• Transactions on Electrical and Electronic Materials
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• 제16권2호
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• pp.74-77
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• 2015

The cure kinetics of a neat epoxy system and epoxy/silica composite were investigated by DSC analysis. A cycloaliphatic type epoxy resin was diglycidyl 1,2-cyclohexanedicarboxylate and curing agent was anhydride type. To estimate kinetic parameters, the Kissinger equation was used. The activation energy of the neat epoxy system was 88.9 kJ/mol and pre-exponential factor was 2.64×10¹² min⁻¹, while the activation energy and pre-exponential factor for epoxy/silica composite were 97.4 kJ/mol and 9.21×10¹² min⁻¹, respectively. These values showed that the silica particles have effects on the cure kinetics of the neat epoxy matrix.

• 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.

• Composites Research
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• 제35권4호
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• pp.288-297
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• 2022

본 연구는 Zirconia(zirconium oxide) 입자가 페놀수지 경화거동에 미치는 영향을 조사하였다. Zirconia 입자의 함량에 따른 페놀수지의 승온 및 등온 경화 거동을 분석하였다. Zirconia 함량을 달리한 페놀수지의 점도 및 열분해 특성을 조사하였다. DSC 분석으로부터 경화도와 경화율을 구하였다. 마지막으로 Zirconia 입자가 첨가된 페놀수지의 DSC 데이터로부터 경화 반응에 대한 활성화 에너지를 계산하였다. 그 결과 zirconia 함량이 높을수록 경화가 지연되고 경화에 필요한 활성화에너지가 더 커지는 경향이 나타났다. 또한 TGA를 이용한 열분해 분석 결과 Zirconia의 함량이 증가할수록 더 적은 중량감소가 관찰됐다. Carbon/Phenol 프리프레그의 표면 점착성은 Zirconia 함량에 따라 부분적으로 변화하였으나 유의한 영향은 없었다.

• Macromolecular Research
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• 제16권6호
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• pp.561-566
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• 2008

NR composites with different curing systems were aged thermally at 60, 70, 80, and $90^{\circ}C$ for 2-185 days in a convection oven, and the changes in the crosslink density were investigated as a function of the accelerated thermal aging. The overall crosslink densities increased with increasing aging time irrespective of the aging temperatures and curing systems. The changes in crosslink density were enhanced by increasing the aging temperature. The degree of the increased crosslink density was in the following order: "the conventional cure system > the semi-EV system > the EV system". For short term thermal aging, the change in crosslink density with the aging time was complicated, particularly for low temperature aging. The activation energies of the change in crosslink density with thermal aging using the conventional and semi-EV cure systems increased and then remained relatively constant with increasing aging time, whereas that of the specimen with an EV cure system tended to increase linearly. The experimental results were explained by the dissociation of the existing polysulfidic linkages and the formation of new cross links through the crosslinking-related chemicals remaining in the sample.

• 공업화학
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• 제5권3호
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• pp.517-523
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• 1994

DGEBA(diglycidyl ether of bisphenol A)/MDA(4,4'-methylene dianiline)/SN(succinonitrile)/HQ(hydroquinone)계의 경화반응 속도론 및 메카니즘을 연구하였다. SN과 HQ는 반응성 첨가제와 촉매로 도입하였다. 경화반응 속도론은 DSC 분석에 의해 Kissinger equation과 fractional-life법을 이용하여 연구하였다. DGEBA/MDA/SN 계의 활성화에너지와 반응차수는 SN의 함량에 관계없이 거의 일정하였고, 촉매로써 HQ가 첨가됨으로 인해 활성화 에너지와 반응시작온도가 낮아졌다. 이들 계의 반응 메카니즘을 고찰하기위하여 SN의 함량에 따라 FT-IR을 측정하였다. 그리고, SN:HQ의 혼합비는 4:1이었다. Diamine으로 경화되는 에폭시 수지의 경화반응 메카니즘은 primary amine-epoxy 반응, secondary amine-epoxy 반응, epoxy-hydroxyl 반응이 일어나는 것으로 알려져 있다. DGEBA/MDA/SN/HQ 계에서는 HQ의 hydroxyl 기가 epoxy 및 amine과 결합하여 전이상태를 형성하여 epoxide ring을 빠르게 개환시켜줌으로써 amine-epoxy반응이 쉽게 일어남을 알았다.

• 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.

