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1 Textile Science and Engineering Vl. 48, N. 1, 2011 ƒ s j p y ky w xá½ Á½» 1 Á w œ w lœw, 1 w» w ( / k) Analysis f Stabilizatin and Carbnizatin Behavirs f Ply(acrylnitrile) Fibers by Stepwise Heating D Hyeng Han, Su Bng Kim, Ki-Yung Kim 1, and Yng Sik Chung Department f Textile Engineering, Chnbuk Natinal University, Jenju , Krea 1 Cnvergent Textile Technlgy Grup, Krea Institute f Industrial Technlgy, Ansan , Krea (Received December 10, 2010/Accepted January 16, 2011) Abstract: The stabilizatin behavir f ply(acrylnitrile)(pan) fibers was mnitred by measuring the changes in density, structural aspects and mechanical prperties during cntinuus stabilizatin prcessing. The effects f the prcessing cnditins, such as the speed f precursr supply, yarn tensin, xidatin temperature, and treatment time, n the mechanical prperties f the final carbn fibers were als examined. The xidized PAN fibers were analyzed by measuring the density and armatizatin index. The change in yarn tensin had critical effects n the final mechanical prperties f the carbn fibers. The maximum mechanical prperties f carbn fibers were btained by prperly cntrlling the stabilizatin cnditins. Keywrds: ply(acrylnitrile), stabilizatin, tensin, residence time 1. k 1950 z k w p wœá» w ƒ y š. w k x š w š, wš k j k w w y š. w š, šk,, v w, / w, û q, ü t ƒ k ù w ƒ w [1].» v f š ƒw k v f k w w, k v f, pitch, plyacrylnitrile(pan) ƒ. p» ƒ PAN w ƒ ƒ š k v f š [2-6]. Crrespndence t Yng Sik Chung 2011 The Krean Fiber Sciety /2011-1/ k œ û ƒ œ ywš w. PAN k œ j. 1. v f œ : w PAN œ w š w š w w. 2. y œ : œ» w ù w 200~300 C ( y œ )w. 3. ky œ : y y»( )w 1000~2000 C (ky)w w. v f l y œ ¾ œ w ƒ k œ m w [3-9]. Fitzer Heine[4] PAN y œ d w 200 C yw wš, w k s³ 25% šw, ü w w» w. w, w y w. Bahl Mancha[5] PAN y PAN 1

2 2 w xá½ Á½» Á ƒ ù y w š, š y ü ù š w, w ky z w k š. ù š y w» w», x š y œ w». w, œ w». PAN v f w y œ PAN yw e w w w wš w. w, y kyw k wš, y y š w š w. 2. x 2.1. e PAN v f s³ 120,000 Jilin Chemical 1K v f w. y e x j» y e w š, ky e š» 3 zne tube furnace w. Figure 1 y e ùk ü PAN v f y PAN v f Figure 1 ùkü y e w w. y 2 1zne mww ƒ zne w w l w. ƒ zne,,, C š w š, 40, 80, 120 min. w Figure 1. Heat treatment scheme fr the stabilized PAN precursr; the tensin f the fibers was measured in the dtted circle psitin. Table 1. Stabilizatin cnditins Residence Speed rate (cm/min.) Lad time (min.) Feeding Heating Winding (g) R40T R80T R120T R80T R80T R80T R120T R120T R120T xw. š 80, 120 min. w d w. œ «w y. Table 1 x w ùkü. v R, T t»w, R T t»w ƒƒ» ùkü. š w v T0 t w PAN v f ky ƒ y PAN ƒ» w 5 C/min C¾ jš 5 C/min. þ ƒ w k w w PAN v f ƒ y ƒ zne» w d w. d (Check Master CN-100R, Kanai Kki) w š œ w w ƒw Figure 1 t m w d w. PAN v f y x ƒ ladder y yƒ (RR/DGA, RAY-RAN POLYTEST) w 1.2~1.85 g/cm ¾ 3 d w. PAN v f y z y» w XRD(PW 1700, Philips, X-ray diffractmeter) w 40 kv, 30 ma CuK α X-ray w Scan speed 4 /min. 2θ 10~60 ¾ d w. ƒ yw PAN kyw z ƒƒ k d w» w UTM(5567A, Instrn C., USA) w. 3. š 3.1. y œ p Figure 2 3 ƒ ùkü

