• 폴리머
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• 제36권6호
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• pp.803-809
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• 2012

에틸렌-테트라플르오르에틸렌(ETFE) 공중합체의 비등온 결정화 거동을 DSC와 imaging FTIR을 이용하여 살펴보았다. 변형 비등온 Avrami 분석 결과, DSC에 의한 열분석의 경우 상대적으로 적은 결정화 엔탈피 변화로 인하여 Avrami 식에 의한 ln[-ln(1-X(t))] vs. ln(t) 곡선이 선형을 이루지 못하는 반면, 결정화에 의한 IR 흡수 강도 image의 변화에 의한 분석 방법인 imaging FTIR의 경우보다 선형적인 결과를 얻음에 따라 imaging FTIR이 ETFE 비등온 결정화 연구에 보다 효과적임을 알 수 있었다. 이와 함께 비등온 결정화에 의한 ETFE의 광학특성을 살펴본 결과, 서냉에 의하여 형성된 ETFE 결정의 빛 산란에 의하여 haze가 증가하며 따라서 투명도가 감소함을 알 수 있으며 비등온 결정화에 의하여 최대 8%의 투과도 감소가 일어남을 확인할 수 있었다. 이상의 결과로부터 결정화를 조절하는 냉각속도가 유리 대체 소재로 사용되고 있는 ETFE 필름의 광투과도 조절에 주요한 가공 변수임을 확인할 수 있었다.

• Elastomers and Composites
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• 제53권1호
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• pp.1-5
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• 2018

In the current research, the curing kinetics of a mixture system consisting of a Bisphenol-A type vinyl ester resin and styrene monomer was studied. Methylethylketone peroxide and cobalt octoate were used as the polymerization initiator and accelerator respectively. Thermograms with several different heating rates were obtained using non-isothermal differential scanning calorimetry. Activation energy values analyzed by the Flynn-Wall-Ozawa isoconversional method showed a three-step change with conversion ${\alpha}$: a slight decrease initially for ${\alpha}$ < 0.1, a constant value of 47.9 kJ/mol in the range 0.1 < ${\alpha}$ < 0.7, and a slow increase for 0.7 < ${\alpha}$. When assuming a constant activation energy of 47.9 kJ/mol, an autocatalytic model of the Sestak-Berggren equation was considered as the proper mathematical model of the conversion function, indicating an overall order of 1.2.

• Elastomers and Composites
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• 제50권2호
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• pp.92-97
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• 2015

A study on reaction kinetics for a PTMG/TDI prepolymer with 2,2'-dichloro-4,4'-methylenedianiline (MOCA), of which formulations may be generally used for fabricating high performance polyurethane elastomers, was peformed using non-isothermal differential scanning calorimetry (DSC). A number of thermograms were obtained at several constant heating rates, and analysed using Flynn-Wall-Ozawa (FWO) isoconversional method for activation energy, $E_a$ and extended-Avrami equation for reaction order, n. Urea formation reaction of the present system was observed to occur through the simple exothermic reaction process in the temperature range of $100{\sim}130^{\circ}C$ for the heating rate of $3{\sim}7^{\circ}C/min$. and could be well-fitted with generalized sigmoid function. Though activation energy was nearly constant as $53.0{\pm}0.5kJ/mol$, it tended to increase a little at initial stage, but it decreases at later stage by the transformation into diffusion-controlled reaction due to the increased viscosity. Reaction order was evaluated as about 2.8, which was somewhat higher than the generally well-known $2^{nd}$ order values for the various urea reactions. Both the reaction order and reaction rate explicitly increased with temperature, which was considered as the indication of occurring the side reactions such as allophanate or biuret formation.

• Bulletin of the Korean Chemical Society
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• 제30권10호
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• pp.2259-2264
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• 2009

A new high-energy organic potassium salt, 2-(dinitromethylene)-1,3-diazepentane potassium salt K(DNDZ), was synthesized by reacting of 2-(dinitromethylene)-1,3-diazepentane (DNDZ) and potassium hydroxide. The thermal behavior and non-isothermal decomposition kinetics of K(DNDZ) were studied with DSC, TG/DTG methods. The kinetic equation is $\frac{d{\alpha}}{dT}$ = $\frac{10^{13.92}}{\beta}$3(1 - $\alpha$[-ln(1 - $\alpha$)]$^{\frac{2}{3}}$ exp(-1.52 ${\times}\;10^5$ / RT). The critical temperature of thermal explosion of K(DNDZ) is $208.63\;{^{\circ}C}$. The specific heat capacity of K(DNDZ) was determined with a micro-DSC method, and the molar heat capacity is 224.63 J $mol^{-1}\;K^{-1}$ at 298.15 K. Adiabatic time-to-explosion of K(DNDZ) obtained is 157.96 s.

