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一维纳米金属氧化物的制备与气敏性能研究

Synthesis and Sensing Property of One Dimensional Metal Oxide Nanocrystal

【作者】 刘欣

【导师】 李殿卿;

【作者基本信息】 北京化工大学 , 化学, 2010, 硕士

【摘要】 本文分别采用水热法和溶剂热法合成出具有一维纳米结构的氧化锌,运用XRD、SEM、TEM、EDX和XPS等分析测试手段对一维纳米氧化锌的晶体结构、形貌、结晶度和材料表面组成进行了表征。通过比较和讨论合成方法、温度和时间对氧化锌产品的影响,优化了合成工艺。本文考察了不同碱比和表面活性剂对氧化锌晶体生长的影响,研究和讨论了氧化锌在水热反应中的生长机理。以低温水热合成法的产品,比较了表面活性剂SDS和CTAB对于气敏性能的影响。对以CTAB为表面活性剂采用低温水热法制备得到的氧化锌进行了气敏选择性能的测试,并通过改变焙烧温度和焙烧时间研究了焙烧过程对于氧化锌气敏性能的影响。通过改变合成方法和合成条件,优化合成了一维纳米氧化锡晶体。在此基础上对纳米氧化锡进行了金属钯的掺杂与表面修饰,运用XRD、SEM、TEM、EDX和XPS等分析测试手段对产品的晶体结构、形貌、结晶度和材料表面组成进行了表征。在采用乙醇溶剂热法制备纳米氧化锡的过程中,为了考察晶体生长的动力学与热力学因素,通过正交实验比较了时间与温度、碱比与初始浓度对氧化锡晶体形貌的影响。讨论了不同焙烧温度下氧化锡的气敏性质,并通过表面修饰改进了纳米氧化锡的气敏性能。

【Abstract】 One-dimensional (ID) ZnO nanocrystals have been synthesized by hydrothermal and solvothermal process. The morphology, crystallinity, surface component and structure of crystals were characterized by SEM, TEM, XRD and XPS analysis. In order to optimize the process of ZnO synthesis, several methods and different synthesis condition have been compared and discussed.For investigated crystal growth mechanism, the ZnO nanocrystal syntheses by different base ratio and surfactant have been conducted in hydrothermal process. By comparing SDS-assisted and CTAB-assisted low-temperature hydrothermal synthesis, the effect of surfactant on the performance of gas sensing material was studied. The gas sensing selectivity of ZnO nanocrystal synthesis by CTAB-assisted low-temperature hydrothermal process was measured. And the effect of calcination temperature and time on ZnO response was systematically studied.In order to optimize the process, One-dimensional SnO2 nanocrystals have been synthesized by several methods. In order to modify the surface of SnO2 nanocrystal, Pd metal was doped on the SnO2 as secondary component. The morphology, crystallinity, surface component and structure of crystals were characterized by SEM, TEM, XRD, EDX and XPS analysis.In order to study the dynamics and thermodynamics of crystal growth factors, an orthogonal experiment was designed to investigate the effect of time and temperature, alkali concentration and the initial concentration on morphology of tin oxide crystals. The effect of calcination temperature on SnO2 response was discussed. In order to improve the gas sensing performance, the surface of SnO2 nanocrystal was modified.

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