硫化镉光电薄膜的制备及表征
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摘要
硫化镉(CdS)是优良的半导体光电材料,在太阳能电池、光电子器件、光催化材料和非线性光学器件上有着广阔的应用前景。特别是关于大尺度的CdS薄膜制备及应用,完成该方面的研究工作,将会促进光电技术及其应用的发展。
本文比较详细的介绍了不同空间维度的CdS材料的研究现状、制备方法及应用前景等。
理论部分：首先,介绍了化学水浴沉积法制备CdS薄膜的生长机理。其次,介绍了真空蒸发法制备CdS薄膜的实验设备、操作流程、成膜原理及表征CdS薄膜的检测手段。
实验部分：首先,介绍了化学水浴沉积法制备CdS薄膜。在CBD法沉积CdS薄膜的实验中,发现CdS薄膜的生长受到多种因素的影响如：反应溶液的初始浓度、沉积时间、沉积温度、超声震荡和溶液搅拌速度等。这些因素中决定CdS薄膜厚度的主要是反应溶液的初始浓度及沉积温度。而且,后期的退火处理对CdS薄膜的结构、形貌、透射率也有很大影响。经过分组对比实验并且用XRD谱、SEM图、Raman谱、透射谱、荧光光谱等表征CdS薄膜而得出制备质量优异的CdS薄膜的最佳条件为：CdCl2的浓度范围选取为0.01～0.02mol/L,NH4Cl的浓度范围选取为0.02～0.04mol/L, SC(NH2)2的浓度范围选取为0.01-0.015mol/L, pH值范围选取为10-11,反应温度控制在85-90℃,沉积时间为20-30min,退火温度为400℃。且适当的超声震荡可使薄膜缺陷减少、厚度均匀和透射率提高等。在以上条件下,制备出大面积(20cm×20cm)的CdS薄膜,并测试了光导电特性。
其次,介绍了真空蒸发法制备CdS薄膜。经一系列实验并且用透射谱、XRD谱、SEM图等表征手段研究蒸发电流、沉积时间、退火处理等制备参数对CdS薄膜的透射率、结构和表面形貌的影响。当其他条件不变时,在蒸发电流小于100A的情况下,CdS薄膜沉积速率随着蒸发电流的增加而变快,同时薄膜的结晶性变好；当其他条件不变时,沉积时间在16min以内与CdS薄膜厚度的增长几乎是线性的；后期的退火处理,会使CdS粒子具有一定的能量,可以在一定范围内运动,随着退火处理温度的增加,粒子获得的动能更多,可移动的范围更大,能形成更大的粒子团,而且更加均匀,结晶性越好,400℃退火后的CdS薄膜结构、导电性及光学特性最佳。最后得到CdS薄膜的最佳制备条件为：蒸发电流：100A,退火温度：400℃,沉积时间：15min。
最后,用提拉法制备CdS/Cu2S双层膜。分别用化学水浴沉积法和真空蒸发法制备出的CdS薄膜浸渍到CuCl的溶液中,然后用提拉法制备出CdS/Cu2S双层膜。由真空蒸发法的CdS薄膜而制备的CdS/Cu2S双层膜的亮电阻及膜的均匀性等都优于由CBD法的CdS薄膜而制备的CdS/Cu2S双层膜。实验过程中发现,在未经退火处理的CdS薄膜上沉积Cu2S时,易脱落,退火处理高于500℃时,双层膜缺陷多。经测试CdS/Cu2S双层膜的光导电性优于CdS单层膜的。
Cadmium sulfide (CdS) is an excellent compound semiconductor photoelectric material, and showing potential application prospects in solar cells,optoelectronic devices,photocatalytic materials,nonlinear optical devices and so on.The large scale of CdS films research and application are especially important that study on it may boost the development of optoelectronic technology and its applications.
In this dissertation thesis the different spatial dimensions preparation of CdS were introduced. The recent advances and applications were reviewed.
Theoretical parts, first of all, it presented the desposition process and growth mechanism of CdS thin films prepared by the chemical bath deposition. Then introduced the laboratory equipment, operational processes, film deposition theory of CdS thin films prepared by vacuum evaporation,and detection means of characterize of CdS thin film.
