硫化物半导体纳米材料的可控制备及性能调控
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摘要
硫化物半导体是重要的宽带隙无机半导体化合物材料,因其优异的特性已经迅速成为短波半导体光电材料研究的国际热点。研究纳米材料的控制生长技术以实现按照应用需求有目的性地合成特定形貌和尺度的纳米材料,是当前纳米材料研究领域亟待解决的重要科学问题。本文选取极具应用前景的硫化物半导体材料作为研究对象,研究其结构生长和形貌演化的内在规律,探索与奇特形貌相关的奇特物理性能。研究的重点集中在纳米材料的控制生长方法、纳米结构动力学控制规律以及形貌演化与实验参数的关系。
主要研究内容及创新点包括以下两点:
(1)对典型稀磁性半导体材料MnS的可控合成及性能调控研究。采用简单的溶剂热法可控合成出MnS的多种新颖花样结构(花状、三脚状、棒状、棱台状),考察了物源选择、反应温度、保温时间、反应物配比和溶剂选择等条件对产物形貌的影响,动态的研究了各形貌产物的形成过程和相互演化的规律,分析发现其形成机制遵循“Ostwaldripening”生长方式。对其顺磁特性和PL发光谱进行了研究,找出了形貌与性能之间的关系,发现花状结构具有较好的磁学和光学性能。
(2)利用简单的无模板化学气相沉积法可控合成ZnS空心微球。利用SEM、EDS、XRD等对产物的形貌结构进行了研究,并对其PL谱进行研究。通过改变硫锌比,可实现对球壳厚度和光学性能调控。随着硫的增多,球壳增厚,PL谱出现光学淬灭。ZnS空心微球的生长过程可由Kirkendall现象来阐明。发展了无模板制备空壳结构的新方法。
Nanostructured Sulfide Semiconductors are very important wide-band-gap inorganic semiconductor materials. Therefore, much attention has been paid to the short-wave photoelectric semiconductor materials because of their excellent properties. Investigation on controlled growth of nanomaterials so as to realize the application tailored design and the synthesis of nanomaterials with specific morphologies and sizes is the tackling issue in the current research on nanomaterials. This present thesis aims to investigate in depth the growth mechanisms and the rules for the morphology evolution of applied sulfide semiconductor nanostructures; explore the novel physical properties correlated with novel structures. The research is mainly focused on controlled growth of nanomaterials, the growth dynamic rules and the correlation between morphology evolution and experimental parameters.
The main contents and originality of the thesis are as follows:
1. Controlled growth and property of typical Dilute Magnetic Semiconductor Manganic sulfide were researched. Many novel Manganic sulfide nanostuctures including flower-like ZnO, three-legged MnS, stick MnS and pyramid MnS has been successfully synthesized via solvothermal method. The effect of various experimental parameters including the sort of sulfide, the temperature at the reaction, reactive time, the ratio of reactant and the sort of solvent were studied on the properties. These nanostructures morphology growth processes and interactional evolution also have been studied. The growth mechanism of the MnS nanostructures is attributed to Ostwald ripening process. The optical properties of the products were also recorded by means of photoluminescence (PL) spectroscopy. Electron paramagnetic resonance measurement revealed the paramagnetic nature of the MnS crystals. That is significant for the investigation of novel physical properties originated from special structures. The optical properties and magnetic nature of the MnS nanoflower are the best than others.
2. ZnS hollow microspheres were prepared via a facile template-free chemical vapor deposition (GVD) route. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy-dispersive X-ray spectrometer (EDX). The optical properties of the products were also recorded by means of photoluminescence (PL) spectroscopy. The growth mechanism of the ZnS microstructures is attributed to Kirkendall process. The quantity of S is deemed as a critical parameter in modulating the shell thickness and PL intensity of ZnS microstructure. A higher S content increase the shell thickness, and cause the luminescence quenching. The growth mechanism of the ZnS microstructures is attributed to Kirkendall process. Hollow sphere structure was synthesized by a new template-free method.
主要研究内容及创新点包括以下两点:
(1)对典型稀磁性半导体材料MnS的可控合成及性能调控研究。采用简单的溶剂热法可控合成出MnS的多种新颖花样结构(花状、三脚状、棒状、棱台状),考察了物源选择、反应温度、保温时间、反应物配比和溶剂选择等条件对产物形貌的影响,动态的研究了各形貌产物的形成过程和相互演化的规律,分析发现其形成机制遵循“Ostwaldripening”生长方式。对其顺磁特性和PL发光谱进行了研究,找出了形貌与性能之间的关系,发现花状结构具有较好的磁学和光学性能。
(2)利用简单的无模板化学气相沉积法可控合成ZnS空心微球。利用SEM、EDS、XRD等对产物的形貌结构进行了研究,并对其PL谱进行研究。通过改变硫锌比,可实现对球壳厚度和光学性能调控。随着硫的增多,球壳增厚,PL谱出现光学淬灭。ZnS空心微球的生长过程可由Kirkendall现象来阐明。发展了无模板制备空壳结构的新方法。
Nanostructured Sulfide Semiconductors are very important wide-band-gap inorganic semiconductor materials. Therefore, much attention has been paid to the short-wave photoelectric semiconductor materials because of their excellent properties. Investigation on controlled growth of nanomaterials so as to realize the application tailored design and the synthesis of nanomaterials with specific morphologies and sizes is the tackling issue in the current research on nanomaterials. This present thesis aims to investigate in depth the growth mechanisms and the rules for the morphology evolution of applied sulfide semiconductor nanostructures; explore the novel physical properties correlated with novel structures. The research is mainly focused on controlled growth of nanomaterials, the growth dynamic rules and the correlation between morphology evolution and experimental parameters.
The main contents and originality of the thesis are as follows:
1. Controlled growth and property of typical Dilute Magnetic Semiconductor Manganic sulfide were researched. Many novel Manganic sulfide nanostuctures including flower-like ZnO, three-legged MnS, stick MnS and pyramid MnS has been successfully synthesized via solvothermal method. The effect of various experimental parameters including the sort of sulfide, the temperature at the reaction, reactive time, the ratio of reactant and the sort of solvent were studied on the properties. These nanostructures morphology growth processes and interactional evolution also have been studied. The growth mechanism of the MnS nanostructures is attributed to Ostwald ripening process. The optical properties of the products were also recorded by means of photoluminescence (PL) spectroscopy. Electron paramagnetic resonance measurement revealed the paramagnetic nature of the MnS crystals. That is significant for the investigation of novel physical properties originated from special structures. The optical properties and magnetic nature of the MnS nanoflower are the best than others.
2. ZnS hollow microspheres were prepared via a facile template-free chemical vapor deposition (GVD) route. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy-dispersive X-ray spectrometer (EDX). The optical properties of the products were also recorded by means of photoluminescence (PL) spectroscopy. The growth mechanism of the ZnS microstructures is attributed to Kirkendall process. The quantity of S is deemed as a critical parameter in modulating the shell thickness and PL intensity of ZnS microstructure. A higher S content increase the shell thickness, and cause the luminescence quenching. The growth mechanism of the ZnS microstructures is attributed to Kirkendall process. Hollow sphere structure was synthesized by a new template-free method.
引文
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