• Korean Journal of Materials Research
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• v.2 no.4
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• pp.257-262
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• 1992

The cure kinetics of a diglycidyl ether of bisphenol A (DGEBA) with 4, 4'-methylene dianiline (MDA) added succinonitrile was studied through the dynamic run method by applying the data to the Kissinger equation which analyses the effect of the heating rate on the temperature at maximum reaction rate using Differential Scanning Calorimetry (DSC) analyzer in the range of 3$0^{\circ}C$-35$0^{\circ}C$. In the DGEBA/MDA system with SN, the activation energy ($E_a$) and the pre-exponential factor (A) were calculated. From these results, the rate constants (k) were obtained according to the different SN contents.

• Applied Chemistry for Engineering
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• v.10 no.7
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• pp.1046-1051
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• 1999

Cure behavior and thermal stability of the different ratio of diglycidylether of bisphenol A(DGEBA)/trimethylolpropane triglycidylether(TMP) epoxy blends initiated by 1 wt % N-benzylpyrazinium hexafluoroantimonate (BPH) as a cationic latent catalyst were studied using DSC and TGA, respectively. Latent properties were performed by measurement of the conversion as a function of temperature using dynamic DSC. Dynamic DSC thermograms of DGEBA/TMP blends revealed that the weak peak was formed by complex formation between the hydroxyl groups in DGEBA and BPH, and between epoxides and BPH in low temperature ranges. The strong peak was considered as an exothermic reaction by the formation of three-dimensional network in high temperature ranges. Isothermal DSC revealed that the reaction rate of the blends was found to be higher than that of the neat TMP. The thermal stabilities in the cured resins were increased with increasing the DGEBA content. These results could be interpreted in terms of the stable aromatic structure, existence of hydroxyl group and high molecular weight of DGEBA.

• Elastomers and Composites
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• v.38 no.3
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• pp.213-226
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• 2003

The cure and rheological behavior of diglycidyl ether of bisphenol F/nadic methyl anhydride resin system with the kinds of imidazole were studied using a differential scanning calorimeter (DSC) and a rotational rheometer. The isothermal traces were employed to analyze cure reaction. The DGEBF/ anhydride conversion profiles showed autocatalyzed reaction characterized by maximum conversion rate at $20{\sim}40 %$ of the reaction. The rate constants ($k_1,\;k_2$) showed temperature dependance, but reaction order did not. The reaction order (m+n) was calculated to be close to 3. There are two reaction mechanisms with the kinds oi catalyst. The gel time was determined by using G'-G" crossover method, and the activation energy was obtained from this results. From measurement of rheological properties it was found that the logarithmic 1:elation time of fused silica filled DBEBF epoxy compounds linearly increased with the content of filler and decreased with temperature. The highly filled epoxy compounds showed typical pseudoplastic behavior, and the viscosity of those decreased with increasing maximum packing ratio.

• Journal of the Korean Chemical Society
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• v.47 no.5
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• pp.472-478
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• 2003

In this work, the zeolite/diglycidylether of bisphenol A(DGEBA) systems were investigated in terms of the cure kinetics and mechanical interfacial properties of the composites. The 4, 4-diamino diphenyl methane(DDM) was used as a curing agent for epoxy. Two types of zeolite(PZ) were prepared with 15 and 35 wt% KOH treatments(15-BZ and 35-BZ, respectively) for 24 h, and their surface characteristics were studied by X-ray photoelectron spectroscopy (XPS) and X-ray diffraction(XRD). Cure kinetics of the composites were examined in the context of differential scanning calorimetry(DSC), and mechanical interfacial properties were investigated in critical stress intensity factor($K_{IC}$) and critical strain energy release rate($G_{IC}$). In the results of XPS and XRD, sodium ion(Na) of zeolite was exchanged for potassium ion(K), resulting from the treatment of KOH. Also, $Si_{2p}/Al{2p}$ composition ratios of the treated zeolite were increased, which could be attributed to the weakening of Al-O bond in framework. Cure activation energy($E_a$) of 15-BZ composites was decreased, whereas KIC and $G_{IC}$ were increased, compared with those of the pure zeolite/DGEBA composites. It was probably accounted that the acidity of zeolite was increased by surface treatments and the cure reaction between zeolite and epoxy was influenced on the increased acidity of zeolite.

