微波加热合成特殊形貌微纳米材料研究
摘要
纳米材料是材料学与纳米科技的交叉学科,也是纳米科技中最基础、最富有活力的组成部分,对未来经济和社会发展有着重要影响。纳米材料是三维空间中至少有一维处于纳米尺度范围或者由该尺度范围的物质为基本结构单元所构成的超精细颗粒材料的总称。纳米材料属于微观粒子和宏观物体交界的过渡区域,具有一系列奇特的效应,这些效应的存在使纳米材料呈现出许多奇异的物理、化学性质,因而使纳米材料具有非常广阔的应用前景。
随着人们对纳米材料所具有的特殊性质的逐步认识和对纳米材料应用方面研究的开展,纳米材料制备研究也日趋深入。目前广泛采用的制备纳米材料有很多种,如,气相沉积法、溶剂热反应、模板法、溶胶-凝胶法、热分解法和超声法等。但是这些方法存在诸如污染环境、成本高、反应条件苛刻或昂贵设备等缺点,不利于大批量制备。为了克服这些缺点,我们在对环境友好的微波化学方法,制备了一系列特殊形貌的微纳米材料。
首先,我们通过微波加热制备了CdS纳米颗粒,用XRD检测其物相组成,表明产物为六方相的硫化镉,并计算出了其晶格常数；用FESEM对其形貌进行了表征,CdS尺寸大约为50 nm,产物十分均一；就表面活性剂的浓度、反应温度等对CdS形貌的影响进行了研究,并通过实验结果的分析提出了其可能的反应机理。
其次,我们采用微波加热制备了陀螺形状ZnO微纳米结构,用XRD检测其物相组成,结构表明产物为六方相的ZnO,并计算出了其晶格常数；用FESEM对其形貌进行了表征,ZnO粒径为1μm左右；对溶液中TEA的含量、加热方式及磁子搅拌等对ZnO微纳米结构形貌的影响进行了研究,通过对比不同反应条件所得产物的形貌提出了可能的生长机理。
再次,我们采用微波加热制备了花状ZnO微纳米结构,用XRD检测其物相组成,结构表明产物为六方相的ZnO,并计算出了其晶格常数；用FESEM对其形貌进行了表征；对溶液中TEA的含量、氨水加入量、反应温度等对ZnO微纳米结构形貌的影响进行了研究,通过对比不同反应条件所得产物的形貌提出了可能的生长机理。
最后,我们采用微波加热,快速(5 min)制备出Te纳米线,用XRD检测其物相组成,结构表明产物为六方相；用HRTEM及FESEM对其形貌进行了表征,Te纳米线直径大约为5 nm；然后我们采用制备的Te纳米线为模板制备出一维的CdTe、PbTe和Au纳米线；提出了一维纳米线的可能生长机理。
综上所述,本论文对利用微波化学法制备微纳米材料进行了系统的研究,并在微波加热条件下制备了一系列形貌均一和结晶性完好的微纳米材料。
As the interdisciplinary of material science and nanotechnology, nanomaterials are also the most basic and active area of nanotechnology and have intense influence on the development of economy and society. In general, nanomaterials is at least one dimension in nanometer-scale range or by the scale as the basic structural unit composed of ultra-fine grain materials. As the particle size approaches nanometer scale, their peculiar physical and chemical properties become quite different with broad application potentials and have great potential applications in many fields.
The fabrication of nanomaterials goes deeper with the understanding of their unique properties and the study on nanomaterials' application. Recently, there are many widely used methods to be utilized to synthesize nanomaterials, such as, vapor deposition method, solvothermal reaction, template method, sol-gel method, thermal decomposition method and the ultrasonic method, etc. But these methods have many drawbacks, for instance, environmental pollution, high energy consumption, high cost and rigorous conditions like high temperature and high pressure or usage of expensive equipment. To overcome these shortcomings, we employ environmentally friendly microwave chemistry to synthesis a series of micro-nano materials.
Firstly, CdS nanoparticles with average particle size of 50 nm was prepared with microwave method. XRD results indicate that the products are hexagonal crystal structure. The concentration of surfactants and reacting temperature all play important roles in the final morphologies of CdS nanoparticle. The reacting process was studied and mechanism governing the growth of CdS nanoparticle was discussed.
Secondly, typical spinning top shape ZnO with average particle size of 1.0μm was prepared with microwave method. XRD results indicate that the products are hexagonal crystal structure. The concentration of surfactants, reacting temperature and blending of magneton all play important roles in the final morphologies of ZnO micro-nano structure. The reacting process was studied and mechanism governing the growth of micro-nano structure was discussed.
Thirdly, unusual flower-like ZnO micro-structure was prepared with microwave method. XRD results indicate that the products are hexagonal crystal structure. The concentration of reactants (TEA and ammonia) and reacting temperature all play important roles in the final morphologies of ZnO micro-nano structure. The reacting process was studied and mechanism governing the growth of micro-nano structure was discussed.
Finally, super thin Te nanowire was fast prepared with microwave method in 5 min. XRD results indicate that the products are hexagonal crystal structure. HRTEM and FESEM show that Te nanowire is about 5 nm in diameter. Then we use Te nanowire as sacrificial template to fabricate CdTe, PbTe and Au nanowire. The reacting process was studied and mechanism governing the growth of nanowire was discussed.
