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Department of Polymer Science and Engineering,

Kumoh National Institute of Technology, Gumi, Gyungbuk 730-701, Korea

*Composites Research Lab., Agency for Defense Development, P. O. Box 35-4, Daejeon, Korea

(Received January 10, 2005;accepted February 28, 2005)

5¨Ü žkªKk– v’(precursor) ‚vÒ ª¯W, ’W, JW N6 ÂÆW’² žk² â‚v² Z®

2úêÆ n22 šê² KkÊ:. Þ, 400 × Ê®&r ß®ê žkªKk >&r r3®ê BW² gfâ

– Jnëš /n®ê ^Ê~‚v®  N gꇖ ª kÆr:. ^Ê~‚v® žkªKk– žkª~

šÒ ~ã, ª¯Zî, ÚZ†Vú G KkÎæ& gê®â ®Ê²:. N FÂ&rê žkªKk ~ã

e Ž Û®® Î òFr î® v½Š e ã ª& †Ò  ^Ê~‚v& V®B žkªKk /ž Jî

² Ö&r r3®ê gfâ, ‚v ª N6 žkªKkš Ʋ ^Ê~‚v® Jžk‡š Æ®V :. ^Ê~‚v® g,  e Jžk‡– ~ã e òFr Û®– ¾& ®Ê®V’Æ, 3 vol% Ê®® ã

&r Î’² Zî®B žkªKkš nß®ê ÙÊ ^Ê~‚v& V®B ã ªKkš Vš®†& Vû W^¶ ْ² f>n:.G

Abstract:Stabilization process is absolutely necessary to convert the precursor fibers into chemically, physically, thermally and structurally stable carbon fibers. Especially, it is critically important for rayon fibers experiencing severe weight loss and thermal shrinkage occurring at the stabilization stage below 400 ×. The stabilization of rayon fibers strongly depends not only on stabilization temperature but also on heating rate, chemical pre-treatment, atmosphere, and so on. In the present study, the weight loss, fiber diameter change occurred in the furnace during the stabilization process for rayon fibers produced with various heating rates and in the absence and presence of phosphorous-based flame retardants and the thermal stability of the stabilized fibers were investigated. The result indicates that the weight, diameter and thermal stability of the rayon fibers are significantly affected by the type and amount of the flame retardant used. It is also suggested that the pre-treatment of rayon fibers with a concentration lower than 3 vol% of phosphoric acid is most desirable for further carbonization process of stabilized rayon fibers.

Keywords: rayon fiber, stabilization process, weight loss, fiber diameter, thermal stability, carbon fiber.

†To whom correspondence should be addressed. E-mail: [email protected]

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î ¢zŽ Þ:.¹¹ NB² žkªKk& Wûš N¶ n Þê K kÎæ& V² W^² r e ²W ÆÊ® vkÊ šê®:.

†Òr, N F® ÿW– šÒ® k2® ^Ê~‚v& V®B

žkªKkš ß®† ZR ® Jî² Ö&r r3®ê g

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žkªKk& ÿr ~ã ÆÊ® Wûš Æ®ê ÙÊ:. B

², žkªKkš ² ^Ê~‚v& V² Jžk‡š JgÚs

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šê² J‡ kJÒ † Z¾Ê:.

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®ê þRV Þ:. ¡N, FR-SHê C2 J&ú† ‚vÿ v†Î

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žkª~ê 400 ×Ê’Æ, 150, 175 e 200 ×/h® Ž Û®®

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ZæZN(SEM, JEOL JSM-5900)š ÿ®B V†®V:. ^Ê~

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žkªKk   ^Ê~‚v® Jžk‡& N®ê žkª Kk ~ã– òFr î v⋅Š e ¾® Wûš Æ®† Z

®B JgÚs†(Thermogravimetric Analyzer, TGA 951, Du Pont) Ò ÿ®B 50 cc/min® ÊÆ âVúV vÛnê Þ²‡ ÚZ†

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Figure 1– žkªKk 2 ÿr Ž Û®® ~ã ÆÊ&r 

