硅酸盐学报

碳热还原杂化前驱体合成SiC–TaC纳米复合粉体

作者：李青肖汉宁郭文明胡继林谢文高朋召欧阳唐哲

分类号：TB332

出版年,卷(期):页码：2012,40(5):739-744

DOI：

摘要：

摘要：以五氯化钽(TaCl₅)、正硅酸乙酯(TEOS)和葡萄糖(C₆H₁₂O₆?H₂O)为原料制备了葡萄糖复合凝胶，凝胶经过450℃煅烧得到C–SiO₂–Ta₂O₅杂化前驱体，通过碳热还原前驱体，于1200～1500℃合成了SiC–TaC纳米复合粉体，并用X射线衍射扫描电镜和能谱仪对产物进行表征。结果表明：凝胶中无定型的SiO₂和Ta₂O₅可通过Si—O—Ta键合，均匀分布的Si—O—Ta—C长链使得杂化前驱体内部结合成为牢固的互穿网络结构；TaC于1200℃时得到，而SiC可在1400℃开始合成，反应可在1500℃完成。在不同的钽硅摩尔比下，SiC–TaC纳米复合粉体具有差异性形貌。当钽硅比约为0.02时，SiC与TaC纳米晶粒颗粒分布均匀，同质化明显。随着钽硅比的升高，SiC有从球状转变为纳米线状的趋势

Abstract: A compound gel was firstly prepared with tantalum pentachloride (TaCl₅), tetraethoxysilane (TEOS) and glucose (C₆H₁₂O₆? H₂O) as starting materials, and the gel was then calcined at 450℃ to obtain a C–SiO₂–Ta₂O₅ hybrid precursor. A nanopowder of SiC–TaC was synthesized with the precusor via the carbonthermal reduction at 1200–1500℃. The products were charaterized by using X-ray diffration, scanning electron microscope, energy dispersive. The results show that the amorphous SiO₂ and Ta₂O₅ can be composed by Si—O—Ta bonding, and the evenly-distributed Si—O—Ta—C long chain renders the solid structure of interpenetrating networks inside the hybrid precursor. TaC was obtained at <1200℃, and SiC started to be synthesized at 1400℃, and the whole reaction process could be fully completed at 1500℃. The nanopowder of SiC–TaC presented distinct features at different mole ratios of tantalum to silicon. The particle size distribution of the powder appeared narrower at a mole ratio of tantalum to silicon of 0.02. The morphology of SiC could vary from spherical nanoparticles into curve-shaped nanowires when the mole ratio increased.

基金项目：

国家自然科学基金(No.50972042)

作者简介：

第一作者：李青(1983—)，男，博士研究生。通信作者：肖汉宁(1961—)，男，博士，教授

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