• Composites Research
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• v.37 no.5
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• pp.393-401
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• 2024

Epoxy is a thermosetting polymer with excellent properties such as heat and chemical resistance, making them essential in various industrial fields including electronics. The performance of epoxy is highly dependent on the type of curing agent used. Among them, sulfonium-based latent curing agents are notable for their fast curing speed, high curing hardness, and specificity to certain temperatures, making them attractive for manufacturing anisotropic conductive films in electronic materials where single-component epoxy is required. However, sulfonium-based latent curing agents face challenges in industrial application due to issues with low yield and purity. This study optimized the synthesis conditions for benzyl and naphthyl-type sulfonium curing agents (B-Sul⁺SbF6^-, N-Sul⁺NCyF^-, N-Sul⁺NFSI^-). By adjusting reaction time, reaction temperature, and reactant ratios, yield was maximized, significantly reducing both reaction time and temperature. The three optimized curing agents were evaluated for their thermal and mechanical properties to assess curing behavior and storage stability. The results confirmed that stable curing performance was maintained even after mixing. This study aims to expand the industrial applicability of sulfonium curing agents.

• 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.

• Polymer(Korea)
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• v.25 no.2
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• pp.168-176
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• 2001

The effect of novel N-crotyl-N,N-dimethyl-4-methylanilinium hexafluoroantimonate (CMH) curing agent as a thermal latent initiator on thermal behaviors, rheological properties, and thermal stability of diglycidylether of bisphenol A (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 at a given temperature. The conversion and conversion rate of DGEBA/CMH system increased with increasing the concentration of initiator, due to high activity of CMH. Rheological properties of the system were investigated under isothermal condition using a rheometer The gelation time was obtained from the analysis of storage modulus (G'), loss modulus (G"), and damping factor (tan $\delta$). As a result, the reduction of gelation time was affected by high curing temperature and concentration of CMH, resulting in high degree of network formation in cationic polymerization, due to difference of activity. The thermal stability of the cured epoxy resin was discussed in terms of the activation energy for decomposition and thermal factors determined from TGA measurements.ents.

• Polymer(Korea)
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• v.34 no.3
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• pp.191-197
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• 2010

To improve the curing method of anisotropic conductive film (ACF) at low temperature, it was studied to replace the thermal latent curing agent of imidazole compounds by the curing agent of cationically initiating type. Thermo-mechanical properties such as glass transition temperature, storage modulus, and coefficient of thermal expansion were investigated for the analysis of curing behavior. The reliability of ACF were observed in thermal cycle and high temperature-high humidity test. ACF using cationic initiator showed faster curing, lower CTE, and higher $T_g$ than the case of using imidazole curing agent, which is important for the high temperature stability. Furthermore, ACF using cationic initiator maintained a stable contact resistance in reliability test, although it was cured at low temperature and fast rate. With these results, it was confirmed that the curing method of epoxy had great effect on thermo-mechanical properties and reliability of ACF.

• 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.

• Applied Chemistry for Engineering
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• v.7 no.5
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• pp.963-969
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• 1996

Cure characteristics of DGEBA(diglycidyl ether of bisphenol A)/dicy(dicyandiamide) system containing diuron(3-(3,4-dichloro phenyl) -1,1-dimethylurea) as an accelerator was investigated. The system has shelf life of six months because dicy is insoluble in liquid/solid resins at room temperature. It is generally known that dicy is an adequate curing agent for one component adhesive due to its highly latent property. With increasing the amount of added dicy, reaction heat of DGEBA/dicy system increased and degree of conversion was not varied. For DGEBA/dicy/diuron system, cure temperature decreased about $40^{\circ}C$ and cure reaction became fast by the addition of diuron which activates dicy. $T_g$ of the mixed resin decreased with the amount of accelerator. which was interpreated with molecular structure forming loose chain. Cure kinetics of DGEBA/dicy and DGEBA/dicy/diuron system were explained using Kamal's autocatalytic reaction model. The effect of acceleration was confirmed with that reaction model.

• Proceedings of the International Microelectronics And Packaging Society Conference
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• 2005.09a
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• pp.201-212
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• 2005

[ $Epoxy/BaTiO_3$ ] composite embedded capacitor films (ECFs) were newly designed fur high dielectric constant and low tolerance (less than ${\pm}15\%$) embedded capacitor fabrication for organic substrates. In terms of material formulation, ECFs are composed of specially formulated epoxy resin and latent curing agent, and in terms of coating process, a comma roll coating method is used for uniform film thickness in large area. Dielectric constant of $BaTiO_3\;&\;SrTiO_3$ composite ECF is measured with MIM capacitor at 100 kHz using LCR meter. Dielectric constant of $BaTiO_3$ ECF is bigger than that of $SrTiO_3$ ECF, and it is due to difference of permittivity of $BaTiO_3\;and\;SrTiO_3$ particles. Dielectric constant of $BaTiO_3\;&\;SrTiO_3$ ECF in high frequency range $(0.5\~10GHz)$ is measured using cavity resonance method. In order to estimate dielectric constant, the reflection coefficient is measured with a network analyzer. Dielectric constant is calculated by observing the frequencies of the resonant cavity modes. About both powders, calculated dielectric constants in this frequency range are about 3/4 of the dielectric constants at 1 MHz. This difference is due to the decrease of the dielectric constant of epoxy matrix. For $BaTiO_3$ ECF, there is the dielectric relaxation at $5\~9GHz$. It is due to changing of polarization mode of $BaTiO_3$ powder. In the case of $SrTiO_3$ ECF, there is no relaxation up to 10GHz. Alternative material for embedded capacitor fabrication is $epoxy/BaTiO_3$ composite embedded capacitor paste (ECP). It uses similar materials formulation like ECF and a screen printing method for film coating. The screen printing method has the advantage of forming capacitor partially in desired part. But the screen printing makes surface irregularity during mask peel-off, Surface flatness is significantly improved by adding some additives and by applying pressure during curing. As a result, dielectric layer with improved thickness uniformity is successfully demonstrated. Using $epoxy/BaTiO_3$ composite ECP, dielectric constant of 63 and specific capacitance of 5.1nF/cm2 were achieved.