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摘要：作为一类新型的多功能材料,锗的硫属化合物由于其在催化、光学、光电导体、离子交换、非线性光学、半导体、锂离子电池等方面的应用，近年来日益受到人们的重视。特别是GeS2纳米材料，其制备与应用目前开始渐渐成为了研究者们的关注焦点。但是有关制备手段仍然较为缺乏，尤其缺少一种成熟、稳定的制备方法。
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溶剂热法具有反应条件温和、污染小、成本较低、易于商业化、产物结晶好、团聚少及纯度高等特点，已被广泛应用于各类无机纳米材料的合成。因此本课题采用溶剂热法，以高纯度的GeCl4为锗源制备了具有较高结晶度和纯度的GeS2纳米片，并采用XRD、UV-vis-NIR、TEM、EDX等手段对产物进行表征。探讨反应温度、反应时间、溶剂等影响因素对产物结晶度和纯度的影响，并初步推测其反应机理。22923
毕业论文关键词：二硫化锗；纳米材料；溶剂热法；制备
Preparation of Germanium Disulfide Nanomaterials and Their Properties
Abstract: Germanium chalcogenides are receiving more and more attention in recent years for their applications in catalysis, photonics, photoconductivity, ion exchange, nonlinear optical materials, semiconductors and lithium-ion batteries. They are occurred to be a new kind of multifunctional materials. GeS2 nanomaterials are as well being recognized to be promising in many applications for their unique electronic and optical properties, however, the synthesis of GeX2 nanomaterials is still in its infancy. A mature and stable preparation method is particularly needed for the further study of GeX2 nanomaterials.
As an economic and environmental synthesis method, solvothermal synthesis has been applied to preparations of various kinds of inorganic nanomaterials. What’s more, solvothermal reactions can be taken out in moderate conditions. Based on these, GeS2 nanoplates were prepared in reactions between germanium precursors (GeCl4 with high purity) and sulfur sources under solvothermal conditions. The as-prepared product will be characterized by XRD, TEM, EDX, and UV-vis-NIR. Influences of reaction conditions including temperature, reaction time, solvents and molar ratio on the crystallinity and purity of the products will be studied in this project. Finally, the primary reaction mechanism of the process will be deduced.
Keywords: Germanium disulfide; Nanomaterials; Solvothermal process; Preparation
目录
1 绪论 1
1.1 硫属化合物研究概述 1
1.1.1 锡的硫属化物 2
1.1.2 锑的硫属化合物 2
1.1.3 GeS 2
1.1.4 GeS2的合成 3
1.2 硫属化合物纳米材料合成方法概述 4
1.2.1热注入法 5
1.2.2单元前驱体法 5
1.2.3水热法 5
1.2.4 其他合成方法 6
1.3 溶剂热法简介 6
1.4 研究意义与目的 7
1.4.1 意义 7
1.4.2 目的 8
2 实验部分 9
2.1 仪器与试剂 9
2.1.1 仪器 9
2.1.2 试剂 9
2.2 实验方法 10
2.2.1 GeS2纳米片的制备 10
2.2.2 条件实验 10
2.2.3 样品表征 10
3 结果与讨论 12
3.1 GeS2纳米片的表征 12
3.1.1 XRD分析 12
3.1.2 元素分析 12
3.1.3 形貌分析 13
3.2 条件实验结果讨论 14
3.2.1溶剂种类的影响 14
3.2.2 反应温度的影响 14