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DPSBCB单体的合成表征及聚合物的热性能和成膜性能

Synthesis of DPSBCB and Thermostability and Film-Forming Property of Its Polymers

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【作者】 黄学亮朱方华杨军校张林谢如刚

【Author】 Xueliang Huang1,2,3,Fanghua Zhu1,Junxiao Yang2,Lin Zhang1,Rugang Xie4(1.Research Center of Laser Fusion,China Academy of Engineering Physics,Mianyang 621900,China;2.School of Materials Science and Engineering,Southwest University of Science and Technology,China;3.Laboratory for Matter Characteristic Research at Extreme Condition,Southwest University of Science and Technology,Mianyang 621010,China;4.Department of Chemistry,Sichuan University,Chengdu 610064,China)

【机构】 中国工程物理研究院激光聚变研究中心西南科技大学材料科学与工程学院西南科技大学极端条件物质特性实验室四川大学化学学院

【摘要】 以4-溴苯并环丁烯(4-BrBCB)和烯丙基溴(ABr)为原料,利用Grignard反应一步法合成出4-烯丙基苯并环丁烯(4-ABCB)单体,并通过硅氢加成反应,成功地将硅氧烷引入到BCB单体中,合成出1,3-二(3-苯并环丁烯基丙基)-1,1,3,3-四甲基二硅氧烷(DPSBCB)单体。单体结构利用红外光谱(FT-IR)、核磁共振(1H-NMR、13C-NMR)等进行了表征和确认。DPSBCB单体在热引发条件下开环聚合得到具有一定交联度的可溶性预聚体。最后利用旋涂法制备出聚合物薄膜,分析了聚合物的成膜性能和热性能,结果显示,薄膜的均方根粗糙度(RMS)为0.79 nm,聚合物初始分解温度为445℃。说明DPSBCB聚合物具有良好的成膜性能和优异的热稳定性。

【Abstract】 4-bromobenzocyclobutene and allyl bromide were employed to afford the monomer of 4-allylbenzocyclobutene by Grignard reaction in one-step.The siloxane was introduced into the monomer of BCB to preparation 1,3-bis(3-benzocyclobutenyl propyl)-1,1,3,3-tetramethyl disiloxane(DPSBCB) via hydrosilylation reaction.The structures of the monomers were characterized and confirmed by Fourier transform infrared spectrum(FT-IR),nuclear magnetic resonance spectrum(1H-NMR and 13C-NMR).The prepolymerization reaction of DPSBCB was carried out by thermal initiation to give the soluble prepolymer with some crosslink degree.The thermostability and film-forming property of the film prepared from the prepolymer by spin-coating method were analyzed by thermogravimetry and atomic force microscopy.The results show that the root-mean square(RMS) roughness is 0.79 nm,and the starting mass loss temperature is about 445 ℃.It indicate that DPSBCB exhibits good film-forming property and excellent thermal stability.

【基金】 国家高技术863基金(2009AA8-441011);中国工程物理研究院科学技术发展基金(2008A0302014)
  • 【文献出处】 高分子材料科学与工程 ,Polymer Materials Science & Engineering , 编辑部邮箱 ,2012年04期
  • 【分类号】TQ320.1
  • 【下载频次】152
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