可交联氟化氮杂环聚芳醚的合成及性能  

Synthesis and Properties of Crosslinkable Fluorinated N-Heterocyclic Polyarylether

作　　者：李闯[1,2] 刘秀利 宗立率[1,2] 苑博 王锦艳 蹇锡高[1,2] Chuang Li;Xiuli Liu;Lishuai Zong;Bo Yuan;Jinyan Wang;Xigao Jian(State Key Laboratory of Fine Chemicals,Dalian University of Technology,Dalian 116024,China;Engineering Research Center of Advanced Polymer and Composite Materials,Ministry of Education,Dalian 116024,China;The 10th Research Institute of China Electronics Technology Group Corporation,Chengdu 610036,China)

机构地区：[1]大连理工大学精细化工国家重点实验室,辽宁大连116024 [2]先进高分子及复合材料教育部工程研究中心,辽宁大连116024 [3]中国电子科技集团公司第十研究所,四川成都610036

出　　处：《高分子材料科学与工程》2021年第11期13-21,共9页Polymer Materials Science & Engineering

基　　金：国家自然科学基金-青年基金资助项目(51903028);中国博士后基金面上项目(2017M611217)。

摘　　要：以4-(4-羟基苯基)-2,3-二氮杂萘酮-1-酮(DHPZ)、双酚AF(6F-BPA)、五氟苯乙烯(FSt)和十氟联苯(DFBP)为原料,通过溶液缩聚反应合成了可交联的FSt-FPPE,所得共聚物的结构通过红外光谱和核磁共振确认与设计一致。FStFPPE呈无定形结构,可溶解在N-甲基吡咯烷酮、N,N-二甲基乙酰胺、N,N-二甲基甲酰胺、氯仿、四氢呋喃等有机溶剂中。与交联剂三聚氰酸三烯丙酯(TAC)进行共固化后,聚合物的玻璃化转变温度由235℃提升至255℃。氮气下热分解温度达497℃,800℃时残碳率为53%。固化后聚合物薄膜的拉伸强度为60~67 MPa,拉伸模量为1.05~1.23GPa,断裂伸长率为10%~12%。当TAC含量为1%时,拉伸强度达到最大值67MPa。在介电性能上,固化后介电常数降低,在10MHz~1GHz的频率下,介电常数在2.4~3.0之间。当TAC含量为3%时,介电常数达到最低值2.4。这些结果表明,FSt-FPPE具有优异的综合性能,在微电子领域中具有一定应用价值。Based on 4-(4-hydroxyphenyl)-2,3-phthalazinone-1-one(DHPZ),bisphenol AF(6 F-BPA),pentafluorostyrene(FSt)and decafluorobiphenyl(DFBP),novel crosslinkable FSt-FPPE was synthesized through solution polycondensation reaction,and the structure of the obtained copolymer was confirmed by FT-IR and ^(1)H-NMR.The resulting FSt-FPPE exhibits amorphous nature and can be dissolved in organic solvents such as NMP,DMAc,DMF,CHCl_(3) and THF.After curing by introducing crosslinking agent triallyl cyanurate(TAC),the glass transition temperature of the resultant thermosets is increased from 235℃to 255℃.The thermal decomposition temperature in nitrogen could reach 497℃,and the residual carbon rate at 800℃is 53%.After curing,the tensile strength of the polymer film is 60~67 MPa with the tensile modulus of 1.05~1.23 GPa,and the elongation at break of 10%to 12%.When the TAC content is 1%,the tensile strength reaches the maximum value of 67 MPa.In terms of dielectric properties,the dielectric constant is decreased after curing,and the dielectric constant is between 2.4~3.0 at a frequency of 10 MHz~1 GHz.When the TAC content is 3%,the dielectric constant reaches the lowest value of 2.4.The results evidently suggest FPPEs as commendable candidate for those high-tech electronic applications.

关 键 词：低介电常数 低介电损耗 聚芳醚 杂萘联苯 氟化 

分 类 号：TQ326.53[化学工程—合成树脂塑料工业]