CdSe纳米晶体的研究
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摘要
CdSe属于II-VI族化合物半导体系列,CdSe纳米晶体由于量子效应具备了独特、新颖的性质,可用来制造高效太阳能电池、量子点激光器、生物标签,光压器件以及发光二极管等,具有极大的研发吸引力和应用前景。
参照制备CdSe纳米晶体的TOP-TOPO-HDA路线,本文探讨了该路线下控制CdSe量子点粒径的规律,揭示了表面活性剂的用量和前体注入方式对CdSe量子点粒径的影响。
提出了一种应用新溶剂体系制备CdSe纳米晶体的新方法。新溶剂A更加环境友好,降低了操作难度;价廉,降低了合成成本的90%,致使制备过程更加符合绿色化学的基本原则。在新体系中,成功地合成出CdSe量子点,并利用UV-Vis、PL、XRD、EDX和TEM等对产品进行了表征;考察了反应温度、注入方式、前体浓度,前体比例以及配体浓度对纳米晶体制备的影响;通过优化调节上述因素实现了对CdSe量子点粒径和晶体结构的调控。
在利用HDA单溶剂体系和新溶剂体系制备CdSe纳米晶体时,实现了对其形态的调控。通过控制反应温度,前体加入方式和加入速度,制备出了球形、棒状、多臂和四脚纺锤形等多种形态的CdSe纳米晶体。
为提高纳米粒子的光稳定性和化学稳定性,利用有机、无机钝化方法,对所得的CdSe量子点进行了表面修饰。采用一步法制备了CdSe@ZnSe核壳纳米粒子。利用微乳液方法,将CdSe@ZnSe核壳纳米粒子进一步封装到SiO2纳米粒子中,得到水溶性的CdSe@ZnSe@SiO2核壳壳型纳米粒子,有利于进一步的生物应用。
定量研究了TOP-TOPO-HDA路线下CdSe量子点的结晶动力学,并发展了一种新的扩散控制的生长模型;探讨了新体系中CdSe量子点的结晶动力学规律。利用粒数衡算模型和移动边界算法对CdSe量子点的结晶过程进行了模拟。
本文研究成果尚未见国内外文献报道。
CdSe belongs to the II-VI type semiconductors. CdSe nanocrystals have some novel and excellent properties due to the quantum effects. Hence, the synthesis of CdSe nanocrystals is a very attractive research field. CdSe nanocrystals have great application prospects and could be used to fabricate high performance solar cell, quantum dots lasers, biological labels, photovoltage devices and LEDs et al.
In this dissertation, we investigated the dependence of CdSe nanocrystals size on the manipulative factors according to the TOP-TOPO-HDA route and found the influence of the dosage of surfactants on the size of the CdSe quantum dots (QDs).
A new method was developed to synthesize CdSe nanocrystals. The new solvent A is more environment-friendly and cheaper than the old solvents. The usage of solvent A can slash the cost by 90 percent and make the synthesis obey the principles of green chemistry. Based on this new method, high quality CdSe nanocrystals were synthesized and characterized by UV-Vis, PL, XRD, EDX and TEM, and the size of CdSe QDs could be controlled by adjusting various factors such as the reaction temperature, injection mode, monomers concentration, the ratio between monomers and the ligand concentration et al. The shape control regularities of CdSe nanocrystals was studied both in HDA system and in solvent A, and different shapes such as spheres, rods (wire) and multi-pod et al were obtained.
In order to improve the photostability of the CdSe QDs, the surface modification of CdSe QDs via organic and inorganic passivation has been investigated. The CdSe@ZnSe core-shell nanocrystals were synthesized by a one-pot method both in HDA system and in solvent A. A new core-shell-shell type of nanocrystal, CdSe@ZnSe@SiO2, was synthesized via microemulsion method. The double shells make the nanocrystals compatible to aqueous solution which is essential to the biological application.
The crystallization of CdSe QDs in TOP-TOPO-HDA system was quantitatively determined and the growth of CdSe QDs was found to be a diffusion-controlled process. A new diffusion-controlled growth model has been developed and the simulation results fitted the experimental data quite well. The crystallization kinetics of CdSe QDs in the new solvent was qualitatively determined. According to population balance model and moving boundary algorithm, the simulation study of the crystallization process of CdSe QDs in solvent A was basically completed.
