【摘要】：半導(dǎo)體納米材料由于其比較明顯的量子尺寸效應(yīng)、電子限域效應(yīng)以及良好的抗光漂白性等優(yōu)良性能，同時(shí)其發(fā)光性質(zhì)可以通過(guò)改變尺寸或?qū)ζ鋼诫s離子進(jìn)行精細(xì)調(diào)節(jié)，而被大量運(yùn)用在制造量子點(diǎn)激光器、太陽(yáng)能電池、發(fā)光二級(jí)管、生物DNA標(biāo)記及探針等領(lǐng)域。半導(dǎo)體納米材料摻雜金屬離子后，不僅可以維持原有的優(yōu)良性能，同時(shí)能夠避免斯托克斯現(xiàn)象，并可以進(jìn)一步對(duì)量子點(diǎn)的光學(xué)、電學(xué)等性質(zhì)進(jìn)行調(diào)節(jié)，因此也受到了廣泛的研究開(kāi)發(fā)。傳統(tǒng)制備的納米晶體雖具有尺寸可控且發(fā)光性能優(yōu)良等優(yōu)點(diǎn)，但多采用有機(jī)金屬合成方法，所用試劑價(jià)格不僅昂貴，而且使用的表面活性劑多數(shù)毒性較大，不利于綠色化學(xué)的發(fā)展，更不適用于大規(guī)模生產(chǎn)。 本文采用微波水相合成方法合成了半導(dǎo)體納米晶體CdTe和CdS，并對(duì)其進(jìn)行了摻雜和熒光性質(zhì)的研究。主要取得了以下研究成果： （1）采用微波水相法，在較短時(shí)間內(nèi)合成了高質(zhì)量且尺寸均勻、粒徑較小的球狀碲化鎘（CdTe）半導(dǎo)體納米晶體。通過(guò)粉末X-射線(xiàn)衍射（XRD）測(cè)試，，確定了所得樣品均為結(jié)晶度較好的具有立方閃鋅礦結(jié)構(gòu)的目標(biāo)納米晶體。通過(guò)高分辨透射電鏡（TEM）測(cè)試可以確定所得樣品為粒徑5-6nm的球形顆粒。 在改變反應(yīng)溫度以及時(shí)間的情況下，我們對(duì)所合成的CdTe納米晶體光學(xué)性質(zhì)進(jìn)行了研究：在反應(yīng)時(shí)間一定時(shí)，CdTe納米晶體的紫外吸收峰以及熒光發(fā)射峰隨著溫度升高而發(fā)生紅移，熒光強(qiáng)度基本按照拋物線(xiàn)形式先升高后降低；在反應(yīng)溫度一定時(shí)，隨著時(shí)間的增加，熒光發(fā)射峰紅移，且熒光強(qiáng)度先升高后降低，這些特征都與納米晶體的生長(zhǎng)規(guī)律以及小尺寸效應(yīng)相關(guān)。 （2）采用微波水相法，以巰基丙酸（MPA）為穩(wěn)定劑，利用中心摻雜技術(shù)在不同時(shí)間內(nèi)快速合成了高質(zhì)量的摻雜半導(dǎo)體納米晶體CdS:Cu。銅離子均勻分布在納米晶體的中心內(nèi)部，而且可以通過(guò)CuS核和CdS層的界面擴(kuò)散進(jìn)行陽(yáng)離子交換過(guò)程。通過(guò)XRD測(cè)試發(fā)現(xiàn)所得樣品為立方閃鋅礦結(jié)構(gòu)，通過(guò)TEM測(cè)試發(fā)現(xiàn)所合成的摻雜納米晶體具有良好的晶體結(jié)構(gòu)。尤其是利用中心摻雜技術(shù)摻入的Cu2+離子有效改進(jìn)了CdS在光學(xué)性質(zhì)、量子產(chǎn)率以及光化學(xué)穩(wěn)定性方面的性能。通過(guò)摻雜Cu2+離子使CdS納米晶熒光發(fā)射峰從538nm調(diào)節(jié)到630nm，即呈現(xiàn)紅色熒光。相比于傳統(tǒng)的合成方法，本文所采用中心摻雜方法合成的產(chǎn)物熒光性質(zhì)優(yōu)良，并且具有良好的光化學(xué)穩(wěn)定性，可以長(zhǎng)期穩(wěn)定的存儲(chǔ)。
[Abstract]:Semiconductor nanomaterials have excellent properties such as obvious quantum size effect, electron limiting effect and good photobleaching resistance, and their luminescence properties can be adjusted by changing their size or doping ions. It has been widely used in the fields of quantum dot lasers, solar cells, light-emitting secondary tubes, biological DNA labeling and probes. After doping metal ions, semiconductor nanomaterials can not only maintain the original excellent performance, but also avoid Stokes phenomenon, and further adjust the optical and electrical properties of quantum dots. Therefore, it has also been extensively researched and developed. Although the traditional nanocrystals have the advantages of controllable size and excellent luminescence properties, they are usually synthesized by organometallic methods. The price of the reagents used is not only expensive, but also most of the surfactants used are more toxic. Not conducive to the development of green chemistry, not suitable for mass production. In this paper, semiconductor nanocrystals CdTe and CDs were synthesized by microwave aqueous phase synthesis, and their doping and fluorescence properties were studied. The main results are as follows: (1) the spherical cadmium telluride (CdTe) semiconductor nanocrystals with high quality uniform size and small particle size were synthesized by microwave aqueous phase method in a short time. The results of X-ray diffraction (XRD) show that the samples are all target nanocrystalline with cubic sphalerite structure with good crystallinity. High resolution transmission electron microscopy (TEM) measurements showed that the samples were spherical particles with 5-6nm diameter. The optical properties of the synthesized CdTe nanocrystals were studied by changing the reaction temperature and time. The UV absorption and fluorescence emission peaks of the CdTe nanocrystals were red-shifted with the increase of the temperature when the reaction time was fixed. The fluorescence intensity increased at first and then decreased in the form of parabola, and when the reaction temperature was fixed, the fluorescence emission peak shifted red with the increase of time, and the fluorescence intensity increased first and then decreased. These characteristics are related to the growth law of nanocrystalline and the small size effect. (2) the microwave aqueous phase method and mercaptopropionic acid (MPA) as stabilizer, The high quality doped semiconductor nanocrystalline CDs _ (1) Cu _ (2) was synthesized by the center doping technique in different time. Copper ions are uniformly distributed in the center of the nanocrystalline and can be exchanged through the interface between the CuS nucleus and the CdS layer. The samples were found to have cubic sphalerite structure by XRD test, and the doped nanocrystals were found to have good crystal structure by TEM test. In particular, the Cu2 ion doped by the center doping technique can effectively improve the optical properties, quantum yield and photochemical stability of CdS. The fluorescence emission peak of CdS nanocrystalline was adjusted from 538nm to 630 nm by doping Cu2 ion, that is, red fluorescence. Compared with the traditional synthesis methods, the products synthesized by the central doping method have excellent fluorescence properties and good photochemical stability, and can be stored steadily for a long time.
【學(xué)位授予單位】：吉林大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類(lèi)號(hào)】：TB383.1;O614.242

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