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(precursor) vV kªvÒ Æ& ªKk Rk&r J:
è Jî~& Îòn ª¯W, W² k² ÂÆÒ v®³ ®êÆ n22 ê² RkÊ:.
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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 kªKk vÂ(precursor) vÒ ª¯W, W, JW N6 ÂÆW² k² âv² Z®
2úêÆ n22 ê² KkÊ:. Þ, 400 × Ê®&r ß®ê kªKk >&r r3®ê BW² gfâ
Jnë /n®ê ^Ê~v® N gê ª kÆr:. ^Ê~v® kªKk kª~
Ò ~ã, ª¯Zî, ÚZVú G KkÎæ& gê®â ®Ê²:. N FÂ&rê kªKk ~ã
e Û®® Î òFr î® v½ e ã ª& Ò ^Ê~v& V®B kªKk / Jî
² Ö&r r3®ê gfâ, v ª N6 kªKk Ʋ ^Ê~v® Jk Æ®V :. ^Ê~v® g, e Jk ~ã e òFr Û® ¾& ®Ê®VÆ, 3 vol% Ê®® ã
&r β Zî®B kªKk nß®ê ÙÊ ^Ê~v& V®B ã ªKk V®& Vû W^¶ Ù² 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: dcho@kumoh.ac.kr
W² Jî~V èn³ N6 ~ãê n³ v
& Ê®ê âÚ óV®ê nÊ âÚ fâ²:. v
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kªKk ß® ZR ® Jî² Ö&r r3®ê g
fâ v& N®ê r² :Î òFr Û® e ã, N6
kªKk& ÿr ~ã ÆÊ® Wû Æ®ê ÙÊ:. B
², kªKk ² ^Ê~v& V² Jk JgÚs
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kª v® Jk& N®ê ª¯Zî® Wû Æ®
Z®B kªKk nß® Z& :¢R o Û®® Î
òFr² ^Ê~v® ²Ê î®V:. ß, Î(phosphoric acid, H3PO4, «ª¯e), 3-(hydroxylphenyl phosphinyl)propanoic acid (HIRETAR-205, H-205, (R)KOLON), N6 FR-SH(Flame Retardant- Special Hard) ((R)2ª). N, Î î ¢z òF v
g® ®îÊÆ ê² ã& Ò nÿ· 2² Âs®B ÿ
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®ê þRV Þ:. ¡N, FR-SHê C2 J&ú vÿ vÎ
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³ dip-coating ë² Ó 12Z / ¾2ú6 zf&r Ó 62Z / ÊÆ2þ kªKk ß®V:.
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kªKk ^Ê~v® Jk& N®ê kª Kk ~ã òFr î v⋅ e ¾® Wû 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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Z®B DTG(derivative thermogravimetry) 7v Æ®V:.
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Figure 1 kªKk 2 ÿr Û®® ~ã ÆÊ&r
kªv® gfâ& N®ê Î òFr î® vá
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:. kªKk 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 r®6 nn§
_2ú ¢Ê:. kªKk òFr îÒ ® ^ Ê~v® gfâ~Ê 70% ÊÎ Ù ÒnW² ^Ê~v ê 400 × Ê®&r 3>® ® Rk Æ®Êr ª¯ÂÆ
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² ß² kªKk&r ^Ê~v® gfâV Ó 6
»12% k Z:¢ «Î¶ n Þ:. ÊB² Rê òFr®
îV kª þÞê Z vn~&r Ê ç fâ2ú 6 (char) ¾ óV2ú ¢Ê:. òFr² în
J: W òFr² îr þ¦ gfâ rþRV û
n:. NBî N :.²Ö gfâ R&r òF r g æ ÙÊ VW² ª n®:6 Û«®â ¶)&
ê :â zÊ Þ:.
