硫化锌纳米材料的制备表征和光学性能的研究

发布时间：2018-02-28 22:27

  本文关键词： 半导体纳米材料 水热法 掺杂 光学性质　出处：《山东大学》2017年硕士论文　论文类型：学位论文

【摘要】：自1980年后期开始,掀起了纳米材料的研究热潮,纳米材料独特优异的光学性能吸引着众多科学家。半导体纳米材料,尤其是硫化镉、硫化锌等宽禁带半导体材料作为纳米材料体系中最为经典的一类,以其独特的偏振光学特性和压电特性以及优异的磁、热性能而备受关注。对半导体纳米材料制备条件的摸索,制备条件对纳米材料结构的影响的研究,以及对半导体纳米材料结构与性能之间关系的研究对于整个材料学领域的发展都有重要的意义。本论文主要开展了对硫化锌制备的研究工作,采用水热合成法,通过添加表面活性剂、掺杂等技术,成功制备了不同形貌、结构的硫化锌微球。同时,本论文研究了制备条件下制备的样品的光学性能。初步阐释了不同空心度的硫化锌空心球的形成原因,不同空心度硫化锌空心球对其光学性能的影响机制,不同掺杂元素的硫化锌的发光机制。具体工作如下:(1)采用水热合成法,以谷胱甘肽(GSH)为硫源,以氯化锌(ZnCl2)为锌源,CTAB为表面活性剂,在比较温和的条件下,实现了一步可控制备纳米粒子组装的单分散的六方相纤锌矿硫化锌微球,并研究了其光学性能。用此方法制备硫化锌纳米材料是因为它的制备温度低,易操控。本研究所采用的硫源为谷胱甘肽,比起其它硫源,谷胱甘肽无毒无污染,是一种绿色原料,用此原料制备的硫化锌可以应用在生物领域。本研究中用此方法合成的单分散的六方相纤锌矿纳米硫化锌微球的直径分布在500 nm-1 μm之间。通过调控乙二胺的含量和CTAB的添加与否,可以制备出荧光性能非常好的硫化锌空心、由纳米棒组成的微球。通过对硫化锌微球发光性能的测试得出,在添加CTAB的条件下,当乙二胺的浓度为5 ml时,得到的空心球的荧光效果最好。本文通过CTAB和乙二胺调控反应系统,实现了六方纤锌矿硫化锌空心纳米微球的可控制备,并通过优化制备条件获得了荧光性能最好的硫化锌微球。(2)采用水热法,以醋酸锌、硝酸钆和硫脲作为原料,以PVP作为表面活性剂在相对低温(150 ℃)的环境下得到单分散硫化锌纳米球。用此方法制备的纳米球直径约为40 nm。通过掺杂钆,使硫化锌纳米球的荧光性能发生变化,发现:当钆的掺杂浓度为2%时,得到的硫化锌纳米球的荧光性能达到最优值。与此同时,研究表明,钆的掺杂并不会明显影响硫化锌纳米球的形貌结构和尺寸大小。由于在掺钆硫化锌纳米球表面上具有-NH2等官能团,使得掺钆硫化锌纳米球能够结合具有特定结构的生物大分子,为其在生物方面的应用提供了条件。
[Abstract]:Since the late 1980, there has been an upsurge in the research of nanomaterials. The unique optical properties of nanomaterials have attracted many scientists. Semiconductor nanomaterials, especially cadmium sulphide, have attracted many scientists. As one of the most classical semiconductor materials in nanomaterials, zinc sulphide has attracted much attention for its unique polarizing and piezoelectric properties and excellent magnetic and thermal properties. Study on the effect of preparation conditions on the structure of nanomaterials, The research on the relationship between structure and properties of semiconductor nanomaterials is of great significance for the development of the whole field of materials. Zinc sulfide microspheres with different morphologies and structures were successfully prepared by adding surfactants and doping techniques. In this paper, the optical properties of the samples prepared under the preparation conditions were studied. The reasons for the formation of different hollow zinc sulfide hollow spheres and the influence mechanism of different hollow zinc sulfide hollow spheres on their optical properties were preliminarily explained. The luminescence mechanism of zinc sulfide with different doped elements is as follows: (1) by hydrothermal synthesis, using glutathione (GSH) as sulfur source, zinc chloride (ZnCl _ 2) as zinc source, CTAB as surfactant, under mild conditions, One-step controllable preparation of monodisperse hexagonal wurtzite zinc sulfide microspheres with one step controllable preparation was carried out, and their optical properties were studied. The preparation of zinc sulfide nanomaterials by this method is due to its low preparation temperature. The sulfur source used in this study is glutathione. Compared with other sulfur sources, glutathione is non-toxic and pollution-free and is a green raw material. Zinc sulphide prepared from this raw material can be used in biological field. In this study, the diameter distribution of monodisperse hexagonal wurtzite nanocrystalline zinc sulfide microspheres was in the range of 500 nm-1 渭 m. The content of ethylenediamine was controlled by controlling the content of ethylenediamine. And the addition of CTAB, Zinc sulphide hollow spheres with excellent fluorescence properties were prepared. The luminescent properties of zinc sulfide microspheres were measured by using nanorods. When the concentration of ethylenediamine was 5 ml, the luminescent properties of zinc sulfide microspheres were tested. In this paper, the controlled preparation of hexagonal wurtzite zinc sulfide hollow nanospheres was achieved by CTAB and ethylenediamine control reaction system. The best fluorescent properties of zinc sulfide microspheres were obtained by optimizing the preparation conditions. The hydrothermal method was used. Zinc acetate, gadolinium nitrate and thiourea were used as raw materials, and zinc nitrate, gadolinium nitrate and thiourea were used as raw materials. Monodisperse zinc sulfide nanospheres were prepared by using PVP as surfactant in a relatively low temperature of 150 鈩，

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