高溫溶劑法制備半導(dǎo)體納米晶及其發(fā)光調(diào)制和形貌控制研究
發(fā)布時間：2019-05-18 20:40
【摘要】： 納米粒子是納米技術(shù)研究中的一個基本單元,它給人們提供了研究與尺寸相關(guān)特性的合適對象,因此,納米粒子在納米材料中也占有特別重要的地位,同時在能源、醫(yī)藥衛(wèi)生、電子和計算機、環(huán)境保護、新材料設(shè)計等領(lǐng)域也都有著非常廣泛的應(yīng)用前景。近年來針對半導(dǎo)體納米粒子(納米晶)的制備方法、合成機理的研究一直是科研工作者所關(guān)注的領(lǐng)域,尤其以利用高溫溶劑法制備半導(dǎo)體納米晶所開展的研究工作為代表。目前合成納米晶材料在前驅(qū)體的使用上有相對固定的選擇,如在涉及CdSe納米晶的制備中,除了早期毒性較大的有機金屬鹽(比如二甲基鎘)外,大都選擇氧化鎘作為鎘的前驅(qū)物,其它的離子型化合物則很少涉及;在含汞近紅外發(fā)射半導(dǎo)體納米晶的制備上,由于其高溫下不穩(wěn)定的特點,室溫合成路線就具有很大的優(yōu)勢,但相應(yīng)的研究報道卻很少;在其它諸如金屬氧化物半導(dǎo)體納米晶的制備過程中的一些重要參數(shù)如介質(zhì)的選擇、反應(yīng)溫度的調(diào)節(jié)、反應(yīng)時間的控制以及表面活性劑的運用對反應(yīng)的結(jié)果都具有直接而重要的影響,如何通過相關(guān)實驗的設(shè)計,深入理解其中相關(guān)參數(shù)的作用,從而更加有效地開展納米晶的可控及規(guī)模合成也是目前合成、制備研究中亟待解決的問題。 本論文即以上述問題為出發(fā)點,在高溫溶劑法的基礎(chǔ)上主要開展相關(guān)的合成研究及部分性質(zhì)表征工作,主要包括以下內(nèi)容: (1)選用離子型鎘源作前驅(qū)體成功的在較低的反應(yīng)溫度下制備了ZnSe/CdSe復(fù)合結(jié)構(gòu)納米晶,并對其發(fā)光機理進行了深入的探討。在此基礎(chǔ)上,結(jié)合當前“綠色”環(huán)保的要求,開展了低毒、高效、低能耗的合成方法研究,針對目前廣泛采用的含膦化合物的合成方法,創(chuàng)新性的采用無膦化合物的合成路線制備了較高質(zhì)量的ZnSe納米晶并開展了基于寬帶隙ZnSe半導(dǎo)體納米晶的過渡族元素中心摻雜體系ZnSe:Cu/ZnSe/ZnS復(fù)合結(jié)構(gòu)納米晶的綠色合成制備。通過Cu~(2+)的引入,實現(xiàn)了對ZnSe納米晶的熒光發(fā)射的有效調(diào)節(jié)。適當厚度的ZnS殼層則可以很好的鈍化粒子表面,從而提高熒光發(fā)射強度;通過采用不同粒徑的ZnSe納米晶為核,該復(fù)合結(jié)構(gòu)納米晶的發(fā)射波長可在480~520 nm的范圍內(nèi)實現(xiàn)連續(xù)調(diào)節(jié)。 (2)探索了室溫環(huán)境下高質(zhì)量近紅外納米晶的制備。在CdTe納米晶結(jié)構(gòu)控制合成的基礎(chǔ)上,采用室溫離子交換的間接制備方法實現(xiàn)了HgCdTe近紅外納米晶的制備,并進一步實現(xiàn)了具有近紅外發(fā)射的HgTe納米晶的室溫合成。 (3)利用高溫熱解等方法制備了一系列的金屬氧化物等化合物,在探索新合成方法的同時,著重探討了反應(yīng)溫度、復(fù)合表面活性劑的使用以及前驅(qū)物的選擇對產(chǎn)物結(jié)構(gòu)、成分和性質(zhì)的影響,并對其機理也進行了相應(yīng)的探討。以上工作的開展為下一步開展基于納米晶的器件研究奠定了基礎(chǔ)。
[Abstract]:Nanoparticles are a basic unit in the research of nanotechnology, which provides a suitable object for people to study the characteristics related to size. Therefore, nanoparticles also play a particularly important role in nanomaterials, at the same time in energy, medicine and health. Electronic and computer, environmental protection, new material design and other fields also have a very wide range of application prospects. In recent years, the research on the synthesis mechanism of semiconductor nanoparticles (nanocrystals) has been a field of concern to researchers, especially the research work carried out in the preparation of semiconductor nanoparticles by high temperature solvent method. At present, synthetic nanocrystal materials have a relatively fixed choice in the use of precursors, such as in the preparation of CdSe nanocrystals, in addition to the early toxic organometallic salt (such as dimethyl cadmium), Most of them chose cadmium oxide as the precursor of cadmium, while other ionic compounds were rarely involved. In the preparation of near infrared emission semiconductor nanocrystals containing mercury, due to its unstable characteristics at high temperature, the synthesis route at room temperature has great advantages, but the corresponding research reports are very few. Some important parameters in the preparation of other metal oxide semiconductor nanocrystals, such as the selection of media and the regulation of reaction temperature, The control of reaction time and the use of surfactants have a direct and important influence on the results of the reaction. How to deeply understand the role of the relevant parameters through the design of related experiments. Therefore, more effective controllable and scale synthesis of nanocrystals is also an urgent problem to be solved in the research of preparation. Based on the above problems, this paper mainly studies the synthesis and characterization of some properties on the basis of high temperature solvent method. The main contents are as follows: (1) ZnSe/CdSe composite structure nanocrystals were successfully prepared by using ion cadmium source as precursor at low reaction temperature, and its luminous mechanism was discussed in detail. On this basis, combined with the current requirements of "green" environmental protection, the synthesis methods of low toxicity, high efficiency and low energy consumption were studied, and the synthesis methods of phosphine compounds, which were widely used at present, were studied. High quality ZnSe nanocrystals were prepared by innovative synthesis of phosphine-free compounds, and ZnSe:Cu/ZnSe/ZnS composite structure nanocrystals of transition group element center doping system based on broadband gap ZnSe semiconductor nanocrystals were carried out. Green synthesis of. Through the introduction of Cu~ (2), the fluorescence emission of ZnSe nanocrystals is adjusted effectively. The proper thickness of ZnS shell can passivate the surface of particles, so as to improve the fluorescence emission intensity. By using ZnSe nanocrystals with different particle sizes as cores, the emission wavelength of the composite structure nanocrystals can be adjusted continuously in the range of 480 nm. (2) the preparation of high quality near infrared nanocrystals at room temperature was investigated. On the basis of controlled synthesis of CdTe nanocrystals, HgCdTe near-infrared nanocrystals were prepared by ion exchange at room temperature, and HgTe nanocrystals with near-infrared emission were further synthesized at room temperature. (3) A series of metal oxides and other compounds were prepared by pyrolysis at high temperature. while exploring the new synthesis methods, the reaction temperature, the use of composite surfactants and the selection of precursors on the structure of the products were discussed. The effects of composition and properties were discussed, and the mechanism was also discussed. The above work lays a foundation for the next step of device research based on nanocrystals.
