基于單一來源前驅物溶劑熱法制備金屬硫化物納米材料及其性質的研究
發(fā)布時間：2018-08-09 14:25
【摘要】：金屬硫化物納米材料作為經(jīng)典的硫族半導體材料,因為具有獨特的物理和化學性質而被廣泛地研究,特別是在光催化、超級電容器、生物成像、電池、傳感器及磁性等領域。在室溫條件下通過化學沉淀法合成單一來源反應前驅物,本文在此基礎上,通過改變實驗的操作條件如不同的反應溶劑,不同反應時間以及有無添加聚乙烯吡咯烷酮(PVP)表面活性劑等制備形貌各異的不同金屬硫化物納米材料。研究了單一成分的金屬硫化物納米材料在光催化、吸附方面的性質,同時制備出金屬硫化物/石墨烯復合材料作為超級電容器的電極材料并研究其電容性質。論文包括下面三個部分:1、不同溶劑下合成的CdS納米材料在光催化性質上的研究比較我們選用Cd(NO_3)_2·4H_2O和C_5H_(10)NNaS2'3H_2O(二乙基二硫代氨基甲酸鈉)分別作為鎘源和硫源,用PVP作為表面活性劑,在室溫的條件下通過化學沉淀法制備出單一來源前驅物。將一定量的前驅物分別在乙二醇和乙二胺溶劑中進行高溫高壓反應,制備出形貌各異的CdS納米材料。采用粉末X-射線衍射儀(XRD)、透射電子顯微鏡(TEM)、掃描電子顯微鏡(SEM)、X射線光電子能譜儀(XPS)、BET比表面積等測試手段對合成樣品的組成、結構、形貌、元素價態(tài)以及比表面積進行分析。用氙燈測試不同樣品對染料羅丹明B(RB)的可見光光催化降解性質。結果表明,不同溶劑下合成的CdS納米材料在催化降解RhB中表現(xiàn)出截然不同的降解特征。通過實驗我們對不同CdS納米材料的光催化機理進行探討與比較。2、水熱法制備花球狀的In_2S_3納米材料及其吸附與光催化性質研究我們選用In(NO_3)_3·xH_2O和C_5H_(10)NNaS2·3H_2O分別作為銦源和硫源,不添加任何表面活性劑,在室溫下通過化學沉淀法制備出單一來源前驅物。將一定量的反應前驅物分散在一定體積的水溶劑里,在高溫高壓反應條件下,制備出花型的In_2S_3納米材料。通過將前驅物在相同的溫度下經(jīng)歷不同的反應時間而得到不同形貌的樣品,從而可以分析并推斷出花型形貌的演變過程。采用XRD、TEM、SEM、XPS以及固體紫外漫反射(UV-visDRS)等測試對合成樣品的組成、結構、形貌、元素價態(tài)、以及可見光吸收等進行表征。選擇最佳形貌的In_2S_3納米材料,BET比表面積結果顯示比表面積高達134.08 m2/g。將花型結構的In_2S_3納米材料作為吸附劑對有機染料甲基藍(MB)進行吸附實驗,同時又作為光催化劑對有機染料甲基橙(MO)和抗生素四環(huán)霉素(TC)進行光催化實驗。結果表明,該花型結構的In_2S_3納米材料有著很高的吸附-光催化性質。同時也對導致該材料高的光催化活性的原因進行了分析與討論。3、水熱法制備NixSy/rGO復合材料及其電化學性質研究我們選用Ni(NO_3)_2·4H_2O和C_5H_(10)NNaS2·3H_2O分別作為鎳源和硫源,不添加任何表面活性劑,在室溫下通過化學沉淀法制備出單一來源前驅物。將前驅物與氧化石墨烯溶液混合并在高溫高壓反應條件下,得到NixSy與還原氧化石墨烯的復合材料。運用SEM、XRD測試對樣品的形貌和組分分別進行表征。結果表明該方法制備出的是多種硫化鎳化合物與還原氧化石墨烯的復合材料�？疾炝瞬煌k源和硫源的量對產(chǎn)物組成的影響。選擇一定配比條件下合成的NixSy/rGO復合材料制作成工作電極,在三電極體系中進行電化學性質測試。結果發(fā)現(xiàn),與石墨烯復合的產(chǎn)物比單獨NixSy產(chǎn)物的電容性質好,同時也意外發(fā)現(xiàn)該單一來源前驅物也有一定的電容性質。
[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.
【學位授予單位】：安徽大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：TB383.1
本文編號：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.
【學位授予單位】：安徽大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：TB383.1
【參考文獻】
相關期刊論文 前4條
1 艾翠玲;周丹丹;張嶸嶸;邵享文;雷英杰;;β-In_2S_3的制備及其太陽光下降解土霉素[J];環(huán)境科學;2015年08期
2 趙雪;邱平達;姜海靜;金振興;蔡克迪;;超級電容器電極材料研究最新進展[J];電子元件與材料;2015年01期
3 何鐵石;趙龍;劉志成;魏穎;金振興;;石墨烯基超級電容器電極材料研究進展[J];電子元件與材料;2011年12期
4 王齊;趙進才;叢燕青;張軼;;無定形TiO_2可見光敏化降解染料污染物[J];催化學報;2011年06期
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