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ZnSe量子點(diǎn)制備及光聲與光伏特性研究

發(fā)布時(shí)間:2018-09-19 14:32
【摘要】:本文選取L-半胱氨酸(L-Cys)為配體(修飾劑或保護(hù)劑),采用水相合成法制備Zn Se量子點(diǎn)。以制備過(guò)程中的回流溫度、Zn前體pH值、回流時(shí)間、配體L-半胱氨酸的比例分別為單一變量,以光聲光譜(PA)和表面光電壓譜(SPS)為主要分析手段分析量子點(diǎn)樣品的光聲與光伏特性。借助X射線衍射(XRD)表征方法鑒定ZnSe量子點(diǎn)樣品的晶體結(jié)構(gòu)和粒徑大小。分析得出隨回流溫度、p H值、回流時(shí)間和配體比例變化所制得的樣品都為立方閃鋅礦結(jié)構(gòu),樣品粒子尺寸分別為2.4—3.0nm、2.45—2.52nm、2.48—2.53nm、2.48—2.53nm,粒徑總體小于3nm,證實(shí)所制的樣品確屬量子點(diǎn)尺寸范疇。利用透射電子顯微鏡(TEM)、高分辨透射電子顯微鏡(HRTEM)和電子衍射花樣分析得到樣品近似為球形、分布均勻且為多晶結(jié)構(gòu)。通過(guò)傅里葉變換紅外光譜(FT-IR)和拉曼光譜(Raman)分析樣品的成分與成鍵情況,實(shí)驗(yàn)分析得出,樣品為類ZnSe/ZnS/配體的核/殼式結(jié)構(gòu)。主要借助PA、SPS分析樣品受調(diào)制光照射后的躍遷機(jī)制與能量轉(zhuǎn)換行為,通過(guò)分析得出,樣品在300-400nm、700-800nm光波長(zhǎng)范圍內(nèi)受激輻射主要以晶格振動(dòng)所致的無(wú)輻射躍遷釋放能量;而在400-550nm光波長(zhǎng)范圍內(nèi)則主要以輻射發(fā)光的方式釋放能量;另外550-700nm光波長(zhǎng)范圍內(nèi),受激輻射為輻射躍遷加無(wú)輻射躍遷同時(shí)進(jìn)行釋放能量。證明了PA譜與SPS譜呈現(xiàn)能量互補(bǔ)關(guān)系,樣品具有優(yōu)異的能量轉(zhuǎn)換效率。借助場(chǎng)誘導(dǎo)表面光電壓譜(EFISPS)分析得出樣品表現(xiàn)為N型半導(dǎo)體光伏特性。實(shí)驗(yàn)以90度制備的量子點(diǎn)為測(cè)試樣品,測(cè)試不同調(diào)制頻率10-90Hz的光聲光譜,分析得出光聲響應(yīng)與調(diào)制頻率的關(guān)系很好地符合光聲光熱經(jīng)典理論:R-G理論,并且證明30Hz左右的調(diào)制頻率為儀器的最適宜調(diào)制頻率。
[Abstract]:In this paper, L- cysteine (L-Cys) was used as ligand (modifier or protectant) to prepare Zn Se quantum dots by aqueous phase synthesis. The pH value of Zn precursor, the reflux time and the ratio of ligand L- cysteine were single variables, respectively. The photoacoustic and photovoltaic properties of QDs were analyzed by photoacoustic spectrum (PA) and surface photovoltage spectrum (SPS). The crystal structure and particle size of ZnSe quantum dots were identified by X-ray diffraction (XRD) (XRD) characterization. The results show that the samples prepared with the change of reflux temperature, reflux time and ligand ratio are cubic sphalerite structure. The particle sizes of the samples are 2.48-2.53nmmand 2.48-2.53nmm respectively, and the particle size is less than 3nm. it is proved that the samples are in the range of quantum dot size. By means of transmission electron microscope (TEM),) high resolution transmission electron microscope (HRTEM) and electron diffraction pattern analysis, the sample is approximately spherical, uniformly distributed and polycrystalline. Fourier transform infrared spectroscopy (FT-IR) and Raman spectroscopy (Raman) were used to analyze the composition and bonding of the samples. The experimental results showed that the samples were core-shell structure of ZnSe/ZnS/ like ligands. The transition mechanism and energy conversion behavior of the samples irradiated by modulated light were analyzed by PA,SPS. The results show that the stimulated radiation in the wavelength range of 300-400nm ~ 800nm is mainly due to the non-radiative transition energy caused by lattice vibration. In the range of 400-550nm wavelength, the energy is mainly released in the form of luminescence, and in the range of 550-700nm wavelength, the stimulated radiation is radiative transition and non-radiative transition simultaneously. It is proved that the PA spectrum and the SPS spectrum are energy complementary, and the sample has excellent energy conversion efficiency. Field induced surface photovoltage spectrum (EFISPS) analysis shows that the sample exhibits N-type semiconductor photovoltaic characteristics. The photoacoustic spectra of 10-90Hz with different modulation frequencies were measured by using 90 degree quantum dots as the test sample. The relationship between photoacoustic response and modulation frequency was found to be in good agreement with the classical photoacousto-photothermal theory: R-G theory. It is proved that the modulation frequency of 30Hz is the most suitable modulation frequency of the instrument.
【學(xué)位授予單位】:燕山大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2015
【分類號(hào)】:TQ132.41

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