合成纤维

2018, v.47;No.355(09) 25-31

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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

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

摘要(Abstract):

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SiC_xO_y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(KeyWords): 聚铝碳硅烷;聚硅碳硅烷;仲丁醇铝;高温处理;碳化硅纤维
polyaluminocarbosilane;polysilocarbosilane;aluminum tri-sec-butoxide;high temperature treatment;SiC fiber

Abstract:

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

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

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DOI: 10.16090/j.cnki.hcxw.20180913.011

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