摘要
硒是重要的半导体材料,同时也是生命的必需元素,而纳米尺寸的硒所具有的在材料上的独特性能和在生命中的特殊生物活性更是引起了人们对硒化学的研究热潮。化学液相纳米合成技术具有方法简单、产品的化学组成易控制等优点,在纳米材料的制备方面显示了广阔的应用前景。本论文用几种低温液相合成技术制备纳米硒,旨在寻找有效控制合成各种结构纳米硒的方法。
1.反相微乳液法:以十二烷基硫酸钠为表面活性剂,正丁醇为助表面活性剂,环己烷为溶剂,以硒代硫酸钠的歧化反应为基础制备纳米硒,得到了粒径较均匀的球形颗粒和长径比较大的纳米线。讨论了影响产物形貌的因素和产物形成的机理。
2.有机介质超声法:以无水乙醇作为反应介质,在超声波作用下合成纳米硒,得到了由球形α-晶形硒定向聚集成的纳米线。在聚乙二醇辛基苯基醚(OP)介质中,超声法合成了微米级的OP-Se复合球结构。
3.水溶液体系表面活性剂模板法:以聚乙烯吡咯烷酮(PVP)为模板,用浓HCI自然扩散法和沉淀法,合成了球形、棒状和线状的的纳米硒。分别以十二烷基硫酸钠(SDS)、聚乙二醇辛基苯基醚(OP)、氯代十六烷基吡啶、聚丙烯酰胺、L—苯丙氨酸为模板,用沉淀法合成了线状和球形纳米硒。对模板的保护诱导作用作了阐述,对纳米线的形成路线作了总结。
4.Ag核诱导法:在PVP的保护下以生成的Ag核为晶种合成纳米硒,得到了Se的棒状结构,并有Se纳米管的存在。对Ag核的诱导作用进行了分析与讨论。
Selenium (Se) is not only an important semiconductor material but also an essential element in life. The Se nanoparticles have aroused great interest due to its special properties on material and biological activity in life. In synthesizing Se nanoparticles, chemical technology with low temperature liquid phase, which possesses some virtues such as low reaction temperature, low cost as well as high control ability for the morphology of products, has received much attention. In this thesis, some chemical approaches with low temperature liquid phase have been employed to prepare Se nanoparticles and varied Se nanoparticles were obtained.
1. Reverse microemulsion method Se nanoparticles were prepared by using sodium dodecane (SDS) as surfactant, n-butanol as aid-surfactant and cyclohesane as solvent. The reaction was based the reduction of Na2SeSO3 to elemental Se in acid environment. The uniform spherical Se nanoparticles and Se nanowires were obtained. The factors affecting the morphologies of the products and the formation mechanism of Se nanoparticles were discussed.
2. Organic-medium ultrasonic method Se nanoparticles were prepared under ultrasound irradiation condition in organic solvent. One-dimension selenium nonostructures were obtained under ultrasound irradiation condition in ethanol medium. Spherical OP-Se micronscale compound was prepared under ultrasound irradiation condition in OP medium.
3. Aqueous method using surfactants as soft templates Using polyvinylpyrrolidone (PVP) as a template, Se nanoparticles with various morphologies, such as nanospheres, nanorods and nanowires, were prepared in HCl-diffusing method and precipitation method. Se nanospheres and nanowires were also obtained using other surfactants as templates, such as sodium
dodecylsulfate, polyethylene glycol tert-octylpheneylether, hexadecyl pyridinium chloride, polyacrylamide and L-phenyl alanine. The function of templates to the formation of nanoparticles and the synthesis mechanism were discussed.
4. Ag crystal nucleus method Se nanoparticles were prepared by using Ag crystal nucleus as inducing reagent in the presence of PVP. Se nanorods containing nanotubes were obtained. The function of Ag crystal nucleus was studied.
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