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先驱体法制备的含铝SiC纤维的组成和结构研究

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

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【作者】 余煜玺李效东曹峰王应德王军郑春满冯春祥

【Author】 YU Yu-Xi, LI Xiao-Dong, CAO Feng, WANG Ying-De, WANG Jun, ZHENG Chun-Man, FENG Chun-Xiang (Key Laboratory of Advanced Ceramic Fibers and Composite, National University of Defense Technology, Changsha 410073, China)

【机构】 国防科技大学陶瓷纤维及其复合材料重点实验室国防科技大学陶瓷纤维及其复合材料重点实验室 长沙 410073长沙 410073

【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29 Si、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.

【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, 27A1 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 contains a 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.

【关键词】 先驱体聚铝碳硅烷碳化硅纤维结构
【Key words】 precursorpolyaluminocarbosilaneSiC fibersstructure
【基金】 国家自然科学基金(59972042)
  • 【文献出处】 无机材料学报 ,Journal of Inorganic Materials , 编辑部邮箱 ,2006年01期
  • 【分类号】TQ343.6
  • 【被引频次】19
  • 【下载频次】368
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