Rapid stabilization of pitch fiber precursor by multi-step thermal oxidation

Hayashi Jun-Ichiro, Makoto Nakashima, Katsuki Kusakabe, Shigeharu Morooka, Susumu Mitsuda

Research output: Contribution to journalArticle

12 Citations (Scopus)

Abstract

A multi-step oxidation procedure was developed to stabilize an isotropic pitch fiber prior to carbonization. In the first step, the temperature was raised to 170-220 °C in 1 minute and kept isothermally for 4 minutes. The temperature was then increased in the same manner to 250, 300 and 350 °C. Stabilized fiber precursors were finally carbonized at 1000 °C. The three-step oxidation of 220-250-300 °C required only 15 minutes and stabilized the pitch fiber without fusion. However, the tensile strength of the resultant carbon fiber was 70% of that of the carbon fiber stabilized by a conventional slow heating method (2.5 °C/min to 360 °C). The four-step oxidation, taking 20 minutes in total, was more effective. The tensile strength of the carbon fiber was 82 and 88% by procedures of 220-250-300-300 °C and 220-250-300-350 °C, respectively. Oxidized fibers were characterized by differential scanning calorimetry (DSC) in a nitrogen atmosphere. The three-step oxidation of 220-250-300 °C decreased the heat capacity of the fiber but did not completely stabilize the microstructure of the fiber. The four-step oxidation up to 350 °C, however, diminished the endothermic peak in the DSC profile seen with fibers oxidized by the three-step procedure. The DSC profile of the fiber prepared by the four-step oxidation was very close to that prepared by the slow heating method.

Original languageEnglish
Pages (from-to)1567-1571
Number of pages5
JournalCarbon
Volume33
Issue number11
DOIs
Publication statusPublished - Jan 1 1995

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Stabilization
Oxidation
Fibers
Carbon fibers
Differential scanning calorimetry
Tensile strength
Heating
Hot Temperature
Carbonization
Specific heat
Nitrogen
Fusion reactions
Temperature
Microstructure
carbon fiber

All Science Journal Classification (ASJC) codes

  • Chemistry(all)
  • Materials Chemistry

Cite this

Rapid stabilization of pitch fiber precursor by multi-step thermal oxidation. / Jun-Ichiro, Hayashi; Nakashima, Makoto; Kusakabe, Katsuki; Morooka, Shigeharu; Mitsuda, Susumu.

In: Carbon, Vol. 33, No. 11, 01.01.1995, p. 1567-1571.

Research output: Contribution to journalArticle

Jun-Ichiro, H, Nakashima, M, Kusakabe, K, Morooka, S & Mitsuda, S 1995, 'Rapid stabilization of pitch fiber precursor by multi-step thermal oxidation', Carbon, vol. 33, no. 11, pp. 1567-1571. https://doi.org/10.1016/0008-6223(95)00118-W
Jun-Ichiro, Hayashi ; Nakashima, Makoto ; Kusakabe, Katsuki ; Morooka, Shigeharu ; Mitsuda, Susumu. / Rapid stabilization of pitch fiber precursor by multi-step thermal oxidation. In: Carbon. 1995 ; Vol. 33, No. 11. pp. 1567-1571.
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abstract = "A multi-step oxidation procedure was developed to stabilize an isotropic pitch fiber prior to carbonization. In the first step, the temperature was raised to 170-220 °C in 1 minute and kept isothermally for 4 minutes. The temperature was then increased in the same manner to 250, 300 and 350 °C. Stabilized fiber precursors were finally carbonized at 1000 °C. The three-step oxidation of 220-250-300 °C required only 15 minutes and stabilized the pitch fiber without fusion. However, the tensile strength of the resultant carbon fiber was 70{\%} of that of the carbon fiber stabilized by a conventional slow heating method (2.5 °C/min to 360 °C). The four-step oxidation, taking 20 minutes in total, was more effective. The tensile strength of the carbon fiber was 82 and 88{\%} by procedures of 220-250-300-300 °C and 220-250-300-350 °C, respectively. Oxidized fibers were characterized by differential scanning calorimetry (DSC) in a nitrogen atmosphere. The three-step oxidation of 220-250-300 °C decreased the heat capacity of the fiber but did not completely stabilize the microstructure of the fiber. The four-step oxidation up to 350 °C, however, diminished the endothermic peak in the DSC profile seen with fibers oxidized by the three-step procedure. The DSC profile of the fiber prepared by the four-step oxidation was very close to that prepared by the slow heating method.",
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