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Alternative TitleShapes, Structures Control and Properties of Nano/Micro Particles of Transition Metals Fe, Co, Ni and Cu
Thesis Advisor袁方利 ; 陈运法
Degree Grantor中国科学院研究生院
Place of Conferral北京
Degree Discipline化学工程
Keyword液相合成   纳微金属   催化   电磁性能
Abstract纳微金属材料在催化、气敏、电磁等领域具有广阔的应用前景。发展高效的合成方法,并探索其生长过程,进而实现对纳微金属材料形貌和结构的调控,对于系统研究金属纳微材料与性能的关系,最终使其进入应用领域具有重要意义。本论文以Fe、Co、Ni和Cu四种过渡金属为研究对象,开展了液相法调控其形貌和结构的研究,并对材料形貌、结构与性能之间的关系进行了有益的探索。主要包括以下几方面内容: 1. 采用溶剂热反应,通过多元醇还原制备了纳/微复合等级结构Co。合成的Co颗粒在微米尺度下表现为六边形和Wulff多面体的规则形貌,在纳米尺度下其表面为纳米片组装成的“花状”结构。所得纳/微复合等级结构Co在催化丙三醇氢解制丙二醇中显示了较好的催化性能。 2. 采用水热反应,通过葡萄糖还原制备了纳微空心Cu2O八面体,研究了实心Cu2O八面体空心化过程,并进一步发展了八面体空心化过程,获得了Cu2O空心球。考察了不同形貌Cu2O可见光催化降解对硝基苯酚的活性,结果表明空心Cu2O八面体具有最高的催化活性。 3. 采用溶剂热反应,通过多元醇还原制备了微米级立方体“介晶”Cu,通过调控反应条件可对其表面微观结构进行调控。所制备“介晶”Cu具有较好的导电性能,可用做导电浆料填充材料。 4. 开发了一种孔蚀法制备纳微空心金属颗粒的新方法。通过控制腐蚀条件使实心纳微金属颗粒在含FeCl3的溶液介质中发生“孔蚀”,得到了表面小孔、内部中空的纳微金属颗粒。这种方法应用在Fe、Co、Ni和Cu颗粒中,成功获得了它们的空心颗粒。对“孔蚀”后羰基Fe粉的电磁性能测试表明,“孔蚀”后羰基Fe粉电磁性能较“孔蚀”前有很大提高。 5. 采用溶剂热反应,通过多元醇还原制备了一种“片花”状Ni,其在催化对硝基苯酚加氢中显示了较纳米Ni更高的催化活性。溶剂热条件下通过水合肼还原制备了“棒状”Fe,其表现了很好的电磁性能。
Other AbstractMetal nano/micro materials have exhibited promising applications in catalysis, sensing, and electromagnetic areas. Preparation of nano/micro metals with well-defined shape and structure through effective synthesis methods and investigation of their formation process should be a key precondition to reveal the relations between the shapes and properties, and pave the way to the real application of nano/micro metals. In this dissertation, we focused researches on the synthesis of nano/micro Fe, Co, Ni and Cu with controlled shapes and structures through solution-based methods and the relations between their shapes and properties. It mainly included the following aspects: 1. Hierarchical Co micro/nanocomposites were successfully synthesized through polyol reduction under the solvothermal conditions. The synthesized Co show regular hexagonal and Wulff polyhedron shapes in micrometer scales, while in nanometer scales their surfaces show “flower-like” structure which connected by nanoplates. The prepared hierarchical Co micro/nanocomposites exhibit very good catalytic activities in glycerol hydrogenolysis. 2. Hollow submicrometer Cu2O octahedra were synthesized through glucose reduction under hydrothermal conditions. The mechanism from solid octahedra to hollow octahedra was investigated detailed. By using this method, hollow Cu2O spheres have also been synthesized. Photocatalytic experiments show that hollow octahedral Cu2O particles exhibit a higher photocatalytic activity for the photodegradation of p-Nitrophenol under visible-light illumination than other shaped Cu2O particles. 3. Cubic Cu mesocrystals with edge length several micrometers were synthesized through polyol reduction under solvothermal conditions. The surface microstructures of the Cu mesocrystals can be controlled by adjusting the reaction conditions. The prepared Cu mesocrystals exhibit a good conducting property, and can be used as fill materials for isotropic conductive adhesives. 4. Explored a new method, “pitting corrosion” method, to synthesize hollow micro/nano metals. In this method, solid micro/nano metals were used as starting materials, and they were “pitting corroded” to hollow structure in FeCl3 solution by controlling the corrosion conditions. Hollow micro/nano Fe, Co, Ni, Cu have been successfully synthesized by using this method. Under the same quality filling, the “pitting corroded” Fe powders exhibited better electromagnetic properties than Fe powders not “pitting corroded”. 5. “Flower-like” Ni particles composed by nanoplates were synthesized through polyol reduction under solvothermal conditions. They exhibit higher catalytic activity in p-Nitrophenol hydrogenation than nano Ni particles. Fe rods with length several micrometers were synthesized through N2H4·H2O reduction under solvothermal conditions. They exhibit good electromagnetic properties.
Document Type学位论文
Recommended Citation
GB/T 7714
曹月斌. 过渡金属Fe、Co、Ni和Cu纳微颗粒的形貌、结构调控及性能研究[D]. 北京. 中国科学院研究生院,2011.
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