In summary, a systematic investigation has been conducted on the microwave chemistry assisted preparation of micro-nano materials. And we synthesized a series of uniform and good crystallinity of micro-nano crystal.
随着人们对纳米材料所具有的特殊性质的逐步认识和对纳米材料应用方面研究的开展,纳米材料制备研究也日趋深入。目前广泛采用的制备纳米材料有很多种,如,气相沉积法、溶剂热反应、模板法、溶胶-凝胶法、热分解法和超声法等。但是这些方法存在诸如污染环境、成本高、反应条件苛刻或昂贵设备等缺点,不利于大批量制备。为了克服这些缺点,我们在对环境友好的微波化学方法,制备了一系列特殊形貌的微纳米材料。
首先,我们通过微波加热制备了CdS纳米颗粒,用XRD检测其物相组成,表明产物为六方相的硫化镉,并计算出了其晶格常数；用FESEM对其形貌进行了表征,CdS尺寸大约为50 nm,产物十分均一；就表面活性剂的浓度、反应温度等对CdS形貌的影响进行了研究,并通过实验结果的分析提出了其可能的反应机理。
其次,我们采用微波加热制备了陀螺形状ZnO微纳米结构,用XRD检测其物相组成,结构表明产物为六方相的ZnO,并计算出了其晶格常数；用FESEM对其形貌进行了表征,ZnO粒径为1μm左右；对溶液中TEA的含量、加热方式及磁子搅拌等对ZnO微纳米结构形貌的影响进行了研究,通过对比不同反应条件所得产物的形貌提出了可能的生长机理。
再次,我们采用微波加热制备了花状ZnO微纳米结构,用XRD检测其物相组成,结构表明产物为六方相的ZnO,并计算出了其晶格常数；用FESEM对其形貌进行了表征；对溶液中TEA的含量、氨水加入量、反应温度等对ZnO微纳米结构形貌的影响进行了研究,通过对比不同反应条件所得产物的形貌提出了可能的生长机理。
最后,我们采用微波加热,快速(5 min)制备出Te纳米线,用XRD检测其物相组成,结构表明产物为六方相；用HRTEM及FESEM对其形貌进行了表征,Te纳米线直径大约为5 nm；然后我们采用制备的Te纳米线为模板制备出一维的CdTe、PbTe和Au纳米线；提出了一维纳米线的可能生长机理。
综上所述,本论文对利用微波化学法制备微纳米材料进行了系统的研究,并在微波加热条件下制备了一系列形貌均一和结晶性完好的微纳米材料。
As the interdisciplinary of material science and nanotechnology, nanomaterials are also the most basic and active area of nanotechnology and have intense influence on the development of economy and society. In general, nanomaterials is at least one dimension in nanometer-scale range or by the scale as the basic structural unit composed of ultra-fine grain materials. As the particle size approaches nanometer scale, their peculiar physical and chemical properties become quite different with broad application potentials and have great potential applications in many fields.
The fabrication of nanomaterials goes deeper with the understanding of their unique properties and the study on nanomaterials' application. Recently, there are many widely used methods to be utilized to synthesize nanomaterials, such as, vapor deposition method, solvothermal reaction, template method, sol-gel method, thermal decomposition method and the ultrasonic method, etc. But these methods have many drawbacks, for instance, environmental pollution, high energy consumption, high cost and rigorous conditions like high temperature and high pressure or usage of expensive equipment. To overcome these shortcomings, we employ environmentally friendly microwave chemistry to synthesis a series of micro-nano materials.
Firstly, CdS nanoparticles with average particle size of 50 nm was prepared with microwave method. XRD results indicate that the products are hexagonal crystal structure. The concentration of surfactants and reacting temperature all play important roles in the final morphologies of CdS nanoparticle. The reacting process was studied and mechanism governing the growth of CdS nanoparticle was discussed.
Secondly, typical spinning top shape ZnO with average particle size of 1.0μm was prepared with microwave method. XRD results indicate that the products are hexagonal crystal structure. The concentration of surfactants, reacting temperature and blending of magneton all play important roles in the final morphologies of ZnO micro-nano structure. The reacting process was studied and mechanism governing the growth of micro-nano structure was discussed.
Thirdly, unusual flower-like ZnO micro-structure was prepared with microwave method. XRD results indicate that the products are hexagonal crystal structure. The concentration of reactants (TEA and ammonia) and reacting temperature all play important roles in the final morphologies of ZnO micro-nano structure. The reacting process was studied and mechanism governing the growth of micro-nano structure was discussed.
Finally, super thin Te nanowire was fast prepared with microwave method in 5 min. XRD results indicate that the products are hexagonal crystal structure. HRTEM and FESEM show that Te nanowire is about 5 nm in diameter. Then we use Te nanowire as sacrificial template to fabricate CdTe, PbTe and Au nanowire. The reacting process was studied and mechanism governing the growth of nanowire was discussed.
In summary, a systematic investigation has been conducted on the microwave chemistry assisted preparation of micro-nano materials. And we synthesized a series of uniform and good crystallinity of micro-nano crystal.
引文
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