• 한국복합재료학회:학술대회논문집
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• 한국복합재료학회 2001년도 춘계학술발표대회 논문집
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• pp.110-113
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• 2001

Dielectrometry has been used to monitor the cure of epoxy resin using composite matrix. In this investigation, physical properties of the mixture of epoxy resin(LY564), bisphenol A type, and cycloaliphatic hardener(HY 2954) were observed. Activation energy at maximum tan $\delta$ and gelation point was determined during isothermal scanning. From IonViscosity data, it was found that vitrification peak after gelation was appeared on slow heating rate. It was also measured that the duration time for full cure was necessary and it was about 24 hr at $145^{\circ}C$. Therefore, epoxy resin used in this research is required the extended time for full cure.

• Macromolecular Research
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• 제17권8호
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• pp.585-590
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• 2009

The cure behaviors, dielectric characteristics and fracture toughness of diglycidylether of bisphenol-A (DGEBA)/poly(ethylene terephthalate) (PET) blend system were investigated. The degree of conversion for the DGEBA/PET blend system was measured using Fourier transform infrared (FTIR) spectroscopy. The cure kinetics were investigated by measuring the cure activation energies ($E_a$) with dynamic differential scanning calorimetry (DSC). The dielectric characteristic was examined by dielectric analysis (DEA). The mechanical properties were investigated by measuring the critical stress intensity factor ($K_{IC}$), critical strain energy release rate ($G_{IC}$), and impact strength test. As a result, DGEBAIPET was successfully blended. The Ea of the blend system was increased with increasing PET content to a maximum at 10 phr PET. The dielectric constant was decreased with increasing PET content. The mechanical properties of the blend system were also superior to those of the neat DGEBA. These results were attributed to the increased cross-linking density of the blend system, resulting from the interaction between the epoxy group of DGEBA and the carboxyl group of PET.

• 한국복합재료학회:학술대회논문집
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• 한국복합재료학회 2002년도 추계학술발표대회 논문집
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• pp.265-268
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• 2002

In this work, the blend system of epoxy and PMR-15 polyimide is investigated in terms of the cure behaviors and thermal stabilities. The cure behaviors are studied in DSC measurements and thermal stabilities are also carried out by TGA analysis. DDM (4, 4'-diamino diphenyl methane) is used as curing agent for EP and the content of PMR-15 is varied within 0, 5, 10, 35, and 20 phr to neat EP. As a result, the cure activation energy ($E_a$) is increased at 10 phr of PMR-15, compared with that of neat EP. From the TGA results of EP/PMR-15 blend system, the thermal stabilities based in the initial decomposed temperature (IDT) and integral procedural decomposition temperature (IPDT) are increased with increasing the PMR-15 content. The fracture toughness, measured in the context of critical stress intensity factor ($K_{IC}$) and critical strain energy release rate ($G_{IC}$), shows a similar behavior with $E_a$. This result is probably due to the crosslinking developed by the interactions between intermolecules in the polymer chains.

• 반도체디스플레이기술학회지
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• 제13권4호
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• pp.27-32
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• 2014

The cure properties of self-extinguishing epoxy resin systems with different charge transfer type latent catalysts were investigated, which are composed of YX4000H as a biphenyl epoxy resin, MEH-7800SS as a hardener, and charge transfer type latent catalysts. We designed and used five kinds of charge transfer type latent catalyst and compared to epoxy resin systems with Triphenylphosphine-Benzoquinone(TPP-BQ) as reference system. The cure kinetics of these systems were analyzed by differential scanning calorimetry with an isothermal approach, the kinetic parameters of all systems were reported in generalized kinetic equations with diffusion effects. The epoxy resin systems with Triphenylphosphine-Quinhydrone(TPP-QH), Triphenylphosphine-Benzanthrone(TPP-BT) and Triphenylphosphine-Anthrone(TPP-AT) as a charge transfer type latent catalyst showed a cure conversion rate of equal or higher rate than those with TPP-BQ. These systems with TPP-QH and Triphenylphosphine-Tetracyanoethylene(TPP-TCE) showed a critical cure reaction conversion of equal or higher conversion than those with TPP-BQ. The increases of cure conversion rates could be explained by the decrease of the activation energy of these epoxy resin systems. It can be considered that the increases of critical cure reaction conversion would be dependent on the crystallinity of the biphenyl epoxy resin systems.