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可溶解热塑性聚酰亚胺薄膜的制备和性能研究

Preparation and properties of soluble thermoplastic polyimide films
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摘要 为了改善传统热塑性聚酰亚胺(TPI)的溶液加工性并提高其耐热性和粘接性,采用不同的商品化二酐单体分别与自制的主链含有吡啶和二苯醚结构及活性苯酚侧基或苯侧基的二胺单体通过两步法制备了一系列可溶解热塑性聚酰亚胺(TPI)树脂,随后制备了相应的TPI薄膜以及挠性覆铜板(FCCL)。通过溶解性试验和凝胶渗透色谱(GPC)分析TPI树脂的性能,然后测试分析了TPI薄膜的结构、吸水率、力学性能、热学性能和介电性能,并对其FCCL的相关性能进行测试。结果表明:TPI树脂均能溶解于NMP等强极性有机溶剂,相应薄膜的玻璃化转变温度(T_(g))均为236.8~325.6℃,5%热失重温度(T_(5%))为508.7~553.7℃,800℃残留率(R_(800))均高于64%,热膨胀系数(CTE)为56.36×10^(-6)~78.30×10^(-6)℃^(-1),拉伸强度为64.93~109.18 MPa,断裂伸长率为9.09%~24.60%,吸水率为0.74%~3.75%。综合性能相对较优的TPI-4的介电常数和介质损耗因数也相对较低,相应FCCL的剥离强度达到0.95 N/mm,但只能通过288℃/10 s的耐浮焊测试。此外,TPI-4中极性的苯酚侧基不仅保证了其有机溶解性,对其耐热性和机械强度也有明显的增强作用,同时还降低了其CTE值。具有反应活性的苯酚侧基为TPI的后续化学改性提供了极大的便利,通过加入少量的氰酸酯树脂(CE01)对其进行改性可以明显改善其与热固性PI薄膜或铜箔的粘接性能并提高相应FCCL的耐浮焊性。 In order to improve the solution processability of traditional thermoplastic polyimide(TPI)and enhance its adhesion and heat resistance,several soluble thermoplastic polyimide(TPI)resins were prepared from different commercial dianhydride monomers and self-made diamine monomers with pyridine and diphenyl ether structures and active phenol side groups or benzene side group in the main chain through the two-step method.And then the corresponding TPI films and flexible copper clad laminates(FCCLs)were prepared.The properties of TPI resins were analyzed by solubility test and gel permeation chromatography(GPC).The structure,water absorption,mechanical properties,and dielectric properties of TPI films were tested,and the related properties of the FCCLs were also tested.The results show that all the TPI resins can dissolve in strong polar organic solvents such as NMP,and the glass transition temperature(T_(g))and 5%thermal weight loss temperature(T_(5%))of the corresponding films are in the range of 236.8−325.6℃and 508.7−553.7℃,respectively,and the residue rate at 800℃(R_(800))is higher than 64%.The coefficient of thermal expansion(CTE),tensile strength,elongation at break,and water absorption is in the range of 56.36×10^(-6)−78.30×10^(-6)℃^(-1),64.93−109.18 MPa,9.09%−24.60%,and 0.74%−3.75%,respectively.The dielectric constant and dielectric loss of TPI-4 with better comprehensive properties are also lower than that of other samples,and the peeling strength of the corresponding FCCL reaches 0.95 N/mm,but it can only pass the floating welding test at 288℃for 10 seconds.In addition,the polar phenol side group in TPI-4 not only ensures its organic solubility,but also significantly enhances its heat resistance and mechanical strength,and also reduce its CTE.The existence of reactive phenol side groups provides great convenience for the subsequent chemical modification of TPI.By adding a small amount of cyanate ester resin(CE01)to modify the TPI,the peel strength and the floating welding resistance o
作者 贺娟 牛翔 陈文求 范和平 HE Juan;NIU Xiang;CHEN Wenqiu;FAN Hepin(Hubei Chemistry Research Institute,Jianghan University,Wuhan 430056,China;Haiso Technology Co.,Ltd.,Wuhan 430074,China;Haiso EM(Wuhan)Ltd.,Ezhou 436070,China)
出处 《绝缘材料》 CAS 北大核心 2024年第10期26-33,共8页 Insulating Materials
基金 湖北省科技发展专项(42000023205T000000146)。
关键词 聚酰亚胺 挠性覆铜板 可溶解 热塑性 粘接性 耐热性 polyimide film flexible copper clad laminate soluble thermoplasticity adhesive property heat resistance
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