硫代硫酸钠在制备ZnO纳米材料中的应用
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摘要
ZnO材料具有独特的电、光、磁、机械等性能,在微电子器件和光电器件等领域有广泛的应用前景。这些独特性能不仅取决于材料的组成、结构和尺度,还取决于其维度和形态。这就要求在材料的生长过程中对它们的结构、组分、形状、大小和位置进行控制。因此,实现形态控制生长是目前ZnO研究的一个重要方向,对其工业化生产和应用具有重大意义。表面活性剂因在化学反应体系中具有多种相行为和结构的多样性,成为研究热点。在特种表面活性剂中,有一类含硫基团的表面活性剂,通常含有N、S、O等官能团的有机分子对无机氧化物都有一定的亲和力,这些官能团能通过氢键、电荷吸引或化学吸附等多种方式与无机氧化物颗粒表面发生作用,从而具有改性作用。在化合物中,除了含硫的有机物能形成具有配位能力的硫离子外,无机化合物硫代硫酸钠(Na_2S_2O_3)分子中,一个硫原子氧化数为+6,另一个为-2,价态为-2的硫原子由于在整个阴离子的外围而具有一定的配位能力,此外,ZnO与硫能产生强的相互作用,可以作为硫的吸附剂,将硫代硫酸钠用于ZnO纳米材料的制备很少报道。
本研究将含硫基团的硫代硫酸钠应用到ZnO的制备过程中,不仅在一定程度上实现了对ZnO的形核、生长和形貌的控制,而且获得了一些新型的复合纳米结构,同时有针对性地对有关体系的荧光发射性能进行研究,因此本文主要用硫代硫酸钠开展系列研究工作,主要研究内容如下:
(一)、探索硫代硫酸钠在锌箔-甲酰胺反应体系中对合成ZnO的形貌调控,探讨ZnO纳米结构的生长过程中,硫代硫酸钠所起的作用,发现硫代硫酸钠不仅可以做为表面活性剂而且还起到硫掺杂的双重作用;硫代硫酸钠通过金属-硫配位,吸附在ZnO生长基元的周围,影响ZnO的生长习性而得到各种形貌的ZnO。
(二)、探索硫代硫酸钠在室温下对ZnO纳米晶的形貌调控,并研究硫掺杂ZnO的光致发光性能,室温下制备出多层花形硫掺杂ZnO微晶,通过对其光致发光的研究,发现S掺杂之后的ZnO只存在可见光发射,紫外发射消失,对于ZnO在可见光区的应用具有重要的价值。
(三)、探索室温下油酸对硫代硫酸钠-硝酸锌-六次甲基四胺反应体系的影响,用简单的溶液法制备出空心硫微球。油酸起作为模板和反应剂的双重作用。由于油酸的溶解度很低,整个反应持续两周,但是反应条件简单。
ZnO materials have unique electrical, optical, magnetic, mechanical properties, and have a wide range of applications in micro-electronic and optoelectronic devices These unique properties not only depend on the composition, structure and scale, but also its dimensions and shapes, which require their structure, composition, shape, size and position are controlable. Therefore, to achieve shape-control ZnO is an important area of research, and has great significance for industrial production and application. Phase behavior of surfactant in chemical reaction system and its structural diversity have become a research focus. In the specialty surfactants, there are a kind of sulfur group of surfactants, usually containing N, S, O and other functional groups of organic molecules on inorganic oxides have a certain degree of affinity, These functional groups through hydrogen bonding, charge attract or a variety of ways, such as chemical adsorption and the surface of inorganic oxide particles and thus have a modified function. In the compounds, in addition to the formation of organic sulfur coordination ability with sulfide ions, the inorganic compounds of sodium thiosulfate (Na_2S_2O_3), sulfur atom oxidation number of +6, and the other is -2, -2 valence state of sulfur atom in the anion locates one corner of the tetrahedron and has a capacity of coordination. In addition, sulfur anion can interact with ZnO as a sulfur adsorbent, so the Na_2S_2O_3 can be used for the preparation of ZnO nano-materials.
In this study, it is reasonable to use of S-contained ligands for controllable growth of ZnO nanostructures: to achieve a certain degree of ZnO nucleation, growth and morphology control, and to prepare a series of new nano-composite structures. At the same time the fluorescence emission properties of S-doped flower-like ZnO was studied. Main contents include the following parts:
(1) Studied how Na_2S_2O_3 to control ZnO morphology in the Zn foil-CH_3NO reaction system. The results show that Na_2S_2O_3 not only acts as a surfactant but also sulfur resource for S-doped; Na_2S_2O_3 adsorbs on ZnO through the metal-sulfur coordination, affects the growth habits of ZnO. Therefore, a variety morphologys of ZnO were obtained.
