• Carbon letters
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• v.14 no.2
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• pp.94-98
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• 2013

Isotropic pitch fibers were stabilized and carbonized for preparing carbon fibers. To optimize the duration and temperature during the stabilization process, a thermogravimetric analysis was conducted. Stabilized fibers were carbonized at 1000, 1500, and $2000^{\circ}C$ in a furnace under a nitrogen atmosphere. An elemental analysis confirmed that the carbon content increased with an increase in the carbonization temperature. Although short graphitic-like layers were observed with carbon fibers heat-treated at 1500 and $2000^{\circ}C$, Raman spectroscopy and X-ray diffraction revealed no significant effect of the carbonization temperature on the crystalline structure of the carbon fibers, indicating the limit of developing an ordered structure of isotropic pitch-based carbon fibers. The electrical conductivity of the carbonized fiber reached $3.9{\times}10^4$ S/m with the carbonization temperature increasing to $2000^{\circ}C$ using a four-point method.

• Carbon letters
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• v.3 no.2
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• pp.93-98
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• 2002

Short pitch fibers were prepared from petroleum based isotropic precursor pitch by melt-blown technology. The pitch fibers were stabilized in oxidizing condition, followed by steam activations at various conditions. The fiber surface and pore structures of the activated carbon fibers (ACFs) were respectively characterized by using SEM and applying BET theory from nitrogen adsorption at 77 K. The weight loss of the oxidized fiber was proportional to activation temperature and activation time, independently. The adsorption isotherms of the nitrogen on the ACFs were constructed and analyzed to be as Type I consisting of micropores mainly. The specific surface area of the ACFs proportionally increased with the weight loss at a given activation temperature. The specific surface area was ranged 850~1900 $m^2/g$ with pores of narrow distribution in sizes. The average pore size was ranged 5.8~14.1 ${\AA}$ with the larger value from the more severe activation condition.

• Carbon letters
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• v.4 no.4
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• pp.185-191
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• 2003

Two types of carbon fiber based high modulus- and isotropic-pitch were exposed to isothermal oxidation in air and $CO_2$ gas and the weight change was measured by TGA apparatus. The kinetic equation was introduced $f=1-{\exp}(-at^b)$ and the constant b was obtained in the range of 1.02~1.68 for the isotropic fiber and obtained 0.91~1.93 for the high modulus fiber respectively. In considering the effect of the atmosphere for isothermal oxidation, the value of the constant b obtained in the carbon dioxide was higher than that obtained in the air. Therefore, it was found that the pitch based carbon fiber shows sigmoidal characteristic when it is oxidized in the carbon dioxide. In addition, it was also found that $k_f = 0.5$, which was reaction constant at f = 0.5, was a very useful parameter for evaluation of the oxidation reactivity of pitch based carbon fibers. According to the consideration, it is suggested that the conversion-time curves of the pitch based carbon fibers are correlated by normalized equation $f=1-{\exp}(-A{\tau}^B)$, where ${\tau}=t/t_f= 0.5$.

• Fibers and Polymers
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• v.2 no.4
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• pp.178-183
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• 2001

A pitch precursor for a general purpose carbon fiber was prepared by condensation of pyrolized fuel oil (petroleum residual oil) with bromine under nitrogen blowing. such a condensation raised the softening point of the pitch from 4$0^{\circ}C$ to $265^{\circ}$ with a yield of 43%. The pitch precurosr showed an enhanced aromaticity and enlarged molecular size, which led to a reduction in molecular mobility and optical isotropy. The precursor was spun into fibers of $20\mu\textrm{m}$ diameter at a take-up speed of 700m/min. The fiber was stepwise stabilized in air and carbonized in Ar gas to obtain an isotropic carbon fiber. The carbon fiber exhibited tensile strengths of 500-800 ㎫though the fiber was formed via a crude method. The electric conductivity of the carbon fiber was relatively high, 2.2$\times$$10^2$S/cm, sufficient to be used as electrode materials.

• Carbon letters
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• v.3 no.1
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• pp.33-38
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• 2002

Petroleum based isotropic pitch was spun into short fiber by melt-blown spinning technology. The processing parameters chosen were air velocity, die temperature, and throughput rate of the pitch within the ranges of experimental tolerances. The fiber diameter was reduced to $6{\mu}m$ by increases of hot air velocity, and spin die temperature. Also, the fiber diameter was strongly dependent on the throughput rate of the pitch and jet speed of hot air through the spinnerets. Even fibers with $10{\mu}m$ diameter were produced at throughput rate of $0.17g/min{\cdot}hole$ and at die temperature of $290^{\circ}C$.

