• ETRI Journal
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• v.38 no.6
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• pp.1179-1189
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• 2016

A chemorheological analysis of a no-flow underfill was conducted using curing kinetics through isothermal and dynamic differential scanning calorimetry, viscosity measurement, and solder (Sn/27In/54Bi, melting temperature of $86^{\circ}C$) wetting observations. The analysis used an epoxy system with an anhydride curing agent and carboxyl fluxing capability to remove oxide on the surface of a metal filler. A curing kinetic of the no-flow underfill with a processing temperature of $130^{\circ}C$ was successfully completed using phenomenological models such as autocatalytic and nth-order models. Temperature-dependent kinetic parameters were identified within a temperature range of $125^{\circ}C$ to $135^{\circ}C$. The phenomenon of solder wetting was visually observed using an optical microscope, and the conversion and viscosity at the moment of solder wetting were quantitatively investigated. It is expected that the curing kinetics and rheological property of a no-flow underfill can be adopted in arbitrary processing applications.

• Korean Chemical Engineering Research
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• v.46 no.1
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• pp.200-204
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• 2008

The curing kinetics of diglycidyl ether of bisphenol F (DGEBF) with an asymmetric cycloaliphatic amine curing agent were examined by thermal analysis in both isothermal and dynamic curing conditions. From the residual curing of the samples partially cured in isothermal condition and from the dynamic curing with various heating rates, it was found that there exist two kinds of reactions such as at low temperature and at high temperature regions. It was thus also found that the cure parameters obtained from the isothermal curing kinetic model hardly estimate experimental results for a degree of cure larger than 0.6. The activation energies and frequency factors of these two kinds of reactions were obtained from the dynamic curing experiments with various heating rates. From the curing analysis, it was verified that the total cure kinetics for low degrees of cure is dominated by the cure reaction in the low temperature region.

• Elastomers and Composites
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• v.52 no.4
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• pp.266-271
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• 2017

This study describes the influence of the amount of curing agent and curing temperature on the kinetics of polyurethane elastomers. The urethane prepolymer series was prepared by reacting toluene diisocyanate with polytetramethylene ether glycol at $80^{\circ}C$ for 1 h, and 4,4'-methylene bis(2-chloroaniline) was used as the curing agent. The ratio of the amine group of the curing agent to the isocyanate group of the urethane prepolymer was controlled from 0.85 to 1.05 at curing temperatures ranging from 80 to $120^{\circ}C$. The curing rate of the urethane prepolymer was monitored by observing the change in heat flow during the curing process using differential scanning calorimetry (DSC). As either the content of curing agent or the curing temperature was higher, the conversion rate to the polyurethane elastomer was high. The DSC results were compared with those obtained from using real-time FT-IR.

• Proceedings of the Materials Research Society of Korea Conference
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• 1994.11a
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• pp.125-126
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• 1994

The chemorheological changes and kinetics during curing reaction of an silica filled epoxy system (DGEBA with curing agent Polyxoypropylenediamine) were investigated. This study concentrates on the influence of silica on the reaction kinetics and rheological behavior of the eopxy system. The concentration of the filler was varied 0~200phr. Curing behavior of the silica filled epoxy system was measured at various heating rates with DSC. Conversion was also measured by integrating the obtained DSC curve and Kinetic parameters measured by using the nonlinear regression method. DSC experiments showed that the presence of silica was found to accelerate the progress of the curing reaction and of reduce the heat of reaction compared with that of unfilled epoxy systems . Rheological experiments were conducted on a Physica by using a disposable parallel plate fixture. Material properites were measured such as the elastic modulus(G′), the loss modulus(G"), the loss tangent(tan $\delta$), and the viscosity was at the initial stahe, and the more the silica filler was added, and the lower the gel temperature was in the epoxy system. In this study it is concluded that the curing of the silica filled epoxy system was found to be accelerated, as silica was added to the epoxy compound.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.37 no.1
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• pp.56-62
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• 2024

By introducing curing kinetics and chemo-rheology for the epoxy resin formulation for ultra-high voltage gas insulated switchgear (GIS) Insulating Spacers, a study was conducted to simulate the curing behavior, flow and warpage analysis for optimization of the molding process in automatic pressure gelation. The curing rate equation and chemo-rheology equation were set as fixed values for various factors and other physical property values, and the APG molding process conditions were entered into the Moldflow software to perform optimization numerical simulations of the three-phase insulating spacer. Changes in curing shrinkage according to pack pressure were observed under the optimized process conditions. As a result, it was confirmed that the residence time in the solid state was shortened due to the lowest curing reaction when the curing holding pressure was 3 bar, and the occurrence of deformation due to internal residual stress was minimized.