 žkª‚v® gfâ& N®ê Î òFr î® váŠ

– Û®& V² Wûš JBRê RÊ:. žkªKk– K†Ú Z†&r ß®V’Æ ~ê 400 ×, òFr ãê WW 1 vol% Ê

:. žkªKkš K† g&r ß² Êvê n§‡ ÚZ†® Ê

0 0 0 0 0 0

N o t r e a t m e n t P h o s p h o r i c a c i d H - 2 0 5 F R - S H 75

6468 69 78

72 68 68

76 64

70 65

433

;3 93 73 53 3

Weight loss(%)

483# 4:8# 533#

Heating rate(×/h)

Figure 1. Weight losses of the rayon fibers untreated or treated with different flame retardants of 1 vol%, occurring during stabilization process to 400 × at different heating rates.

V ^Ê~‚v JÚÊ 2 Ê(tar) k‡š r®6 nn§š

_2ú† ¢ŽÊ:. žkªKk  òFr îÒ ®  – ^ Ê~‚v® gfâ~Ê 70% ÊΠٖ ÒnW’² ^Ê~‚v ê 400 × Ê®&r 3>® ’® Rkš Æ®Êr ª¯ÂÆ

ª– ¾. BW² gfâÒ /n®ê JnëÊ r3®† ¢Ž

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»12% k Z:¢š «Î¶ n Þ:. ÊB² Rê òFr®

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n:. NBî N :.’²Ö† – gfâ R&r Ž òF r g æ ÙÊ VW’² ª n®:6 Û«®â ¶)†&

ê :â zÊ Þ:.

Figure 2ê Ž Û® òFr® ãV 400 × Jî~¢ 150 ×/h

® /Ò² ~ã² K†ÚZ† ®&r žkª2†š ¢ 

^Ê~‚v® gfâ& N®ê Wûš JBV:. JîÒ ZV

®  – J: òFr² Zî² & žkªr ^Ê~‚

v® gfâV Z::. òFr® ãV óV¶n³ ή

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r 66»68%® VW’² :â Æ gfâÒ î:. ã V

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(brittleness)Ê ª :ê ٚ wž’² «Î¶ n Þ:. †Ò r Ó 3% Ê®® ã&r ÿ®ê ÙÊ jâ®:6 f>r:.

N6 žkª‚v& >‡Ê Þ’Ê ã ªKk  ê  â‚v C2 >‡Ê ޚ n ޒ² žkªKk& †B®ê ê Z &r ª – ã&r® ÿÊ âûr:.

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®  – ÙJ: Ââ Z::ê ÙÊ:. òFrÒ ÿ®

 ®š ¢ ~ãV æn³ ^Ê~‚v® – Ó 6 µm Ê

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ʖ NV² v®6 Þ’î ‚v²Ê– :â ær ٚ « ζ n Þ:. òFr² Zî®6 žkªr ‚v® Ê î

®  – Ù& šÊ ~ã& †Ò Ó 15»60% k Ââ î

:. î®  – ‚v® – ~ãV 150 ×/h² Vû r ‚v® – ~ã& Ââ Wûš q  ®:. †Òr, ò Fr® ÿ– ^Ê~‚v® žkªKk ã e þ~‡š 6z¶

¢ VW’² ¶Î ~ãV ª jⶠْ² ^r:.

B², Ž Û® òFr g ‚v® fâ r& ÎÊ VW

’² J: þ~W’² †B®ê ْ² f>r:.

Figure 4ê òFr® ãª& †Î žkª ^Ê~‚v® 

ªÒ JBRê RÊ:. nÿ·& B¾n Þê òFr 1 vol%

²Ö† 10 vol%¢® ãWC&r žkªr ^Ê~‚v® 

– ¦2B ªÊ Ó 8.7»9.8 µm® Â†Ò lê ْ² V†

433#

;3#

93#

73#

53#

3#

Weight loss(%)

# 4# 6# 8# 43#

Concentration(vol%)

0 0 0 0 0 0

75 6468 69

75

59 66

62 75

60 62 75

5660

1 3 5

N o t r e a t m e n t P h o s p h o r i c a c i d H - 2 0 5 F R - S H

Figure 2. Weight losses of the rayon fibers untreated or treated with different flame retardants and concentrations, occurring during stabili- zation to 400 × at 150 ×/h.