Figure 2ê Û® òFr® ãV 400 × Jî~¢ 150 ×/h
® /Ò² ~ã² KÚZ ®&r kª2 ¢
^Ê~v® gfâ& N®ê Wû JBV:. JîÒ ZV
® J: òFr² Zî² & kªr ^Ê~
v® gfâV Z::. òFr® ãV óV¶n³ ή
&ê gfâV 64%&r 56%², FR-SH® &ê 69%&r 60%² fâ®V:. N6 H-205Ò ÿ®V ¢ê 1»3 vol%&
r 66»68%® VW² :â Æ gfâÒ î:. ã V
& Î òFr þRê 3 vol% Ê®® ãV N Ê® è
ãJ: VW² ª Ââ çÿ² Ù² f>r:. B², òFr ¾Ê óV¾& Ò kªKk v® >
(brittleness)Ê ª :ê Ù w² «Î¶ n Þ:. Ò r Ó 3% Ê®® ã&r ÿ®ê ÙÊ jâ®:6 f>r:.
N6 kªv& >Ê ÞÊ ã ªKk ê âv C2 >Ê Þ n Þ² kªKk& B®ê ê Z &r ª ã&r® ÿÊ âûr:.
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Figure 3 kªKk 2 ÿ² ~ã& Î ^Ê~v Ò®® 6 ªÒ JBV:. þ6 ~ã&r Vû ¦2 B : òFr² Zî² Ò®® 6® fâV î
® ÙJ: Ââ Z::ê ÙÊ:. òFrÒ ÿ®
® ¢ ~ãV æn³ ^Ê~v® Ó 6 µm Ê
®¢ fâ®V:. kªKkÊ "r & Þ2¯² v>
Ê NV² v®6 Þî v²Ê :â ær Ù « ζ n Þ:. òFr² Zî®6 kªr v® Ê î
® Ù& Ê ~ã& Ò Ó 15»60% k Ââ î
:. î® v® ~ãV 150 ×/h² Vû r v® ~ã& Ââ Wû q ®:. Òr, ò Fr® ÿ ^Ê~v® kªKk ã e þ~ 6z¶
¢ VW² ¶Î ~ãV ª jⶠٲ ^r:.
B², Û® òFr g v® fâ r& ÎÊ VW
² J: þ~W² B®ê Ù² f>r:.
Figure 4ê òFr® ãª& Î kª ^Ê~v®
ªÒ JBRê RÊ:. nÿ·& B¾n Þê òFr 1 vol%
²Ö 10 vol%¢® ãWC&r kªr ^Ê~v®
¦2B ªÊ Ó 8.7»9.8 µm® ÂÒ lê Ù² 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%® VW² ãÒ ÿ®B kª îÒ ®B ^Ê~v® Ê Ââ fânê Z ¶
n Þ¢ r2®B V:. N6 Îî® vÊ VW² :â Ââ v~ «Î¶ n Þ:. ή ãV ó V¾& Ò v® 6 Ó 9.2»10.1 µm êZÒ î:.
Û®® òFr g β Zî®B ^Ê~vÒ kª2
¢V VW² Vû è v v®V¢ ¢ n Þ:. B², òFrÒ ÿ®V ¢ kªr v® >ÊÊ Jî
Rk&r æn ®:. ÊB² ^Ê~v® ªê ´
&r JBV kª Rk&r r3² v® gfâ ª r
² Ò®®ê RÊ:. ÿr Û®® òFrê þ¦ ^Ê~
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ÚÛÞ sV ®î òFr Û®& Ò r² :Ò Ù
² ^r:.
3.3 ?]`|#C£ß#Lð
Figure 5ê KÚZ ®&r 400 ×, 150 ×/h® kªKk Æ Ê&r ^Ê~v® Jk& N®ê òFr Û®® W û JBV:. Figure 5® ®>Öê DTG 7v 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§ /n®
Êr nrn ¢Ê:. Ó 120 × ÊZ& Vnê ^ gfâ
ê kªRk&r kr v²Ê& Ê®ê R² âÒ B¾
®6 Þê ª¯VûV v²Ê²Ö ÊnÊr r3®ê Z
R 2 VRk&r Ûv n Þê â® nÚÊ rÆnÊ r ^îr Ù² f>r:. TGA Rê òFr® ÿÊ ^Ê~
v® ²Ê& ª $ VûÒ k®B kªKk _2ú êÆ B²:ê Ù ZgW² r2®B V:.
