AlOOH核壳、空心球的控制合成与组装及三氧化二铝纳米粉体、薄膜的廉价制备博士毕业论文.doc
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1、中图分类号: 单位代号:10280密 级: 学 号:05820007 博 士 学 位 论 文SHANGHAI UNIVERSITYDOCTORAL DISSERTATION题目AlOOH核壳、空心球的控制合成与组装及Al2O3纳米粉体、薄膜的廉价制备上海大学博士学位论文学位论文原创性声明本人郑重声明:所呈交的论文是本人在导师的指导下独立进行研究所取得的研究成果。除了文中特别加以标注引用的内容外,本论文不包含任何其他个人或集体已经发表或撰写的成果作品。对本文的研究做出重要贡献的个人和集体,均已在文中以明确方式标明。本人完全意识到本声明的法律后果由本人承担。作者签名: 日期: 年 月 日学位论文版
2、权使用授权书本学位论文作者完全了解学校有关保留、使用学位论文的规定,同意学校保留并向国家有关部门或机构送交论文的复印件和电子版,允许论文被查阅和借阅。本人授权 大学可以将本学位论文的全部或部分内容编入有关数据库进行检索,可以采用影印、缩印或扫描等复制手段保存和汇编本学位论文。涉密论文按学校规定处理。作者签名:日期: 年 月 日导师签名: 日期: 年 月 日原 创 性 声 明本人声明:所呈交的论文是本人在导师指导下进行的研究工作。除了文中特别加以标注和致谢的地方外,论文中不包含其他人已发表或撰写过的研究成果。参与同一工作的其他同志对本研究所做的任何贡献均已在论文中作了明确的说明并表示了谢意。 签
3、 名: 日 期: 本论文使用授权说明本人完全了解上海大学有关保留、使用学位论文的规定,即:学校有权保留论文及送交论文复印件,允许论文被查阅和借阅;学校可以公布论文的全部或部分内容。(保密的论文在解密后应遵守此规定)签 名: 导师签名: 日期: 上海大学工学博士学位论文AlOOH核壳、空心球的控制合成与组装及Al2O3纳米粉体、薄膜的廉价制备姓 名:张良苗导 师:陆文聪 教授学科专业:材料学上海大学材料科学与工程学院二零零八年八月A Dissertation Submitted to Shanghai University for the Degree of Doctor in Philosop
4、hyControlled Synthesis and Self-assembly of AlOOH and Low-cost Preparation of Al2O3 Nanopowders and Nanomembranes PhDCandidate:Liangmiao ZHANG Supervisor:Prof. Wencong LUMajor:Materials ScienceSchool of Materials Science and Engineering Shanghai UniversityAugust, 2008摘 要纳米材料因为它们所具有的独特的磁学、电学、光学性质,一直是
5、科学家研究的热点。目前研究的难点是如何合理的控制材料的定向生长,进而实现对其尺寸、维度、组成、晶体结构乃至物性的调控,深入研究结构与物性的关联、并最终实现按照人们的意愿设计合成功能材料。本论文总结了纳米材料的结构、制备、形成机理和性质等方面的进展,把液相合成方法拓展到新颖、特殊结构的设计合成与生长,在研究形成机制及所获得新型纳米结构的物性等方面进行了有益的探索;并在纳米氧化铝粉体、薄膜的廉价制备以及所设计路线工业化生产的可能性方面进行了大胆的尝试。论文中取得了一批创新性成果,主要内容概括如下:1. 建立了纳米Al2O3空心球的乳液界面控制合成新技术,通过对实验过程中影响空心球形成的各种因素进行
6、考察,阐述了其形成机理。表面活性剂的加入量是反应中最重要的影响因素,它影响乳液中水核的存在形状,最终影响产物的形貌。通过增加表面活性剂Span80的量至1.5g,使之形成带状水核,成功合成了竹叶状Cu(OH)2单晶。通过煅烧得到了表面具有纳米孔的CuO纳米带。并对其带状结构的光学性质进行了初步研究,为进一步探索该类独特结构的优异物理化学性质奠定了坚实的基础。2. 利用柠檬酸根可以和很多金属离子络合而控制水解速率及产物结晶方向的特点,在醇-水混合溶剂作用下合成出纳米AlOOH的核壳结构。高倍透射电镜照片显示:其二级结构是由纳米薄片以及其卷曲而成的纳米管组成。核壳结构的形成可归因为酸性条件下表面晶
7、核溶解-再沉淀的过程,不同反应时间产物的透射电镜阐述了这一机制。由于其具有大的比表面积、均一的孔径分布,在吸附与分离、催化等领域将展示良好的应用前景。初步研究表明其在室温条件下显示出较强的对刚果红染料的吸附性能。3. 发展了溶剂热法,选择丙酮-水作混合溶剂,调控合成了AlOOH的空心球。通过SEM,TEM,XRD,BET和PL等手段对产物的结构和形貌进行了表征。深入研究了实验参数对产物形貌的影响,探讨了AlOOH的三维结构的形貌与发光性能之间的关系。通过这些新型纳米结构的合成,发展了一条简单有效的制备金属氧化物核壳及空心球纳米结构的途径,并为新的合成方法学的建立奠定了基础。4. 建立了以废铝料
8、为原料制备高纯度纳米氧化铝的新流程。废铝料经过与硫酸氢铵反应,利用重结晶技术,实现了硫酸铝铵的纯化。硫酸铝铵与碳酸氢铵等反应得到了碳酸铝铵,经过煅烧最终得到了纯度可达99.99%粒径分布集中在49nm的a-Al2O3。并对中间产物碳酸铝铵的合成过程进行实验设计,利用支持向量机方法处理实验数据,得到了控制收率的优化区间。本流程既处理了废料,又为纳米氧化铝的工业化生产找到了一条廉价的工艺路线。5. 建立了从废料中提取的无机盐出发,采用溶胶-凝胶法制备氧化铝纳滤膜的方法。深入研究了影响薄膜开裂的各种影响因素(例如支撑体的孔径大小,氧化铝含量,干燥控制剂的选择和用量,浸渍时间,干燥和煅烧条件等),制得
9、了表面无开裂、无针孔缺陷的不对称膜。并应用数据挖掘方法处理实验数据,得到了不开裂膜制备条件的半经验方程式。关键词:氧化铝,勃姆石,乳液合成,溶剂热合成,一维纳米结构ABSTRACTNanomaterials have drawn continuous research attention because of their unique electrical, optical and magnetic properties different from that of bulk materials. But the main challenge in this area is how to pr
10、ecisely control the sizes, dimensionalities, compositions and crystal structures in nanoscale, which may serve as a powerful tool for the tailoring of physical/chemical properties of materials in a controllable way. In this dissertation, based on the comprehensive and thorough investigation of a lot
11、 of literatures, I gave a concise review on the structures, properties, applications and preparation methods. Following that, solution-based routes were developed to realize the chemical synthesis of special and novel nanomaterials. Furthermore, valuable explorations have been carried out on the res
