在油酸—石蜡体系下CdS/CdSe量子点的制备及其光学性能研究
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摘要
量子点是准零维的荧光半导体纳米材料，一般是由II-VI族或者是III-V族元素组成的，直径在1-10nm之间，也称为“人造原子”。量子点由于其特殊的效应，吸收光谱宽，发射光谱窄而且呈对称分布，光化学稳定等特点，在化学催化、电子器件、光纤通信光电器件、半导体器件、太阳能电池、生物荧光探针等方面有着广阔的应用前景。目前，最常用的制备光学性能好的量子点的方法是有机金属合成法。虽然这个方法可以制备质量较高的量子点，但是由于所使用的溶剂TOP和TOPO存在较多的缺点，其高成本高污染等缺点阻碍了量子点的应用推广。因此，探寻廉价绿色，简单易行，毒性小，对环境污染少，反应条件温和的新方法，在量子点的制备中，仍是一个非常重要的研究领域。另外，改善粒子的表面性能以及开发出新的光化学性质，进而实现电子器件的研制，将更是具有重要的科学意义和使用价值。
本论文使用液体石蜡作为反应溶剂，油酸作为配位剂，深入探索了CdS、CdSe量子点的油相绿色合成工艺，并对制备的量子点进行了多种表征并研究其光学特性。对该绿色合成工艺进行多反应条件的测试，通过改变反应时间、反应物浓度、反应温度等条件对制备的量子点的尺寸进行控制，进一步完善其制备CdS、CdSe量子点的流程，增强产物的可控性。对制备的稳定的CdS、CdSe量子点进行了表面修饰工作，重点通过包裹CdS形成CdSe/CdS核壳结构量子点以增强其荧光量子产率。对修饰方法进行了深度摸索并总结出一套行之有效的工艺流程。
利用高分辨透射电子显微镜(HRTEM)、X射线衍射仪(XRD)、荧光光谱仪(PL)和紫外-可见吸收光谱仪(UV-vis)对样品进行表面形貌、粒径分析、晶体结构表征和光学性能测试。结果表明使用这种方法制备出了分散性好、粒径均一、尺寸小、荧光好的CdS量子点、CdSe量子点、CdSe/CdS核壳结构量子点。通过实验可以看出对量子点进行包覆后其光学性能有一定的提高。
Quantum dots (QDs), also known as“man-made”atomic, are quasi-zero-dimensionalfluorescence semiconductor nanomaterials, which are 1-10 nm in diameter and generallycomprised of II-VI group or III-V group elements. Due to its special effects, such as broadabsorption spectrum, narrow emission spectrum and symmetrical distribution, photochemicalstability and so on, quantum dots have widespread application prospects in chemical catalysis,electronic devices, optical fiber communication components, semiconductor devices, solarcells, biological fluorescence probes and so on. Recently, the most common method tosynthesize excellent optical performance quantum dots is the metal organic synthesis.Although high quality quantum dots could be obtained, the high cost and high pollutiondefects of the solvent TOP and TOPO hinder the application of quantum dots. For this reason,seeking a cheap, green, simple and easy, low toxic, less pollution and mild reaction conditionis still very important in the filed of quantum dots preparation. In addition, it is moresignificant and valuable to achieve the development of electronic devices through improvingthe surface and photochemical properties of the particles.
In this thesis, paraffin liquid is chosen as solvent, oleic acid as the complex agent, CdS,CdSe quantum dots are successfully synthesized via green oil phase synthetic process,characterized by various measures and its optical properties have been investigated. In orderto control the size of as-prepared quantum dots, the influences of reaction time, concentrationof reactants and reaction temperature in the green synthetic process have been investigated tofurther improve the process of the preparation of CdS, CdSe quantum dots and enhance thecontrollability of the products. Surface modification on the preparation of the steady CdS,CdSe quantum dots is also employed, mainly through wrapping CdS to form CdSe/CdScore-shell quantum dots, aims at enhancing the fluorescence quantum yield. The method ofmodification has been explored and a set of effective processes been summarized.
Surface morphology, crystal structure characterization and optical performance areinvestigated by high-resolution transmission electron microscopy (HRTEM), X-ray diffraction(XRD), fluorescence spectrometer (PL) and ultraviolet-visible absorption spectrometer(UV-vis). The results show that well dispersion, uniform particle size, small size, goodfluorescence CdS quantum dots, CdSe quantum dots and CdSe/CdS core-shell quantum dotsare prepared in this method. It can be seen that the optical performance of quantum dots isimproved through the experiment.
