• 한국안전학회지
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• 제31권1호
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• pp.66-73
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• 2016

Lyocell fibers were used as a precursor in order to improve yield and strength of cellulose-based precursor while manufacturing activated carbon fiber(ACF). Lyocell fibers as a precursor for the preparation of ACF were surface-modified by reaction with 3-aminopropyltriethoxysilane(APTES) and pre-treated with KOH and H3PO4. Using aforementioned precursor, ACFs were prepared by a series of stabilization, carbonization and activation process at high temperatures. On each process, FT-IR, TGA, UTM and SEM were used to observe fibers' physical properties including structure and porous surfaces. FT-IR results proved that surface modification was achieved during stabilization, carbonization and activation process. TGA results during carbonization process found that surface modified fibers with APTES 0.02 mol(A2) showed higher thermostability, and extended pre-treatment increased yield. Especially, yield was found to have an increase of 10~20 wt% with surface modification during activation process. UTM results showed that tensile strength has the same order of concentration of APTES after surface modification, however, was found to show lower tensile strength than lyocell fibers after stabilization process. SEM results revealed that more homogeneous porosity control could be proceed after modifying the surface for the effective removal of hazardous substances.

• 한국세라믹학회지
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• 제34권9호
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• pp.963-968
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• 1997

Coal tar pitch was used to study the effect of the pyrolysis conditions to produce mesophase pitch used as a matrix precursor for carbon/carbon composites. The pyrolysis conditions were presented in all cases that the total pressure was 1 atm and the first stage temperature was changed from 25$0^{\circ}C$ to 34$0^{\circ}C$ to remove the low molecular weight compounds in the pitch, and then, heated to 40$0^{\circ}C$ to form anisotropic mesophase as the second stage temperature. The first stage temperature was very affected to form resulting anisotropic mesophase pitch. The resulting mesophase pitches show a significantly increased anisotropic contents upto 30$0^{\circ}C$. However, the contents of mesophase were decreased above 30$0^{\circ}C$. It was the reason that the first stage temperature had been control the number of free radicals to react the aromatic compounds in the pitch to form high molecular weight compound. Therefore, the two stage pyrolysis method could be very effectively used to control various contents of anisotropic polyaromatic mesophase compared to continuous to continuous heating method.

• 한국재료학회지
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• 제3권3호
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• pp.292-299
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• 1993

본 연구에서는 탄소/탄소복합재료의 마모특성에 대한 탄소섬유 길이의 영향을 고찰하였다. 매트릭스 precursor로 레졸형의 페놀수지와 강화재로 표면처리를 하지않은 PAN계 단섬유형 탄소섬유를 사용하여 액상함침법으로 1회의 고온열처리 공정과 4회의 탄화공정을 통하여 탄소/탄소복합재료를 제조하였다. Disk-on-disk형의 마모시험기를 통하여 상대 마찰재로 AISI 304 stainliss steel을 사용하여 0.6MPa(61 ${\times}{10^3}$Kg/$m^2$)의 압력과 0.71m/sec의 미끄러짐 속도하에서 측정된 탄소/탄소복합재료의 마찰계수는 0.2-0.3이었다. 마찰계수에 대한 섬유의 길이의 영향은 크게 나타나지 않았지만, 마모 속도는 섬유의 길이가 증가함에 따라 증가하는 경향이 나타났다. 본 실헙 결과를 섬유 강화 플라스틱의 마모 모델을 적용하여 고찰하여 본 결과, 섬유의 길이가 증가함에 따라 탄소/탄소복합재료의 마모 속도가 증가되는 경향은 생성된느 마모조각의 크기가 커기기 때문에 나타난 현상으로 판단되었다.

• Korean Chemical Engineering Research
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• 제43권6호
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• pp.745-750
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• 2005

등방성 피치계 탄소섬유 및 활성탄소섬유를 얻기 위한 프리커서 피치를 제조하기 위하여 NCB(naphtha cracking bottoms) oil을 열처리온도, 처리시간, 질소유량을 변화시키면서 개질하였다. 개질된 피치의 수율, 연화점, 원소분석, 분자량분포를 측정하고 용융방사하여 최적의 개질조건을 얻었다. 질소유량 1.25 vvm, 열처리온도 $380^{\circ}C$, 처리시간 3 h 일 때 약 $240^{\circ}C$의 연화점을 갖는 방사성이 우수한 프리커서 피치를 제조할 수 있었다. 이때의 수율은 약 21 wt％, C/H 몰비는 1.07에서 1.34로, 방향족화도는 0.85에서 0.88으로 증가하였고, 벤젠 및 퀴놀린 불용분은 각각 30.0 wt％, 1.5 wt％ 이었다, 방사 온도는 프리커서 피치의 연화점보다 약 $50^{\circ}C$ 높았으며 분자량은 250~1,250 범위에 분포되어 있지만 80％ 이상은 250~700의 좁은 범위에 몰려있었다.

• Carbon letters
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• 제11권3호
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• pp.176-183
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• 2010

PAN precursor fibers were produced via wet-spinning process, and effects of polymerization and spinning processes, especially the stretching process, were investigated on mechanical properties and micro-morphologies of precursor fibers. An increase in molecular weight, dope solid and densification and a decrease in surface defects were possible by controlling polymerization temperature, the number of heating rollers for densification and the jet stretch ratio, which improved the mechanical properties of precursor fibers. The curves for strength, modulus, tensile power and diameter as a function of stretch ratio can be divided into three stages: steady change area, little change area and sudden change area. With the increase of stretch ratio, the fiber diameter became smaller, the degree of crystallization increased and the structure of precursor fibers became compact and homogeneous, which resulted in the increase of strength, modulus and tensile power of precursor fibers. Empirical relationship between fiber strength and stretch ratio was studied by using the sub-cluster statistical theory. It was successfully predicted when the strengths were 0.8 GPa and 1.0 GPa under a certain technical condition, the corresponding stretch ratio of the fiber were 11.16 and 12.83 respectively.

