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NMP로부터 제조된 Melt-blown흑연섬유의 안정화조건에 따른 미세구조와 전기화학적 특성
김찬,양갑승,고장면,박상희,박호철,김영민,Kim Chan,Yang Kap Seung,Ko Jang Myoun,Park Sang Hee,Park Ho Chul,Kim Young-Min 한국전기화학회 2001 한국전기화학회지 Vol.4 No.3
용융분사법으로 나프탈렌계 메조페이스 피치(mP)를 방사하여 산화안정화 속도를 변화시켜 흑연화 섬유의 모폴러지를 제어하였으며, 흑연화 섬유를 이용하여 Li-ion 이차전지 부극을 제조하여 충$\cdot$방전 거동 및 용량을 측정하였다. 용융분사조건에 따라 제조된 피치섬유의 직경은 $4{\mu}m$로부터 $16{\mu}m$까지 다양하였다 이중에서 직경 $10{\mu}m$인 피치섬유를 선택하여 세가지 승온속도 조건 $2^{\circ}C/min,\;5^{\circ}C/min,\;10^{\circ}/min$에서 산화안정화 후 $1000^{\circ}C$에서 탄소화하여 $2650^{\circ}C$에서 흑연화 한 결과, 섬유 단면이 산화안정화 조건 $2^{\circ}C/min$의 경우는 라디알 구조, $5^{\circ}C/min$의 것은 라디알-랜덤 구조, $10^{\circ}C/min$의 경우는 skin-core 구조를 형성하였고, 승온속도가 큰 경우일수록 이흑연화성이 컷다. 이것은 큰 승온속도에서는 탄소화$\cdot$흑연화 과정에서 섬유표면에서만 산화안정화가 일어나고, 내부에서는 피치분자가 유동성이 커 승온과정에서 고결정성의 흑연구조가 발달한 것으로 추측된다. 따라서 이흑연화성이 큰 $10^{\circ}C/min$에서 산화안정화 한 것이 충전방전 용량이 $2^{\circ}C/min$의 경우에 비해서 1.3배로 약 400mAh/g, 충방전 효율도 $96.8\%$로 가장 우수한 특성을 나타냈다. Naphthalene derived mesophase pitch WP) was spun into short fibers by using melt-blown technology. The pitch fibers oxidative stabilization were carried out heating rates of $2^{\circ}C/min,\;5^{\circ}C/min\;and\; 10^{\circ}/min$. The heating rate was a key factor to maximate the capacity of the Li-ion secondary battery through controlling the morphology of the graphitized fiber. The diameters of the melt-blown fibers prepared were in the range of $4{\mu}m\~16{\mu}m$ with functions of air jet speed, air temperature and the temperature of the nozzle. The graphitized fibers of $10{\mu}m$ diameters showed various morphological structure with heating rate of the stabilization. Radial, radial-random and skin-core cross-sectional structure of the fibers were observed at the respective heating rate of $2^{\circ}C/min\;5^{\circ}C/min\;and\;10^{\circ}C/min$. Most crystalline structure of graphite was obtained from the fiber stabilized at heating rate of $10^{\circ}C/min$ exhibiting the best anode performance with 400 mAh/g of capacitance and $96.8\%$ of charge/discharge efficiency.
이홍범,김찬,양갑승,국윤환,Lee, Hong-Bum,Kim, Chan,Yang, Kap-Seung,Kook, Yoon-Hwan 한국섬유공학회 1995 한국섬유공학회지 Vol.32 No.4
In order to introduce a functionality to coal tar pitch, dienophiles such as p-benzoquinone(BQ) and maleic anhydride(U) were used in the chemical modification reaction. The coal tar pitch was reacted with BQ or MA at 160℃ under nitrogen atmosphere. Thermal behavior of'the reaction product was examined by sofiening point measurement and thermogravimetric analysis(TGA) under nitrogen atmosphere. TGA results revealed that the weight loss of the reaction product is reduced with the amount of BQ used in the reaction. The result comes fiom the formation of intermolecular cross links between the pitch molecules. The sofiening point of the reaction products increased with the amount of the BQ or MA used in the reaction. BQ was more effective than MA in increasing the sofiening point of coal tar pitch. The coal tar pitch ryacted with 200wt% BQ showed dimensional stability with heat treatment up to 500℃. The concentration ewut of BQ and MA on solubility in various solvents was tested by sequential extraction method. The insoluble fiaction of the reaction product increased with increase of BQ, whereas M showed an opposite effect. On the basis of courier transform-infiared(FT-lR) spectroscopic result, BQ acts not only as a dienophile of Diels-Alder reaction agent but also as a crosslinking agent, whereas H acts mainly as a dienophile.