• 한국산학기술학회논문지
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• 제9권5호
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• pp.1125-1129
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• 2008

폴리프로필렌(polypropylene, PP)/옥수수전분(corn starch) 마스터뱃취(MB)(전분 MB) 블렌드를 PP 함량을 90, 80, 70, 60 wt%로 변화시키며 실험실 규모의 Brabender mixer를 이용하여 $200^{\circ}C$에서 제조하였다. PP/전분MB 블렌드의 화학구조, 기초 열적특성 및 비등온결정화거동을 적외선분광기 (FT-IR), 시차주사열용량분석기(DSC) 그리고 열중량분석기(TGA)를 이용하여 관찰하였다. PP/전분MB 블렌드의 제조는 수산기의 존재여부를 통해 확인하였다. 용융온도 및 엔탈피에는 큰 변화가 나타나지 않음을 알 수 있었고, 블렌드의 분해온도는 전분MB 함량에 따라 감소하고 있음을 보여주었다. PP/전분MB 블렌드의 비등온결정화 거동은 Avrami 방정식을 이용하여 분석하였다. Avrami 지수의 경우 PP는 2.71-3.97의 값을 나타내었고, PP/전분MB 블렌드의 경우는 1.48-1.99 값을 보여주었다. 활성화에너지는 Kissinger 방법에 의해서 계산되었고, PP의 경우 233 kJ/mol, PP90은 484 kJ/mol, PP80은 541 kJ/mol, PP70은 553 kJ/mol, 그리고 PP60은 422 kJ/mol이었다.

• 대한화학회지
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• 제57권1호
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• pp.109-114
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• 2013

The effects of aluminum nanoparticles (AlNs) on the thermal decomposition of ammonia perchlorate (AP) were investigated by DSC, TG-DSC and DSC-TG-MS-FTIR. Addition of AlNs resulted in an increase in the temperature of the first exothermic peak of AP and a decrease in the second. The processing of non-isothermal data at various heating rates with and without AlNs was performed using Netzsch Thermokinetics. The dependence of the activation energy calculated by Friedman's isoconversional method on the conversion degree indicated the decomposition process can be divided into three steps. They were C1/D1/D1 for neat AP, determined by Multivariate Non-linear Regression, and changed to C1/D1/F2 after addition of AlNs into AP. The isothermal curves showed that the thermal stability of AP in the low temperature stage was improved in the presence of AlNs.

• 한국세라믹학회지
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• 제32권12호
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• pp.1331-1336
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• 1995

The glass-ceramics for ferro-electric were made from compositions of 70PbO.16TiO2.8SiO2.4B2O3.2AlPO4 (wt%) and 67.5PbO.20TiO2.8.5SiO2.2B2O3.2AlPO4 (wt%). The crystallization kinetics for PbTiO3 crystalline phase formation from glass was studied using non-isothermal DSC techniques. The values of activation energy, ΔE using variables of heating rate and temperature were calculated at various reaction fractions obtained from peak area over DSC. The results indicated that activation energy was lowest at 60% reaction fractions and the activation energy of glass containing 20.0 wt% TiO2 is higher than that of glass containing 16.0 wt% TiO2. The crystallization mechanism was three dimensional growth (n=4).

• 한국추진공학회:학술대회논문집
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• 한국추진공학회 2011년도 제36회 춘계학술대회논문집
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• pp.421-424
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• 2011

본 연구에서는 열분석법을 이용하여 혼합 액체연료의 수치해석에 필요한 여러 가지 인자를 측정하였다. 이러한 열분석법에는 열중량 분석방법(TGA, Thermo-Gravimetric Analyzer)과 시차 주사열량 측정법(DSC, Differential Scanning Calorimetry)이 있다. 열중량 분석방법을 통한 비등온 실험(non-isothermal experimental) 결과를 토대로 Freeman Carroll의 수학적인 후처리 방법을 이용하여 미지의 액체연료의 구성 성분에 대한 동역학적 변수인 활성화 온도와 반응차수로 각각 6128.2 K와 1.4를 얻었다. 그 외 다양한 수학적 처리 방법에 따른 동역학적 변수의 값을 구해보았고, 계산 결과는 처리방법에 따라 약간의 차이를 보였다.

• 한국연초학회지
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• 제5권2호
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• pp.55-62
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• 1983

Cellulose의 열분해 반응에 대한 Kinetic Parameter를 구하기 위하여 Thermogravimetry(TG)와 Differential Scanning Calorimetry(DSC)를 이용하는 네가지 비등온법을 고찰하였다. 그 결과 DSC에 의한 가열속도법과 TG에 의한 근사법이 가장 간편하였고Kinetic Parameters의 신뢰도도 매우 높았다. Cellulose 열분해 반응에서 반응차수는 1/2차였고 활성화에너지는 42kca1/mo1로 나타났다.

• Journal of Welding and Joining
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• 제33권5호
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• pp.41-46
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• 2015

The snap cure NCP(non-conducive paste) adhesive material is essentially required for the high productivity flip chip bonding process. In this study, the accessibility of DEA(dielectric analysis) method for the evaluation of snap cure behavior was investigated with comparison to the isothermal DSC(differential scanning calorimetry) method. NCP adhesive was mainly formulated with epoxy resin and imidazole curing agent. Even though there were some noise in the dielectric loss factor curve measured by DEA, the cure start and completion points could be specified clearly through the data processing of cumulation and deviation method. Degree of cure by DEA method which was measured from the variation of the dielectric loss factor of adhesive material was corresponded to about 80% of the degree of cure by DSC method which was measured from the heat of curing reaction. Because the adhesive joint cured to the degree of 80% in the view point of chemical reaction reveals the sufficient mechanical strength, DEA method is expected to be used effectively in the estimation of the high speed curing behavior of snap cure type NCP adhesive material for flip chip bonding.