摘要
本论文旨在补充和发展无机微纳结构材料的合成与组装方法，利用前驱体煅烧路线控制合成多孔无机材料，以及利用生物分子模板法设计制备微纳结构的仿生材料。研究中，通过调节实验选用合理的合成路线，制备了微纳结构的多孔氧化物(氧化镁，氧化铜)和无机仿生材料(硫化镉和氧化锌)，并对其形貌尺寸的控制和合成机理进行了探索性的研究。论文主要内容总结如下：
1．利用生物小分子甘氨酸作模板，硝酸铜水溶液作铜源，制备了大孔的氧化铜。利用溶剂、反应温度、铜源和反应物浓度等实验参数对产物的影响，对CuO产物的形貌实现了有效的控制，并在前人工作和实验结果的基础上提出了大孔CuO可能的生长机理。此外，用甘氨酸为模板，还通过水热过程成功地合成了CdS树枝晶。
2．在前人研究的基础上，将模板法和煅烧技术相结合用于多孔金属氧化物的制备。利用不同的高分子聚合物，比如聚乙烯吡咯烷酮(PVP)，葡聚糖为模板试剂，研究其对反应途径的影响，实现了对多孔MgO形貌的有效控制。实验证明，不同的溶剂、不同的模板以及模板的用量，对产物的形貌有很大的影响。此实验路径进一步完善了煅烧合成反应路线，也加深了我们对煅烧合成技术的认识。
3．建立了通过高温热解无机盐溶液前驱体制备微纳结构金属氧化物晶体的简便路线。具体提出了煅烧一种无机盐水溶液来合成多孔MgO纳米片的方法并将其成功地推广到蘑菇状ZnO微晶的制备方面。与传统的方法相比，此水溶液热解过程具有以下优势：①丰富和发展了液相法制备微纳材料的新方法与新技术，扩展了水溶液制备微纳材料的领域；②操作方便灵活，原料廉价易得，无需昂贵设备；③在空气中直接反应，不需要任何保护气体。该路线有望用于其他金属氧化物微纳材料的合成上。
4．在总结前人工作的基础上，丰富和发展了传统水热、溶剂热合成技术。用混合溶剂热法合成了金属有机物前驱体，然后使其热解，可以得到一种新颖的晶态材料—骨状MgO纳米晶。详细研究了溶剂热过程中的反应条件，比如浓度、温度、溶剂和时间对最后产物形貌的影响。并探讨了骨状MgO纳米晶的可能生长机理。又利用水热法和前驱体法相结合制备了花状ZnO微晶，该晶体是由纳米片自组装而成。
This dissertation is intended to supplement and develop precursor calcinations routes to synthesize porous inorganic materials and use templates to prepare micro- or nano-scale biomimetic inorganic materials. On the basis of previous work, we have developed some novel mild routes to fabricate porous metal oxides (MgO and CuO) and micron- or nano-scale inorganic biomimetic materials (CdS and ZnO). The control of the morphology and size of the products has also been investigated. The details are summarized as follows:
1. The macroporous CuO has been produced with glycine as template and Cu(NO_3)_2 aqueous solution as copper source. The morphologies of the products could be tuned through varying solvent, reaction temperature, copper sources and the reactants concentrations. On the basis of the experimental results and previous literatures, a possible growth mechanism has also been proposed. Moreover, CdS dendrites have been successfully generated using glycine as structure-directing agent.
2. On the basis of previous work, combined the traditional templating method with the calcination technique, a template-assisted calcination route has been applied to synthesize porous materials. The morphologies of porous MgO could be controlled through using different templates, such as poly (vinyl pyrrolidone) (PVP) and dextran. Studies found that the templates had an important role on the products. The experimental route has perfected clacinations reactions and can be easily extended into the preparation of other metal oxides crystals. All above studies has increased our understanding on the calcinations techniques and provided efficient routes to porous inorganic materials.
3. A facile thermal decomposition route has been developed for the synthesis of metal oxides using inorganic salt solution as precursors. The porous MgO nanoplates have been produced through calcinations of only aqueous Mg(NO_3)_2 solution. The method has also been applied to grow mushroom-like ZnO microcrystals by using Zn(NO_3)_2 solution as precursor instead of Mg(NO_3)_2 solution. Compared with previous methods, our new route has the following features: (i) the system does not need any protective gases; (ii) the raw materials are inexpensive, and the manipulation is simple; (iii) the route has enriched the methods of preparing micro- or nano-scale materials. 4. Based on previous literatures, a feasible solvothermal/hydrothermal approach was enriched and developed. The material with novel morphology — bone-like MgO nanocrystals has been achieved by the thermal decomposition of an organic metal precursor, which was pre-prepared by a solvothermal process. Some crucial factors, such as the solvothermal temperature, the volume ratio of absolute alcohol to water, and the amount of Mg powders, affected the products formation. This is the first report related to the synthesis of nanobones. The products growth mechanism was also discussed. The tlower-like ZnO microcrystals have been synthesized through a precursor process followed by a hydrothermal process. The microcrystals are self-assembled by nanoplates. The precursor is pre-obtained by a precipitation reaction.
引文
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