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二氧化硅基复合微球的制备与表征

Preparation and Characterization of Silica-based Composite Microspheres

【作者】 金莉莉

【导师】 魏先文;

【作者基本信息】 安徽师范大学 , 无机化学, 2006, 硕士

【摘要】 纳米复合材料可以通过对具有不同性能材料的微观复合,实现对各种性质如光、电、磁等的优化,满足各种用途的需要,而半导体纳米材料由于在太阳能转化、光催化及光电子工业等具有潜在的应用价值,成为了实验和理论研究的焦点。本论文旨在合成具有电磁性能的SiO2基复合材料并研究其性能,通过改变反应条件优化合成复合材料,探究复合材料的结构与性能的关系,以期拓展纳米SiO2基复合材料的应用范围。1.采用St?ber方法制备了单分散的、直径分别为100纳米和140纳米的非晶态SiO2微球。合成了SiO2 /普鲁士蓝纳米复合微球,并经X—射线粉末衍射(XRD)、透射电镜(TEM)表征。探讨了FeCl3的质量分数、溶剂等对复合结构的影响,并且研究了SiO2 /普鲁士蓝复合微球修饰电极的电化学行为。实验结果表明,包覆在SiO2微球上的普鲁士蓝是晶态的,较大的FeCl3质量分数有利于形成连续的包覆;利用三乙醇胺—水—乙醇作溶剂得到的复合结构粒径较用乙醇—水作溶剂得到的复合结构粒径小,用复合微球修饰的电极对过氧化氢的还原有较好的催化作用。2.为了避免FeNi合金的纳米结构被氧化,通过正硅酸乙酯的水解,合成了SiO2 / FeNi纳米复合物,对其结构进行了XRD、TEM、扫描电镜(SEM)、振动样品磁强计(VSM)表征。实验结果表明,SiO2包覆层厚度可以通过改变TEOS的浓度调控,随着SiO2包覆层厚度的增加,复合物样品的饱和磁化强度降低,而样品中金属FeNi所产生的饱和磁化强度基本不变。该法简单方便,且SiO2包覆层厚度可控,为合成SiO2基复合磁性材料及拓展其应用奠定基础。

【Abstract】 Nanocomposites not only combine the advantageous properties of two component, exhibit excellent optical, electrical, catalytic, and mechanical properties that single-phase material does not have, but also have potential application in catalysis, electronics and nonlinear optics. Semiconductor nanoparticles have been extensively studied from experimental and theoretical viewpoints, owing to their potential applications in solar energy conversion, photocatalysis and the optoelectronic industry. The thesis is focused on the synthesis and characterization of SiO2 based nanocomposites with unique properties, and seeking after the changes of properties and structure by changing the concentrations of reactant, solvents, in order to broaden applied areas of SiO2.1. Monodipersed, amorphous SiO2 microspheres with diameters of 100 nm and 140 nm, respectively, were prepared by St?ber method. SiO2 / Prussian Blue nanocomposites were synthesized and characterized by X-ray powder diffraction (XRD) and transmission electron microscope (TEM). The influence of experimental parameters such as mass fractions of FeCl3, solvent etc. on the composites nanostructures was studied. The results indicated that larger mass fraction of FeCl3 was in favor of forming more continuous crystal cladding layers on SiO2 microspheres and that the

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