aanlysis System w œ» 5 C/min 1000 C¾ y w. 3. š Fig. 1 w ve j d w y ùküš. ve ƒ w ƒ û ƒ û w. š ƒ 500 C w ƒ w w y û. w ve 330~440 C 26 cp ùkü. w 1% ve ƒ š ƒ w 2% ƒw ve ƒ ƒ w w 10% ve 335~365 C w wz

3 k ve ƒw w k w e y 645 Fig. 1. Viscsities f pitches with idine as a functin f temperature. Fig. 2. TG graphs f pitch with Idine as a functin f temperature. 350 cp ùkü. š û ù kü w ƒw š. w ve y w ƒ w 480 C ùš Bhatia, Aggarwal, Chari šw w 450 C ve ü w yw k y w w w ƒ wš š 500 C y ù ƒ w ew. 9) w ve ƒ w ƒ û š w 10% 365 C l ƒ w» w. Fig. 2 ve v. w ƒw 1000 C z ky š. š w 10% 61.3 wt% ky ùkü w ve ky 36.8 wt% 24.5 wt%ù. Bhatia šw û w yw w ƒ ùš ve Fig. 3. DTG f pitches with idine as functin f temperature. ƒw w ky š ew. 9) w ve ƒ y ù š û w yw w 3 w w yw { w ky q w. w w ƒ w Fig. 1 ƒ w w q. Fig. 3 ve d w v. ve ƒ š. š 3œ ù kù 1 š 315 C w ù 2, 3 š w ve ƒƒ 450 C 485 C ùkù w 10 wt% 2, 3 š 360 C 462 C ùkù û w. 315 C ù ƒ w yw ƒ w { x w ùkù q. 2, 3 š y veü w yw»»(functinal Grup ) e»(-ch 3 ), e»(-ch 2 ) w -CHI, -CIO, -CIOO, -CI w w y ƒ ƒ û y»» w veü w yw w ù q. Fig. 4 w y β-resin y ùkü v. w ƒw β-resin ƒwš. β-resin ve ü w yw w w w š y š r w aliphatic side»»(functinal Gru p) w w e w 46«6y(2009)

4 646 Ÿ Á xá Á x Á xzá Fig. 4. β-resin(wt%) f pitches as a functin f idine cntents. x w w. Fig. 2 w ƒ ky w w β-resin ƒ» š q. Fig. 5 y z xr t k IR rp w. js ƒ š ky ƒw we ve ww w 2wt% ve w ky, y w. ve w Dvj»ƒ w ùkü D/G f. w w»»(functinal Grup) y ùš y»» w veü w yw 3 ƒ w y w w w r w q. Fig. 6 y z xr ùkü XRD v. ve w 002»ƒ w Fig. 6. XRD curves f graphite samples as a functin f treatment. w. XRD mw y w as-received raw pitch w y ƒ 80.5% v e w y 51.2% w ƒ j w w. Fig. 5 w RAMAN w y»»(functinal Grup) w q w. Fig. 7 ve w ve w ky, yw xr œ», 10 C/min 1000 C¾ yw. ky xr, xr y ƒ xr 50 C ù yƒ y ƒ y ¾., y xr y š y w 17% w Fig. 5. Raman curves f graphite samples as a functin f treatment. w wz

5 k ve ƒw w k w e y 647 y 51.2% w w w. ky xr, xr y ƒ xr 50 C ù yƒ y ƒ y ¾., y xr y š y w 17% w. Acknwledgment Fig. 7. TG graphs f carbn and graphite samples as a functin f temperature.. ky z ky ü w ƒ w y w w y ƒ w q w. š û ƒ yƒ w š ù ƒ w w 3 w û ù, d w wš 3 w e w yƒ y (xidatin site)» w q w. 4. w ƒw ve ƒ ƒwš û ùkü w ƒw š. ve veƒ y ƒ w ƒ û. w w ƒw ky. w ƒ ky w w β-resin ƒ», ùkü D/G f. w ve»» (Functinal Grup) y ùš y»» w w yw 3 ƒ w y w w w r w q. as-received raw pitch w y ƒ 80.5% ve w w» y w,. REFERENCES 1. H. Kajiura, Y. Tanabe, and E. Yasuda, Carbnizatin and Graphitizatin Behavir f Idine-Treated Cal Tar Pitch, Carbn, (2006). 2. H. J. Jung, Y. J. Chung, D. W. Ch, and Y. S. Lim, A Sudy n the Cnditin f Cal Tar Pitch t frm Mesphase as a Matrix Precusr f Crbn/Carbn Cmpsites, J. Kr. Ceram. Sc., (1997). 3. C. Q. Ren., T. H. Li, Q. L. Lin, H. Li, and X. Y. Sun, Preparatin f Carbn Materials by Mdeling f Impregnating Cal-Tar Pitch int Carbn Prefrm, J. Mat. Pr. Tech., (2007). 4. J. Fernandez, A. Figueras, E. Granda, J. Bermej, and R. Menendez, Mdificatin f Cal Tar Pitch by Air-Blwing-I. Variatin f Pitch Cmpsitin and Prperties, Carbn, (1995). 5. J. Fernandez, A. Figueras, E. Granda, J. Bermej, and R. Menendez, Mdificatin f Cal Tar Pitch by Air-Blwing-II. Influence f Cke Structure and Prperties, Carbn, (1995). 6. S. M. Oh and Y. D. Park, Cmparative Sudies f the Mdificatin f Cal-Tar Pitch, Fuel, (1999). 7. S. Bnnamy, Carbnizatin f Varius Precursrs: Effect f Heating Rate, Carbn, (1999). 8. B. Petrva, T. Budinva, N. Petrv, M. F. Yardim, E. Ekinci, and M. Razvigrva, Effect f Different Oxidatin Treatments n the Chemical Structure and Prperties f Cmmercial Cal Tar Pitch, Carbn, (2005). 9. Bhatia, R. K. Aggarwal, S. S. Chari, and G. C. Jain, Rhelgical Characteristics f Cal Tar and Petrleum Pitches with and withut Additives, Carbn, (1977). 46«6y(2009)