• Elastomers and Composites
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• v.42 no.1
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• pp.47-54
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• 2007

Reaction kinetics of polyurethane elastomers (PU) were studied using dynamic DSC and TGA for three PU samples of general purpose (Sample A), high temperature cross-likable CASE purpose with MOCA (Sample B), and RT cross-likable CASE purpose grade (Sample C). From DSC results, sample with MOCA(Sample B) showed lower shift of peak temperature, while showing broader thermograms than those of general purpose grade (Sample A). On the other hand, RT cross-linkable PU grade (Sample C) showed an interesting double mode reaction patterns, i.e., a lower temperature reaction at about $70\;^{\circ}C$, and a higher temperature reaction in the range of $140{\sim}170\;^{\circ}C$, indicating that it requires 2-step reaction process in order to complete the reaction. Once the cross-linking reaction completed, however, TGA results showed that all the samples would be considered to have similar chemical structures, showing similar decomposition processes. Sample C, especially, had showed decomposition properties of both Sample A and Sample B. Formation activation energies calculated from Kissinger method showed 10.39, 65.85, 36.52(Low $T_p$) and 18.21(High $T_p$) kcal/mol, while decomposition activation energies were 31.94, 30.84, 24.16 kcal/mol, respectively.

• Polymer(Korea)
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• v.24 no.1
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• pp.105-112
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• 2000

Using a commercial epoxy/carbon fiber composite prepreg (DMS 2224) as a model system, the cure kinetics of vitrifying thermoset system were analyzed by isothermal and dynamic-heating experiments. Focusing on the processing condition of high performance composite systems, a phenomenological kinetic model was developed by using differential scanning calorimetry (DSC) and reaction kinetics theories. The model system exhibited a limited degree of cure as a function of isothermal temperature seemingly due to the diffusion-controlled reaction rates. The diffusion-controlled cure reaction was incorporated in the development of the kinetic model, and the model parameters were determined from isothermal experiments. The first order reaction was confirmed from the characteristic shape of isothermal cure thermograms, and the activation energy wes 78.43 kJ/mol. Finally, the proposed model was used to predict a complex autoclave thermal condition, which was composed of several isothermal and dynamic-heating stages.

• Journal of Conservation Science
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• v.32 no.2
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• pp.223-234
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• 2016

Two-component epoxy resin is widely used in the cultural heritage restoration field. However according to mixing ratio of resin and hardener, curing property, mechanical strength and chemical structure differ which have possibility to effect the stability of cultural heritage. Result of questionnaire survey shows hands-on workers in the conservation field tend to mix the epoxy resin with his or her eye measurement when the using amount is small or mix additional hardener to shorten the pot life of epoxy resin. This research aims to analyze the curing property, mechanical strength and chemical structure of rapid curing type epoxy resin and medium curing type one depending on relative ratio of 0.25~4 of hardener to resin. When the amount of hardener was 0.5~2 times more than the resin, exothermic heat and curing speed were both increased. In case of included hardener to resin was lower than official ratio, mechanical strength (tensile shear strength, tensile strength and compressive strength) became higher along with active cross-linking bonding of the epoxy resin. Medium curing type epoxy relatively had lower exothermic heat and slower reaction during curing process. It was observed to be put to definite point of mechanical strength under lower content of hardener than official ratio. While, hardener ratio more than twice the resin slowed down the curing greatly and lowered the adhesion strength also. In conclusion, under the lower mixing rate of hardener than official ratio would show relatively fast reaction with similar mechanical strength. Over the official ratio on the other hand, material property drops rapidly. Accordingly, mixing ratio of epoxy resin is expected to be influential to the stability of cultural heritage.

• Polymer(Korea)
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• v.24 no.1
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• pp.65-71
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• 2000

The latent properties and cure kinetics of an acid anhydride-cured epoxy resin have been investigated by a near-infrared (NIR) reflection spectroscopy. The assignments of the latent properties and cure behaviors were performed by the measurements of the NIR reflectance for epoxide and hydroxyl groups at different temperatures. A comprehensive analysis of the origin, location, and shifts during reaction of all major NIR absorption peaks in the spectral range from 4000 to 7100 $cm^{-1}$ / was provided. The extent of reaction was determined from NIR absorption band at the 4530 $cm^{-1}$ / depending on epoxide concentration and cure temperature.

• Composites Research
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• v.17 no.6
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• pp.44-51
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• 2004

To determine the effect of numbers of nitrogen atom bonded at ethyl group included in main chain of linear amine curing agents of epoxy-cure systems on the thermal and mechanical properties, standard epoxy resin DGEBF was cured with DETA, TETA and TEPA in a stoichiometrically equivalent ratio. From this work, the effect of curing agents of the DGEBF/amine systems oil the thermal and mechanical properties was significantly influenced by numbers of nitrogen atom of curing agents. The results showed that heat of reaction increased, and maximum exothermic temperature decreased with the decrease of numbers of nitrogen atom. In case of cured systems, density and maximum conversion(%) had no relation to numbers of nitrogen atom, but flexural modulus and tensile modulus increased with the decrease of numbers of nitrogen atom in main chain. Thermal stability, shrinkage(%), Tg, tensile and flexural strength showed irregular tendency having nothing to do with numbers of nitrogem atom at a sight. This findings imply that the differences in the maximum conversion(%) about the chain length of curing agents affect the thermal and mechanical properties.