【學(xué)位授予單位】：吉林大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2010
【分類號】：TB383.1
本文編號：2480320
[Abstract]:Nanoparticles are a basic unit in the research of nanotechnology, which provides a suitable object for people to study the characteristics related to size. Therefore, nanoparticles also play a particularly important role in nanomaterials, at the same time in energy, medicine and health. Electronic and computer, environmental protection, new material design and other fields also have a very wide range of application prospects. In recent years, the research on the synthesis mechanism of semiconductor nanoparticles (nanocrystals) has been a field of concern to researchers, especially the research work carried out in the preparation of semiconductor nanoparticles by high temperature solvent method. At present, synthetic nanocrystal materials have a relatively fixed choice in the use of precursors, such as in the preparation of CdSe nanocrystals, in addition to the early toxic organometallic salt (such as dimethyl cadmium), Most of them chose cadmium oxide as the precursor of cadmium, while other ionic compounds were rarely involved. In the preparation of near infrared emission semiconductor nanocrystals containing mercury, due to its unstable characteristics at high temperature, the synthesis route at room temperature has great advantages, but the corresponding research reports are very few. Some important parameters in the preparation of other metal oxide semiconductor nanocrystals, such as the selection of media and the regulation of reaction temperature, The control of reaction time and the use of surfactants have a direct and important influence on the results of the reaction. How to deeply understand the role of the relevant parameters through the design of related experiments. Therefore, more effective controllable and scale synthesis of nanocrystals is also an urgent problem to be solved in the research of preparation. Based on the above problems, this paper mainly studies the synthesis and characterization of some properties on the basis of high temperature solvent method. The main contents are as follows: (1) ZnSe/CdSe composite structure nanocrystals were successfully prepared by using ion cadmium source as precursor at low reaction temperature, and its luminous mechanism was discussed in detail. On this basis, combined with the current requirements of "green" environmental protection, the synthesis methods of low toxicity, high efficiency and low energy consumption were studied, and the synthesis methods of phosphine compounds, which were widely used at present, were studied. High quality ZnSe nanocrystals were prepared by innovative synthesis of phosphine-free compounds, and ZnSe:Cu/ZnSe/ZnS composite structure nanocrystals of transition group element center doping system based on broadband gap ZnSe semiconductor nanocrystals were carried out. Green synthesis of. Through the introduction of Cu~ (2), the fluorescence emission of ZnSe nanocrystals is adjusted effectively. The proper thickness of ZnS shell can passivate the surface of particles, so as to improve the fluorescence emission intensity. By using ZnSe nanocrystals with different particle sizes as cores, the emission wavelength of the composite structure nanocrystals can be adjusted continuously in the range of 480 nm. (2) the preparation of high quality near infrared nanocrystals at room temperature was investigated. On the basis of controlled synthesis of CdTe nanocrystals, HgCdTe near-infrared nanocrystals were prepared by ion exchange at room temperature, and HgTe nanocrystals with near-infrared emission were further synthesized at room temperature. (3) A series of metal oxides and other compounds were prepared by pyrolysis at high temperature. while exploring the new synthesis methods, the reaction temperature, the use of composite surfactants and the selection of precursors on the structure of the products were discussed. The effects of composition and properties were discussed, and the mechanism was also discussed. The above work lays a foundation for the next step of device research based on nanocrystals.
【學(xué)位授予單位】：吉林大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2010
【分類號】：TB383.1
【引證文獻】
中國博士學(xué)位論文全文數(shù)據(jù)庫 前1條
1 王美平;CdTe及其核殼結(jié)構(gòu)納米晶的水相合成與熒光性能研究[D];成都理工大學(xué);2012年
，本文編號：2480320
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