12、earch on their growth mechanism and properties and attempts have been made on low-cost preparation of alumina nanopowders and the possibilities of large scale production. The research conclusions provide some original and innovative results, and the main points are summarized as follows:1. A new and
13、 feasible emulsion route was established to control the synthesis of Al2O3 hollow spheres. The reaction was accomplished at the organic/aqueous biphasic boundary. Based on a series of comparative experiments under different reaction conditions, the probable formation mechanism of Al2O3 hollow sphere
14、s was proposed to be emulsion-morphology controlled growth process. The Al2O3 hollow spheres could be tailored by using different concentration of surfactant. In addition, Cu(OH)2 bamboo-leaf-like single crystals were successfully synthesized by increasing the surfactant amounts to 1.5g. It could be
15、 converted to a porous structure (CuO) after removing the Span80 molecules via calcination. The optical properties of these CuO nanostructures were studied with UV-vis spectra measurements and found to exhibit blue shifts in UV-vis spectra and possess larger band gaps compared with those of bulk cry
16、stals.2. The AlOOH core/shell microspheres were successfully synthesized in large-scale via a one-step template-free solvothermal route. Most shells of the spheres composed of loosely stacked nanoplatelets and nanotubes as second order structure. Based on the evolution process of the products at var
17、ious stages of the reaction, a possible mechanism was proposed to the formation of core-shell structures, which involved a surface reaction-dissolution-recrystallization process. Citrtate anion, as a coordination agent and shape modifier, plays a key role in determining the morphology of the final p
18、roducts. The as-prepared AlOOH core-shell superstructures are powerful in the removal of Congo red pollutant from waste water. Taking into account the high BET surface area and excellent porous properties, this novel structure is expected to be useful in many other applications, such as catalysts, s
19、orbents, ceramics, and optical nanodevices. 3. A solvothermal method using the mixed solvent of water and acetone was developed to prepare AlOOH hollow spheres. The structure and morphology of the products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), field e
20、mission scanning electron microscopy (FE-SEM), Brunauer-Emmett-Teller (BET) and room-temperature photoluminescence (PL) spectra, etc. The effect of the important experiment parameters on the morphology of the final products was deeply investigated. And we also investigated the dependent relationship
21、 between morphologies and PL. And this work may provide new insights into preparing other inorganic core/shell spheres with complicated structure.4. A new synthetic strategy has been established to prepare nano-alumina of high purity with exhausted aluminum scraps as the raw material. Aluminium ammo
22、nium sulphate (AA) with high purity was obtained via the reaction of aluminum scrap reacted with ammonium bisulfate and recrystallization several times. And aluminium ammonium carbonate hydroxide (AACH) was synthesized via the reaction of AA reacted with ammonium bicarbonate. The precursor was calci
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