박주현,김진봉,양갑승,이무성,Park, Ju-Hyeon,Kim, Jin-Bong,Yang, Kap-Seung,Lee, Moo-Sung 한국섬유공학회 2007 한국섬유공학회지 Vol.44 No.3
매트릭스가 폴리스티렌이고 분산상이 폴리부타디엔인 스타형 블록공중합체의 물성을 개선하고 고분자 전해질의 매트릭스로서의 사용 가능성을 확인하기 위하여 스타형 폴리스티렌-부타디엔 공중합체의 수소화/술폰화 개질 실험을 행하였고, 다음의 결과를 얻었다. 1. 수소화제로 p-toluenesulfonylhydrazide/tri-n-propyl amine을 사용하였으며, 온도에 따른 수소화 반응 속도의 변화로부터 구한 스타형 SB 공중합체의 수소화 반응 활성화 에너지는 89kJ/mol이었다. 2. 수소화 반응에 의해 부타디엔 단위가 지방족 탄화수소로 변화되어 분산상인 PB 영역의 유리전이온도가 $50^{\circ}C$ 정도 증가하였으나, 열안정성은 다소 감소하였다. 3. 수소화된 SB(H-SB)를 acetyl sulfate를 사용하여 술폰화한 결과, $65^{\circ}C$의 반응온도에서 60분 이상 반응시키면 한계 술폰화 정도에 도달하며, 술폰화제이 양이 증가할수록 술폰화 정도는 증가하였다. 그러나, 한계 술폰화제의 양을 넘어서면 불용의 전해질이 얻어진다. 4. 술폰화 정도가 증가함에 따라 포화함수율과 이온전도도 모두 증가하며, 23 mol% 정도 술폰화된 경우 함수율과 이온전도도는 각각 18%, $1.6{\times}10^{-3}S/cm$이었다. Hydrogenation and sulfonation of a star-type styrene-butadiene copolymer (SB), in which styrene domain is matrix, were carried out in order to investigate the possibility for polymer electrolyte. Mixtures of ${\rho}-toluenesulfonylhydrazide$ and tri-n-propyl amine and acetyl sulfate were used as hydrogenating and sulfonating agents, respectively. Activation energy for the hydrogenation of SB was 89 kJ/mol. The degree of sulfonation in hydrogenated SB (H-SB) was dependent on the reaction time and the amount of acetyl sulfate. After 60 min at $65^{\circ}C$, the degree of sulfonation does not change further and insoluble products were also obtained above 40 mol% of the degree of sulfonation. Both the water uptake and proton conductivity of sulfonated H-SB (SH-SB) were increased with the degree of sulfonation. For the SH-SB with 23 mol% of sulfonic acid moiety, ionic conductivity was $1.6{\times}10^{-3}S/cm$.
정전방사에 의한 PAN계 활성화 탄소 나노섬유 전극 제조와 EDLC 응용
김찬,김종상,이완진,김형섭,양갑승,Kim, Chan,Kim, Jong-Sang,Lee, Wan-Jin,Kim, Hyung-Sup,Edie, Dan D.,Yang, Kap-Seung 한국전기화학회 2002 한국전기화학회지 Vol.5 No.3
PAN(polyacrylonitrile)을 DMF(dimethylformamide) 용매에 용해하여 정전방사법에 의해 평균 직경 400 nm의 나노섬유 웹을 제조하였다. 제조된 나노섬유 웹은 산화 안정화, 활성화 공정을 거쳐 활성화 탄소 나노섬유를 제조하여, 전기화학적 특성과 비축전 용량을 측73하였다. 활성화 탄소 나노섬유의 비표면적은 $1230m^2/g-800m^2/g$으로 일반 활성탄소 섬유의 거동과는 다르게 활성화 온도가 증가할수록 감소하는 경향을 나타냈으며, 활성화 에너지 값은 29.2kJ/mol로 활성화 온도에 크게 영향을 받지 않고, 급격한 반응이 일어남을 알 수 있었다. 비축전 용량은 활성화 온도가 $700^{\circ}C,\;750^{\circ}C,\;800^{\circ}C$의 경우 27 F/g, 25 F/g, 22 F/g으로 활성화 온도가 증가할수록 비표면적에 비례하여 낮아지는 경향을 나타냈다. Poly(acrylonitrile)(PAN) solutions in dimethylformamide(DMF) were electrospun to prepare webs consisting of 400nm ultra-fine fibers. The webs were oxidatively stabilized, activated by steam and resulted to be activated carbon fibers(ACFs). The specific surface area was $800\~1230 m^2/g$, which showed a trend of a decrease of the surface area with an increase in activation temperature, showing opposite behavior to the other ACFs. The activation energy of the stabilized fibers for the steam activation was determined as 29.2 kJ/mol to be relatively low indicating the easier activation than that of other carbonized fibers. The ACF webs were characterized by pore size and specific surface uea which would be related to the specific capacitance of the electrical double layer capacitor (EDLC). The specific capacitances measured were 27 F/g, 25 F/g, 22 F/g at the respective activation temperature of $700^{circ}C,\;750^{\circ}C\;800^{\circ}C$, showing similar trend with the specific surface area i.e., the higher activation temperature was, the lower specific capacitance resulted.
손유선(You Sun Son),양갑승(Kap Seung Yang),박상희(Sang Hee Park),권해용(Hae Yong Kweon),김수일(Su Il Kim),조종수(Chong Su Cho) 한국키틴키토산학회 2001 한국키틴키토산학회지 Vol.6 No.1
N/A Chitosan fiber spun through circular nozzle was immersed into alginate solution to enhance mechanical properties of the fiber for suture application. The tensile strength of the chitosan fiber increased with an increase of molecular weight and concentration of the chitosan. The dry tenacity of chitosan fiber (cps 15.7) was enhanced by treatment with alginate solution from 0.56 g/d to 1.71 g/d due to the formation of polymeric electrolyte complex between chitosan as polycation and alginate as polyanion. The optimum condition of treatment concentration and time of alginate to enhance mechanical properties of chitosan fiber was 0.5 wt% and 12 hrs, respectively. The morphology of the chitosan fiber after treatment with alginate showed smoother than that of chitosan fiber only.