【作者】 宋吉明；

【导师】 张胜义；

【作者基本信息】 安徽大学 ， 无机化学， 2005， 硕士

【摘要】 科学技术的迅速发展,对材料提出了更高的要求。为了克服单一材料的局限性,获得各种特殊性能的新材料,人们越来越多地借助于复合技术。材料的复合不仅能减少贵重原料的使用量,降低制备成本,而且还能使材料优势互补,获得性质优异的新材料。由固-气、气-液、液-固、液-液、固-固等不同物相接触所形成的界面具有独特的结构和性质,借助界面来制备复合材料、纳米材料是当前材料研究领域的热点之一。本论文就是利用液-液界面的特殊结构和性质,让纳米微粒在该界面上生长,制备了不同形貌的纳米硒、纳米铜、纳米银及纳米级硒-铜、硒-银复合物,对界面生长机理进行了探讨,并研究了所得产物的光电性质等。 1.纳米硒的制备及表征:以二氧化硒为硒源,用水合肼还原,同时加入一定量的表面活性剂,以防止纳米粒子的团聚。向反应后的溶液中加入正丁醇,振荡,静置,形成油-水界面,纳米粒子聚集在界面上生长。考察了温度、还原剂用量、超声、表面活性剂的种类等因素的影响。制得了棒、线、球形纳米粒子。并用透射电镜(TEM)、扫描电镜(SEM)、热重-差热(TG-DSC)、X-射线粉末衍射(XRD)、紫外-可见分光光度法(UV-Vis)等分析测试技术对样品进行了表征。 2.纳米铜的制各及表征:用硫酸铜溶液与适当的还原剂反应,在表面活性剂聚乙烯吡咯烷酮(PVP)的存在下制得铜纳米粒子,然后使初始产物在正丁醇-水界面生长,制得了球形、带状、棒状、片状等不同形貌的纳米铜。在纳米材料制备过程中,创造性地引入亚硫酸钠作抗氧剂,成功地除去了溶液中的氧;通过调节溶液的酸碱度控制还原剂的电位,避免了氧化铜及氧化亚铜的生成,得到了纯净的纳米铜。用TEM、SEM、UV、XRD对样品进行了表征。 3.纳米银的制各及表征:由于银离子是一种较强的氧化剂,在水溶液中见光易分解。本章采用银氨溶液作为氧化剂代替硝酸银,以葡萄糖作还原剂,该体系反应温和,易于控制。通过界面生长,制各了均匀球形、等腰三角形、梯形、六边形等银纳米粒子,用TEM、SEM、UV、XRD表征了产物的形貌,研究了产物的物相和光电性质。 4.纳米硒-铜、硒-银复合物的制备及表征:在上述实验的基础上,选用一种还原更多还原

【Abstract】 Nowadays, more and more nano-materials with excellent quality are demanded due to the rapid development of the science and technology. In order to obtain new nano-materials with good functions, the complex technology has often been applied. The complex technology can not only reduce the amount of expensive material, but also make the new materials more excellent than single material. The interfaces formed between different substances such as solid-gas, gas-liquid, liquid-solid, liquid-liquid, have particular structures and properties. The preparation of complex materials and nano-materials by interface-growth has attracted much attention. In this thesis, various nanoparticles with different morphologies, such as selenium, copper, sliver and the composites of selenium-copper, selenium-sliver, were prepared by liquid-liquid interface-growth process. The interface-growth mechanism of nanoparticles has been discussed and the photoelectric properties of the products have been determined.1. Preparation and characterization of Se nanoparticles: In water solution, SeO2 was first deoxidized into elemental Se by hydrazine monohydrate in the existence of surfactant. Then n-butanol was added into the reaction solution under stirring. Rod-like, sting-like and sphere-like Se nanostructures were obtained by the butanol-water interface-growth process. The effect factors such as temperature, the amount of reducing agent, ultrasound, surfactants were discussed. The products obtained were characterized with transmission electron microscopy(TEM), scanning electron microscopy (SEM) , thermogravimetry(TG) , differential scanning calorimetry (DSC), ultra-violet-visible (UV-Vis) and x-ray diffraction ( XRD) .2. Preparation and characterization of Cu nanoparticles: Cu nanoparticles were prepared through the reduction of CuSO4 by proper reducing agent inaqueous solution. Other conditions like the ones mentioned above. In order to avoid the oxidation of Cu in aqueous solution, sodium sulfite(Na2SO3) was used to get ride of the oxygen. Using polyvinylpyrrolidone (PVP) as the soft template. Cu nanoparticles with different morphologies, such as particle-like, rod-like, bolt-like, dendrite-like, flake-like, were obtained through liquid-liquid interface growth process. The products were characterized with TEM、 SEM、 UV-Vis and XRD.3. Preparation and characterization of Ag nanoparticles : Through the reaction of [Ag (NH3) 2]+ with mild reducer glucose, Ag nanoparticles with uniform sphericity, isosceles triangle, trapezium and hexagon, were prepared by liquid-liquid interface-growth process. The morphology, material phase and photoelectric property of the products have been studied.4. Preparation and characterization of Se-Ag and Se-Cu composites: The solution of Se(Ⅳ)-Cu(Ⅱ) or Se(Ⅳ)-Ag(Ⅰ) was deoxidized with single reducing agent. Se nanoparticles could react with Cu nanoparticles producing CuSe nanoparticles because nanoparticles have higher activity than its bulk. The results of characterization have indicated that the products with different component were obtained in liquid-liquid interface by adjusting the proportion of Se and Cu or Ag. Interestingly, the nanoparticles with core/sphere and double layers were also obtained in the synthesis of Se-Ag complex.更多还原