• Korean Journal of Materials Research
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• v.3 no.3
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• pp.215-222
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• 1993

Malononitrile(MN) as a reactive additive was added to Diglycidyl ether of bisphenol A (DGEBA)/Methylene dianiline (MDA) system in order to modify a thermosetting epoxy resin. Cure ki. netics and cure mechanism of this modified system were investigated by using DSC(differential scanning calorimetry) and FT-IR(fourier transform infrared spectrometry). Cure kinetics gave an information that the DGEBA/MDA system modified with MN should cure at over $110^{\circ}C$ after curing at about $80^{\circ}C$ for the complete curing. The activation energy of the first cure was nearly constant and that of the second cure was increased as the MN content was increased. Cure mechanism for the system was investigated with the samples cured every $30^{\circ}C$, from $80^{\circ}C$ to $170^{\circ}C$, for Ihr. It was known that the cure reactions of the epoxy-diamine system were composed of PA -E, SA - E and E-OH reactions. Beside these three reactions, in the DGEBA/MDA/MN system PA-CN and CN-OH reaction was found.

• Korean Journal of Materials Research
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• v.9 no.4
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• pp.373-377
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• 1999

The cure mechanicsm and cure kinetics of diglycidyl ether of bisphenol A(DGEBA)/4,4'-methylene dianiline(MDA)/nitrile(MN, SN, GN) systems were studied by FT-IR and DSC to develop new applications in the biomedical polymer fields. The network structure of the DGEBA/MDA system was changed to the chain-extended network structure by the addition of nitriles. The reactions contributed to the chain extension were the primary amine-nitrile and hydroxyl-nitrile reactions. The chain-extended network structure could be indirectly proved by the decrement of T\ulcorner and the increment of impact strength with the increasing nitrile content. The cure rate of DGEBA/MDA/nitrile system was lower than that of DGEBA/MDA system due to the disturbance of nitrile group in the reaction of primary amine and epoxide groups.

• Bulletin of the Korean Chemical Society
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• v.20 no.11
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• pp.1329-1334
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• 1999

The curing characteristics of diglycidyl ether of bisphenol A (DGEBA) with diaminodiphenylmethane (DDM) as a curing agent were studied using differential scanning calorimetry (DSC), rheometrics mechanical spectrometry (RMS), and dielectric analysis (DEA). The isothermal curing kinetics measured by DSC were well represented with the generalized auto-catalytic reaction model. With the temperature sweep, the inverse relationship between complex viscosity measured by RMS and ionic conductivity obtained from DEA was established indicating that the mobility of free ions represented by the ionic conductivity in DEA measurement and the chain segment motion as revealed by the complex viscosity measured from RMS are equivalent. From isothermal curing measurements at several different temperatures, the ionic conductivity contribution was shown to be dominant in the dielectric loss factor at the early stage of cure. The contribution of the dipole relaxation in dielectric loss factor became larger as the curing further proceeded. The critical degrees of cure, at which the dipolar contribution in the dielectric loss factor starts to appear, increases as isothermal curing temperature is increased. The dielectric relaxation time at the same degree of cure was shorter for a sample cured at higher curing temperature.

• 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.

• Elastomers and Composites
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• v.53 no.2
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• pp.52-56
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• 2018

The present study examines the transformation of dynamic DSC data into the equivalent isothermal data for the formation kinetics of a polyurethane elastomer. The reaction of 2'-dichloro-4,4'-methylenedianiline (MOCA) with a PTMG/TDI-based isocyanate prepolymer was evaluated. DSC measurement was performed in the dynamic scanning mode with several different heating rates to obtain the reaction thermograms. Then, the data was transformed into the isothermal data through a procedure based on Ozawa analysis. The main feature of this procedure was the transformation of $({\alpha}-T)_{\beta}$ curves from dynamic DSC into $({\alpha}-t)_T$ curves using the isoconversional $(t-T)_{\alpha}$ diagram. Validity was discussed for the relationship between the dynamic DSC data and the transformed isothermal results.

• 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.7 no.2
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• pp.356-361
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• 1996

Cure kinetics of diglycidyl ether of bisphenol A(DGEBA)/4,4'-methylene dianiline(MDA) with hydroquinone-phenyl glycidyl ether(HQ-PGE) as a reactive additive, which was preliminarily synthesized, was investigated by DSC and FT-IR analyses. Kissinger equation and Arrhenius' equation were used to calculate activation energy and pre-exponential factor. When HQ-PGE was added to DGEBA/MDA system, it reduced activation energy of system. When the 5 phr of HQ-PGE was added to DGEBA/MDA system, activation energy was 7.8 kcal/mol by FT-IR analysis and 11.3 kcal/mol by DSC, in comparison with the system without HQ-PGE, activation energy decreased about 30% and 9%, respectively. According to these results, HQ-PGE, introducing agent of this system, acted as a catalyst.

• Applied Chemistry for Engineering
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• v.26 no.5
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• pp.538-542
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• 2015

In this work, effects of the blend composition composed of 0, 10, 20, 30 and 40 wt% of nylon 6 to epoxy (diglycidylether of bisphenol-A, DGEBA) resin were investigated in terms of cure kinetics and thermal stability by differential scanning calorimeter (DSC) and thermogravimetric analysis (TGA). As the content of the nylon 6 increased, the maximum exothermic temperature ($T_{max}$) and the value of cure activation energy ($E_a$) decreased. The maximum exothermic temperature of the blending samples decreased with increasing in nylon 6 content, resulting in the decrease in curing activation energy of them due to the rapid curing reaction with epoxy resin in this system. From TGA analysis results of the DGEBA/nylon 6, the thermal stability based on the thermal stability index ($A^*{\cdot}K^*$) and integral procedure decomposition temperature (IPDT) increased with increase in the nylon 6 content. This was because of the combination of DGEBA and nylon 6 having good heat resistance, resulting in improving thermal stability of the DGEBA/nylon 6.

• Proceedings of the Korean Society For Composite Materials Conference
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• 1999.11a
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• pp.73-76
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• 1999

Near infrared spectroscopy techniques were used to study the cure reactions of epoxy resin system based on diglycidyl ether of bisphenol A(DGEBA) resins cured with 4, 4' diaminodiphenyl sulfone (DDS) hardner. Stoichiometric DGEBA/DDS resin formulation was involved in this study. The infrared absorption spectra of the prepared formulation were obtained on an FTIR spectrometer operating in the region of 11000 to 4000$cm^{-l}$. The chemical group peaks of interest in a DFEBA/DDS spectrum were identified by a comparative study with individual spectra of DGEBA and DDS monomers. Where necessary, special model compounds were used to identify unknown bands, such as the primary amine band at 4535$cm^{-l}$. The absorption bands of interest were integrated to quantify the areas and then converted to molar concentrations. This series of quantitative analyses of the major chemical groups led us to understand not only the reaction mechanism but also the cure kinetics. In this paper, the reaction mechanisms observed in stoichiometric DGEBA/DDS resin formulation and the various properties of the resin system as a function of cure temperature are described.

• Proceedings of the Korean Society For Composite Materials Conference
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• 2000.11a
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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.