纳米硫化物和氧化物的湿化学合成与形貌控制研究
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摘要
纳米结构及其相关的复合结构具有许多有趣的与尺寸和形貌相关的性能。利用纳米结构材料的特殊性能可以设计全新的电子、光子、传感等纳米器件,具有广阔的潜在应用前景。本论文针对己有纳米材料制备方法存在的工艺复杂、成本较高的问题,采用设备条件要求不高、适应性强的湿化学方法,选择典型的半导体材料为研究对象,通过对反应介质、结构导向剂以及制备工艺的精心选择和设计,在相对温和、简单的条件下实现了对纳米材料在尺寸和形貌等方面的可控合成,并对生长机理进行了探讨。论文主要内容归纳如下:
1.采用水热法成功合成了Mn~(2+)掺杂MS(M=Zn、Cd)纳米棒,探讨了Mn~(2+)含量对光谱性能的影响。结果表明随着Mn~(2+)含量的增加,其直径基本不变,但长度变短,形貌变的较杂乱,并且伴随有颗粒产生。MS纳米棒的紫外吸收光谱和荧光光谱都逐渐红移,表明Mn~(2+)是一种重要的光谱调节元素,能有效的调节MS纳米棒的光学性能。
采用十二烷基苯磺酸钠辅助水热法制备了ITO交叉棒。研究了不同温度下合成的前驱体的微结构和形貌,并在此基础上对粉末择优取向生长机理进行了探讨。结果表明,在113℃下合成的前驱体的择优取向最为明显,该温度下前驱体的生长主要沿着[100]晶向择优取向并且具有最好的空间交叉棒形貌。提出了水热合成过程中产生的密实粒子或短棒以“棒-棒”相接的生长模式形成更长的棒状或者交叉棒的生长机理。
2.利用简单的自组装化学反应,将CuS均匀地包覆于PSA乳胶粒模板的表面,形成PSA/CuS的核/壳结构微球,用有机溶剂溶去PSA乳胶粒模板后,可以得到壳厚20nm、孔直径120nm且大小均匀表面光滑的CuS空心微球。采用超声振动法,利用PEG作为结构诱导软模板成功制备了Bi_2S_3纳米棒,分析了不同时间Bi2S3纳米棒的生长形貌,提出了“粒子-粒子”自组装连接生成Bi2S3纳米棒的生长机理,并通过紫外吸收光谱估算出了Bi_2S_3纳米棒的光学带隙宽度。
3.采用乙二胺/水溶剂热法,选择不同的硫源,合成了具有双层十二对称结构的Cu_(2-x)S晶体,探讨了不同乙二胺/水体积比对形貌的影响,提出了双层十二对称结构是源于六边形微盘组装而成的生长机理。
采用二甘醇溶剂热法合成了包含少量水合氯化铟(InCl_3·3H_2O)的In(OH)_3晶体,它们可呈现出棉花状、刺球状和海胆状复杂而有趣的形貌,探讨了温度对形貌变化的影响及相应的生长过程。
4.采用微乳液法,通过调节微乳液中起始溶液的pH值,合成了CeO_2的纳米球和纳米棒晶体。分析了样品的组成和结构,探讨了形貌对CeO_2纳米晶的比表面积和光谱性能的影响,估算了不同形貌CeO_2纳米晶的光学带隙宽度。
5.采用水热法制备了聚合物PVP表面修饰ZnO纳米棒,比较了改性前后ZnO纳米棒的晶体结构和光学性质。结果表明,PVP对改性后对ZnO的晶体结构影响不大,但增加了ZnO纳米棒在紫外区域的吸收,而对其在紫外区域的屏蔽能力和在可见光区域的透过能力影响不大。353nm处弱的发射峰表明ZnO晶体的表面已经被钝化,与氧有关的缺陷被PVP所修饰。
Nanomaterials and relatived composites have many interesting properties relating size and morphology. Novel electrons, photons and sensors can be designed by their especial structure. Most of the developed synthetic routes to nanomaterials are complicated in process, expensive in cost, this work of the dissertation has explored a series of new wet chemical methods, which present low requirements in equipment and strong adaptability, to synthesize some typical semiconductor nanocrystals with controllable sizes and morphologies under relatively mild and simple conditions by carefully selecting the reaction media, structure-directing agents and processes. Relatived mechanisms were discussed. The main points can be summarized as follows:
1. Mn~(2+) doped MS(M=Zn, Cd) nanorods were successfully synthesized through hydrothermal route. With the increase of Mn~(2+) in the samples, the morphology of products become disorder accompanying some nanoparticles. The diameter of nanorods retains almost the same, but the length becomes shorter. Mn~(2+) enters the position of M2+(M=Zn, Cd) by substitution. Both the absorption band edge and the PL emission spectroscopy of MS nanorods shifted gradually to longer wavelength with the increase of Mn~(2+). The results confirm that the doped Mn~(2+) is the major luminescent component and can effectively adjust the optical properties of ZnS nanorods.
