基于单一来源前驱物溶剂热法制备金属硫化物纳米材料及其性质的研究
发布时间：2018-08-09 14:25
【摘要】：金属硫化物纳米材料作为经典的硫族半导体材料,因为具有独特的物理和化学性质而被广泛地研究,特别是在光催化、超级电容器、生物成像、电池、传感器及磁性等领域。在室温条件下通过化学沉淀法合成单一来源反应前驱物,本文在此基础上,通过改变实验的操作条件如不同的反应溶剂,不同反应时间以及有无添加聚乙烯吡咯烷酮(PVP)表面活性剂等制备形貌各异的不同金属硫化物纳米材料。研究了单一成分的金属硫化物纳米材料在光催化、吸附方面的性质,同时制备出金属硫化物/石墨烯复合材料作为超级电容器的电极材料并研究其电容性质。论文包括下面三个部分:1、不同溶剂下合成的CdS纳米材料在光催化性质上的研究比较我们选用Cd(NO_3)_2·4H_2O和C_5H_(10)NNaS2'3H_2O(二乙基二硫代氨基甲酸钠)分别作为镉源和硫源,用PVP作为表面活性剂,在室温的条件下通过化学沉淀法制备出单一来源前驱物。将一定量的前驱物分别在乙二醇和乙二胺溶剂中进行高温高压反应,制备出形貌各异的CdS纳米材料。采用粉末X-射线衍射仪(XRD)、透射电子显微镜(TEM)、扫描电子显微镜(SEM)、X射线光电子能谱仪(XPS)、BET比表面积等测试手段对合成样品的组成、结构、形貌、元素价态以及比表面积进行分析。用氙灯测试不同样品对染料罗丹明B(RB)的可见光光催化降解性质。结果表明,不同溶剂下合成的CdS纳米材料在催化降解RhB中表现出截然不同的降解特征。通过实验我们对不同CdS纳米材料的光催化机理进行探讨与比较。2、水热法制备花球状的In_2S_3纳米材料及其吸附与光催化性质研究我们选用In(NO_3)_3·xH_2O和C_5H_(10)NNaS2·3H_2O分别作为铟源和硫源,不添加任何表面活性剂,在室温下通过化学沉淀法制备出单一来源前驱物。将一定量的反应前驱物分散在一定体积的水溶剂里,在高温高压反应条件下,制备出花型的In_2S_3纳米材料。通过将前驱物在相同的温度下经历不同的反应时间而得到不同形貌的样品,从而可以分析并推断出花型形貌的演变过程。采用XRD、TEM、SEM、XPS以及固体紫外漫反射(UV-visDRS)等测试对合成样品的组成、结构、形貌、元素价态、以及可见光吸收等进行表征。选择最佳形貌的In_2S_3纳米材料,BET比表面积结果显示比表面积高达134.08 m2/g。将花型结构的In_2S_3纳米材料作为吸附剂对有机染料甲基蓝(MB)进行吸附实验,同时又作为光催化剂对有机染料甲基橙(MO)和抗生素四环霉素(TC)进行光催化实验。结果表明,该花型结构的In_2S_3纳米材料有着很高的吸附-光催化性质。同时也对导致该材料高的光催化活性的原因进行了分析与讨论。3、水热法制备NixSy/rGO复合材料及其电化学性质研究我们选用Ni(NO_3)_2·4H_2O和C_5H_(10)NNaS2·3H_2O分别作为镍源和硫源,不添加任何表面活性剂,在室温下通过化学沉淀法制备出单一来源前驱物。将前驱物与氧化石墨烯溶液混合并在高温高压反应条件下,得到NixSy与还原氧化石墨烯的复合材料。运用SEM、XRD测试对样品的形貌和组分分别进行表征。结果表明该方法制备出的是多种硫化镍化合物与还原氧化石墨烯的复合材料。考察了不同镉源和硫源的量对产物组成的影响。选择一定配比条件下合成的NixSy/rGO复合材料制作成工作电极,在三电极体系中进行电化学性质测试。结果发现,与石墨烯复合的产物比单独NixSy产物的电容性质好,同时也意外发现该单一来源前驱物也有一定的电容性质。
[Abstract]:As a classic sulphur semiconductor material, metal sulfide nanomaterials have been widely studied because of their unique physical and chemical properties, especially in the fields of photocatalysis, supercapacitors, bioimaging, batteries, sensors, and magnetic fields. At room temperature, the precursor of a single source reaction is synthesized by chemical precipitation method at room temperature. On the basis of the changes of the operating conditions such as different reaction solvents, different reaction times and the addition of polyvinylpyrrolidone (PVP) surfactant, different metallic sulfide nanomaterials have been prepared. The properties of the single component Metal Sulfide Nanomaterials in photocatalytic activity and adsorption are studied. The metal sulfides / graphene composites are prepared as electrode materials for supercapacitors and study their capacitive properties. The following three parts are included: 1, the photocatalytic properties of CdS Nanomaterials Synthesized under different solvents are compared with Cd (NO_3) _2. 4H_2O and C_5H_ (10) NNaS2'3H_2O (two ethyl two thiocarbamate). A single source precursor was prepared by chemical precipitation under the condition of room temperature as a surface active agent with PVP as a source of cadmium and sulfur, respectively. A certain amount of precursors were subjected to high temperature and high temperature reaction in ethylene glycol and ethylenediamine solvent, and the CdS nanomaterials with different morphologies were prepared. The powder X- ray diffractometer (XRD) was used for transmission. Electron microscopy (TEM), scanning electron microscopy (SEM), X ray photoelectron spectroscopy (XPS), BET specific surface area and other testing methods were used to analyze the