单分散Fe_3O_4和核/壳结构Fe_3O_4/ZnS纳米材料的可控合成与性能研究
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摘要
材料的尺寸、形貌、组成和结构等直接影响材料的性能,因此如何探索一种材料制备方法,实现材料微观结构的有效控制,进而达到材料性能的“人工裁剪”来满足实际需求,已成为当前材料学研究中的热点问题。单分散Fe3O4纳米晶因其具有独特的物理、化学性能及其在生物、医药等领域的潜在应用而被广泛关注。本论文主要通过溶剂热法,利用有机前驱在高沸点的有机溶剂中高温分解制备单分散Fe3O4纳米晶,探讨了实验参数对产物尺寸、形貌和结构的影响,并对其形成机制及性能进行了研究。主要内容如下：
(1)发展了一种溶剂热合成单分散Fe3O4球形纳米颗粒的方法,通过控制反应条件得到了形貌均一、尺寸在6-12nm的Fe3O4球形纳米颗粒。磁学性能研究表明Fe3O4纳米颗粒在2K和300K时分别呈现出铁磁性和超顺磁性的特点,且产物的颗粒尺寸对磁性能有着显著的影响。
(2)在上述工作的基础上,通过引入表面活性剂,成功制备了形貌均一、尺寸为12nm的Fe3O4纳米立方块。通过调控反应参数,可以实现对Fe3O4纳米立方块尺寸和形貌的有效调控,基于实验结果,提出了其可能的形成机制与生长模型。
(3)以Fe3O4纳米球为核,通过超声辅助成功制备了Fe3O4/ZnS核/壳结构纳米材料。通过调节硫源和锌源的量可以控制壳层的厚度。研究表明Fe3O4/ZnS核/壳结构纳米材料具有良好的磁学性能和光学性能。
Previous studies suggest that the size, shape, composition and structure of nanomaterials directly influence their properties. Thus, it is of great importance to develop a synthetic method to achieve the controlment of the microstructures of nanomaterials and further realize the artificial tailoring of their properties to satisfy the practical requirement. Monodisperse Fe3O4 nanocrystals have aroused extensive interest due to their unique physical and chemical properties and potential applications in biological and medical fields. In this thesis, a solvothermal method was developed to synthesize monodisperse magnetic nanocrystals through thermal decomposition of organometallic precursors in the high boiling point organic solvent. The effect of various experimental parameters on the size, shape and structure of products was investigated. In addition, the formation mechanism and properties of final products were carefully discussed. The content is summarized as follows:
(1) A solvothermal method was developed to synthesize the monodisperse Fe3O4 spherical nanoparticles. The uniform Fe3O4 nanoparticles with diameter around 6-12nm were obtained by controlling reaction conditions. Magnetic study reveals that the as-synthesized Fe3O4 nanoparticles are ferromagnetic at 2K while they are superparamagnetic at 300K. And the impact of sizes of final products on the magnetic properties was significant.
(2) Based on the above method, the uniform Fe3O4 nanocubes with sizes of 12nm were successfully synthesized under the aid of surfactants. The sizes and shapes of the nanocubes were availably controlled by adjusting the reaction parameters. Moreover, the formation mechanism and growth model of Fe3O4 nanocubes were provided based on the experimental results.
(3) Fe3O4/ZnS core-shell structured nanomaterials were prepared through a simple ultrasonic-assisted way using Fe3O4 nanospheres as cores. The thickness of the shell can be controlled via adjusting the amount of sulfur source and zinc source. Properties investigation indicated nanomaterials with core-shell structure exhibited excellent magnetic and luminescent properties.
(1)发展了一种溶剂热合成单分散Fe3O4球形纳米颗粒的方法,通过控制反应条件得到了形貌均一、尺寸在6-12nm的Fe3O4球形纳米颗粒。磁学性能研究表明Fe3O4纳米颗粒在2K和300K时分别呈现出铁磁性和超顺磁性的特点,且产物的颗粒尺寸对磁性能有着显著的影响。
(2)在上述工作的基础上,通过引入表面活性剂,成功制备了形貌均一、尺寸为12nm的Fe3O4纳米立方块。通过调控反应参数,可以实现对Fe3O4纳米立方块尺寸和形貌的有效调控,基于实验结果,提出了其可能的形成机制与生长模型。
(3)以Fe3O4纳米球为核,通过超声辅助成功制备了Fe3O4/ZnS核/壳结构纳米材料。通过调节硫源和锌源的量可以控制壳层的厚度。研究表明Fe3O4/ZnS核/壳结构纳米材料具有良好的磁学性能和光学性能。
Previous studies suggest that the size, shape, composition and structure of nanomaterials directly influence their properties. Thus, it is of great importance to develop a synthetic method to achieve the controlment of the microstructures of nanomaterials and further realize the artificial tailoring of their properties to satisfy the practical requirement. Monodisperse Fe3O4 nanocrystals have aroused extensive interest due to their unique physical and chemical properties and potential applications in biological and medical fields. In this thesis, a solvothermal method was developed to synthesize monodisperse magnetic nanocrystals through thermal decomposition of organometallic precursors in the high boiling point organic solvent. The effect of various experimental parameters on the size, shape and structure of products was investigated. In addition, the formation mechanism and properties of final products were carefully discussed. The content is summarized as follows:
(1) A solvothermal method was developed to synthesize the monodisperse Fe3O4 spherical nanoparticles. The uniform Fe3O4 nanoparticles with diameter around 6-12nm were obtained by controlling reaction conditions. Magnetic study reveals that the as-synthesized Fe3O4 nanoparticles are ferromagnetic at 2K while they are superparamagnetic at 300K. And the impact of sizes of final products on the magnetic properties was significant.
(2) Based on the above method, the uniform Fe3O4 nanocubes with sizes of 12nm were successfully synthesized under the aid of surfactants. The sizes and shapes of the nanocubes were availably controlled by adjusting the reaction parameters. Moreover, the formation mechanism and growth model of Fe3O4 nanocubes were provided based on the experimental results.
(3) Fe3O4/ZnS core-shell structured nanomaterials were prepared through a simple ultrasonic-assisted way using Fe3O4 nanospheres as cores. The thickness of the shell can be controlled via adjusting the amount of sulfur source and zinc source. Properties investigation indicated nanomaterials with core-shell structure exhibited excellent magnetic and luminescent properties.
引文
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