Indium-tin oxide (ITO) precursor powderswere synthesized by hydrothermal method. The effects of temperature on the preferred orientation morphologies of the precursor powders were studied. Thereby their preferred orientation growth mechanisms were deduced. The effects of temperature on the phase structures and morphologies of the precursors were remarkable. ITO precursors synthesized at 113℃had the most obvious preferred orientation and grew mainly along the [100] direction and exhibited the best morphology of intersecting-rods.
2. CuS hollow spheres with a wall thickness about 20 nm and a pore diameter about 150 nm have been successfully prepared using the PSA latex template approach by a layer-by-layer self-assembly technique. Growth mechanism of CuS hollow spheres was discussed.
Bi2S3 nanorods has successfully fabricated by sonochemical aqueous solution using PEG as structure-directing agent. The Bi2S3 nuclei show an obvious tendency to arrange themselves in rod-like arrays over extended length scales under soft template. The growth mode of particle?to?particle by self-assembly under soft template is proposed. The band gap energy of Bi_2S_3 nanorods was estimated at about 1.36 eV by UV-Vis absorption spectroscopy.
3. Novel twelve-fold symmetrical Cu2-xS single crystals were synthesized by En/H2O solvothermal process,, and they were built up by two layers of about 80–100 nm in thickness. The possible growth process had been discussed. In(OH)3 with cotton-like, bur-like and pod-like morphologies were synthesized at different temperatures by diglycol-mediated solvothermal processes. The effect of temperature on morphology was discussed and growth mechanism was proposed.
4. CeO2 nanocrystals with different morphologies were synthesized by adjusting the pH value of the starting solution in water-in-oil microemulsion. Results show that the morphologies of CeO_2 were transformed from granular, to spherical, and to rod-like with the pH of the starting solution varying from 5, to 8, and to11. All samples were indexed to the phase of CeO_2 and Ce(OH)_4, and the molar ratio of CeO_2 to Ce(OH)_4 could be deduced about 0.25. The morphologies of CeO_2 nanocrystals had a little influence on the specific surface area, UV-Vis spectra and PL spectra. The band gap energies of different morphological samples were estimated by UV-Vis spectroscopic method.
5. ZnO nanorods modified by PVP were obtained by hydrothermal technique. Comparison of the amount of ZnO nanorods synthesized in the presence or absence of PVP reveals that PVP plays an important role in the preparation ZnO nanorods, but doesn’t alter the crystalline structure of ZnO. The optical property of the ZnO nanomaterials could be modified by PVP. ZnO nanorods increase in absorption at UV region, and don’t influence the UV-shielding ability and transparency in the visible light region of ZnO. A weak UV emission at 353 nm of PL spectra exhibits the surface of ZnO is passivated and oxygen-related defects were supplied by PVP.
1.采用水热法成功合成了Mn~(2+)掺杂MS(M=Zn、Cd)纳米棒,探讨了Mn~(2+)含量对光谱性能的影响。结果表明随着Mn~(2+)含量的增加,其直径基本不变,但长度变短,形貌变的较杂乱,并且伴随有颗粒产生。MS纳米棒的紫外吸收光谱和荧光光谱都逐渐红移,表明Mn~(2+)是一种重要的光谱调节元素,能有效的调节MS纳米棒的光学性能。
采用十二烷基苯磺酸钠辅助水热法制备了ITO交叉棒。研究了不同温度下合成的前驱体的微结构和形貌,并在此基础上对粉末择优取向生长机理进行了探讨。结果表明,在113℃下合成的前驱体的择优取向最为明显,该温度下前驱体的生长主要沿着[100]晶向择优取向并且具有最好的空间交叉棒形貌。提出了水热合成过程中产生的密实粒子或短棒以“棒-棒”相接的生长模式形成更长的棒状或者交叉棒的生长机理。
2.利用简单的自组装化学反应,将CuS均匀地包覆于PSA乳胶粒模板的表面,形成PSA/CuS的核/壳结构微球,用有机溶剂溶去PSA乳胶粒模板后,可以得到壳厚20nm、孔直径120nm且大小均匀表面光滑的CuS空心微球。采用超声振动法,利用PEG作为结构诱导软模板成功制备了Bi_2S_3纳米棒,分析了不同时间Bi2S3纳米棒的生长形貌,提出了“粒子-粒子”自组装连接生成Bi2S3纳米棒的生长机理,并通过紫外吸收光谱估算出了Bi_2S_3纳米棒的光学带隙宽度。
3.采用乙二胺/水溶剂热法,选择不同的硫源,合成了具有双层十二对称结构的Cu_(2-x)S晶体,探讨了不同乙二胺/水体积比对形貌的影响,提出了双层十二对称结构是源于六边形微盘组装而成的生长机理。
采用二甘醇溶剂热法合成了包含少量水合氯化铟(InCl_3·3H_2O)的In(OH)_3晶体,它们可呈现出棉花状、刺球状和海胆状复杂而有趣的形貌,探讨了温度对形貌变化的影响及相应的生长过程。
4.采用微乳液法,通过调节微乳液中起始溶液的pH值,合成了CeO_2的纳米球和纳米棒晶体。分析了样品的组成和结构,探讨了形貌对CeO_2纳米晶的比表面积和光谱性能的影响,估算了不同形貌CeO_2纳米晶的光学带隙宽度。
5.采用水热法制备了聚合物PVP表面修饰ZnO纳米棒,比较了改性前后ZnO纳米棒的晶体结构和光学性质。结果表明,PVP对改性后对ZnO的晶体结构影响不大,但增加了ZnO纳米棒在紫外区域的吸收,而对其在紫外区域的屏蔽能力和在可见光区域的透过能力影响不大。353nm处弱的发射峰表明ZnO晶体的表面已经被钝化,与氧有关的缺陷被PVP所修饰。