composition, structure, morphology, valence state and specific surface area of the synthesized samples. The visible light photocatalytic degradation of rhodamine B (RB) by different samples was tested by xenon lamp. The results showed that different solubility was different. The CdS Nanomaterials Synthesized under the agent showed distinct degradation characteristics in the catalytic degradation of RhB. Through the experiment, we explored and compared the photocatalytic mechanism of different CdS nanomaterials..2, In_2S_3 nanomaterials and their adsorption and photocatalytic properties were prepared by hydrothermal method. We selected In (NO_3) _3. XH_2O and C_5H_ (10) NNaS. 2. 3H_2O as an indium source and a sulfur source, without any surfactants, to prepare a single source precursor by chemical precipitation method at room temperature. A certain amount of reaction precursors are dispersed in a certain volume of water solvent, and the flower type In_2S_3 nanomaterials are prepared under high temperature and high pressure conditions. The precursors are in the same way. Samples of different morphologies were obtained at different reaction times at temperature, and the evolution process of flower morphology could be analyzed and deduced. XRD, TEM, SEM, XPS and solid ultraviolet diffuse reflectance (UV-visDRS) were used to characterize the composition, structure, morphology, valence state, and visible absorption of the synthetic samples. In_2S_3 nanomaterials of appearance, BET specific surface area results show that the specific surface area is up to 134.08 m2/g., and the In_2S_3 nanomaterials of the flower structure are used as adsorbents to adsorb organic dye methyl blue (MB), and also as photocatalyst for organic dye methyl orange (MO) and anti biotic tetracycline (TC) photocatalytic experiment. The results show that the photocatalyst is used as a photocatalyst. In_2S_3 nanomaterials with this type of flower structure have high adsorption and photocatalytic properties. At the same time, the reasons for the photocatalytic activity of high photocatalytic activity of the material are also analyzed and discussed..3, NixSy/rGO composites and their electrochemical properties are studied by hydrothermal method. We choose Ni (NO_3) _2. 4H_2O and C_5H_ (10) NNaS2. 3H_2O respectively as the nickel source. A single source precursor was prepared by chemical precipitation at room temperature without any surface active agent. The precursor was mixed with the solution of graphene oxide and the composite of NixSy and reduced graphene oxide was obtained under the condition of high temperature and high pressure. The morphology and composition of the samples were characterized by SEM and XRD. The results showed that a variety of nickel sulfide compounds and reduced graphene oxide were prepared by this method. The influence of the amount of different CD sources and sulfur sources on the composition of the products was investigated. The NixSy/rGO composites prepared under certain proportions were made into working electrodes, and the electrochemical properties were tested in the three electropolar bodies. The results were found, The composite with graphene has better capacitive properties than NixSy alone, and the precursor from a single source also has certain capacitive properties.
