液态聚碳硅烷制备含铝碳化硅陶瓷前驱体——聚铝碳硅烷  

LIQUID POLYCARBOSILANE DERIVED Al-CONTAINING SiC CERAMIC PRECURSORS——POLYALUMINOCARBOSILANE

作　　者：杨露姣[1] 杨景明[1] 余煜玺[1] 程璇[1] 张颖[1] 

机构地区：[1]厦门大学材料学院材料科学与工程系特种先进材料福建省重点实验室,福建厦门361005

出　　处：《硅酸盐学报》2009年第12期1970-1974,共5页Journal of The Chinese Ceramic Society

基　　金：特种先进材料福建省重点实验室项目(2006L2003);国家自然科学基金重点项目(50532010)资助

摘　　要：通过液态聚碳硅烷与乙酰丙酮铝反应,合成了一系列的聚铝碳硅烷,考察了原料配比和反应温度的影响。结果显示:改变合成温度或乙酰丙酮铝的加入量,聚铝碳硅烷呈现从液态到固态的转变。增加乙酰丙酮铝的配比或提高合成温度,可增加聚铝碳硅烷中铝的质量分数,在360℃合成的产物中铝的质量分数接近理论值;增加铝的质量分数或提高合成温度,可增大聚铝碳硅烷的分子量及其多分散系数。360℃以下聚铝碳硅烷的数均分子量随着铝的质量分数的增加呈线性增加。红外光谱及核磁共振分析结果均显示,铝元素的引入伴随着Si—H键的消耗,通过AlOx(x=4,5,6)基团使液态聚碳硅烷分子部分交联长大,高铝含量的样品具有较高的交联程度。The Al-containing SiC ceramic precursors, polyaluminocarbosilane （PACS）, were synthesized via the reactions of liquid polycarbosilane （L-PCS） and aluminum acetylacetonate （Al（AcAc）3） with different ratios at 300 ℃ and 360 ℃ respectively. The results reveal that the PACS phases vary from liquid to solid at various of reaction temperatures or the amounts of Al（AcAc）3 input. The Al content introduced increases with the increases of reaction temperature and the amount of Al（AcAc）3 input. The value of Al content was similar to the theoretical value calculated from the amounts and ratio of the reactants at 360 ℃. The molecular mass and polydispersity indexes also increases with the increases of Al content in the PACS or the reaction temperatures. The values of number average mass of the PACS produced at 360 ℃ increased linearly with the increase of Al contents. The Fourier transform infrared spectroscopy, nuclear magnetic resonance （including 1H, 29Si and 27Al NMR） results indicate that Al was introduced into the L-PCS by consuming Si—H bonds and forming AlOx （x = 4, 5, 6） groups, in which the L-PCS molecules cross-linked making the molecular mass increase. The degree of cross-linking in the PACS increased when the Al content increased.

关 键 词：聚铝碳硅烷 液态聚碳硅烷 陶瓷先驱体 结构表征 

分 类 号：TB303[一般工业技术—材料科学与工程]