• Proceedings of the Korean Society for Technology of Plasticity Conference
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• 2009.10a
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• pp.323-327
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• 2009

Silicone is recently used for LED chip encapsulment due to its good thermal stability and optical transmittance. In order to predict residual stress which causes optical briefringence and mechanical warpage of silicone, finite element analysis was conducted for both curing and cooling process during silicone molding. For analysis of curing process, a cure kinetics model was derived based on the differential scanning calorimetry(DSC) test and applied to the material properties for finite element analysis. Finite element simulation result showed that the curing as well as the cooling process should be designed carefully so as to reduce the residual stress although the cooling process plays the bigger role than curing process in determining the final residual stress state.

• Transactions of Materials Processing
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• v.24 no.2
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• pp.101-106
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• 2015

Recently, silicone is being used for LED chip lens due to its good thermal stability and optical transmittance. In order to predict residual stresses, which cause optical birefringence and mechanical warpage of silicone, a finite element analysis was conducted for the curing of silicone during molding. For the analysis of the curing process, a dynamic cure kinetics model was derived based on the results of a differential scanning calorimetry (DSC) testing and applied to the material properties for finite element analysis. Finite element simulation results showed that a step cure cycle reduced abrupt reaction heat and showed a decrease in the residual stresses.

• Journal of the Korean Wood Science and Technology
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• v.40 no.2
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• pp.110-122
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• 2012

This study investigated the effects of layered clay on the thermal curing behavior and tensile properties of resole phenol-formaldehyde (PF) resin/clay/cellulose nanocomposites. The thermal curing behavior of the nanocomposite was characterized using conventional differential scanning calorimetry (DSC) and temperature modulated (TMDSC). The addition of clay was found to accelerate resin curing, as measured by peak temperature ($T_p$) and heat of reaction (${\Delta}H$) of the nanocomposite’ curing reaction increasing clay addition decreased $T_p$ with a minimum at 3~5% clay. However, the reversing heat flow and heat capacity showed that the clay addition up to 3% delayed the vitrification process of the resole PF resin in the nanocomposite, indicating an inhibition effect of the clay on curing in the later stages of the reaction. Three different methods were employed to determineactivation energies for the curing reaction of the nanocomposite. Both the Ozawa and Kissinger methods showed the lowest activation energy (E) at 3% clay content. Using the isoconversional method, the activation energy ($E_{\alpha}$) as a function of the degree of conversion was measured and showed that as the degree of cure increased, the $E_{\alpha}$ showed a gradual decrease, and gave the lowest value at 3% nanoclay. The addition of clay improved the tensile strengths of the nanocomposites, although a slight decrease in the elongation at break was observed as the clay content increased. These results demonstrated that the addition of clay to resole PF resins accelerate the curing behavior of the nanocomposites with an optimum level of 3% clay based on the balance between the cure kinetics and tensile properties.

• 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.35 no.3
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• pp.196-202
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• 2011

The cure kinetics of a bisphenol A epoxy resin and polyoxypropylene diamine curing agent system are investigated in both dynamic and isothermal conditions by differential scanning calorimetry (DSC). In dynamic experiments, the shift of exothermic peaks obtained at different heating rates is used to obtain activation energy of overall cure reaction based on the methods of Ozawa and Kissinger. Isothermal DSC data at different temperatures are fitted to an autocatalytic Kamal kinetic model. The kinetic model is in a good agreement with the experimental data in the initial stage of cure. A diffusion effect is incorporated to describe the later stage of cure, predicting the cure kinetics over the whole range of curing process. Also, dynamic mechanical analysis is performed to evaluate the storage modulus and average molecular weight between crosslinkages.