400 × ÖR&rÖ 2~W² r3² gfâê wk& ÿ r kªvV 400 ×¢ Jîr ÙÊ ¢Ê:. Òr N Ê® ~&r v® JÚÊ n§Ê ßnÊr nrÚÊ ê VW² r3²:. î² &ê òFr Û®& VÊ Ó 500 × ÊZ&r kªv® Jk Æ® v®:ê Ù
® òFr îÒ ® ÙJ: :â è Jk J Î nÊ, H-205® &ê zÞz k 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 Ù² Æn:. B² 800 × ÖR&r ân~ ή
V VW² è Ù² î:.
^Ê~v ²Ê β Zî² kªKk ß®B
^Ê~v&r 500 × Ê® gæ:Ê Vû ¶Êâ ß nê ~V VW² :ê : :Î ¦ òFrJ: Î
Ê ^Ê~v® ªKk _r²r þRW² 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(%)
ê Ù ZgW² r2®B V:. W^² òFr® ÿ ^Ê
~v& Ê®ê Þ2³: NO rÆ®ê n§ _®²
ã² Êê ªKk Rk ª¯W² ª2úê C¶
¶ n Þ:ê Ù² J6n6 Þ:.11NB² ÊB² òFrê kª~&r F²zú ÂÆ® nn§ _2ú6 nr Ê
Æ B²:.
Figure 6 400 ×, 175 ×/h, KÚZ&r kªv®
Jk& N®ê Î ã® Wû JBV:. òFrÒ ÿ®
B rÆr kªv® Jk î® ÙJ:
ê û ¢ n Þ:. Êê Figure 5&r _r j oÊ, v² Ê& îr òFrV 500 × ÊZ&r r3®ê JÚÊ Z ¢
& ª¯ÂÆV ®nÊr nrÊ rÆn ¢Ê:. B² 5»10 vol%® VW² è Î ã&r îr kªv 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, β î² 6~&r®
gfâV Ó 24»35 × k ~&r ²r®â Òîê Ù «Î¶ n Þ:. Ó 600 × Ê&r® Jk Î ã
V èn³ :â èâ î:. ^Ê~v ²Ê& în Þ ê Î Ú kª Rk& vW² K g® â n§®
B ²æ&r k² ª k²:. kªKk / Î
²Ö pyrophosphoric acid metaphosphoric acidÒ Æ& phopho- us² ®r12 ÚÊ TGA wk g ã JÚÊ ÆÊ& ÎònÊ r êV gfâÒ ^î®V Ù² f>r:.
Figure 7 3 vol% ã® FR-SH òFrÒ ÿ®B ^Ê~v Ò K g 400 ×&r kªKk v& V®B ~
ã ª& Ò r3®ê gfâÒ JBV:. kªv® 500 × Ê®&r® Jk 150, 175 e 200 ×/h ~ã& ®Ê
¦2B Wû q ®:. ~ãV æn³ 500 × Ê
&r® gfâ Âê è ~ ² Ê/®V:. Êê
~ã&r kªKk ߶ ^Ê~vê G~ÆÊ® J î² Ö&r ª 2Z / kªn ¢Ê:.
4. û«
Û®® Î òFr Î, H-205 e FR-SH² WW Zîr
^Ê~v& V®B nß² kªKk Rk&r Jî² Ö
&r r3² gfâ e v® 6 ªÒ Ʋ Rê W^² ¾® Îÿ·® îV ^Ê~v® kª& Vû þ RW² B²:ê Ù r2®B R:. B² Î, H-205 e FR-SHÒ V ¦¶ ¢, kªKk ^Ê~v& V
®B Þ² ÚZ&r wk² Jk Ús R 500 × Ê
&r® ²V gæ:Ê Òîê ~V ή Vû
Æ, 700 × Ê&r® ân~Ê VW² è:ê Ù²Ö
ÎÊ kª ^Ê~v® ª_r² çÿ®B ªn§ã
Ò ¶Êâ ®Æ ^Ê~ âv&r® ªn~ û& B
¶ n Þ Ù² "n:.
[÷£# KÜN FÂê ^zKRV¯¦® ¯vF &&
®Ê nßn² Ê& f2:.
S+S
1. M. M. Tang and R. Bacon, Carbon, 2, 211 (1964).
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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).
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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, 3rd Ed., J.-B. Donnet, T. K. Wang, and J. C. M. Peng, Editors, Marcel Dekker, New York, Chapter 1 (1998).
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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(%)