本论文使用液体石蜡作为反应溶剂，油酸作为配位剂，深入探索了CdS、CdSe量子点的油相绿色合成工艺，并对制备的量子点进行了多种表征并研究其光学特性。对该绿色合成工艺进行多反应条件的测试，通过改变反应时间、反应物浓度、反应温度等条件对制备的量子点的尺寸进行控制，进一步完善其制备CdS、CdSe量子点的流程，增强产物的可控性。对制备的稳定的CdS、CdSe量子点进行了表面修饰工作，重点通过包裹CdS形成CdSe/CdS核壳结构量子点以增强其荧光量子产率。对修饰方法进行了深度摸索并总结出一套行之有效的工艺流程。
利用高分辨透射电子显微镜(HRTEM)、X射线衍射仪(XRD)、荧光光谱仪(PL)和紫外-可见吸收光谱仪(UV-vis)对样品进行表面形貌、粒径分析、晶体结构表征和光学性能测试。结果表明使用这种方法制备出了分散性好、粒径均一、尺寸小、荧光好的CdS量子点、CdSe量子点、CdSe/CdS核壳结构量子点。通过实验可以看出对量子点进行包覆后其光学性能有一定的提高。
Quantum dots (QDs), also known as“man-made”atomic, are quasi-zero-dimensionalfluorescence semiconductor nanomaterials, which are 1-10 nm in diameter and generallycomprised of II-VI group or III-V group elements. Due to its special effects, such as broadabsorption spectrum, narrow emission spectrum and symmetrical distribution, photochemicalstability and so on, quantum dots have widespread application prospects in chemical catalysis,electronic devices, optical fiber communication components, semiconductor devices, solarcells, biological fluorescence probes and so on. Recently, the most common method tosynthesize excellent optical performance quantum dots is the metal organic synthesis.Although high quality quantum dots could be obtained, the high cost and high pollutiondefects of the solvent TOP and TOPO hinder the application of quantum dots. For this reason,seeking a cheap, green, simple and easy, low toxic, less pollution and mild reaction conditionis still very important in the filed of quantum dots preparation. In addition, it is moresignificant and valuable to achieve the development of electronic devices through improvingthe surface and photochemical properties of the particles.
In this thesis, paraffin liquid is chosen as solvent, oleic acid as the complex agent, CdS,CdSe quantum dots are successfully synthesized via green oil phase synthetic process,characterized by various measures and its optical properties have been investigated. In orderto control the size of as-prepared quantum dots, the influences of reaction time, concentrationof reactants and reaction temperature in the green synthetic process have been investigated tofurther improve the process of the preparation of CdS, CdSe quantum dots and enhance thecontrollability of the products. Surface modification on the preparation of the steady CdS,CdSe quantum dots is also employed, mainly through wrapping CdS to form CdSe/CdScore-shell quantum dots, aims at enhancing the fluorescence quantum yield. The method ofmodification has been explored and a set of effective processes been summarized.
Surface morphology, crystal structure characterization and optical performance areinvestigated by high-resolution transmission electron microscopy (HRTEM), X-ray diffraction(XRD), fluorescence spectrometer (PL) and ultraviolet-visible absorption spectrometer(UV-vis). The results show that well dispersion, uniform particle size, small size, goodfluorescence CdS quantum dots, CdSe quantum dots and CdSe/CdS core-shell quantum dotsare prepared in this method. It can be seen that the optical performance of quantum dots isimproved through the experiment.
引文
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[2]娄文静，陈淼．有机-无机复合CdS纳米晶的制备及表征[J]．材料科学与工程学报．2005, 23(6):891-894．
[3]惠浩浩，杨伟，张清华，马红菊，马平，许乔．溶胶-凝胶法制备疏水性自组装SiO2薄膜[J]．应用光学．2011, 32(4): 761-766．
[4]滕立东，王介峰，张晓凯．Sol-Gel法制备纳米CdS微晶掺杂玻璃复合材料的工艺研究[J]．山东轻工业学院学报．1996, 10(2): 59-63．
[5] S. M. Reda. Synthesis and optical properties of CdS quantum dots embedded in silica matrix thin filmsand their applications as luminescent solar concentrators[J]. Acta Mater. 2008, 56(2): 259-264.
[6]赵丰华，陈平清，霍延平，蓝邦．溶剂热法合成CdS纳米晶及其光学性质研究[J]．分析测试学报．2010, 29(3): 242-246．
[7]丛日敏，罗运军，李国平，谭惠民．PAMAM树形分子模板法原位合成发紫光CdS量子点的研究[J]．无机化学学报．2005, 21(11): 1763-1766．
[8] Dayang Wang, Yaan Cao, Xintong Zhang, Zhiqiang Liu, Xinming Qian, Xin Ai, Fengqi Liu, DejunWang, Yubai Bai, Tiejin Li and Xinyi Tang. Size control of CdS nanocrystals in block copolymermicelle[J]. Chem. Mater. 1999, 11(2): 392-398.
[9]桑文斌，彭小雷，史伟民，刘祖刚，钱永彪，王林军，闵嘉华，刘引烽．溶胶络合转化法制备CdS纳米微晶及其特性研究[J]．功能材料．2000, 31(5): 508-509．
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