• Carbon letters
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• v.14 no.1
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• pp.58-61
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• 2013

In this work, the effect of catalysts on the mechanical properties of carbon fibers-reinforced epoxy matrix composites cured by cationic latent thermal catalysts, i.e., N-benzylpyrazinium hexafluoroantimonate (BPH) was studied. Differential scanning calorimetry was executed for thermal characterization of the epoxy matrix system. Mechanical interfacial properties of the composites were studied by interlaminar shear strength (ILSS), critical stress intensity factor ($K_{IC}$), and specific fracture energy ($G_{IC}$). As a result, the conversion of neat epoxy matrix cured by BPH was higher than that of one cured by diaminodiphenyl methane (DDM). The ILSS, $K_{IC}$, $G_{IC}$, and impact strength of the composites cured by BPH were also superior to those of the composites cured by DDM. This was probably the consequence of the effect of the substituted benzene group of BPH catalyst, resulting in an increase in the cross-link density and structural stability of the composites studied.

• The Korean Journal of Rheology
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• v.10 no.2
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• pp.92-97
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• 1998

열잠재성 경화제인 N-benzylpyrazinium hexafluoroantimonate (BPH)를 이용하여 함 량에 따른 DGEBA계 에폭시 수지의 경화반응에서의 유변학적 특서 및 반응속도를 연구하 였다. 경화시의 활성화 에너지를 Barrett 방법을 이용한 동적 DSC 측정방법으로 조사 하였 다. DSC 실험 결과 BPH의 함량이 증가할수록 활성화 에너지는 감소함을 알수 있었다. Rheomter를 이용하여 DGEBA/BPH 계의 유변학적 특성을 등온경화와 tdmdhsrud화 조건하 에서 살펴보았다. BPH의 함량이 증가함에 따라 겔화점 도달시간 빠르게 나타나는데 이는 낮아진 활성화 에너지에 기인한 것으로 사료된다. 두 번째 damping 피크를 이용하여 유리 화점을 측정하여 Time-Temperature-Transformation (T-T-T) cure diagram을 작성한 결 과 열잠재성 경화제의 특성인 일정온도 이상에서 활성이 나타남을 확인할수있었다.

• 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.

• 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.

• Composites Research
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• v.17 no.5
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• pp.47-53
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• 2004

In this work, two thermal latent catalysts, i.e., N-benzylpyrazinium hexafluoroantimonate (BPH) and benzyl-2,5-dimethylpyrazinium hexafluoroantimonate (BDPH), were synthesized. The cure behaviors and thermal stabilities of diglycidylether of bisphenol A (DCEBA) epoxy resins initiated by 1 wt.% of the catalysts were investigated by DSC, NIR, TCA, and DMA Latent properties of the catalysts were examined by conversion of epoxy resins using NIR from $100^{\circ}C$ to $180^{\circ}C$ From the resultes of near-IR, DGEBA/BPH system showed higher conversion than that of DGEBA/BDPH system. The thermal stabilities of DGEBA/BDPH system based on the initial decomposition temperature (IDT) and integral procedural decomposition (IPDT) were relatively lower than those of DCEBA/BPH system. These could be attributed to the hindered structure of BDPH, resulting in decreasing the thermal stability in the DGEBA/BDPH 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.

• Macromolecular Research
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• v.10 no.1
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• pp.34-39
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• 2002

Cure behavior of an epoxy resin was investigated at different cure temperatures (110, 120, 130, 140, and 150 $^{\circ}C$) and cure times in the presence of 2 wt% of an N-benzylpyrazinium hexafluoroantimonate (BPH) cationic catalyst by means of differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA). The glass transition temperature ( $T_{g}$) and chemical conversion (x) at the different temperatures were determined from DSC thermograms. The $T_{g}$ and x vs. In time data were superposed up to $T_{g}$ = 10$0^{\circ}C$ and x = 0.70 by shifting horizontally at a reference temperature of $T_{g}$ = 13$0^{\circ}C$. It is interesting that the $T_{g}$ and x of the superposed data increase rather slowly in the early stage of cure and rapidly thereafter. Therefore, the increase of the $T_{g}$ and x can be divided into two regions; $R_{I}$= -18.4(= $T_{go}$ ) ~5$^{\circ}C$ and $R_{II}$ = 5 ~ 10$0^{\circ}C$ in $T_{g}$, and $R_{I}$ : 0~0.24 and $R_{II}$ : 0.24~0.70 in x. The $R_{I}$ is closely related to the initiation reactions between BPH and epoxy and between hydroxy group and epoxy in this epoxy/catalyst system. From the kinetic analysis of the $T_{g}$-shift, activation energy was 12.5 kcal/mol. The relationship between $T_{g}$ and x was also considered. The gelation and vitrification times for different cure temperatures were obtained from DMA curves.urves. DMA curves.urves.

• Elastomers and Composites
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• v.39 no.1
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• pp.42-50
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• 2004

In this work, the diglycidylether of bisphenol A (DGEBA) and modified polyurethane (PU) blends were initiated by N-benzylpyrazinium hexafluoroantimonate (BPH). The cure and fracture toughness of neat DGEBA with the addition of PU were investigated. The cure properties of DGEBA/PU blend system were examined by DSC and near-IR measurements. The fracture touhtness were investigated by measuring the critical stress intensity factor ($K_{IC}$) and the critical strain energy release rate ($G_{IC}$). According to the results, the maximum values of owe activation energy ($E_a$) and conversion (${\alpha}$) were found at 10 phr of PU. Also the $K_{IC}$ showed a similar behavior with the results of conversion. These results were probably due to increase of crosslinking density in the blends resulted from increase of the hydrogen bonding between the hydroxyl groups of DGEBA and isocyanate groups of PU.

• Composites Research
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• v.35 no.2
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• pp.53-60
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• 2022

This study uses Diglycidyl ether of terephthalylidene-bis-(4-amino-3-methylphenol) (DGETAM), an amine hardener 4,4'-diaminodiphenylethane (DDE) and cationic catalyst N-benzylpyrazinium hexafluoroantimonate (BPH) to make epoxy film. For analysis, ¹H_NMR and FT-IR were used to verify proper synthesis, and the liquid crystallinity of DGETAM was checked using Differntial Scanning Calorimetry and Polarized Optical Microscopy. Thermal conductivity of the sample was measured using Laser Flash Apparatus. Thermal stability as well as thermal conductivity is important when used as a packaging material. Activated energy is the energy needed to generate a response, which can be used to estimate the energy required to maintain physical properties. It was obtained using the Arrhenius equation based on the data measured by isothermal decomposition using Thermogravimetric Analysis. Measurement of the thermal conductivity of epoxy films showed higher thermal conductivity when DDE was used, and it was found that thermal conductivity had an effect on thermal stability, given that it represented an activation energy similar to a film with BPH upon 5% decomposition.

• Polymer(Korea)
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• v.24 no.1
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• pp.65-71
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• 2000

The latent properties and cure kinetics of an acid anhydride-cured epoxy resin have been investigated by a near-infrared (NIR) reflection spectroscopy. The assignments of the latent properties and cure behaviors were performed by the measurements of the NIR reflectance for epoxide and hydroxyl groups at different temperatures. A comprehensive analysis of the origin, location, and shifts during reaction of all major NIR absorption peaks in the spectral range from 4000 to 7100 $cm^{-1}$ / was provided. The extent of reaction was determined from NIR absorption band at the 4530 $cm^{-1}$ / depending on epoxide concentration and cure temperature.