• Polymer(Korea)
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• v.27 no.3
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• pp.176-182
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• 2003

The fluorine-containing epoxy resin, 2-trifluorotoluene diglycidylether (FER) was prepared by reaction of 2-chloro-${\alpha}$,${\alpha}$,${\alpha}$-trifluorotoluene with glycerol diglycidylether in the presence of pyridine catalyst. Curing behavior of FER/DDM system was investigated using dynamic and isothermal DSC. Cure activation energy (Ea) was determined by Flynn-Wall-Ozawa's equation. The rheological properties of FER/DDM system were studied under isothermal condition using a rheometer. Cross-linking activation energy (Ec) was determined from the Arrhenius equation based on gel time and curing temperature. As a result, the chemical structure of FER was confirmed by FT-IR, $\^$13/C NMR, and $\^$19/F NMR spectroscopy. The cure activation energy of FER/DDM system was 55.4 kJ/mol and conversion and conversion rate were increased with the curing temperature. The cross-linking activation energy of FER/DDM system was 41.6 kJ/mol and gel time was decreased with the curing temperature.

• Elastomers and Composites
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• v.51 no.2
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• pp.81-92
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• 2016

1,3-Diphenylguanidine (DPG) is commonly used as a secondary accelerator which not only acts as booster of cure but also activating silanization reaction. The aim of this study is to increase the interaction between silica and rubber by using DPG. In this study, mixing was proceeded in two steps. The T-1 compound is mixed DPG with silica and silane coupling agent in the kneader at high temperature which is named as $1^{st}$ mixing step. T-3 compound is mixed DPG with curatives in the two-roll mill at low temperature which is named as $2^{nd}$ mixing step. The T-2 compound is mixed a half of DPG in $1^{st}$ mixing step and the remainder is mixed in $2^{nd}$ mixing step. Total DPG content was equal for all compounds. When DPG is mixed with silica, silane coupling agent during the $1^{st}$ mixing step, a decrease in cure rate and an increase in scorch time can be seen. This indicates that DPG is adsorbed on the surface of silica. during rubber processing. However, bound rubber content is increased and dynamic properties are improved. These results are due to the highly accelerated silanization reaction. However, there are no significant difference in 100%, 300% modulus.

• Restorative Dentistry and Endodontics
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• v.29 no.4
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• pp.386-398
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• 2004

Objectives: The purpose of this study was to observe the reaction kinetics and the degree of polymerization of composite resins when cured by different light sources and to evaluate the effectiveness of the blue Light Emitting Diode Light Curing Units (LED LCUs) compared with conventional halogen LCUs. Materials and Methods: First, thermal analysis was performed by a differential scanning calorimeter (DSC). The LED LCU (Elipar Freelight, $320{\;}mW/\textrm{cm}^2$) and the conventional halogen LCU (XL3000, $400{\;}mV/\textrm{cm}^2$) were used in this study for curing three composite resins (SureFil, Z-250 and AEliteFLO). Second. the degree of conversion was obtained in the composite resins cured according to the above curing mode with a FTIR. Third, the measurements of depth of cure were carried out in accordance with ISO 4049 standards. Statistical analysis was performed by two-way ANOVA test at 95% levels of confidence and Duncan's procedure for multiple comparisons. Results: The heat of cure was not statistically different among the LCUs (p > 0.05). The composites cured by the LED (Exp) LCUs were statistically more slowly polymerized than by the halogen LCU and the LED (Std) LCU (p < 0.05). The composite resin groups cured by the LED (Exp) LCUs had significantly greater degree of conversion value than by the halogen LCU and the LED (Std) LCU (p =0.0002). The composite resin groups cured by the LED (Std) LCUs showed significantly greater depth of cure value than by the halogen LCU and the LED (Exp) LCU (p < 0.05).

