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Synthesis and characterization of mesoporous zirconia nanocomposite using self-assembled block copolymer template.

机译:使用自组装嵌段共聚物模板合成和表征介孔氧化锆纳米复合材料。

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摘要

Mesoporous zirconia has properties such as high surface area, uniform pore size distribution, and large pore volume, thus attracting great attention from the research community. Self-assembled structures have been used as directing agents to synthesize mesoporous zirconia. Here, we investigated the use of block copolymers conjugated to cationic biomolecules such as lysozyme, as well as cationic block copolymers as templates to synthesize mesoporous zirconia in completely aqueous media. Based on the Pluronic-lysozyme conjugate template, we further studied the effects of preparation conditions, including calcination temperature, precursor concentration, and precipitating pH. Several technics such as TGA, XRD, TEM, and N2 sorption were employed to characterize the zirconia samples. The results showed that tetragonal zirconia started to form after 300°C calcination and became fully crystallized after 500°C, grew larger when heated to higher temperatures, and began to form monoclinic phase after 900°C calcination. Our modified templates enhanced the thermal stability and increased the surface area of zirconia samples. The results also indicated that low precursor concentration and alkali media helped to decrease the zirconia particle size as well as increase the specific surface area. The surface area of the as-synthesized zirconia sample exhibited an increase before 500°C and a decrease after that, the highest specific surface area, 348 m2/g, achieved after 500°C calcination which was obtained using 0.08mol/L precursor at pH=10.
机译:介孔氧化锆具有比表面积大,孔径分布均匀和孔体积大等特性,因此引起了研究界的广泛关注。自组装结构已被用作导向剂来合成中孔氧化锆。在这里,我们研究了共轭嵌段共聚物与阳离子生物分子(如溶菌酶)以及阳离子嵌段共聚物作为模板在完全水性介质中合成介孔氧化锆的用途。基于Pluronic-溶菌酶偶联物模板,我们进一步研究了制备条件的影响,包括煅烧温度,前体浓度和沉淀pH。几种技术(例如TGA,XRD,TEM和N2吸附)用于表征氧化锆样品。结果表明,四方氧化锆在300°C煅烧后开始形成,在500°C之后完全结晶,在加热至更高温度时变得更大,在900°C煅烧后开始形成单斜晶相。我们改良的模板提高了热稳定性,并增加了氧化锆样品的表面积。结果还表明,低前驱物浓度和碱性介质有助于减小氧化锆的粒径并增加比表面积。合成后的氧化锆样品的表面积在500°C之前呈现出增加的趋势,而在此之后呈现降低的趋势,在500°C的煅烧后,使用0.08mol / L的前驱体在200°C时可获得的最高比表面积为348 m2 / g。 pH = 10。

著录项

  • 作者

    Ge, Qinwen.;

  • 作者单位

    Iowa State University.;

  • 授予单位 Iowa State University.;
  • 学科 Materials science.
  • 学位 M.S.
  • 年度 2012
  • 页码 86 p.
  • 总页数 86
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

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