• Current Research on Agriculture and Life Sciences
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• 제30권1호
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• pp.41-50
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• 2012

As a part of abating formaldehyde emission of urea-formaldehyde resin, this study was conducted to investigate the rmalcure kinetics of both neat and modified urea-formaldehyde resins using differential scanning calorimetry. Neat urea-formaldehyde resins with three different formaldehyde/urea mol ratios (1.4, 1.2 and 1.0) were modified by adding three different additives (sodium bisulfite, sodium hydrosulfite and acrylamide) at two different levels (1 and 3wt%). An isoconversional method at four different heating rates was employed to characterize thermal cure kinetics of these urea-formaldehyde resins to obtain activation energy ($E{\alpha}$) dependent on the degree of conversion (${\alpha}$). The $E{\alpha}$ values of neat urea-formaldehyde resins (formaldehyde/urea = 1.4 and 1.2) consistently changed as the ${\alpha}$ increased. Neat and modified urea-formaldehyde resins of these two F/U mol ratios did show a decrease of the $E{\alpha}$ at the final stage of the conversion while the $E{\alpha}$ of neat urea-formaldehyde resin (formaldehyde/urea = 1.0) increased as the ${\alpha}$ increased, indicating the presence of incomplete cure. However, the change of the $E{\alpha}$ values of all urea-formaldehyde resins was consistent to that of the Ea values. The isoconversional method indicated that thermal cure kinetics of neat and modified urea-formaldehyde resins showed a strong dependence on the resin viscosity as well as diffusion control reaction at the final stage of the conversion.

• 소성∙가공
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• 제24권2호
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• pp.101-106
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• 2015

Recently, silicone is being used for LED chip lens due to its good thermal stability and optical transmittance. In order to predict residual stresses, which cause optical birefringence and mechanical warpage of silicone, a finite element analysis was conducted for the curing of silicone during molding. For the analysis of the curing process, a dynamic cure kinetics model was derived based on the results of a differential scanning calorimetry (DSC) testing and applied to the material properties for finite element analysis. Finite element simulation results showed that a step cure cycle reduced abrupt reaction heat and showed a decrease in the residual stresses.

• 유변학
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• 제11권2호
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• pp.135-142
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• 1999

열잠재성 개시제인 N-benzylpyrazinium hexafluoroantimonate (BPH)를 에폭시 수지에 페놀-노볼락 수지의 혼합비가 각각 0, 5, 10, 20 그리고 40 wt.%로 구성된 혼합물에 1 wt.% 첨가 시킨 후 혼합 조성비에 따른 경화 동력학, 열안정성 그리고 유변학적 특성에 관하여 연구하였다. 열잠재특성은 동적 DSC를 이용하여 반응 온도에 대한 전화량을 구하여 측정하였다. 본 양이온 BPH 시스템은 에폭시-페놀 경화 시스템의 열잠재성 개시제로서 유용하다는 것이 입증되었다. 페놀-노볼락 수지의 농도 증가는 브랜드 시스템의 잠재온도 감소와 경화 활성화 에너지($E_a$) 증가를 나타내었다. 브랜드 시스템의 열안정성과 유변학적 특성은 TGA와 rheometer를 사용한 등온 실험을 통하여 각각 조사하였다. 결과로서, TGA를 이용하여 구한 열안정성과 분해 활성화 에너지($E_t$) 그리고 rheometer에 의한 gel time과 가교 활성화 에너지($E_c$)는 페놀-노볼락 수지가 20~40 wt.% 조성범위에서 혼합될 때 증가하였다. 이는 페놀 수지내의 수산기 그룹, 에폭시 수지내의 에폭사이드환 그리고 BPH간의 3차원 가교 반응에 기인한다.

• Transactions on Electrical and Electronic Materials
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• 제13권4호
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• pp.204-207
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• 2012

Epoxy nanocomposite was synthesized through the exfoliation of organoclay in an epoxy matrix, which was composed of diglycidyl ether of bisphenol A (DGEBA), 4,4'-methylene dianiline (MDA) and malononitrile (MN). Organoclay was prepared by treating the montmorillonite with octadecyl trimethyl ammonium bromide (ODTMA). The exfoliation of the organoclay was estimated by wide angle X-ray diffraction (WAXD) analysis. In order to measure the cure rate of DGEBA/MDA (30 phr)/MN (5 phr)/organoclay (3 phr), differential scanning calorimetry (DSC) analysis was performed at various heating rates, and the data were interpreted by Kissinger equation. Thermal degradation kinetics of the epoxy nanocomposite were studied by thermogravimetric analysis (TGA), and the data were introduced to the Ozawa equation. The activation energy for cure reaction was 45.8 kJ/mol, and the activation energy for thermal degradation was 143 kJ/mol.