45 43

; 9 7 5 3

Fiber diameter(µm)

483# 4:8# 533#

Heating rate(×/h)

0 2 4 6 8 0

2 N o t r e a t m e n t P h o s p h o r i c a c i d H - 2 0 5 F R - S H

5.8 9.3 9 8.7

7.1 9.2

8.8 8.1

7 9.39 9.2

Figure 3. A comparison of average diameters of the rayon fibers untreated or treated with flame retardants of 1 vol% and then stabilized to 400 × at different heating rates.

0 2 4 6 8 0 2

5.8 9.39 8.7

5.8 9.3 9.1 9

5.8 9.7

8.9 9.8

5.8 9.4 N o t r e a t m e n t

P h o s p h o r i c a c i d H - 2 0 5 F R - S H

45#

43#

;#

9#

7#

5#

3#

Fiber Diameter(µm)

4# 6# 8# 43#

Concentration(vol%)

Figure 4. A comparison of average diameters of the rayon fibers untreated or treated with flame retardants and concentrations and then stabilized to 400 × at 150 ×/h.

n:. ß, 1»3 vol%® VW’² – ãÒ ÿ®B žkª îÒ ®B ^Ê~‚v® Ê Ââ fânê Zš ¶

n Þ¢š r2®B V:. N6 Îî®  ‚vÊ  VW’² :â Ââ v~š «Î¶ n Þ:. ή ãV ó V¾& †Ò ‚v® 6– Ó 9.2»10.1 µm êZÒ î:.

Ž Û®® òFr g Î’² Zî®B ^Ê~‚vÒ žkª2

†š ¢V VW’² Vû è– ‚vš v®V¢š ¢ n Þ:. B², òFrÒ ÿ®Vš ¢ žkªr ‚v® >ÊÊ Jî

Rk&r æn  ®:. ÊB² ^Ê~‚v® ªê ´

&r JBV žkª Rk&r r3² ‚v® gfâ ª– r

² Ò®®ê RÊ:. ÿr Ž Û®® òFrê þ¦ ^Ê~‚

v® Ê k‡š fâ2úêÆ †B² ÙÊ ÚÛ®:. ÒnW’² Î òFrV ^Ê~‚v® žkª& çÿ®ê n§ ª:î–

š ÚÛÞ sV  ®’î òFr Û®& †Ò r² :Ò Ù

’² ^r:.

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Figure 5ê K†ÚZ† ®&r 400 ×, 150 ×/h® žkªKk Æ Ê&r  ^Ê~‚v® Jžk‡& N®ê òFr Û®® W ûš JBV:. Figure 5® ®>Öê DTG 7vš î:. ÿ² òFr ãê 3 vol%² /Ò®V:. òFr îÒ ®  – ÙJ:

î² Ù® 500 × ÊZ&r® gæ:Ê ª Ââ r3®V:.

Êê ‚v²Ê& îr Òk® òFrV JÚÊ n§š /n®

Êr nrn† ¢ŽÊ:. Ó 120 × ÊZ& V†nê ^† gfâ

ê žkªRk&r k‡r ‚v²Ê& Ê®ê R² âÒ B¾

®6 Þê ª¯Vû†V ‚v²Ê’²Ö† ÊnÊr r3®ê Z

R 2 VšRk&r Ûv n Þê â® nÚÊ rÆnÊ r ^îr ْ² f>r:. TGA Rê òFr® ÿÊ ^Ê~

‚v® ²Ê& ª $– Vû†Ò k‡®B žkªKkš _2ú êÆ †B²:ê ٚ ZgW’² r2®B V:.

400 × ÖR&rֆ 2~W’² r3² gfâê wk& ÿ r žkª‚vV 400 ×¢ Jîr Ùʆ ¢ŽÊ:. †Òr N Ê® ~&r ‚v® JÚÊ n§Ê ßnÊr nr‡ÚÊ ê VW’² r3²:. î² &ê òFr Û®& VÊ Ó 500 × ÊZ&r žkª‚v® Jžk‡– Æ® v®:ê ٚ

®  òFr îÒ ®  – ÙJ: :â è– Jžk‡š J Î nÊ, H-205® &ê zÞz – žk‡š î:. DTG

RÒ JÊ, ή ÿ– 500 × Ê® gfâ ãV Vû

¶Êâ Òîê ~Ò 559 ×&r 533 ײ Ó 26 × V ê ê nÊ, H-205– FR-SHê Ó 10»20 × óV2r Rê ْ² Æn:. B² 800 × ÖR&r  ân~– ή 

V VW’² è– Ù’² î:.

