基于聚硅碳硅烷与仲丁醇铝制备含铝碳化硅纤维  

Synthesis of Aluminum-Containing SiC Fibers Based on Polysilancarbosilane and Aluminum Tri-Sec-Butoxide

作　　者：甄霞丽 裴学良 钟希强 何流 黄庆 苏新艳[1] ZHEN Xia-li;PEI Xue-liang;ZHONG Xi-qiang;HE Liu;HUANG Qing;SU Xin-yan(School of Material Science and Engineering,Shanghai University,Shanghai 200444,China;Engineering Laboratory of Nuclear Energy Materials,Ningbo Institute of Material Technology ＆ Engineering,Chinese Academy of Sciences,Ningbo 315201,Zhejiang,China)

机构地区：[1]上海大学材料科学与工程学院,上海200444 [2]中国科学院宁波材料技术与工程研究所核能材料工程实验室,浙江宁波315201

出　　处：《合成纤维》2018年第9期25-31,共7页Synthetic Fiber in China

基　　金：国家自然科学基金重大研究计划项目(91426304);ADS项目(XDA03010305)

摘　　要：采用聚硅碳硅烷和仲丁醇铝常压高温反应合成碳化硅纤维先驱体——聚铝碳硅烷。通过GPC、FT-IR、元素分析、X射线光电子能谱分析等表征发现：其组成以Si—C、Si—O、O—Al等化学键结构为主,重均分子质量为2 600,软化点在190～200℃之间。经熔融纺丝制得聚铝碳化硅纤维,其预氧化后陶瓷产率达到75%,高温处理后得到的含铝SiC纤维。随着温度的升高,该纤维组成逐渐由无序结构转化为晶体结构,其中的SiCxOy不稳定相在1 500℃开始分解,但晶粒尺寸基本维持在10 nm左右,无过度长大。含铝SiC纤维表现出良好的耐温性能,1500℃高温处理后纤维表面没有明显缺陷。As the precursor of SiC fiber, polyaluminocarbosilane（PACS） was synthesized by the high temper-ature reaction of polysilocarbosilane（PSCS） with aluminum tri-sec-butoxide（ASB）. The PACS was charac-terized by GPC, FT-IR, element analysis and XPS. The results show that the PACS, with the Si—C, Si—Oand O—Al as the main chemical bond structure, has weight molecular weight of 2 600 and the softeningpoint of 190～200 ℃. After melt-spinning and oxidation crosslinking, the PACS fiber has a high ceramicyield of about 75%. After heat-treatment, the SiC fiber is obtained from PACS fiber. With increasing theheat-treatment temperature, the SiC fiber composition is gradually transformed from disordered structure in-to crystal structure, and the unstable SiCxOyphase also starts to decompose at 1 500 ℃. But the crystallitysize is still maintained at about 10 nm, and there is no excessive growth. The obtained SiC fiber shows excel-lent temperature resistance, and the fiber surface can keep smooth and no obvious defects at 1 500 ℃.

关 键 词：聚铝碳硅烷 聚硅碳硅烷 仲丁醇铝 高温处理 碳化硅纤维 

分 类 号：TQ343.6[化学工程—化纤工业]