纳米硒化物的制备及其电化学性质研究
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摘要
硒化物纳米材料具有良好的光学性质、电学性质、磁学性质、光电及热电性能等,在太阳能电池、红外探测器、光电器件、热电装置、化学传感器等领域有广泛的应用前景。因此,对硒化物纳米材料的合成和性质研究是当前纳米材料研究领域的热点之一。
本文是以预先合成的三方相t-Se纳米管作为反应模板,分别与不同的金属无机盐反应,利用水热法分别合成了硒化铅纳米管、硒化铋纳米管和硒化锡纳米盘,采用扫描电子显微镜(SEM)、X-射线衍射仪(XRD)、X-射线光电子能谱(XPS)、热重分析(TG)等对产物的结构和组成进行了表征,探讨了产物的形成机理,并利用循环伏安法对产物的电化学性质进行了研究。
论文主要内容如下：
1.硒化铅纳米管的制备及其电化学性质研究
首先利用本课题组设计的方法制备t-Se纳米管,然后以t-Se纳米管为反应模板,利用水热合成法将其与Pb(NO3)2反应制备PbSe纳米管。一系列实验结果表明,反应温度和反应物中Pb和Se的不同摩尔比对产物的组成有很大的影响。利用多种表征手段对所得产物的形貌和组成进行了表征,探讨了PbSe纳米管的形成机理。同时,研究了PbSe纳米管在不同介质体系中的电化学性质。
2.硒化铋纳米管的制备及其电化学性质研究
以预先制备的硒纳米管作反应模板,以Bi(N03)3为铋源、N2H4·H20为还原剂,利用水热合成法在160℃的条件下制备了六方相的H-Bi2Se3纳米管。利用SEM、XRD、XPS等现代分析测试手段对所得的产物进行了表征,通过一系列实验,研究了反应温度、反应物之间的摩尔比对产物的影响,并对Bi2Se3纳米管的形成机理进行了探讨。利用线性扫描和循环伏安法研究了Bi2Se3纳米管在不同介质中的电化学行为,考察了扫描范围、扫描速度、电解质溶液等因素对Bi2Se3纳米管电化学性质的影响。
3.硒化锡纳米盘的制备及其电化学性质研究
利用N2H4·H20的强还原性,在水热条件下将混合溶液中的Se4+,Sn2+分别还原为硒纳米粒子和锡纳米粒子。由于新生成的单质硒纳米粒子和单质锡纳米粒子活性很高,因此同时生成的这两种纳米粒子很容易结合形成SnSe2分子。通过一系列的实验,讨论了反应温度和反应物之间的摩尔比对产物的影响,探讨了SnSe2纳米盘的形成机理。最后,研究了SnSe2纳米盘在不同介质体系中的电化学性质。
Selenide nanomaterials have unique optical, electrical, magnetic, photoelectric and thermoelectric properties, which makes them potential applications in solar cells, infrared detectors, photoelectric device, thermoelectric device and chemical sensors. Therefore, the study for selenide nanomaterials is a hot point in nanomaterial field.
In this paper, PbSe nanotubes, Bi2Se3 nanotubes and SnSe2 nanoplates were respectively prepared by hydrothermal synthesis, in which the t-Se nanotubes were used as engaged-template that reacted with relevant metal ions. The selenides as-obtained were characterized by Scanning Electron Microscope (SEM), X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Thermogravimetric Analysis (TGA), etc. Furthermore, the formation mechanism of selenide nanomaterials was disscussed, and their electrochemical property was studied by the cyclic voltammetry.
Our main work as follows:
1. Synthesis and Electochemical Behavior of PbSe nanotubes
First, the t-Se nanotubes were synthesized as our report. Then, with the hydrothermal synthesis, the t-Se nanotubes as-obtained were used as template reagent that reacted with Pb(NO3)2 to form PbSe nanotubes. Through a series of experiments, it was found that the reaction temperature and the molar ratio of reactants play an important role in formation of the PbSe nanotubes. The products obtained were characterized by XRD, TEM, SEM, XPS, etc. In addition, the formation mechanism and electochemical property of the PbSe nanotubes were studied.
2. Synthesis and Electochemical property of Bi2Se3 nanotubes.
By using the t-Se nanotubes prepared, Bi(NO3)3, and N2H4·H2O as Se source, Bi source and reducing agent respectively, the hexagon Bi2Se3 nanotubes were obtained at 160℃with hydrothermal synthesis. The products as-obtained were characterized by XRD, TEM, SEM, XPS, etc. Based on a series of experiments and characterizations, the effect factors and the formation mechanism of the Bi2Se3 nanotubes were discussed. Furthermore, the electrochemical behavior of the Bi2Se3 nanotubes was studied by the voltammetric technique in different medium, and the effect factors on the cyclic voltammograms of Bi2Se3 nanotubes, such as potential region, scan rate and the acidity of electrolyte solution, were discussed.
3. Synthesis and Electochemical property of SnSe2 nanoplates.
Depending on the strong deoxidization of N2H4 H2O, the Se4+ and Sn2+ in solution were respctively reduced to Se and Sn nanoparticles under hydrothermal condition. These fresh elemental nanoparticles, with high reactivity, could react with each other to form SnSe2 nanoparticles. The products as-obtained were characterized by XRD, TEM and SEM. By a series of experiments, the effect of the reaction temperature and the molar ratio of Sn and Se in precursors on the phase and composition of product was studied, and the formation mechanism of the SnSe2 nanoplates was disscussed. Finally, we also studied the electochemical property of the SnSe2 nanoplates.