^Ê~‚v ²Êš Î’² Zî²  žkªKkš ß®B

– ^Ê~‚v&r 500 × Ê® gæ:Ê Vû ¶Êâ ß nê ~V VW’² :ê :– :Î ¦ òFrJ: Î

Ê ^Ê~‚v® ªKk _r²r þRW’² çÿ¶ n Þ:

Figure 5. TGA(top) and DTA(bottom) thermograms measured in N2 for the stabilized rayon fibers without and with flame retardant treatments.

0 0 0 0 0 0 0

No Treatment Phosphoric Acid H - 205 FR - SH

# 3# 533# 733# 933# ;33#

Temperature(×) 453

433

;3 93 73 53 3

Weight(%)

.3 .2 .1 .0 .1

No Treatment Phosphoric Acid H - 205 FR - SH

559 533

569 579

# 3# 533# 733# 933# ;33#

Temperature(×) 314

313

0314 0315 0316

Deriv. weight(%)

Figure 6. TGA(top) and DTA(bottom) thermograms measured in N2 for the stabilized rayon fibers without and with phosphoric acid treatment at different concentrations.

0 0 0 0 0 0 0

No Treatment 1 vol%

3 vol%

5 vol%

10 vol%

3# 533# 733# 933# ;33#

Temperature(×) 453#

433#

;3#

93#

73#

53#

3#

Weight(%)

.3 .2 .1 .0 .1

No Treatment 1 vol%

3 vol%

5 vol%

10 vol%

559 524 524 535 535

3# 533# 733# 933# ;33#

Temperature(×) 314#

313#

0314#

0315#

0316#

Deriv. Weight(%)

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~‚v& Ê®ê Þ2³: NOš rÆ®ê n§š _®²

㒲 Êê ªKk Rkš ª¯W’² ª2úê C¶š

¶ n Þ:ê ْ² J6n6 Þ:.¹¹NB² ÊB² òFrê ž kª~&r –F²zú ÂÆ® nn§š _2ú6 nr Ê

Æ †B²:.

Figure 6– 400 ×, 175 ×/h, K†ÚZ†&r  žkª‚v®

Jžk‡& N®ê Î ã® Wûš JBV:. òFrÒ ÿ®

B rÆr žkª‚v® Jžk‡– î®  – ÙJ: š

ê ûš ¢ n Þ:. Êê Figure 5&r _r j– oÊ, ‚v² Ê& îr òFrV 500 × ÊZ&r r3®ê JÚÊ Z ¢

Ž& ª¯ÂÆV ®nÊr nr’Ê rÆn† ¢ŽÊ:. B² 5»10 vol%® VW’² è– Î ã&r îr žkª‚v ê 1»3 vol%® – ã&rJ: 400 × Ê&r ã JÚÊ&

®² gæ:Ê ª è– ~&r r3®V:. DTG R&r î

n  6 rÆr ‚v® 500 × Ê® gfâê Ó 559 ×

&r Vû ¶Êâ ßr nÊ, Î’² î²  6~&r®

gfâV Ó 24»35 × k – ~&r ²r®â Òîê ٚ «Î¶ n Þ:. Ó 600 × Ê&r® Jžk‡– Î ã

V èšn³ :â èâ î:. ^Ê~‚v ²Ê& în Þ ê Î ‡Ú– žkª Rk& vW’² K† g® ■n§®

B ²‡æ&r žk² ª’š k‡²:. žkªKk /ž Î

’²Ö† pyrophosphoric acid– metaphosphoric acidÒ Æ& phopho- us² ®r¹² ‡ÚÊ TGA wk g ã JÚÊ ÆÊ& ÎònÊ r êV gfâÒ ^î®Vš ْ² f>r:.