• Journal of Industrial and Engineering Chemistry
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• v.67
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• pp.358-364
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• 2018

An isotropic pitch precursor for fabricating carbon fibres was prepared by co-carbonization of ethylene bottom oil(EBO) and polyvinyl chloride (PVC). Various pre-treatments of EBO and PVC, and a high heating rate of $3^{\circ}C/min$ with no holding time, were evaluated for their effects on the oxidative stabilization process and the mechanical stability of the resulting fibres. Our stabilization process enhanced the volatilization, oxidative reaction and decomposition properties of the precursor pitch, while the addition of PVC both decreased the onset time and accelerated the oxidative reaction. Aliphatic carbon groups played a critical role in stabilization. Microstructural characterization indicated that these were first oxidised to carbon-oxygen single bonds and then converted to carbon-oxygen double bonds. Due to the higher heating rate and lack of a holding step during processing,the resulting thermoplastic fibers did not completely convert to thermoset materials, allowing partially melted, adjacent fibres to fuse. Fiber surfaces were smooth and homogeneous. Of the various methods evaluated herein, carbon fibers derived from pressure-treated EBO and PVC exhibited the highest tensile strength. This work shows that enhancing the naphthenic component of a pitch precursor through the co-carbonization of pre-treated EBO with PVC improves the oxidative properties of the resulting carbon fibers.

• Carbon letters
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• v.5 no.2
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• pp.51-54
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• 2004

Isotropic pitch-based carbon fiber was isothermally activated in $CO_2$ atmosphere. Structural parameters of the isotropic carbon fibers and activated carbon fibers (ACFs) were evaluated by X-ray diffraction (XRD). The $d_{002}$ and La of the carbon fibers were measured to be 4.04 ${\AA}$ and 23.6 ${\AA}$ and those of ACFs were 4.29 ${\AA}$ and 22.7 ${\AA}$, respectively, representing less ordered through activation process. The pores in the ACFs were characterized by BET, and they showed super-high specific surface area of maximum value 3,495 $m^2/g$ from average pore size of 8.3 ${\AA}$ at 59% burn-off. It was recognized that 8-9 ${\AA}$ was optimum range of pore size for efficient creation of high specific surface area. The average size of the pores formed at higher temperature ($1100^{\circ}C$) was larger than that of the pores formed at lower temperature ($900^{\circ}C$).

• Carbon letters
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• v.10 no.3
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• pp.202-207
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• 2009

Pitch-based carbon fiber tows were prepared from naphtha cracking bottom oil by reforming and carbonization. The relationship between exothermic heat and carbon contents of the fiber was investigated by changing the carbonization conditions. The carbon contents and the crystallinities of isotropic pitch-based carbon fibers were 86.8~93.8 wt% and 33.7~40.1%, respectively, which were linearly proportional to the increase of carbonization temperature from 700 to $1000^{\circ}C$. The exothermic heat (temperature increase) of fiber tows was measured in a short time, which was also linearly proportional to the increase of carbon contents due to the increase of crystallinity, even though the crystallinity was low. Therefore, the carbon contents or carbonization degree of fibers can rapidly and indirectly be estimated by measuring the surface temperature increase of fibers.

• Carbon letters
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• v.21
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• pp.51-60
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• 2017

Isotropic pitch-based fibers produced from coal tar pitch with the melt-blowing method were carbonized at temperatures ranging from 800 to $1600^{\circ}C$ to investigate their crystalline structure and physical properties as a function of the carbonization temperature. The in-plane crystallite size ($L_a$) of the carbonized pitch fiber from X-ray diffraction increased monotonously by increasing the carbonization temperature resulting in a gradual increase in the electrical conductivity from 169 to 3800 S/cm. However, the variation in the $d_{002}$ spacing and stacking height of the crystallite ($L_c$) showed that the structural order perpendicular to the graphene planes got worse in carbonization temperatures from 800 to $1200^{\circ}C$ probably due to randomization through the process of gas evolution; however, structural ordering eventually occurred at around $1400^{\circ}C$. For the carbonized pitch powder without stabilization, structural ordering perpendicular to the graphene planes occurred at around $800-900^{\circ}C$ indicating that oxygen was inserted during the stabilization process. Additionally, the shear stress that occurred during the melt-blowing process might interfere with the crystallization of the CPF.

• Carbon letters
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• v.1 no.1
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• pp.6-11
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• 2000

Coal tar pitch was chemically modified with 10 wt% benzoquinone (BQ) to raise the softening point of isotropic pitch precursor and the precursor was melt-spun into pitch fibers, stabilized, carbonized and activated with steam at $900^{\circ}C$. The weight loss of carbon fiber-benzoquinone (CF-BQ) increased with the increase of activation time like other fibers, but was lower than those of Kureha fiber at the same activation time in spite of larger geometric surface area. Those adsorption isotherms fitted into 'Type I' according to Brunauer, Deming, Deming and Teller classification. However, there was very thin low-pressure hysteresis that lower closure points of the hysteresis are about 0.42-0.45. From the pore size distribution curves, there might be some micropores having narrow-necked bottle; a series of interconnected pore is more likely than discrete bottles. FT-IR studies showed that the functional groups such as carboxyl, quinone, and phenol were introduced to ACFs-BQ surface after steam activation. Methylene blue decolorization and iodine adsorption capacity of ACF-BQ increased linearly with the increase of specific surface area and was larger than that of ACF-Kureha at the same specific surface area.