• 한국세라믹학회지
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• 제37권3호
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• pp.280-287
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• 2000

Adsorption behavior and amount of phenolic resin followed silica (SiO2) formation onto silicon nitride(Si3N4) surface were investigated using electrokinetic sonic amplitude (ESA) technique and with UV spectrometer, to fabricate Si3N4/SiC nano-composite based on reaction between SiO2 formed and phenolic resin absorbed onto Si3N4 particle. The amount of SiO2 formed and carbon from phenolic resin absorbed onto Si3N4 surface were calculated quantitatively to adjust the reaction between SiO2 and phenolic resin, resulting in no residual SiO2 and carbon. As a result, pre-heated tempeature for optimized reaction was below 25$0^{\circ}C$, in which there was no residual SiO2 and carbon.

• 한국세라믹학회지
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• 제34권1호
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• pp.56-62
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• 1997

탄화된 PAN 섬유, 페놀수지, 세라믹 결합체를 혼합하여 탄소섬유-세라믹복합체를 제조한 후 활성화시켜 PAN 섬유의 탄화온도에 따른 활성탄소섬유-세라믹복합체의 비표명적과 굽힘 강도변화를 연구하였다. 안정화 PAN 섬유를 80$0^{\circ}C$와 100$0^{\circ}C$에서 각각 탄화시켜 얻은 두 종류의 탄소섬유를 복합체 제작시편의 원료로 사용하였다. 탄소섬유-세라믹복합체를 10~90분간 CO2로 85$0^{\circ}C$에서 활성화시켜 얻은 두 종류의 활성복합체에 대한 물성 측정결과, 80$0^{\circ}C$로 PAN 섬유를 탄화시켜 만든 활성복합체의 burn-off이 37%에서 76%로 증가될 때 비표면적은 493m2/g에서 1090m2/g으로 증가하였으며, 굽힘강도는 4.5 MPa에서 1.4MPa로 감소하였다. 이 값들은 안정화 PAN 섬유의 탄화온도를 100$0^{\circ}C$로하여 활성복합체 시편이 나타내는 값보다 약 2배 정도 큰 값이었다. 비표면적, 굽힘강도 측정결과와 미세조직 관찰결과, PAN 섬유의 탄화온도가 활성복합체의 비표면적과 굽힘강도에 미치는 영향은 활성화시 탄소섬유와 페놀수지탄화체 또는 세라믹 필름간에 발생되는 결합력과 상대적인 수축율에 의해 결정되는 활성복합체의 구조특성에 기인된 것으로 해석하였다.

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

• Composites Research
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• 제34권1호
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• pp.23-29
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• 2021

탄소섬유는 단위 중량 당 높은 강도 및 모듈러스를 갖기 때문에 고성능 복합 재료 제조 시 탄소보강재로 많이 사용된다. 그러나 탄소 섬유를 제조하는 공정에서 많은 시간과 높은 에너지를 소모하여 제조비용이 크게 증가하기 때문에 상용화에 어려움을 겪고 있다. 따라서 생산 비용 절감을 위하여 제조 공정에 사용되는 에너지를 대체할 수 있는 고속의 저 에너지원을 적극적으로 찾아 연구할 필요가 높아졌다. 폴리아크릴로니트릴(PAN) 전구체(Precursor)로 상용화 된 탄소 섬유는 180~300℃의 대기 분위기에서 안정화 과정이 이루어지고, 1600℃ 이하의 불활성 가스 분위기에서 탄화하여 탄소 섬유를 생산할 수 있다. 이 두 공정은 많은 시간과 높은 에너지를 사용하지만, 고성능 탄소 섬유를 생산하는 데 필수적이며 중요하다. 따라서 최근에는 공정 시간을 단축하고 에너지 소비를 줄일 수 있는 플라즈마, 전자 빔 및 마이크로파와 같은 다양한 다른 에너지원을 보조적으로 사용 함으로써 저 에너지·고속 안정화 공정 기술이 시도되고 있다. 본 연구에서는 플라즈마 공정과 열처리를 연속적으로 수행하여 PAN 전구체 안정화 공정을 연구하였으며, 모폴로지, 구조적 변화, 열적 및 물리적 특성 변화를 연구하였다.

• Carbon letters
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• 제12권3호
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• pp.131-137
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• 2011

Kenaf fibers, cellulose-based natural fibers, were used as precursor for preparing kenafbased carbon fibers. The effects of carbonization temperature ($700^{\circ}C$ to $1100^{\circ}C$) and chemical pre-treatment (NaOH and $NH_4Cl$) at various concentrations on the thermal change, chemical composition and fiber morphology of kenaf-based carbon fibers were investigated. Remarkable weight loss and longitudinal shrinkage were found to occur during the thermal conversion from kenaf precursor to kenaf-based carbon fiber, depending on the carbonization temperature. It was noted that the alkali pre-treatment of kenaf with NaOH played a role in reducing the weight loss and the longitudinal shrinkage and also in increasing the carbon content of kenaf-based carbon fibers. The number and size of the cells and the fiber diameter were reduced with increasing carbonization temperature. Morphological observations implied that the micrometer-sized cells were combined or fused and then re-organized with the neighboring cells during the carbonization process. By the pre-treatment of kenaf with 10 and 15 wt% NaOH solutions and the subsequent carbonization process, the inner cells completely disappeared through the transverse direction of the kenaf fiber, resulting in the fiber densification. It was noticeable that the alkali pre-treatment of the kenaf fibers prior to carbonization contributed to the forming of kenaf-based carbon fibers.