Study on the Curing System of Phenolic Hydroxyl-substituted Spirofluorene-xanthene-type Polyimide-modified Cyanate Ester Resin
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氰酸酯树脂(cyanate ester resin,CE)具有优异的机械性能、良好的热稳定性和极小的尺寸收缩率,广泛用于电子封装等领域.本文利用合成的酚羟基取代的螺芴-咕吨型全刚性聚酰亚胺(PI-OH)对双酚A型氰酸酯树脂(bisphenol A cyanate ester,BADCy)进行改性.研究发现,PI-OH侧链上的酚羟基可以显著降低BADCy的固化温度,与未改性树脂相比,固化放热峰值温度降低了约142 ℃.室温下,PI-OH(10％)/BADCy的储能模量和杨氏模量分别为2614 MPa和5010 MPa,与纯BADCy相比,分别提高了34％和10.2％.此外,PI-OH(8％)/BADCy的拉伸强度和拉伸模量分别提高了63.9％和128.4％,虽然玻璃化转变温度(Tg)略有下降,但其热降解温度(Td5％)和统计耐热指数(Ts)均得到提升.同时,由于PI-OH侧链含有大量疏水性的三氟甲基基团,PI-OH(10％)/BADCy体系的吸水率仅为0.73％,降低了47.9％.这一进展对于降低BADCy树脂的固化温度、制备具有良好热稳定性和机械性能的氰酸酯树脂材料具有重要意义.
Cyanate ester resins(CE),which have excellent mechanical properties,good thermal stability and very small dimensional shrinkage,are widely used in electronic packaging and other fields.In this study,the synthesized phenolic hydroxyl-substituted spirofluorene-xanthene-type fully rigid polyimide(PI-OH)was used to modify bisphenol A-type cyanate ester resin(BADCy).It was found that the phenolic hydroxyl groups on the side chain of PI-OH could significantly reduce the curing temperature of BADCy,and the peak exothermic temperature of curing was reduced by about 142 ℃ compared with that of the unmodified resin.At room temperature,the energy storage modulus and Young's modulus of PI-OH(10％)/BADCy were 2614 MPa and 5010 MPa,respectively,which were increased by 34％and 10.2％,respectively,compared with those of pure BADCy.In addition,the tensile strength and tensile modulus of PI-OH(8％)/BADCy were increased by 63.9％and 128.4％,respectively,and its thermal degradation temperature(Td5％)and statistical heat resistance index(Ts)were enhanced,although the glass transition temperature(Tg)was slightly decreased.Meanwhile,the water absorption of the PI-OH(10％)/BADCy system was only 0.73％,which was reduced by 47.9％,due to the large number of hydrophobic trifluoromethyl groups in the side chain of PI-OH.This progress is of great importance for the production of low-temperature curable cyanate ester resin materials with good thermal stability and mechanical properties.
Phenol hydroxyl polyimideBisphenol A cyanate esterCuring temperatureHigh temperature resistance
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