Nanomaterials and relatived composites have many interesting properties relating size and morphology. Novel electrons, photons and sensors can be designed by their especial structure. Most of the developed synthetic routes to nanomaterials are complicated in process, expensive in cost, this work of the dissertation has explored a series of new wet chemical methods, which present low requirements in equipment and strong adaptability, to synthesize some typical semiconductor nanocrystals with controllable sizes and morphologies under relatively mild and simple conditions by carefully selecting the reaction media, structure-directing agents and processes. Relatived mechanisms were discussed. The main points can be summarized as follows:
1. Mn~(2+) doped MS(M=Zn, Cd) nanorods were successfully synthesized through hydrothermal route. With the increase of Mn~(2+) in the samples, the morphology of products become disorder accompanying some nanoparticles. The diameter of nanorods retains almost the same, but the length becomes shorter. Mn~(2+) enters the position of M2+(M=Zn, Cd) by substitution. Both the absorption band edge and the PL emission spectroscopy of MS nanorods shifted gradually to longer wavelength with the increase of Mn~(2+). The results confirm that the doped Mn~(2+) is the major luminescent component and can effectively adjust the optical properties of ZnS nanorods.
Indium-tin oxide (ITO) precursor powderswere synthesized by hydrothermal method. The effects of temperature on the preferred orientation morphologies of the precursor powders were studied. Thereby their preferred orientation growth mechanisms were deduced. The effects of temperature on the phase structures and morphologies of the precursors were remarkable. ITO precursors synthesized at 113℃had the most obvious preferred orientation and grew mainly along the [100] direction and exhibited the best morphology of intersecting-rods.
2. CuS hollow spheres with a wall thickness about 20 nm and a pore diameter about 150 nm have been successfully prepared using the PSA latex template approach by a layer-by-layer self-assembly technique. Growth mechanism of CuS hollow spheres was discussed.
Bi2S3 nanorods has successfully fabricated by sonochemical aqueous solution using PEG as structure-directing agent. The Bi2S3 nuclei show an obvious tendency to arrange themselves in rod-like arrays over extended length scales under soft template. The growth mode of particle?to?particle by self-assembly under soft template is proposed. The band gap energy of Bi_2S_3 nanorods was estimated at about 1.36 eV by UV-Vis absorption spectroscopy.
3. Novel twelve-fold symmetrical Cu2-xS single crystals were synthesized by En/H2O solvothermal process,, and they were built up by two layers of about 80–100 nm in thickness. The possible growth process had been discussed. In(OH)3 with cotton-like, bur-like and pod-like morphologies were synthesized at different temperatures by diglycol-mediated solvothermal processes. The effect of temperature on morphology was discussed and growth mechanism was proposed.
4. CeO2 nanocrystals with different morphologies were synthesized by adjusting the pH value of the starting solution in water-in-oil microemulsion. Results show that the morphologies of CeO_2 were transformed from granular, to spherical, and to rod-like with the pH of the starting solution varying from 5, to 8, and to11. All samples were indexed to the phase of CeO_2 and Ce(OH)_4, and the molar ratio of CeO_2 to Ce(OH)_4 could be deduced about 0.25. The morphologies of CeO_2 nanocrystals had a little influence on the specific surface area, UV-Vis spectra and PL spectra. The band gap energies of different morphological samples were estimated by UV-Vis spectroscopic method.
5. ZnO nanorods modified by PVP were obtained by hydrothermal technique. Comparison of the amount of ZnO nanorods synthesized in the presence or absence of PVP reveals that PVP plays an important role in the preparation ZnO nanorods, but doesn’t alter the crystalline structure of ZnO. The optical property of the ZnO nanomaterials could be modified by PVP. ZnO nanorods increase in absorption at UV region, and don’t influence the UV-shielding ability and transparency in the visible light region of ZnO. A weak UV emission at 353 nm of PL spectra exhibits the surface of ZnO is passivated and oxygen-related defects were supplied by PVP.
引文
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