节点文献
功能材料的制备与组装
【作者】 朱琳；
【导师】 李志华；
【作者基本信息】 山东师范大学 ， 物理化学， 2011， 硕士
【摘要】 空心纳米材料和稀土钒酸盐材料是功能钠米材料的主要组成部分。空心结构材料具有低密度、高比表面、热力学稳定性、单分散性、良好的生物相容性以及空心部分能容纳其他材料等优点。其在药物运载与释放、催化剂、光子晶体、纳米粒子合成反应器等领域有重要的应用,已成为当今纳米材料的前沿和热点。稀土钒酸盐材料在紫外灯照射下具有稳定的发光效率,在PDP和FED等领域有着广泛的应用,被认为是很有使用价值的发光基质。随着纳米材料技术的发展,钒稀土发光材料也步入新的研究领域。本文主要通过常温酸腐蚀法、水热合成法、溶剂热法分别制备了介孔材料,空心材料、稀土发光材料,并对所制备的材料进行了XRD,TEM,SEM,TGA,EDS等结构表征,对部分实验反应机理进行了探讨。本论文主要包括以下几部分:1以SiO2为模板,PVP为表面活性剂,在常温下采用酸侵蚀的方法制备多孔的具有空腔结构的二氧化硅球,产物分散性好,大小均匀。采用TEM、FTIR、TGA/DTA对制备的产物进行表征,系统的分析了反应条件的影响,并对反应机理进行解释.2利用水热法合成出空心结构的SiO2?Ln2O3纳米材料。本实验的创新在于酸性条件下合成,不同与一般文献报道的碱性环境,并系统分析反应时间、稀土的浓度对产物形貌的影响。采用TEM、HRTEM、SEM、XRD对制备的产物进行表征,并解释了反应机理,对掺Eu的SiO2空心球进行荧光测试。由于空心球的表面具有多孔性,我们进行药物释放试验。实验结果表明SiO2空心球具有较高的载药量,释放前后药物的性质未发生变化,可以用作布洛芬释放的药物载体。3采用溶剂热法,制备了发光YVO4 : Eu纳米球。本实验选用DMF为反应的溶剂可以降低稀土盐的水解率,从而较为容易控制反应条件。通过优化、调整反应条件,实现了具有发光效应的YVO4:Eu纳米球的制备,并对反应过程进行了研究。通过试验总结了pH、反应时间对产物形貌的影响,颗粒大小在30 nm左右。并通过XRD、TEM、FTIR、固体荧光光谱对样品进行表征。
【Abstract】 As an important component of the functional material, hollow materials and vanadium rare-earth luminescence materials are applied with a great value.Hollow nanostructures have been one of the research frontier. They have the advantages of low density、high specific surface area、thermal stability、monodispersity、good compatibilities with other materials and different material can be combined into the hollow interiors et al. So they play an important role in our life.Such as delivery vehicle of drugs、efficient catalyst、photonic building and the reactor of the nanoparticles.The vanadium rare-earth luminescence materials have their stable luminous efficiency illuminated by vacuum ultraviolet and successfully applied in the field of PDP and FED .With the development of the nanotechnology , the vanadium rare-earth luminescence materials will step into a new step development phase.In this paper, porous silica , hollow materials and rare-earth luminescence materials were prepared via acid etching method , hydrothermal synthesis and solvothermal method , and by applying various characterizing methods, such as XRD, TEM, SEM, TGA, EDS et al. Some experiments are discussed about the reaction mechanism. The main contents were as follows:1 Well dispersed porous silica spheres were prepared via acid etching method .The reaction conditions were as follows: SiO2 as the template ,HF aqueous solution, PVP as the surfactant The products were characterized by means of transmission electron microscopy(TEM) ,Fourier transform infrared(FTIR)and DTA/TGA.The reaction mechanism was also explored.2 Hydrothermal method has been employed to fabricated hollow-structure SiO2:Ln materials. This experiment’s innovation is that the hollow materials are prepared under acidic condition, which is different from the report in the literature of alkaline condition. We also studied impact of the particles prepared in the condition ,the reaction temperature and the concentration of Ln3+ were the important influencing factors. The structure of the proucts was characterized by TEM , HRTEM, SEM, XRD.The optical properties of Eu-doped fluorescent silica were also characterized by flourence.Due to the porousness in the surface of the silica, the drug releasing and loading behaviors of hollow silica. were also studied.Through the testing ,the resuluts indicated that the hollow silica has high storage capacities and favorable drug released behavior.It is important that the properties of the drugs were not changed in the loading and released process.The synthesized hollow silica has potential for controlled drug IBU deliverty.3 The YVO4 : Eu were prepared under the solvothermal condition using the DMF as the solvent which can decrease the rate of the hydrolysis rate of Re salts.so that the reaction process can be controlled easily. Through optimizing the reaction conditions, monodispersed YVO4:Eu spheres were obtained and the reaction process were explored.,pH and reaction time were also discussed, the YVO4:Eu spheres diameters were about 30nm. The structure was characterized by TEM, SEM, and so on.