• Fibers and Polymers
• /
• 제1권2호
• /
• pp.97-102
• /
• 2000

Pitch precursors were synthesized from coal tar(CT) and pyrolysis fuel oil(PFO, petroleum residue oil) at relatively low temperature of $250^{\circ}$, in the presence of horontrifluorideidiethyletherate complex(BFDE) as a catalyst and nitrobenzene(NB) as a co-catalyst. The softening point, nitrogen content and carbon yield increased with an increase of concentration of NB. The pitch precursors with good spinnability were prepared by removing the volatile components through $N_2$ blowing. The precursor pitches were spun through a circular nozzle, stabilized at $310^{\circ}$ and finally carbonized at $1000^{\circ}$. The optically anisotropic structure formed at the absence of NB was changed into isotropic structure, showing a decrease in size of the flow domain. The hollow carbon fiber could be prepared in the process of stabilization. The results proposed that the morphology of carbon materials could be controlled by changing the concentration of catalyst and/or co-catalyst and/or stabilization condition that affect on the mobility of molecules during carbonization.

• Carbon letters
• /
• 제3권2호
• /
• pp.93-98
• /
• 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
• /
• 제21권
• /
• pp.51-60
• /
• 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
• /
• 제1권3_4호
• /
• pp.165-169
• /
• 2001

The C-type mesophase pitch-based carbon fiber (C-MPCF) was prepared throuch C-type spinnerette and compared the mechanical properties to those of round type mesophase pitch fiber (R-MPCF) and C-type isotropic pitch fiber (C-iPCF). The tensile strength and modulus of C-MPCF were about 18.6% and 35.7% higher than those of R-MPCF. The tensile strength of C-MPCF was 62% higher than that of C-iPCF of the same $8{\mu}m$ thickness because of more linear transverse texture, which could be easily converted to graphitic crystallinity during heat treatment. The torsional rigidity of C-MPCF was 2.37 times higher than that of R-MPCF. The electrical resistivity of C-MPCF was $8{\mu}{\Omega}{\cdot}m$. The C-iPCF shows far lower electrical resistivity than R-iPCF as well as the mesophase carbon fiber because of better alignment of texture to the fiber axis.

• Journal of Industrial and Engineering Chemistry
• /
• 제67권
• /
• pp.358-364
• /
• 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.

• 한국재료학회지
• /
• 제13권11호
• /
• pp.742-748
• /
• 2003

The structural parameters such as Lc, La and d of $CO_2$activated isotropic carbon fibers(ACFs) were obtained from XRD in order to understand a development mechanism of micropores. And the structural parameters were compared with specific surface area(SSA) data. The $d_{002}$, Lc, and La of the original fiber were measured to be 4.04$\AA$, 6.2$\AA$, and 23.6$\AA$, respectively. Carbonization of outer-parts and oxidization of inner-parts of the original fibers were far from completeness. It was observed that the structural changes of the ACFs during activation take place severely, therefore the carbonization and the oxidization of the fibers take place simultaneous with pore developments. The $d_{002}$ of the ACFs was increased to be 2.80$\AA$, and the La of the ACFs was decreased to be 17.0$\AA$ by activation. It was shown that the pores are developed continuously from the outer-parts to the inner-parts of the fibers, therefore the SSA increases as a result of the development of pores fully to the inner-parts of the fiber when the burn-off degree was over :39%. It seems that the (002) planes of crystallites contribute to the micropore wall related to the super high SSA.SSA.

• Carbon letters
• /
• 제11권4호
• /
• pp.304-310
• /
• 2010

To manufacture a carbon/carbon composite the coal tar pitch was used as the matrix precursor and the PAN (polyacrylonitrile)-based carbon fiber was used as the reinforcing material to weave 3-directional preform. For pressure carbonization HIP equipment was used to produce a maximum temperature of $1000^{\circ}C$ and a maximum pressure of 100 MPa. The carbonization was induced by altering the dwell temperature between $250^{\circ}C$ and $420^{\circ}C$, which is an ideal temperature for the moderate growth of the mesophase nucleus that forms within the molten pitch during the pressure carbonization process. The application of high pressure during the carbonization process inhibits the mesophase growth and leads to the formation of spherical carbon particles that are approximately 30 nm in size. Most particles were spherical, but some particles were irregularly shaped. The spread of the carbon particles was larger on the surface of the carbon fiber than in the interior of the matrix pocket.

• Carbon letters
• /
• 제16권2호
• /
• pp.107-115
• /
• 2015

Impact damages induced by a low-velocity impact load on carbon fiber reinforced polymer (CFRP) composite plates fabricated with various stacking sequences were studied experimentally. The impact responses of the CFRP composite plates were significantly affected by the laminate stacking sequences. Three types of specimens, specifically quasi-isotropic, unidirectional, and cross-ply, were tested by a constant impact carrying the same impact energy level. An impact load of 3.44 kg, corresponding to 23.62 J, was applied to the center of each plate supported at the boundaries. The unidirectional composite plate showed the worst impact resistance and broke completely into two parts; this was followed by the quasi-isotropic lay-up plate that was perforated by the impact. The cross-ply composite plate exhibited the best resistance to the low-velocity impact load; in this case, the impactor bounced back. Impact parameters such as the peak impact force and absorbed energy were evaluated and compared for the impact resistant characterization of the composites made by different stacking sequences.

• 한국복합재료학회:학술대회논문집
• /
• 한국복합재료학회 2002년도 추계학술발표대회 논문집
• /
• pp.38-42
• /
• 2002

An apparatus was developed to repetitively apply a $-196^{\circ}C$ thermal load to coupon-sized mechanical test specimens. Using this device, IM7/5250-4 (carbon / bismaleimide) cross-ply and quasi-isotropic laminates were submerged in liquid nitrogen ($LN_2$) 400 times. Ply-by-ply micro-crack density, laminate modulus, and laminate strength were measured as a function of thermal cycles. Quasi-isotropic samples of IM7/977-3 (carbon / epoxy) composite were also manually cycled between liquid nitrogen and an oven set at $120^{\circ}C$ for 130 cycles to determine whether including elevated temperature in the thermal cycle significantly altered the degree or location of micro-cracking. In response to thermal cycling, both materials micro-cracked extensively in the surface plies fellowed by sparse cracking of the inner plies. The tensile modulus of the IM7/5250-4 specimens was unaffected by thermal cycling, but the tensile strength of two of the lay-ups decreased by as much as 8.5%.

• 한국추진공학회:학술대회논문집
• /
• 한국추진공학회 2003년도 제20회 춘계학술대회 논문집
• /
• pp.151-155
• /
• 2003

An apparatus was developed to repetitively apply a -196 $^{\circ}C$ thermal load to coupon-sized mechanical test specimens. Using this device, IM7/5250-4 (carbon / bismaleimide) cross-ply and quasi-isotropic laminates were submerged in liquid nitrogen (L$N_2$) 400 times. Ply-by-Ply micro-crack density, laminate modulus, and laminate strength were measured as a function of thermal cycles. Quasi-isotropic samples of IM7/977-3 (carbon / epoxy) composite were also manually cycled between liquid nitrogen and an oven set at 120 $^{\circ}C$ for 130 cycles to determine whether including elevated temperature in the thermal cycle significantly altered the degree or location of micro-cracking. In response to thermal cycling, both materials micro-cracked extensively in the surface plies followed by sparse cracking of the inner plies. The tensile modulus of the IM7/5250-4 specimens was unaffected by thermal cycling, but the tensile strength of two of the lay-ups decreased by as much as 8.5 %.