【学位授予单位】：安徽大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TB383.1
本文编号：2174366
[Abstract]:As a classic sulphur semiconductor material, metal sulfide nanomaterials have been widely studied because of their unique physical and chemical properties, especially in the fields of photocatalysis, supercapacitors, bioimaging, batteries, sensors, and magnetic fields. At room temperature, the precursor of a single source reaction is synthesized by chemical precipitation method at room temperature. On the basis of the changes of the operating conditions such as different reaction solvents, different reaction times and the addition of polyvinylpyrrolidone (PVP) surfactant, different metallic sulfide nanomaterials have been prepared. The properties of the single component Metal Sulfide Nanomaterials in photocatalytic activity and adsorption are studied. The metal sulfides / graphene composites are prepared as electrode materials for supercapacitors and study their capacitive properties. The following three parts are included: 1, the photocatalytic properties of CdS Nanomaterials Synthesized under different solvents are compared with Cd (NO_3) _2. 4H_2O and C_5H_ (10) NNaS2'3H_2O (two ethyl two thiocarbamate). A single source precursor was prepared by chemical precipitation under the condition of room temperature as a surface active agent with PVP as a source of cadmium and sulfur, respectively. A certain amount of precursors were subjected to high temperature and high temperature reaction in ethylene glycol and ethylenediamine solvent, and the CdS nanomaterials with different morphologies were prepared. The powder X- ray diffractometer (XRD) was used for transmission. Electron microscopy (TEM), scanning electron microscopy (SEM), X ray photoelectron spectroscopy (XPS), BET specific surface area and other testing methods were used to analyze the composition, structure, morphology, valence state and specific surface area of the synthesized samples. The visible light photocatalytic degradation of rhodamine B (RB) by different samples was tested by xenon lamp. The results showed that different solubility was different. The CdS Nanomaterials Synthesized under the agent showed distinct degradation characteristics in the catalytic degradation of RhB. Through the experiment, we explored and compared the photocatalytic mechanism of different CdS nanomaterials..2, In_2S_3 nanomaterials and their adsorption and photocatalytic properties were prepared by hydrothermal method. We selected In (NO_3) _3. XH_2O and C_5H_ (10) NNaS. 2. 3H_2O as an indium source and a sulfur source, without any surfactants, to prepare a single source precursor by chemical precipitation method at room temperature. A certain amount of reaction precursors are dispersed in a certain volume of water solvent, and the flower type In_2S_3 nanomaterials are prepared under high temperature and high pressure conditions. The precursors are in the same way. Samples of different morphologies were obtained at different reaction times at temperature, and the evolution process of flower morphology could be analyzed and deduced. XRD, TEM, SEM, XPS and solid ultraviolet diffuse reflectance (UV-visDRS) were used to characterize the composition, structure, morphology, valence state, and visible absorption of the synthetic samples. In_2S_3 nanomaterials of appearance, BET specific surface area results show that the specific surface area is up to 134.08 m2/g., and the In_2S_3 nanomaterials of the flower structure are used as adsorbents to adsorb organic dye methyl blue (MB), and also as photocatalyst for organic dye methyl orange (MO) and anti biotic tetracycline (TC) photocatalytic experiment. The results show that the photocatalyst is used as a photocatalyst. In_2S_3 nanomaterials with this type of flower structure have high adsorption and photocatalytic properties. At the same time, the reasons for the photocatalytic activity of high photocatalytic activity of the material are also analyzed and discussed..3, NixSy/rGO composites and their electrochemical properties are studied by hydrothermal method. We choose Ni (NO_3) _2. 4H_2O and C_5H_ (10) NNaS2. 3H_2O respectively as the nickel source. A single source precursor was prepared by chemical precipitation at room temperature without any surface active agent. The precursor was mixed with the solution of graphene oxide and the composite of NixSy and reduced graphene oxide was obtained under the condition of high temperature and high pressure. The morphology and composition of the samples were characterized by SEM and XRD. The results showed that a variety of nickel sulfide compounds and reduced graphene oxide were prepared by this method. The influence of the amount of different CD sources and sulfur sources on the composition of the products was investigated. The NixSy/rGO composites prepared under certain proportions were made into working electrodes, and the electrochemical properties were tested in the three electropolar bodies. The results were found, The composite with graphene has better capacitive properties than NixSy alone, and the precursor from a single source also has certain capacitive properties.
【学位授予单位】：安徽大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TB383.1
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