硅改性BPA-PA酚醛环氧树脂导电胶的合成及性能

doi:10.16085/j.issn.1000-6613.2021-1945

摘要/Abstract

摘要：

以双酚A多聚甲醛酚醛树脂（BPA-PA酚醛树脂）、二甲基二甲氧基硅烷和环氧氯丙烷为原料，通过酯交换反应和亲核取代反应得到硅改性BPA-PA酚醛环氧树脂。采用傅里叶变换红外光谱（FTIR）、X射线光电子能谱（XPS）分析进行结构确证。结合非等温DSC、T-β外推直线和FTIR分析研究了最佳固化工艺条件。探讨了不同硅烷添加量对硅改性BPA-PA酚醛环氧树脂性能的影响。最后以硅改性BPA-PA酚醛环氧树脂为基体树脂，加以导电填料和助剂，制备出中温型导电胶。对导电胶进行拉伸剪切强度、体积电阻率和热重测试分析，结果显示：自制硅改性BPA-PA酚醛环氧树脂导电胶拉伸剪切强度达到20.18MPa、体积电阻率达到7.44×10^-4Ω·cm，残炭量达到68.89%。相对市售E-51环氧树脂所制导电胶，自制硅改性BPA-PA酚醛环氧树脂导电胶拉伸剪切强度提高5.73MPa，体积电阻率降低3.86×10^-4Ω·cm，残炭量提高7.49%。

关键词: 硅改性, BPA-PA酚醛环氧树脂, 导电胶, 固化工艺条件, 黏结性能, 导电性能, 耐热性能

Abstract:

Using bisphenol A paraformaldehyde phenolic resin (BPA-PA phenolic resin), dimethyldimethoxysilane and epichlorohydrin as raw materials, silicon-modified BPA-PA phenolic epoxy resin was obtained through transesterification and nucleophilic substitution reactions. FTIR and XPS were used for structural confirmation. Combining non-isothermal DSC, T-β extrapolation line and FTIR analysis, the optimal curing process conditions were studied. The effects of different silane addition levels on the properties of silicon-modified BPA-PA phenolic epoxy resin were discussed. Finally, silicon-modified BPA-PA phenolic epoxy resin was used as the matrix resin, and conductive fillers and additives were added to prepare a medium-temperature conductive adhesive. Conduct tensile shear strength, volume resistivity and thermogravimetric test analysis of its conductive adhesive were tested and analyzed. The results showed that the self-made silicon modified BPA-PA phenolic epoxy resin conductive adhesive had a tensile shear strength of 20.18MPa, a volume resistivity of 7.44×10^-4Ω·cm and a residual carbon content of 68.89%. Compared with the conductive adhesive made of commercially available E-51 epoxy resin, the self-made silicon-modified BPA-PA phenolic epoxy resin conductive adhesive increased tensile shear strength by 5.73MPa and reduced volume resistivity by 3.86×10^-4Ω·cm with increasing amount of residual carbon by 7.49%.

Key words: silicon modified, BPA-PA phenolic epoxy resin, conductive adhesive, curing process conditions, bonding performance, electrical conductivity, heat resistance

中图分类号:

TQ433

郭睿, 李平安, 赵云飞. 硅改性BPA-PA酚醛环氧树脂导电胶的合成及性能[J]. 化工进展, 2022, 41(8): 4473-4480.

GUO Rui, LI Ping’an, ZHAO Yunfei. Synthesis and performance of silicon modified BPA-PA phenolic epoxy resin conductive adhesive[J]. Chemical Industry and Engineering Progress, 2022, 41(8): 4473-4480.

图/表 11

图1 硅改性BPA-PA酚醛环氧树脂的合成及原理

图2 硅改性BPA-PA酚醛环氧树脂的红外光谱

图3 硅改性BPA-PA酚醛环氧树脂的X射线光电子能谱

图4 硅改性BPA-PA酚醛环氧树脂固化反应的非等温DSC曲线

图5 特征温度线性拟合外推直线

图6 混合体系进行不同固化时间的红外光谱

图7 不同硅烷添加量（质量分数）所制硅改性BPA-PA酚醛环氧树脂的TGA曲线

图8 不同硅烷添加量所制硅改性BPA-PA酚醛环氧树脂的SEM

图9 不同硅烷质量分数所制硅改性BPA-PA酚醛环氧树脂的水接触角

图10 硅改性BPA-PA酚醛环氧树脂导电胶的拉伸剪切强度及体积电阻率

图11 硅改性BPA-PA酚醛环氧树脂导电胶的TGA曲线

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