一种PI感光干膜的制备与性能

Preparation and properties of PI photosensitive dry film

为开发一种分辨率高、力学性能优异的聚酰亚胺(PI)感光干膜,首先采用4,4'-联苯醚二酐(ODPA)与2,2-双(3-氨基-4-羟基苯基)六氟丙烷(BAHF)等合成了碱溶性PI树脂。再将该树脂与交联剂、引发剂、偶联剂等进行复配,制备了光敏性PI胶液,最后将该光敏性PI胶液涂布在载体聚对苯二甲酸乙二酯(PET)薄膜上,经烘干、冷却,覆上聚乙烯膜(PE膜),获得PI感光干膜。利用凝胶渗透色谱、傅里叶变换红外光谱、光学显微镜等对碱溶性PI树脂和感光干膜的性能进行表征。结果表明,成功制备碱溶性PI树脂,亚胺化率为82%,厚度为15μm的PI感光干膜经曝光显影后具有优异的分辨率,为10μm。通过动态热机械分析仪、热重分析等对200℃固化的PI感光干膜的力学性能、耐热性和耐药性进行了研究。结果表明,200℃固化的感光干膜在30℃时的拉伸强度达到101 MPa,断裂伸长率达到7.3%,5%热失重温度为352℃,10%热失重温度为385℃,在590℃的质量保持率为44%,并且在丙酮、N-甲基吡咯烷酮、30%HNO_(3),30%H_(2)SO_(4),1%HF等试剂中的质量变化率均小于1%。综上,PI感光干膜具有优异的分辨率、热稳定性和耐药性。

In order to develop a kind of polyimide(PI)photosensitive dry film with high resolution and excellent mechanical properties,alkali-soluble PI resin was synthesized by using 4,4'-diphenyl ether dianhydride(ODPA)and 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane(BAHF).The photosensitive polyimide adhesive was prepared by mixing the resin with crosslinking agent,initiator and coupling agent.Finally,the photosensitive polyimide was coated on the carrier polyethylene terephthalate(PET)film,after drying,cooling,coated with polyethylene(PE)film,polyimide photosensitive dry film was obtained.The properties of alkali-soluble polyimide resin and photosensitive dry film were characterized by gel permeation chromatography,Fourier transform infrared spectroscopy and microscope.The results show that alkali-soluble polyimide resin is successfully prepared,and the imidization rate is 82%.The PI photosensitive dry film with a thickness of 15μm shows excellent resolution after exposure and development.The mechanical properties,heat resistance and drug resistance of photosensitive dry film cured at 200℃are studied by dynamic thermomechanical analysis and thermogravimetric analysis.The results show that the tensile strength of the film cured at 200℃reaches 101 MPa at 30℃,the elongation at break reaches 7.3%,the thermal weight loss temperature of 5%is 352℃,the thermal weight loss temperature of 10%is 385℃,and the quality retention rate of the film at 590℃is 44%.The mass change rates in acetone,N-methylpyrrolidone,30%HNO_(3),30%H_(2)SO_(4) or 1%HF are all less than 1%.In summary,the photosensitive dry film has excellent resolution,thermal stability and drug resistance.