Figure 7– 3 vol% ã® FR-SH òFrÒ ÿ®B ^Ê~‚v Ò K† g 400 ×&r žkªKk   ‚v& V®B ~

ã ª& †Ò r3®ê gfâÒ JBV:. žkª‚v® 500 × Ê®&r® Jžk‡– 150, 175 e 200 ×/h Ž ~ã& ®Ê

¦2B Wûš q  ®:. ~ãV æn³ 500 × Ê

&r® gf⠒Âê è– ~ ’² Ê/®V:. Êê –

~ã&r žkªKkš ߶  ^Ê~‚vê G~ÆÊ® J î² Ö&r ª Š 2Z /ž žkªn† ¢ŽÊ:.

4. û«

Ž Û®® Î òFr Î, H-205 e FR-SH² WW Zîr

^Ê~‚v& V®B nß² žkªKk Rk&r Jî² Ö

&r r3² gfâ e ‚v® 6 ªÒ Ʋ Rê W^² ¾® Îÿ·® îV ^Ê~‚v® žkª& Vû þ RW’² †B²:ê ٚ r2®B R:. B² Î, H-205 e FR-SHÒ V š¦¶ ¢, žkªKk   ^Ê~‚v& V

®B Þ²‡ ÚZ†&r wk² Jžk‡ Ús R 500 × Ê

&r® ²V gæ:Ê Òîê ~V ή  Vû ’

Æ, 700 × Ê&r® ân~Ê VW’² è:ê ْ²Ö†

ÎÊ žkª ^Ê~‚v® ª_r² çÿ®B ªn§ã

Ò ¶Êâ ®Æ ^Ê~ â‚v&r® ªn~ û& †B

¶ n ޚ ْ² "n:.

[÷£# KÜN FÂê ^zKRV¯¦® ¯vFš &&

®Ê nßn’² Ê& f2:.

S+S

1. M. M. Tang and R. Bacon, Carbon, 2, 211 (1964).

2. R. Bacon and M. M. Tang, Carbon, 2, 221 (1964).

3. R. Bacon, in Chemistry and Physics of Carbon, P. L. Walker, Jr. and P. A.

Thrower, Editors, Marcel Dekker, New York, vol. 9, p. 1 (1973).

4. L. H. Peebles, in Carbon Fibers: Formation, Structure, and Properties, CRC Press, Chapter 2 (1995).

5. J. V. Duffy, J. Appl. Polym. Sci., 15, 715 (1971).

6. J. E. Hendrix and G. L. Drake, Jr., J. Appl. Polym. Sci., 16, 41 (1972).

7. F. Shafizadeh and A. G. W. Bradbury, J. Appl. Polym Sci., 23, 1431 (1979).

8. B. F. Jones and R. G. Duncan, J. Mater. Sci., 6, 289 (1971).

9. A. C. Pastor, F. Rodriquez-Rinoso, H. Marsh, and M. A. Martinez, Carbon, 37, 1275 (1999).

10. D. Cho, J. Lee, and J. K. Park, J. Soc. Adhesion and Interface(Korea), 5, 10 (2004).

11. O. P. Bahl, Z. Shen, J. G. Lavin, and R. A. Ross, in Carbon Fibers, 3^rd Ed., J.-B. Donnet, T. K. Wang, and J. C. M. Peng, Editors, Marcel Dekker, New York, Chapter 1 (1998).

12. D. Cho, H. S. Kang, H. C. Park, H. S. Ha, B. I. Yoon, and K. S. Kim, Polymer(Korea), 20, 650 (1996).

Figure 7. TGA(top) and DTA(bottom) thermograms measured in N2 for the rayon fibers treated with FR-SH of 3 vol% and then stabilized to 400 × at different heating rates.

0 0 0 0 0 0 0

150 ^OC 175 ^OC 200 ^OC

# 3# 533# 733# 933# ;33#

Temperature(×) 453

433

;3 93 73 53 3

Weight(%)

3 2 1 0 1

150 ^OC 175 ^OC 200 ^OC

579

571 547

# 3# 533# 733# 933# ;33#

Temperature(×) 314#

313#

0314#

0315#

0316#

Deriv. weight(%)