(2) Studied the effect of Na_2S_2O_3 to nanocrystalline ZnO regulation of morphology at room temperature and studying the S-doped ZnO photoluminescence properties. At room temperature we got sulfur-doped flower-like ZnO. Through its photoluminescence study, we found that sulfur-doped ZnO only have visible light emission, ultraviolet emission disappeared which has an important value for ZnO application in the visible region.
(3) Studied the impact of oleic acid for C_6H_(12)N_4-Zn(NO_3)_2-Na_2S_2O_3 reaction system. In conclusion, hollow microspheres of sulfur have been synthesized via a simple solution route at room temperature and ambient conditions for the first time. Oleic acid acts as both template and reagent. For the low solubility of oleic acid, process of the formation of sulfur hollow microspheres lasts as long as two weeks but benifits simple raction conditions.
本研究将含硫基团的硫代硫酸钠应用到ZnO的制备过程中,不仅在一定程度上实现了对ZnO的形核、生长和形貌的控制,而且获得了一些新型的复合纳米结构,同时有针对性地对有关体系的荧光发射性能进行研究,因此本文主要用硫代硫酸钠开展系列研究工作,主要研究内容如下:
(一)、探索硫代硫酸钠在锌箔-甲酰胺反应体系中对合成ZnO的形貌调控,探讨ZnO纳米结构的生长过程中,硫代硫酸钠所起的作用,发现硫代硫酸钠不仅可以做为表面活性剂而且还起到硫掺杂的双重作用;硫代硫酸钠通过金属-硫配位,吸附在ZnO生长基元的周围,影响ZnO的生长习性而得到各种形貌的ZnO。
(二)、探索硫代硫酸钠在室温下对ZnO纳米晶的形貌调控,并研究硫掺杂ZnO的光致发光性能,室温下制备出多层花形硫掺杂ZnO微晶,通过对其光致发光的研究,发现S掺杂之后的ZnO只存在可见光发射,紫外发射消失,对于ZnO在可见光区的应用具有重要的价值。
(三)、探索室温下油酸对硫代硫酸钠-硝酸锌-六次甲基四胺反应体系的影响,用简单的溶液法制备出空心硫微球。油酸起作为模板和反应剂的双重作用。由于油酸的溶解度很低,整个反应持续两周,但是反应条件简单。
ZnO materials have unique electrical, optical, magnetic, mechanical properties, and have a wide range of applications in micro-electronic and optoelectronic devices These unique properties not only depend on the composition, structure and scale, but also its dimensions and shapes, which require their structure, composition, shape, size and position are controlable. Therefore, to achieve shape-control ZnO is an important area of research, and has great significance for industrial production and application. Phase behavior of surfactant in chemical reaction system and its structural diversity have become a research focus. In the specialty surfactants, there are a kind of sulfur group of surfactants, usually containing N, S, O and other functional groups of organic molecules on inorganic oxides have a certain degree of affinity, These functional groups through hydrogen bonding, charge attract or a variety of ways, such as chemical adsorption and the surface of inorganic oxide particles and thus have a modified function. In the compounds, in addition to the formation of organic sulfur coordination ability with sulfide ions, the inorganic compounds of sodium thiosulfate (Na_2S_2O_3), sulfur atom oxidation number of +6, and the other is -2, -2 valence state of sulfur atom in the anion locates one corner of the tetrahedron and has a capacity of coordination. In addition, sulfur anion can interact with ZnO as a sulfur adsorbent, so the Na_2S_2O_3 can be used for the preparation of ZnO nano-materials.
In this study, it is reasonable to use of S-contained ligands for controllable growth of ZnO nanostructures: to achieve a certain degree of ZnO nucleation, growth and morphology control, and to prepare a series of new nano-composite structures. At the same time the fluorescence emission properties of S-doped flower-like ZnO was studied. Main contents include the following parts:
(1) Studied how Na_2S_2O_3 to control ZnO morphology in the Zn foil-CH_3NO reaction system. The results show that Na_2S_2O_3 not only acts as a surfactant but also sulfur resource for S-doped; Na_2S_2O_3 adsorbs on ZnO through the metal-sulfur coordination, affects the growth habits of ZnO. Therefore, a variety morphologys of ZnO were obtained.
(2) Studied the effect of Na_2S_2O_3 to nanocrystalline ZnO regulation of morphology at room temperature and studying the S-doped ZnO photoluminescence properties. At room temperature we got sulfur-doped flower-like ZnO. Through its photoluminescence study, we found that sulfur-doped ZnO only have visible light emission, ultraviolet emission disappeared which has an important value for ZnO application in the visible region.
(3) Studied the impact of oleic acid for C_6H_(12)N_4-Zn(NO_3)_2-Na_2S_2O_3 reaction system. In conclusion, hollow microspheres of sulfur have been synthesized via a simple solution route at room temperature and ambient conditions for the first time. Oleic acid acts as both template and reagent. For the low solubility of oleic acid, process of the formation of sulfur hollow microspheres lasts as long as two weeks but benifits simple raction conditions.
引文
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