• Applied Chemistry for Engineering
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• v.16 no.2
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• pp.292-295
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• 2005

The curing time of the phenolic resin for the processing of brake pad is very important factor for reducing the processing cost. The curing time could be investigated by examining the reaction time of the phenolic resin and hexamethylenediamine. The reaction time has been studied by FT-IR, Differential Scanning Calolimetric Analysis (DSC), and Thermogravimetric Analysis (TGA).

• Proceedings of the Korean Society of Precision Engineering Conference
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• 2004.05a
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• pp.13-13
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• 2004

나노테크놀러지 중의 한 가지인 나노임프린트 리소그래피 기술은 수 ∼ 수십 나노 급의 선폭을 가지는 스탬프(stamp)를 전자빔 리소그래피(electron beam lithography)를 이용하여 제작한 후 스탬프에 형성된 패턴과 동일한 형상을 원하는 곳에 모사하는 기술이다. 이 기술은 크게 열을 가하는 방식과 UV 경화성 수지를 이용한 방식으로 나뉜다. 열을 가하는 나노임프린트 리소그래피 방식의 경우는 열 경화성 수지를 이용하여 고온 조건에서 스탬프를 고압으로 눌러 원래의 형상을 모사하며, UV 나노임프린트는 광경화 반응을 이용하여 수지를 경화 시켜 모사하는 차이점이 있다.(중략)

• Polymer(Korea)
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• v.24 no.6
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• pp.837-844
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• 2000

The cure behavior of commercial epoxy molding compounds (EMC) commonly used for IC package was studied at constant cure temperatures as well as at constant heating rates using differential scanning calorimetry (DSC), rheometer, and dielectric analyzer (DEA). The cure kinetics were obtained using autocatalytic reaction model according to the Ryan Dutta method after assuming m+n equal to 2. The prediction of reaction rates by the model equation corresponded well to experimental data at all temperatures except for 10$0^{\circ}C$. The phase transitions such as gelation and vitrification occurred during network formation. At each isothermal cure temperature, $T_{g}$ was measured in accordance with cure time, and the vitrification point was attained when $T_{g}$ was equal to $T_{cure}$. The temperature dependence of gel points and vitrification points showed good agreement with Arrhenius relation. DEA using parallel plate electrode was effective for the monitoring of EMC cure. we knew that if the resin systems are materials of comparable quality, $_{gel}$$T_{g}$ is constant regardless of accelerator concentration in TTT (Time-Temperature-Transformation) diagram.

• Polymer(Korea)
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• v.33 no.4
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• pp.290-296
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• 2009

The morphology and mechanical properties of epoxy/polyamide/MPD/2E4MZ-CN reactive blends with various amount of catalyst were investigated. The cure behaviors, mechanical strengths, and morphological changes of the epoxy blend systems were analyzed by using DSC, UTM, and SEM, respectively. The amount of catalyst ranged from 0 to 3 phr, and the cure reaction occurred at $170^{\circ}C$ for 30 min. The maximum peaks in heat flow during cure reactions appeared at slightly lower temperature with increasing catalyst content, indicating that the cure reactions start at lower temperature by adding catalyst and polyamide rarely hinders the cure reaction paths. The co-continuous morphology was found in epoxy/polyamide(20 phr) blends and by adding catalyst to the blends much clearer and uniform co-continuous phase was observed. The surface tension of the mechanical test specimen was increased due to the AP plasma surface treatment, and then adhesion strength was increased by over 20% by adding 2 phr of catalyst to the blends. When considering morphological tuning of the blends by means of catalyst incorporation, it is expected that the increased elongation and adhesion strength can be achieved in the structural adhesive systems.

• Analytical Science and Technology
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• v.17 no.3
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• pp.225-229
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• 2004

The effect of the silicon acrylate as a reactive additive on the UV-curing photopolymerization reaction was studied by micro raman technique. For the study, acrylate systems and Darocur 1173 were used as oligomer and monomers, and a photo initiator, respectively. The content of silicon acrylate was within the range of 0-3 wt%. The extent of photo-polymerization reaction as a function of depth from the air interface was obtained from the conversion ratio of acrylate double bond calculated from the intensities of measured bands at $1410cm^{-1}$ and at $1635cm^{-1}$. Micro raman spectroscopic technique can be an useful tool for the investigation of the factors, which can affect the reaction progress, such as oxygen inhibition, composition of the formulations, depth, etc.