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作 者:马馨雨 刘立柱[1,2] 张笑瑞[1,2] 吕彤 MA Xinyu;LIU Lizhu;ZHANG Xiaorui;LV Tong(School of Materials Science and Engineering,Harbin University of Science and Technology,Harbin 150040,China;Key Laboratory of Engineering Dielectric and Its Application,Ministry of Education(Harbin University of Science and Technology),Harbin 1580080,China)
机构地区:[1]哈尔滨理工大学材料科学与工程学院,哈尔滨150040 [2]工程电介质及其应用教育部重点实验室(哈尔滨理工大学),哈尔滨150080
出 处:《材料科学与工艺》2019年第3期47-52,共6页Materials Science and Technology
摘 要:以2,2′-二甲基-4,4′-二氨基联苯(m-TB)为二胺单体,均苯四甲酸二酐(PMDA)和3,3′,4,4′-联苯四甲酸二酐(BPDA)为二酐单体,N,N′-二甲基乙酰胺(DMAc)为溶剂,采用常规的两步法制备了一系列不同二酐比例的热塑性聚酰亚胺,并通过红外光谱仪、X-射线衍射仪、热重分析仪、紫外光谱仪、动态热分析仪、溶解性测试等对共聚聚酰亚胺的结构和性能进行表征.结果表明:在1780、1720、1500、1380、1050和725cm^-1处出现明显的吸收峰,说明成功制备了聚酰亚胺材料;共聚聚酰亚胺只在PMDA与BPDA物质的量比为0.2∶0.8时存在结晶峰,其他比例时均为非晶聚合物;亚胺化后的共聚聚酰亚胺在DMSO、DMAc、DMF、NMP和m-cresol中有溶解性,证明成功制备出热塑性聚酰亚胺薄膜;热塑性共聚PI起始分解温度大于500℃,800℃时的质量保持率在50%以上,具有良好的热稳定性;随着聚合物中BPDA含量的提高,热塑性聚酰亚胺薄膜的玻璃化转变温度呈现下降的趋势.当紫外光波长达到400 nm时,薄膜的透光率高达57.6%,当波长为760nm时,薄膜透光率均达到100%,成功制备了透光率较高的聚酰亚胺薄膜.A series of thermoplastic copolyimides with different dianhydride ratios were synthesized via the conventional two-step method by using 2,2′-dimethyl-4,4′-diaminobiphenyl(m-TB) as the diamine monomer, and pyromellitic dianhydride(PMDA) and 3,3′,4,4′-biphenyl tetracarboxylic dianhydride(BPDA) as the dianhydride monomer in N,N-dimethylacetamide. The structure and properties of the copolymerized polyimide were characterized by infrared spectrometer, X-ray diffractometer, thermogravimetric analyzer, ultraviolet spectrometer, dynamic thermal analyzer, and solubility test.Results show that there was obvious absorption at 1 780, 1 720, 1 500, 1 380, 1 050, and 725 cm^-1,indicating thatthe polyimide material was successfully prepared. The copolymerized polyimide only had a crystallization peak when the ratio of PMDA to BPDA was 0.2∶0.8, whilethe other proportions were all amorphous polymers. The imidized copolyimide had solubility in DMSO, DMAc, DMF, NMP, and m-cresol, suggesting that the thermoplastic polyimide film was successfully prepared. The thermoplastic copolyimide had good thermal stability when the initial decomposition temperature was higher than 500 ℃, and the residue at 800 ℃ was above 50%. With the increaseof BPDA content in the polyimide, the glass transition temperature showeda downward trend. The transmittance of the films reached 57.6% and 100% when the wavelength of ultraviolet light reached 400 nm and 760 nm, indicating that the polyimide film with high transmittance was successfully prepared.
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