• Carbon letters
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• v.25
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• pp.89-94
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• 2018

In this study, we tried to prepare an isotropic spinnable pitch which can be useful to prepare the general purpose carbon fiber through the co-carbonization of biomass tar with ethylene bottom oil under two different preparation methods (atmospheric distillation, pressurized distillation). The results showed that the ethylene bottom oil added co-carbonization was very effective to decrease of the oxygen contents for obtaining a stable spinnable pitch. The pressurized distillation was more effective to reduce the oxygen functional groups of pitches than atmospheric distillation. The obtained spinnable pitch by the pressurized distillation showed higher pitch yield of 42% and lower oxygen content of 9.12% than the spinnable pitch by the atmospheric distillation. The carbon fiber derived from the pressurized distillation spinnable pitch by carbonization at $800^{\circ}C$ for 5 min showed that the higher tensile strength of carbon fiber was increased up to 800 MPa.

• Carbon letters
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• v.2 no.3_4
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• pp.170-175
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• 2001

A petroleum-based isotropic pitch fiber spun by melt-blown method was oxidized in air flow at various conditions. The oxidized pitch fiber obtained was tested for its infusibility and its elemental composition during the process of stabilization. The structural changes were traced by using solvent solubility, FT-IR spectroscopy, and elemental analysis. The samples showed a gradual increase in weight with increasing the oxidization temperature. The weight gain of sample oxidized at $320^{\circ}C$ for 10 min was about 4.5%. The concentration of the pyridine and toluene soluble fraction decreased with an increase in stabilization temperatures. The oxygen uptaken in the stabilization process converted aliphatic side chains into the carbonyl groups. As stabilization proceeded, the more ether and carboxylic acid groups were formed through the oxidations of aldehyde and primary alcohol, and then the carboxylic acid was dehydrated to be aromatic anhydride.

• 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 $290^{\circ}C$.

• 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.

• Journal of Industrial and Engineering Chemistry
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• v.67
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• pp.276-283
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• 2018

For the first time, polyvinyl chloride (PVC) was used as an easily-handled chlorine source for preparation of isotropic pitch-based carbon fiber (IPCF) incorporating ethylene bottom oil (EO) as a raw material. Pitch precursors were prepared by the chlorination-dehydrochlorination triggered by chlorine radicals originated from PVC; aromatization and poly-condensation reactions occurred by polyene-type radicals from PVC. Radical production and co-carbonization were facilitated by pretreatments of EO through vacuum distillation, bromination, and additional heat treatment. Pitches were prepared by the co-carbonization of pretreated EO and EO containing 20 wt% PVC, and had higher yields and better spinnability than those by simple distillation.

• 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.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 ${\tau}=t/t_f= 0.5$.

• 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.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.7 no.2
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• pp.114-118
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• 2006

Isotropic pitch-based carbon fiber has been activated by steam diluted in nitrogen in order to characterize the microporosity. Especially, 40 wt% burn-off ACFs were prepared from different conditions to compare the pore structure and size. The ACFs were thinly sliced to investigate the inside pores by TEM and image analyzer. As expected, the adsorption characteristics of these ACFs were quite different from one another because of different pore structure and size. Most pores are not slit-shaped but rather round. Small round micropores become broad and irregular as increasing the activation time and temperature.