3 다단가열에 따른 폴리아크릴로니트릴 섬유의 안정화 및 탄화 거동 분석 Degree f tensin as an indicatr during stabilizatin with a residence time f 80 min. Figure 2. Changes in density accrding t the stabilizatin residence times Density (g/cm3) Temperature Sample ( C) Stabilizatin Carbnizatin R40T R80T R120T Table 2. Table 3. cnditins Changes in density accrding t the stabilizatin Sample R80T20 R80T70 R80T190 R120T70 R120T150 R120T190 Degree f tensin as an indicatr during stabilizatin with a residence time f 120 min. Figure 3. 프이다. 장력의 발생원인은 각 zne에 해당되는 온도에서 분자간의 결합에 의해 분자구조의 수축에 의한 구조 변화 의 발생으로 생각할 수 있다. 초기 장력은 장력을 제어하 기 위해 공급부분에 발생하는 저항과 처음 챔버에서 발생 되는 장력이 연동되어 높게 나타난 것으로 생각된다. Figure 2와 3에서 초기 장력 이후 장력이 온도에 따라 증가하지만, C zne의 2번째 챔버에서 감소가 일어나는 것을 확인 할 수 있다. 이는 Fitzer[4]의 논문에서 나타난 수축 그래프 와 유사한 결과로써, 연속적인 안정화 장치에서는 물리적 수축에서 화학적 수축으로 변하는 온도가 C에서 나타 나는 것으로 생각된다. 또한, C zne의 2번째 챔버에 서 장력이 크게 증가되는 것을 확인할 수 있다. 이는 PAN 의 선형적인 구조가 C에서 활발히 구조변화가 일어나 기 때문으로 해석된다. 공정조건에 따라 전체적인 장력의 Textile Science and Engineering, Vl. 48, N. 1, Density (g/cm3) Stabilizatin Carbnizatin ± ± ± ± ± 크기는 다르지만 거의 비슷한 유형의 그래프를 나타내는 것으로 확인할 수 있다. 안정화 및 탄화 공정 후 밀도 분석 안정화 공정 후 PAN 프리커서의 밀도는 구조 변화에 따 른 구조 치밀화를 통해 차이가 나타나고, 이를 알아보기 위 하여 밀도 분석을 하였다. Table 2와 3에 각각 체류시간과 온도에 따른 안정화 공정 후 밀도 값과 안정화 공정 시 장 력 변화를 준 프리커서의 밀도 값을 나타내었다. Table 2에서 체류시간과 온도에 따라 밀도 값이 상승하 는 것을 확인할 수 있다. 이는 온도에 따라 점차 ladder 구 조와 같은 구조 변화가 진행되는 것으로 생각할 수 있다[2]. 밀도 값이 클수록 구조 치밀화가 많이 진행된 것으로 볼 수 있는데, 체류 시간별 최종 밀도 값이 이를 뒷받침한다. Table 3을 보면, 장력을 가한 것보다 장력을 제거한 샘플의 밀도 값이 더 높게 나타나는 것을 확인할 수 있다. 이는 장 력을 가하지 않으면 에너지를 받은 분자사슬의 배향이 풀 리면서 사슬 간의 가교결합이 더욱 용이할 것으로 생각된다. 탄화 공정 후에도 섬유의 turbstatic 구조 형성으로 인해 3.2.

4 4 w xá½ Á½» Á ƒ w, ky œ œ w w. Figure 4. XRD patterns f stabilized PAN fibers at different stabilizatin residence times. Figure 5. XRD patterns f the stabilized PAN fibers with different tensins at a stabilizatin residence time f 80 min. Table 4. Changes in AI values accrding t the stabilizatin cnditin Sample Armatizatin index R40T R80T R120T R80T R80T R80T R120T R120T R120T AI(armatizatin index) Figure 4 PAN v f y w» w XRD w w. PAN XRD vj 17 ùkùš y œ z 17 24~25 vj yƒ [5]. Figure 4 17 vjƒ ƒw š, 24~25 vjƒ ùkù y w, ƒ ladder y». Figure 5 80 min. w PAN v f XRD v ùkü. 17 w w v ƒ w v j y. ƒw w š. w, ƒw, ƒ ù w ù w ƒ. ƒ v AI Table 4 ùkü. š y ùkü AI m XRD[5] DSC [6] ù ký XRD w. AI ƒw ¼ ladder y w». j ù û, š w v AI w. yw w w» w yw š ƒw w w w» ƒ ky z p Table 5 ƒ v ky œ z k d w ùkü. Table 5 ¼ ƒ w y w. w y y w, ù û w. û w y œ Table 5. Mechanical prperties f the carbn fibers prepared by stabilizatin under different cnditins after carbnizatin up t 1200 C Sample Strength (MPa) Mdulus (GPa) R40T R80T R120T R80T R80T R80T R120T R120T R120T

5 ƒ s j p y ky 5 w ladder y w w w w ù» š, ƒ w w w ù» ƒ. 4. PAN v f ƒ š ³ y»» w y ww š,, PAN yw e w r. w y ƒ š ky w k wš y y w. PAN y œ w ƒw, C ƒ ù kù yw w y w. wš, w ƒw. œ z PAN v f XRD v y š, AI mw w y w. ky z d mw y w w w š, w w. :» ( y M ) w. š x 1. P. Mrgan, Carbn Fibers and Their Cmpsites, Taylr & Francis, USA, 2005, pp G. Henrici-Olive and S. Olive, The Chemistry f Carbn Fiber Frmatin frm Plyacrylnitrile, Mnsnt Textiles Cmpany, USA, 1982, pp M. S. A. Rahaman, A. F. Ismail, and A. Mustafa, A Review f Heat Treatment n Plyacrylnitrile Fiber, Plym Degrad Stabil, 2007, 92, E. Fitzer, W. Frhs, and M. Heine, Optimizatin f Stabilizatin and Carbnizatin Treatment f PAN Fibers and Structural Characterizatin f the Resulting Carbn Fibers, Carbn, 1986, 24(4), O. P. Bahl and L. M. Mancha, Characterizatin f Oxidised PAN Fibres, Carbn, 1974, 12, J. S. Tsai, The Relatinship Between Oxidized degree and Carbnizatin Temperature fr Carbn Fiber, Sample J, 1993, 29(5), J. S. Tsai and H. N. Hsu, Determinatin f the Armatizatin Index fr Oxidized Plyacrylnitrile Fibre by the Differential Scanning Calrimetry Methd, J Mater Sci, 1992, 11, A. Sedghi, R. Eslami Farsani, and A. Shkuhfar, The Effect f Cmmercial Plyacrylnitrile Fibers Characterizatins n the Prduced Carbn Fibers Prperties, J Mater Prc Technl, 2008, 198, J. Liu, P. H. Wang, and R. Y. Li, Cntinuus Carbnizatin f Plyacrylnitrile Based Oxidized Fibers: Aspects n Mechanical Prperties and Mrphlgical Structure, J Appl Plym Sci, 1994, 52, Textile Science and Engineering, Vl. 48, N. 1, 2011

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