可纺性bn(c)有机先驱体的合成与陶瓷化分析-synthesis and ceramic analysis of spinnability bn ( c ) organic precursor.docxVIP
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可纺性bn(c)有机先驱体的合成与陶瓷化分析-synthesis and ceramic analysis of spinnability bn ( c ) organic precursor
的成型性。热分析研究表明,先驱体热裂解反应主要发生在 120°C,180°C, 300°C 温度段,120~180°C 主要发生残留的 B-Cl 键与 N-H 键的反应释放 HCl 气 体以及部分有机基团的分解,即先驱体进一步聚合的过程。300°C 附近主要进 行 C-C 键与 N-H 键的反应释放含有 C,H 元素气体的过程。根据热分解特征, 建立了 先驱 体陶 瓷化 结构 演化 模型 ,深入 研究了 结构 演化 机制 。元 素分 析表 明,经氨气 1100°C 处理后产物的 C 含量进一步降低,为 1.24wt%,陶瓷网络结 构由 B-N 键构成。研究了三氯硼吖嗪/烯丙基胺体系先驱体的流变行为,结果表明先驱体为剪 切变稀流体,剪切速率为 560s-1 ,温度 80°C,先驱体的粘度稳定,有利于纺 丝。采用该先驱体制备了 BN(C)微纳米纤维,用熔融挑丝法获得的纤维直径约为 10μm,长度可达 30cm,用静电纺丝法制备的纤维经 1550°C 热处理后直径为 200nm。分别研究了热处理气氛对纤维形貌和结构的影响,结果表明 N2 处理的 纤维形貌没有明显变化,氨气处理有明显的除 C 作用,同时对纤维造成一定刻 蚀,在 1100°C 氨化这种刻蚀作用明显。高温氮化,会由于结构调整和原子重排 作用,纤维缺陷会得到修复,在 1550°C 氮化修复作用明显。制备的 BN 和 BCN 纤维有着优良的抗氧化性,在空气气氛中 BN 纤维 800°C 时仅约有 5%的 热失重,而 BCN 纤维到 1200°C 约有 10%的热失重,抗氧化性明显优于 C 纤 维。关键词:三氯硼吖嗪;有机先驱体;BN(C)纤维;流变性;结构演化AbstractHexagnal BN(C) materials have large number merits of corrosion resistance, oxydation resistance, low density, high temperature resistance and superior high temperature mechanical property and microwave transparency. So it can be used as structure materials, reenforcement of composites, solid lubricant, carrier of catalysts. But there are some difficulties to fabricate BN(C) fibers and in various shapes. And impurities of precursor may limit the superior properties of BN(C) materials. The main reason is that there are limited BN(C) precursor, so the key issue is to fine a high purity, shaping-well precurosr. Trichloroborazine (TCB) is a solid molecular crystalline, containing B-N ring, Cl,and H elements. It has been first synthesized in 1967, but there are little reports about BN(C) micro/nano materials derived from TCB backbones. In this dissertation, TCB was used as raw material, and its reacting directivity and selectivity are systemic studied. High purity and shaping-well precurosr have been synthesized by TCB, aniline (allylamine) which act as bridging molecues, and BN(C) micro/nano materials were further prepared. The outcomes testified that TCB/aniline(allylamine) is a kind of surperior precursor to prepare BN(C) micro/nano materials. The main conl
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