参照制备CdSe纳米晶体的TOP-TOPO-HDA路线,本文探讨了该路线下控制CdSe量子点粒径的规律,揭示了表面活性剂的用量和前体注入方式对CdSe量子点粒径的影响。
提出了一种应用新溶剂体系制备CdSe纳米晶体的新方法。新溶剂A更加环境友好,降低了操作难度;价廉,降低了合成成本的90%,致使制备过程更加符合绿色化学的基本原则。在新体系中,成功地合成出CdSe量子点,并利用UV-Vis、PL、XRD、EDX和TEM等对产品进行了表征;考察了反应温度、注入方式、前体浓度,前体比例以及配体浓度对纳米晶体制备的影响;通过优化调节上述因素实现了对CdSe量子点粒径和晶体结构的调控。
在利用HDA单溶剂体系和新溶剂体系制备CdSe纳米晶体时,实现了对其形态的调控。通过控制反应温度,前体加入方式和加入速度,制备出了球形、棒状、多臂和四脚纺锤形等多种形态的CdSe纳米晶体。
为提高纳米粒子的光稳定性和化学稳定性,利用有机、无机钝化方法,对所得的CdSe量子点进行了表面修饰。采用一步法制备了CdSe@ZnSe核壳纳米粒子。利用微乳液方法,将CdSe@ZnSe核壳纳米粒子进一步封装到SiO2纳米粒子中,得到水溶性的CdSe@ZnSe@SiO2核壳壳型纳米粒子,有利于进一步的生物应用。
定量研究了TOP-TOPO-HDA路线下CdSe量子点的结晶动力学,并发展了一种新的扩散控制的生长模型;探讨了新体系中CdSe量子点的结晶动力学规律。利用粒数衡算模型和移动边界算法对CdSe量子点的结晶过程进行了模拟。
本文研究成果尚未见国内外文献报道。
CdSe belongs to the II-VI type semiconductors. CdSe nanocrystals have some novel and excellent properties due to the quantum effects. Hence, the synthesis of CdSe nanocrystals is a very attractive research field. CdSe nanocrystals have great application prospects and could be used to fabricate high performance solar cell, quantum dots lasers, biological labels, photovoltage devices and LEDs et al.
In this dissertation, we investigated the dependence of CdSe nanocrystals size on the manipulative factors according to the TOP-TOPO-HDA route and found the influence of the dosage of surfactants on the size of the CdSe quantum dots (QDs).
A new method was developed to synthesize CdSe nanocrystals. The new solvent A is more environment-friendly and cheaper than the old solvents. The usage of solvent A can slash the cost by 90 percent and make the synthesis obey the principles of green chemistry. Based on this new method, high quality CdSe nanocrystals were synthesized and characterized by UV-Vis, PL, XRD, EDX and TEM, and the size of CdSe QDs could be controlled by adjusting various factors such as the reaction temperature, injection mode, monomers concentration, the ratio between monomers and the ligand concentration et al. The shape control regularities of CdSe nanocrystals was studied both in HDA system and in solvent A, and different shapes such as spheres, rods (wire) and multi-pod et al were obtained.
In order to improve the photostability of the CdSe QDs, the surface modification of CdSe QDs via organic and inorganic passivation has been investigated. The CdSe@ZnSe core-shell nanocrystals were synthesized by a one-pot method both in HDA system and in solvent A. A new core-shell-shell type of nanocrystal, CdSe@ZnSe@SiO2, was synthesized via microemulsion method. The double shells make the nanocrystals compatible to aqueous solution which is essential to the biological application.
The crystallization of CdSe QDs in TOP-TOPO-HDA system was quantitatively determined and the growth of CdSe QDs was found to be a diffusion-controlled process. A new diffusion-controlled growth model has been developed and the simulation results fitted the experimental data quite well. The crystallization kinetics of CdSe QDs in the new solvent was qualitatively determined. According to population balance model and moving boundary algorithm, the simulation study of the crystallization process of CdSe QDs in solvent A was basically completed.
引文
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