苯并噁嗪树脂的应用研究进展

针对苯并噁嗪树脂的工业应用,综述了近年来苯并噁嗪树脂的单体合成、树脂改性及固化研究的现状.     

苯并噁嗪树脂的合成及应用

本文综述了苯并 口恶嗪树脂的合成、性能、改性和应用。     

单环苯并噁嗪树脂热解的ReaxFF反应动力学模拟

采用ReaxFF动力学方法模拟了非交联固化单环苯并噁嗪树脂在不同温度下的热解特性。模拟结果表明,N桥键的断裂是热解的主要引发反应,H_2,H_2O和大分子碳团簇是热解的主要产物。随着反应温度升高,H_2的数量急剧增加,而H_2O的数量反而降低,高温有利于促进相对分子质量较大的碳团簇的形成,还观察到了CO,NH_3,N_2和HCN等小分子产物。用ReaxFF动力学方法模拟所得的气体产物以及含类似石墨烯结构的碳团簇与实际实验结果一致,ReaxFF动力学模拟方法可以作为一种研究苯并噁嗪树脂高温热解反应的有效途径。     

苯并噁嗪树脂的研究与应用进展

3,4-二氢-3-取代基-2H-1,3-苯并噁嗪(简称苯并噁嗪),是一类新型的高性能热固性树脂,在加热和(或)催化剂的作用下发生开环聚合,生成含氮且类似酚醛树脂的网状结构,人们将这种新型树脂称作开环聚合酚醛树脂.自上世纪九十年代初以来,有关苯并噁嗪的研究工作取得了快速发展.本文较系统概述了国内外在苯并噁嗪中间体的合成、固化反应、结构与性能关系、应用开发等方面取得的进展,侧重介绍了四川大学在苯并噁嗪研究和应用方面取得的成果.     

苯并(噁)嗪树脂体系在湿法缠绕工艺中的应用研究

采用旋转黏度计测定了苯并(口恶)嗪(BZ)树脂体系的黏度-温度曲线以及黏度-时间曲线,并计算BZ体系的固化动力学参数,从而确定固化工艺;在特定固化工艺条件下将BZ树脂初步缠绕内径60mm的碳管,测试其相关的力学性能,为BZ树脂体系应用于湿法缠绕工艺提供一定的依据。测试结果表明,该树脂体系室温下黏度为0.35Pa·s,满足湿法缠绕工艺的要求;固化工艺参数T_i=173℃,T_p=197℃,T_f=214℃,而固化制度为100℃/1h+120℃/1h+140℃/1h+160℃/1h+180℃/2h+200℃/2h;碳管的水压测试达到19MPa。     

双酚A型苯并噁嗪与酚醛型环氧树脂共混体系的固化反应与热性能

将双酚A型苯并噁嗪(Ba)和酚醛型环氧树脂(F-51)按照不同的质量比进行熔融共混,并固化制备了浇铸体。研究结果表明:环氧树脂的加入降低了苯并噁嗪的黏度,改善了苯并噁嗪的加工工艺性。随着环氧树脂含量的增加,Ba/F-51共混体系的DSC固化反应峰值温度向高温方向移动。在F-51环氧树脂的加入量低于50%的范围内,随环氧树脂加入量增加,Ba/F-51共混树脂的交联密度和玻璃化转变温度均有明显提高,其中Ba/F-51=1.5体系的Tg最高为173.4℃,比纯苯并噁嗪提高了17.4℃。     

苯并噁嗪树脂的共混改性研究进展

综合论述了针对苯并(口恶)嗪树脂的共混改性研究进展,分别从热固性树脂、热塑性树脂、橡胶和聚氨酯弹性体等4个方面,对苯并(口恶)嗪树脂所进行的改性研究情况进行了论述.     

氧化石墨烯原位合成苯并噁嗪树脂改性材料的制备

本文采用原位合成法制备氧化石墨烯／苯并噁嗪树脂改性材料,初步对复合材料的傅里叶红外光谱、微观结构以及其性能肖氏硬度和抗压强度进行了探讨。结果表明,由苯并噁嗪树脂和氧化石墨烯／苯并噁嗪材料红外分析对比分析,氧化石墨烯有利于材料的合成和交联,而从金相显微镜对材料表面观察发现,过量的氧化石墨烯加入对复合材料的抗压强度整体性能有一定程度的影响;氧化石墨烯／苯并噁嗪树脂改性材料的肖氏硬度随氧化石墨烯含量增加而增大,且明显改善材料的硬度,在加入0．3％氧化石墨烯后,材料肖氏硬度可达到35H以上,抗压强度也有明显改善,在加入0．1％的氧化石墨烯后材料的抗压强度可以达到15．8MPa,氧化石墨烯的加入能有效的改善材料的性能。     