• Korean Chemical Engineering Research
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• 제46권1호
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• pp.200-204
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• 2008

비대칭성 고리형 지방족 아민 경화제를 이용한 diglycidyl ether of bisphenol F(DGEBF) 계열의 에폭시의 경화 반응을 등온 및 동적 경화 실험을 통하여 분석하였다. 등온 부분경화 실험 및 동적 경화반응을 통하여 아민 경화제의 비대칭성으로 인해 경화 반응이 저온부 및 고온부분의 두 가지 반응으로 구성되어 있다는 것을 확인하였고, 따라서 경화도가 0.6 이상인 영역에서는 등온경화반응 모델식을 이용하여 실험값을 예측하기는 어렵다는 것을 확인하였다. 승온 속도를 여러 가지로 변화시키며 동적 경화반응을 분석하여 저온부 및 고온부 각각의 반응에 대한 활성화에너지 및 속도상수를 알아보았고, 경화 초기에는 저온부의 반응이 주가 되는 것을 확인하였다.

• 한국윤활학회:학술대회논문집
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• 한국윤활학회 1999년도 제30회 추계학술대회
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• pp.49-56
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• 1999

A material was formulated with Phenol novolac and HEXA only. The cure kinetics and thermal characteristics of phenol novolac with various HEXA contents were peformed by differential scanning calorimetry and thermal gravimetric analysis. All kinetic parameters of the curing reaction including the reaction order, activation energy, and rate constant were calculated and reported. The results indicate that the curing reaction goes through an autocatalytic kinetic mechanism. The friction and wear characteristics of this material were determined using friction material testing machine. The friction coefficient of phenol novolac with various HEXA contents was determined using the PV(pressure & velocity) factor. The most stable and highest friction coefficient with a various pressure and velocity condition was found at HEXA 10 wt.% material. The specific wear rate per unit sliding distance with a various HEXA contents was reported.

• Elastomers and Composites
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• 제48권2호
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• pp.161-166
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• 2013

비등온 TGA 실험방법을 이용하여 가교 사이트가 서로 다른 chlorine cure-site ACM 고무와 carboxylic cure-site ACM 고무 두 종류에 대하여 열분해 거동을 연구하였다. 분해 반응이 최대인 점의 온도는 모든 승온 속도에서 carboxylic cure-site ACM 고무의 열분해 특성이 상대적으로 더 안정함을 보여 주었다. Kissinger의 해석 방법에 의한 활성화에너지는 chlorine cure-site ACM 및 carboxylic cure-site ACM 고무에 대하여 각각 118.6 및 105.5 kJ/mol로 나타났으며, Flynn-Wall-Ozawa의 해석방법에서의 전환율 0.1~0.2 범위의 평균과 유사한 값을 나타내었다. 반응차수 해석으로부터 두 시험편 모두 일반적인 고무와 유사한 다중 복합반응에 의하여 열분해 반응이 진행됨을 알 수 있었다.

• Design & Manufacturing
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• 제8권2호
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• pp.46-49
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• 2014

Silicone is recently used for LED chip lense due to its good thermal stability and optical transmittance. In order to predict residual stress which causes optical briefringence and mechanical warpage of silicone, finite element analysis was conducted for curing process during silicone molding. For analysis of curing process, a dynamic cure kinetics model was derived based on the differential scanning calorimetry(DSC) test and applied to the material properties for finite element analysis. Finite element simulation result showed that the slow cure reduced abrupt reaction heat and it was predicted decrease of the residual stress.

• 한국복합재료학회:학술대회논문집
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• 한국복합재료학회 2000년도 추계학술발표대회 논문집
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• pp.34-37
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• 2000

The effect of novel N-crotyl-N,N-dimethyl-4-methylanilinium hexafluroantimonate (CMH) curing agent on cure behavior and thermal properties of DGEBA epoxy cationic system was investigated. From DSC measurements of DGEBA/CMH system, it was shown that this system exhibits an excellent thermal latent characteristic in a given temperature and reveals complex cure behavior as indicated by multiple exotherms. The conversion and conversion rate of DGEBA/CMH system increased with increasing the concentration of initiator due to high activity of CMH. Viscoelastic properties during gel formation of DGEBA with CMH were investigated by rheological techniques under isothermal condition. The gel time obtained from the modulus crossover. point t(G')=G", was affected by high curing temperature and concentration of CMH, resulting in high degree of network formation in cationic polymerization. The thermal stabilities were discussed in terms of the activation energy for decomposition and thermal factors determined from TGA measurements.ents.

• 폴리머
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• 제24권1호
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• pp.105-112
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• 2000

본 연구에서는 항공기 구조용 재료로 쓰이는 탄소섬유/에폭시 복합재료 프리프레그(DMS 2224)를 모델시스템으로 하여 등온환경과 등속도 가열환경에서 경화반응 속도를 연구하였다. 이 복합재료의 공정온도에서의 가공공정을 묘사할 수 있는 현상학적인 반응속도 모델을 differential scanning calorimetry (DSC)와 이론을 통하여 제안하였다. 등온환경에서의 실험으로부터 반응특성곡선을 관찰한 결과 경화반응이 1차 반응함수임을 확인하였고, 활성화 에너지는 78.43 kJ/mo1을 얻었다. 이 프리프레그는 경화온도에 따라 한계경화도를 보여주어 유리화가 존재함을 확인하였고 이를 1차 반응속도 모델에 적용시킨 결과, 유리화 이후의 확산우세현상을 포함한 반응속도 모델을 제안하였다. 제안된 모델식을 이용하여 등온/등속도 가열환경을 포함한 실제 경화공정을 성공적으로 표현할 수 있었다.