• The Korean Journal of Rheology
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• v.10 no.4
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• pp.227-233
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• 1998

The effects of 1 mol% N-benzylpyrazinium hexafluoroantimonate(BPH) as a thermal latent initiator and blend compositions composed of cycloaliphatic and DGEBA epoxies were investigated in the rheological properties and cure kinetics. Latent properties were performed by measurement of the conversion as a function of reaction time using isothermal DSC at $150^{\circ}C$ and $50^{\circ}C$ Rheological properties of the blend systems were investigated in terms of isothermal experiments using a rheometer. The gelation time was obtained from the evaluation of storage modulus (G'), loss modulus (G") and damping factor (tan$\delta$)). Cross-linking activation energy ($E_c$) was also determined from the Arrhenius equation based on gel time and curing temperature. As a result, the gel time and cross-linking activation energy increased with increasing DGEBA composition. The cure activation energies ($E_a$) were obtained by Kissinger method using dynamic DSC thermograms. In this work, the cure activation energy decreased with increasing CAE concentration, which might be resulted from the short repeat units, simple side-groups and viscosity of reaction media.edia.

• Korean Chemical Engineering Research
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• v.47 no.2
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• pp.169-173
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• 2009

Effects of variations sulfur/accelerator ratio on cross-linking and thermal degradation behavior of NR/CR rubber compounds were studied using both dynamic DSC and non-isothermal TGA. DSC thermograms of the given samples were obtained with several different heating rates, and after cross-liked in DSC, TGA thermograms with the same samples also obtained. Kissinger analysis was applied to assess the activation energies for the cross-linking and thermal decomposition processes. Results showed that the formation and thermal decomposition reaction of the samples occurred in the overall temperature range of $120{\sim}180^{\circ}C$ and $350{\sim}450^{\circ}C$, respectively, exhibiting that data could be well-fittable by Kissinger method. Furthermore, formation activation energy by DSC was estimated as $83.0{\pm}5.0kJ/mol$, which was much smaller than that of degradation by TGA, $147.0{\pm}2.0kJ/mol$. From these results, it was considered that, although variations of sulfur/accelerator ratio in the present experiments affected little on the formation mechanism and/or thermal degradation, they could play roles as the catalysts which lower the activation energy of formation. Because of stabilization after formation reaction, however, they have no more effects on the lowering the activation energy, showing higher values when decomposition, caused by main-chain scissions.

• 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.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.13 no.5
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• pp.2408-2413
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• 2012

Effects of stanous catalyst on the cross-linking reaction characteristics of multi-functional fluoropolymer with blocked-hexamethylene diisocyanate(HMDI) were studied by dynamic DSC and non-isothermal thermogravimetric analysis (TGA). Results showed that cross-linking reaction occurred around $230-250^{\circ}C$ aftr the solvent and phenol, blocking agent, were removed upto the $150^{\circ}C$. It was considered that the reaction mechanism of the multi-functional fluoropolymer with HMDI might not be changed by the catalyst, however, the reaction rate became extremely faster upto to 100 times, showing the change of activation energy 81.8 kJ/mol for non-catalytic system to 61.7 kJ/mol for 1 phr catalytic system.

• The Korean Journal of Rheology
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• v.11 no.2
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• pp.135-142
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• 1999

The effects of 1 wt.% N-benzylpyrazinium hexafluoroantimonate (BPH) as a thermal latent initiator and blend compositions composed of 0, 5, 10, 20 and 40 wt.% of phenol-novolac resin to epoxy resin were investigated in terms of cure kinetics, thermal stabilities and rheological properties. Thermal latent properties of BPH were measured from the conversion as a function of reaction temperature on a dynamic DSC. This cationic BPH system turned out to be an effective thermal latent initiator in the epoxy-phenol curing system. And the increase of phenol-novolac resin concentration led to the decrease in the latent temperature and to the increase of cure activation energy ($E_a$) of the blend system. The thermal stability and activation energy ($E_t$) for decomposition, gel-time and activation energy ($E_c$) for cross-linking from rheometer increased within the composition range of 20~40 wt.% of phenol-novolac resin. This implies that the three-dimensional cross-linking may take place among hydroxyl group within phenol resin, epoxide ring within epoxy resin and BPH.

• Elastomers and Composites
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• v.35 no.2
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• pp.122-131
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• 2000

In this work, the effect of chemical surface treatments on morphology of carbon blacks was investigated in terms of cure behavior and tearing energy ($G_T$) of carbon blacks/rubber composites. As experimental results, the polar or nonpolar chemical treatment led to a significant physical change of carbon black morphology. The cure activation energies (Ea) and frequency factor (A) obtained from Kissinger equation decreased with improving the dispersion of carbon flacks, resulting in high reactivity. However, a significant advantage of carbon black/rubber composites is gained by carbon blacks treated in basic (BCB) or nonpolar (NCB) chemical solution, resulting in increasing the tearing energy. These results could be explained by changes of dispersion, agglomerate, surface functional group, void volume, and cross-linking density of carbon black/rubber composites.

• Elastomers and Composites
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• v.22 no.1
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• pp.20-28
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• 1987

The characteristic of the dielectric relaxation in silicone rubbers were studied in the frequency range of $1{\times}10^2{\sim}3{\times}10^6Hz$ at the temperature range of $30^{\circ}{\sim}170^{\circ}C$. As the results of the study, it has been confirmed that the silicone rubber containing the cross-linking agants of 2,5-bis(tert-butylperoxy)-2, 5-dimethyl hexane exhibit the dissipation spectra of two kind(${\alpha},\;{\beta}$ dissipation) due to the siloxane and methyl groups. Particularly, the maximum value of dielectric loss spectra of silicone rubber combinning the cross-linking agents of 0.7phr to 1.0phr are on the increasing in high frequency region, but the specimen of above 1.0phr become smaller again. The energy and the entropy of activation on the molicular motion obtained 18.32 kcal/mole and $1.48ca1/mole{\cdot}deg$ in measuring condition respectively.

• Macromolecular Research
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• v.17 no.8
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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.

• Elastomers and Composites
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• v.25 no.2
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• pp.112-116
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• 1990

In this study, as one way of developing the new cross-linking method that is curable in water, kinetic analysis of solution reaction between CR and silane coupling agents was attemped. First, CR was reacted with silane coupling agents in solution state. According to the time, reaction quantity was pursued by gas chromatography. Also, reaction rate coefficient and activation energy were calculated from the reaction quantity. Silane coupling agents which were used in this study were MPS, CPS and VES.

• Polymer(Korea)
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• v.25 no.2
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• pp.177-185
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• 2001

In this work, the cure kinetics and rheological properties of difunctional epoxy(diglycidylether of bisphenol A, DGEBA)/polysulfone (PSF) blends were investigated using differential scanning calorimeter and rheometer. From the DSC results of the blends, the temperature of the exothermic peak and cure activation energy (E) using a half-width method were increased with increasing the PSF content to neat epoxy resin up to 30 wt%. However, a marginal decrease in the blend system was shown in E. The conversion ($\alpha$) and conversion rate (d$\alpha$/dt) were decreased as the content of PSF increases. Rheological properties of the blend system were investigated under isothermal condition using a rheometer. Cross-linking activation energy (E$_{c}$) was determined from the Arrhenius equation based on gel time and curing temperature. As a result, the E$_{c}$ showed a similar behavior with E which could be resulted from high viscosity of PSF and the phase separation between DGEBA and PSF.PSF.f PSF and the phase separation between DGEBA and PSF.PSF.