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主管单位 中华人民共和国
工业和信息化部
主办单位 中国材料研究学会
哈尔滨工业大学
主编 苑世剑 国际刊号ISSN 1005-0299 国内刊号CN 23-1345/TB

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引用本文:马馨雨,刘立柱,张笑瑞,吕彤.热塑性共聚聚酰亚胺薄膜的合成及性能研究[J].材料科学与工艺,2019,27(3):47-52.DOI:10.11951/j.issn.1005-0299.20180030.
MA Xinyu,LIU Lizhu,ZHANG Xiaorui,LÜ Tong.Synthesis and performance of thermoplastic copolyimide film materials[J].Materials Science and Technology,2019,27(3):47-52.DOI:10.11951/j.issn.1005-0299.20180030.
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热塑性共聚聚酰亚胺薄膜的合成及性能研究
马馨雨1,刘立柱1,2,张笑瑞1,2,吕彤1
(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)
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1 780、1 720、1 500、1 380、1 050和725 cm-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760 nm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.
关键词:  共聚聚酰亚胺  热塑性  溶解性  耐热性  透光率
DOI:10.11951/j.issn.1005-0299.20180030
分类号:O631.1
文献标识码:A
基金项目:
Synthesis and performance of thermoplastic copolyimide film materials
MA Xinyu1, LIU Lizhu1,2, ZHANG Xiaorui1,2, Lü Tong1
(1. School of Materials Science and Engineering, Harbin University of Science and Technology, Harbin 150040, China; 2. Key Laboratory of Engineering Dielectric and Its Application,Ministry of Education(Harbin University of Science and Technology), Harbin 150080, China)
Abstract:
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.
Key words:  copolyimide  thermoplastic  solubility  heat resistance  transmittance

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