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二元溶剂热中无机含氧酸盐微纳米材料的化学制备

Synthesis of Oxysalt Micro and Nanomaterials in a Binary Solution

【作者】 薛飞

【导师】 钱逸泰;

【作者基本信息】 中国科学技术大学 , 无机化学, 2009, 硕士

【摘要】 本论文主要探索在二元溶剂热的条件下合成磷酸盐纳米材料和钼酸盐微尺度材料,并对所制备的微纳米材料进行了鉴定和表征,对它们的生长过程也进行了研究。主要内容总结如下:1.溶剂热条件下BiPO4纳米材料的制备。以Bi(NO3)3和NaH2PO4为原料,在无表面活性剂或者高分子聚合物辅助的情况下,通过溶剂热途径制备了尺寸在100-150 nm之间的六方相纳米茧和直径在50-150 nm之间,长度范围为0.5-1.0μm之间的单斜相纳米棒,并研究了随着时间的变化六方相纳米茧到单斜相纳米棒的转化过程,在水热条件下我们也发现了相同的相转化过程,并伴随着纳米棒到八面体状微晶的形貌转化。此外,我们还讨论了甘油和水的溶剂比对产品形貌的影响。对所得的六方相纳米茧和单斜相纳米棒的荧光性质进行了研究。2.溶剂热条件下三维CaMoO4茧状微结构和SrMoO4花生状微结构的制备。以CaCl2 ,SrCl2和Na2MoO4为原料,通过溶剂热方法合成了平均直径是500 nm,平均长度是1.5μm的钼酸钙茧状微结构和直径大约是500 nm,长度大约在1.5μm的钼酸锶花生状微结构,在他们的生长过程中我们观察到了一个熟化-分裂-定向组装的过程。并且我们还讨论了溶剂比和反应物浓度比对最终产物的影响。对它们的荧光性质也进行了简单的讨论。

【Abstract】 The aim of this dissertation is to explore the synthesis of phosphates nanomaterials and molybdates micromaterials by solvothermal method. The as-prepared phosphates nanomaterials and molybdates micromaterials are characterized and their growth mechanism is also investigated. The major contents can be summarized as follows:1. Solvothermal process to synthesize hexagonal phase BiPO4 nano-cocoons and monoclinic phase BiPO4 nanorods. By using Bi(NO3)3 and NaH2PO4 as the reaction materials, without the presence of any surfactants or polymers, hexagonal phase BiPO4 nano-cocoons with the sizes of 100-150nm, monoclinic phase BiPO4 nanorods with diameters of 50-150 nm, lengths of 0.5-1.0μm have been successfully prepared. The phase and morphology evolution from the initially formed hexagonal phase nano-cocoons to monoclinic phase BiPO4 nanorods were investigated by studying intermediate products of different reaction time. The similar phase transformation from hexagonal phase BiPO4 to monoclinic phase BiPO4 in the hydrothermal condition at 160°C was also observed, accompanying with a morphology transformation from nanorods to octahedron-like microcrystals. Moreover, we found that the volume ratio of glycerol and water had a great impact on the shapes of finial products. Experimental results revealed that BiPO4 nanostructures exhibited photoluminescence properties.2. Cocoon-like CaMoO4 microstructures and peanut-like SrMoO4 mirostructures constructed from nanocrystals have been solvothermally synthesized in a binary solution of glycerol and water. A shape evolution of ripening-cleavage-oriented aggregation can be observed in the growth process of CaMoO4 cocoon-like and SrMoO4 peanut-like microstructures. It was found that the amount of reactants and the volume ratio of glycerol to water in the solvothermal condition had a great impact on the shapes and sizes of the products. The photoluminescence properties of cocoon-like CaMoO4 and peanut-like SrMoO4 architectures were also investigated.

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