本文是以预先合成的三方相t-Se纳米管作为反应模板,分别与不同的金属无机盐反应,利用水热法分别合成了硒化铅纳米管、硒化铋纳米管和硒化锡纳米盘,采用扫描电子显微镜(SEM)、X-射线衍射仪(XRD)、X-射线光电子能谱(XPS)、热重分析(TG)等对产物的结构和组成进行了表征,探讨了产物的形成机理,并利用循环伏安法对产物的电化学性质进行了研究。
论文主要内容如下：
1.硒化铅纳米管的制备及其电化学性质研究
首先利用本课题组设计的方法制备t-Se纳米管,然后以t-Se纳米管为反应模板,利用水热合成法将其与Pb(NO3)2反应制备PbSe纳米管。一系列实验结果表明,反应温度和反应物中Pb和Se的不同摩尔比对产物的组成有很大的影响。利用多种表征手段对所得产物的形貌和组成进行了表征,探讨了PbSe纳米管的形成机理。同时,研究了PbSe纳米管在不同介质体系中的电化学性质。
2.硒化铋纳米管的制备及其电化学性质研究
以预先制备的硒纳米管作反应模板,以Bi(N03)3为铋源、N2H4·H20为还原剂,利用水热合成法在160℃的条件下制备了六方相的H-Bi2Se3纳米管。利用SEM、XRD、XPS等现代分析测试手段对所得的产物进行了表征,通过一系列实验,研究了反应温度、反应物之间的摩尔比对产物的影响,并对Bi2Se3纳米管的形成机理进行了探讨。利用线性扫描和循环伏安法研究了Bi2Se3纳米管在不同介质中的电化学行为,考察了扫描范围、扫描速度、电解质溶液等因素对Bi2Se3纳米管电化学性质的影响。
3.硒化锡纳米盘的制备及其电化学性质研究
利用N2H4·H20的强还原性,在水热条件下将混合溶液中的Se4+,Sn2+分别还原为硒纳米粒子和锡纳米粒子。由于新生成的单质硒纳米粒子和单质锡纳米粒子活性很高,因此同时生成的这两种纳米粒子很容易结合形成SnSe2分子。通过一系列的实验,讨论了反应温度和反应物之间的摩尔比对产物的影响,探讨了SnSe2纳米盘的形成机理。最后,研究了SnSe2纳米盘在不同介质体系中的电化学性质。
Selenide nanomaterials have unique optical, electrical, magnetic, photoelectric and thermoelectric properties, which makes them potential applications in solar cells, infrared detectors, photoelectric device, thermoelectric device and chemical sensors. Therefore, the study for selenide nanomaterials is a hot point in nanomaterial field.
In this paper, PbSe nanotubes, Bi2Se3 nanotubes and SnSe2 nanoplates were respectively prepared by hydrothermal synthesis, in which the t-Se nanotubes were used as engaged-template that reacted with relevant metal ions. The selenides as-obtained were characterized by Scanning Electron Microscope (SEM), X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Thermogravimetric Analysis (TGA), etc. Furthermore, the formation mechanism of selenide nanomaterials was disscussed, and their electrochemical property was studied by the cyclic voltammetry.
Our main work as follows:
1. Synthesis and Electochemical Behavior of PbSe nanotubes
First, the t-Se nanotubes were synthesized as our report. Then, with the hydrothermal synthesis, the t-Se nanotubes as-obtained were used as template reagent that reacted with Pb(NO3)2 to form PbSe nanotubes. Through a series of experiments, it was found that the reaction temperature and the molar ratio of reactants play an important role in formation of the PbSe nanotubes. The products obtained were characterized by XRD, TEM, SEM, XPS, etc. In addition, the formation mechanism and electochemical property of the PbSe nanotubes were studied.
2. Synthesis and Electochemical property of Bi2Se3 nanotubes.
By using the t-Se nanotubes prepared, Bi(NO3)3, and N2H4·H2O as Se source, Bi source and reducing agent respectively, the hexagon Bi2Se3 nanotubes were obtained at 160℃with hydrothermal synthesis. The products as-obtained were characterized by XRD, TEM, SEM, XPS, etc. Based on a series of experiments and characterizations, the effect factors and the formation mechanism of the Bi2Se3 nanotubes were discussed. Furthermore, the electrochemical behavior of the Bi2Se3 nanotubes was studied by the voltammetric technique in different medium, and the effect factors on the cyclic voltammograms of Bi2Se3 nanotubes, such as potential region, scan rate and the acidity of electrolyte solution, were discussed.
3. Synthesis and Electochemical property of SnSe2 nanoplates.
Depending on the strong deoxidization of N2H4 H2O, the Se4+ and Sn2+ in solution were respctively reduced to Se and Sn nanoparticles under hydrothermal condition. These fresh elemental nanoparticles, with high reactivity, could react with each other to form SnSe2 nanoparticles. The products as-obtained were characterized by XRD, TEM and SEM. By a series of experiments, the effect of the reaction temperature and the molar ratio of Sn and Se in precursors on the phase and composition of product was studied, and the formation mechanism of the SnSe2 nanoplates was disscussed. Finally, we also studied the electochemical property of the SnSe2 nanoplates.
引文
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