• Journal of Hydrogen and New Energy
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• v.22 no.6
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• pp.827-834
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• 2011

Epoxy/graphite/expanded graphite composites have been prepared in various weight ratios and thermal degradation and electrical properties were estimated in order to use for the bipolar plate materials in PEMFC. Thermogravimetric analysis (TGA) showed that the epoxy/graphite system cured by a curing agent GX-533 was most proper because its weight loss until $80^{\circ}C$ at which PEMFC would be operated was 0.3 wt%, and differential scanning calorimetry (DSC) analysis showed its cure temperature would be sufficient at $80^{\circ}C$. The activation energy for the cure reaction was 132.0 kJ/mol and the pre-exponential factor was $1.76{\times}10^{17}min^{-1}$. Electrical conductivity on the surface of the bipolar plate prepared under a pressure of 200 $kgf/cm^2$ was increased from 4 to 25 $S/cm^2$ by increasing expanded graphite (EG) content from 50 phr to 90 phr. The percolation threshold was initiated around 75 phr and the corrosion rate at 80 phr was 1.903 $uA/cm^2$.

• Applied Chemistry for Engineering
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• v.8 no.6
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• pp.960-966
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• 1997

The effects of epoxy resins and content of catalyst on the cure characteristics were studied by FT-IR, DSC and dynamic viscometer for the thermal properties and rheological properties of the catalytic (N-Benzylpyrazinium hexafluoroantimonate, BPH) epoxy thermosetting system. Compared with DSC results of DEGBF containing 0.5wt% BPH, the DSC thermograms of DGEBA containing 0.5wt% BPH indicated that the reaction was faster than that of DGEBF/BPH and the conversion rate of DGEBA/BPH was high in the initial stage of the reaction. As the concentration of BPH increases, the reaction and conversion rates show similar value in both the cases. The influence of hydroxyl group of epoxy resin on gel point defined from the crossover point of storage modulus (G') and loss modulus (G") could be explained by the formation of 3-dimensional network in the initial stage owing to the curing reaction between epoxides and hydroxyl groups of epoxy resin. This was consistent with the gel point obtained from DSC, FT-IR and moduli crossover. The activation energy (Et) obtained from the crossover point (G'/G"=1) are $31-39kJ.mol^{-1}$ for various BPH compositions in case of two epoxy systems.

• Journal of Adhesion and Interface
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• v.15 no.1
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• pp.22-30
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• 2014

Self-photoinitiating acrylate (SPIA) which can undergo self-initiation under UV irradiation was synthesized by a Michael addition in the presence of a base catalyst. The SPIA polymerizations were investigated by photo-differential scanning calorimeter (photo-DSC) and surface physical properties such as pendulum hardness and pencil hardness. The results showed that the SPIA can cure upon UV irradiation by itself without a photoinitiator. But we found out that both the curing rate and the conversion were too low for the self-curing reaction of SPIA. In order to improve the SPIA curing properties, we introduced the SPIA/cationic hybrid system and observed the effects of the addition of commercial free radical type monomer and photoinitiator on the curing behaviors. SPIA/cationic hybrid system was the best suitable to improve the SPIA curing properties. The kinetic analysis indicated that the cationic monomer and photoinitiator apparently accelerated the cure reaction and rate of the hybrid SPIA system, mostly due to the synergistic effect of cationic monomer and photoinitiator increasing the mobility of active species and the generation of reactive species (free radical, cation) during the photopolymerization process. The physical properties showed that, unlike typical free radical system, the hybrid systems did not show oxygen inhibition effect because of cationic reaction on the coating surface.