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.
Study on the Curing System of Phenolic Hydroxyl-substituted Spirofluorene-xanthene-type Polyimide-modified Cyanate Ester Resin
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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