无机材料学报

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先驱体法制备的含铝SiC纤维的组成和结构研究

余煜玺, 李效东, 曹峰, 王应德, 王军, 郑春满, 冯春祥   

  1. 国防科技大学陶瓷纤维及其复合材料重点实验室, 长沙 410073
  • 收稿日期:2004-11-12 修回日期:2005-01-17 出版日期:2006-01-20 网络出版日期:2006-01-20

Composition and Structure of Polymer-derived Aluminium-containing SiC Fibers

YU Yu-Xi, LI Xiao-Dong, CAO Feng, WANG Ying-De, WANG Jun, ZHENG Chun-Man, FENG Chun-Xiang   

  1. Key Laboratory of Advanced Ceramic Fibers and Composite, National University of Defense Technology, Changsha 410073, China
  • Received:2004-11-12 Revised:2005-01-17 Published:2006-01-20 Online:2006-01-20

摘要: 先驱体聚铝碳硅烷经熔融纺丝、空气预氧化处理、1300℃烧成可制得SiC(OAl)纤维(称为KD-A), 该纤?维再经1800℃烧结转变为SiC(Al)纤维(称
为KD-SA). 采用了元素分析、AES、SEM、XRD、RMS以及29Si、13C、27Al魔角自?旋固体核磁共振等测试方法对纤维的组成和结构进行了研究.
元素分析结果表?明KD-A的化学组成为SiC1/31O0.25Al0.018, KD-SA为SiC1.03O0.013Al0.024. AES表明, KD-A和KD-SA的表面和内部组成
不同. SEM表明KD-A、KD-SA表面光滑平坦, ?没出现孔洞、裂纹、沟槽等表面缺陷. XRD、RMS以及29Si、13C、27Al核磁共振的分析结果表明:
KD-A包含较多的不定形游离C, O以不?定形SiCxOy复合相的形式存在, Al与复合相中的O相连存在于复合相中, 复合相在纤维中是连续相, 少量
的β-SiC微晶分散在其中, 是非晶SiC纤维; KD-SA含有大量的β-SiC晶粒, 少量的α-SiC和Al2O3, 是近化学计量比的多晶SiC纤维.

关键词: 先驱体, 聚铝碳硅烷, 碳化硅纤维, 结构

Abstract: A ceramic fiber with the SiC(OAl) composition, named KD-A, was prepared by the melt-spinning of precursor polyaluminocarbosilane, air-curing, and pyrolizing at 1300℃.
The KD-A fiber was converted into SiC(Al) fiber, named KD-SA, by sintering at 1800℃. The composition and structure of the two kinds of
fibers were characterized by chemical element analysis, AES, SEM, XRD, RMS, and 29Si, 13C, 27Al MAS NMR. The compositions of KD-A
and KD-SA fibers are in the formula SiC1.31O0.25Al0.018 and SiC1.03O0.013Al0.024, respectively. The compositions of
KD-A and KD-SA fibers on the surface are different from that of inside of the fibers. The surfaces of KD-A and KD-SA fibers are smooth and even, and there are no
hole, crack and groove. KD-A fiber contains free carbon, small amount of β-SiC micro-crystal and aluminium embedded in an intergranular phase SiCxOy, which is
ascribed to a non-crystalline SiC fiber. KD-SA fiber containsa large number of β-SiC, a small amount of α-SiC and Al2O3,
which is ascribed to a crystalline SiC fiber with a nearly stoichiometric composition.

Key words: precursor, polyaluminocarbosilane, SiC fibers, structure

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