氨基丁腈橡胶改性苯并噁嗪树脂的研究

用氨基封端的液体丁腈橡胶(ATBN)对苯并噁嗪树脂(BB)进行改性,通过研究不同配比ATBN/BB体系的性能,确定了随ATBN含量增加,共混体系的黏度和固化行为、固化产物的相形态、固化物的机械性能和耐热性能的变化规律。     

低介电常数聚合物研究进展

本文介绍了降低聚合物介电常数的方法,原理.对有机和杂化聚合物在低介电常数材料方面的应用作了分类介绍.对各类聚合物列举了合成实例,并简要介绍了聚合物的介电常数和热性能.     

Porous low dielectric constant materials for microelectronics

Materials with a low dielectric constant are required as interlayer dielectrics for the on-chip interconnection of ultra-large-scale integration devices to provide high speed, low dynamic power dissipation and low cross-talk noise. The selection of chemical compounds with low polarizability and the introduction of porosity result in a reduced dielectric constant. Integration of such materials into microelectronic circuits, however, poses a number of challenges, as the materials must meet strict requirements in terms of properties and reliability. These issues are the subject of the present paper.     

POSS基低介电常数多孔薄膜的制备与性能研究

通过4，4’-二（4-烯丙氧基苯甲酸）苯酯与POSS分子的硅氢化反应，合成了POSS交联聚合物。用FTIR、XRD对聚合物结构进行了表征，利用椭偏仪测量了薄膜的折射率和介电常数。通过改变单体与POSS投料摩尔比，可制备出k＜2.5的低介电常数薄膜。     

Mechanical characterization of zeolite low dielectric constant thin films by nanoindentation

With semiconductor technologies continuously pushing the miniaturization limits, there is a growing interest in developing novel low dielectric constant materials to replace the traditional dense SiO₂ insulators. In order to survive the multi-level integration process and provide reliable material and structure for the desired integrated circuits (IC) functions, the new low-k materials have to be mechanically strong and stable. Therefore the material selection and mechanical characterization are vital for the successful development of next generation low-k dielectrics. A new class of low-k materials, nanoporous pure-silica zeolite, is prepared in thin films using IC compatible spin coating process and characterized using depth sensing nanoindentation technique. The elastic modulus of the zeolite thin films is found to be significantly higher than that of other low-k materials with similar porosity and dielectric constants. Correlations between the mechanical, microstructural and electrical properties of the thin films are discussed in detail.     

UV light-induced deposition of low dielectric constant organic polymer for interlayer dielectrics

The photo-induced conversion of polyamic acid spun onto Si and quartz substrates into thin polyimide films at low temperature using 172 nm radiation from a Xe₂^* excimer lamp is described. The degree of imidization of the polyimide films during the UV curing at different exposure times and temperatures was investigated using Fourier transform infrared spectroscopy. Compared with conventional furnace processing, the photo-induced curing of the polyimide provided both reduced processing time and temperature. Ellipsometry, UV spectrophotometry, capacitance-voltage and current-voltage measurements were employed to characterize the polymer films and indicated them to be of high quality. In particular, the current-voltage measurements showed that the leakage current density of the irradiated polymer was over an order of magnitude smaller than has been obtained in layers prepared by thermal processing.     

Effect of thermal treatment on carbon-doped silicon oxide low dielectric constant materials

Carbon-doped silicon oxide (SiOCH) low dielectric constant (low-k) material is a good candidate for advanced interconnect technology. Good thermal stability of the dielectric is required due to the many thermal processes involved during IC fabrication. The thermal stability of tetramethylcyclotetrasiloxane (TMCTS) based plasma-enhanced chemical vapor deposition (PECVD) carbon doped low-k material with annealing temperature from 400 to 800 degrees C in N2 was studied. The thermal stability temperature of TMCTS based carbon doped low-k material is 600 degrees C. Above 600 degrees C annealing, the thermal energy can break Si-CH3, Si-C, Si-H, and C-H bonds leading to outgasing, which results in film composition change, weight loss, and thickness shrinkage. Film composition changes, especially carbon loss and oxygen incorporation, can degrade its reliability extremely. Carbon is desorbed in the form of CH4, CO, and other hydrocarbon.