Experimental parts, first of all, presented CdS thin films prepared by the chemical bath deposition. The growth behaviors of CBD-CdS thin films may be influenced by the experimental conditions, such as, the initial reaction solution concentration, deposition time, deposition temperature, ultrasonic vibration and the solution stirring speed. In these conditions factors, the initial reaction solution concentration and deposition temperature were the main conditions factors to determine the thickness of CdS thin films. In addition, post-annealing treatment had greatly affected on the structure, surface morphology and transmittance of CdS thin films. After comparing experimental groups and the characterization of CdS thin films by XRD spectra, SEM graph, Raman spectroscopy, transimission spectroscopy, fluorescence spectroscopy that we have obtained the optimum conditions to deposit CdS thin films in the CBD process. The optimum ranges were:CdCl2 concentration in the range of 0.01 to 0.02mol/L, NH4Cl concentration in the range of 0.02 to 0.04mol/L, SC(NH2)2 concentration in the range of 0.01 to 0.015mol/L, pH value in the range of 10 to 11, temperature in range of 85 to 90℃, deposition time general during from 20 to 30 min, annealing temperature 400℃, and appropriate ultrasonic vibration could benefict reduction film defects reduce the film defects, make thickness uniform and improve transmission rate, ect. In the conditions above, we prepared the large area (20cm×20cm) of CdS thin films, and tested the optical and electrical properties.
Secondly, it presented CdS thin films prepared by the vacuum evaporation. Analysis of preparation parameters include evaporation current, deposition time and annealing treatment influencing on the transmittance, structure and surface morphology of the CdS thin films by doing a series of experiment tests and using transmission spectroscopy, XRD spectra, Raman spectroscopy, SEM graph of characterization. When other conditions remained unchanged, the current less than 100A that deposition rate of the CdS thin films increased with the current becomed faster, while the crystallinity of films changed for the better. When other conditions remain unchanged, deposition time in less than 16min and the growth of CdS film thickness was almost linear. Post-annealing treatment would lead to CdS particles with a certain energy that could move within a certain range, as the annealing temperature increased, the particles gained more kinetic energy could be moved to larger and larger particles, and more uniform crystalline better. After annealing at 400℃, the structure, conductivity and optical properties of CdS thin films would be the best. So the optimum ranges were:evaporation current 100A, annealing temputer 400℃, deposition time 15min.
Finally, we prepared CdS/Cu2S bilayers by pulling method. Using the chemical bath deposition and vacuum evaporation prepared CdS thin films respectively, then dipping into a solution of CuCl and pulling out to be CdS/Cu2S bilayers. The light resistance and uniformity of CdS/Cu2S bilayers prepared by vacuum evaporation CdS thin films were excellent. In the experiment found that the CdS thin films without annealing and then depositing Cu2S was easy to fall off, annealing above 500℃the bilayer membrane deficit. After tested the photoelectric of CdS/Cu2S bilayers better than CdS monolayer.
本文比较详细的介绍了不同空间维度的CdS材料的研究现状、制备方法及应用前景等。
理论部分：首先,介绍了化学水浴沉积法制备CdS薄膜的生长机理。其次,介绍了真空蒸发法制备CdS薄膜的实验设备、操作流程、成膜原理及表征CdS薄膜的检测手段。
实验部分：首先,介绍了化学水浴沉积法制备CdS薄膜。在CBD法沉积CdS薄膜的实验中,发现CdS薄膜的生长受到多种因素的影响如：反应溶液的初始浓度、沉积时间、沉积温度、超声震荡和溶液搅拌速度等。这些因素中决定CdS薄膜厚度的主要是反应溶液的初始浓度及沉积温度。而且,后期的退火处理对CdS薄膜的结构、形貌、透射率也有很大影响。经过分组对比实验并且用XRD谱、SEM图、Raman谱、透射谱、荧光光谱等表征CdS薄膜而得出制备质量优异的CdS薄膜的最佳条件为：CdCl2的浓度范围选取为0.01～0.02mol/L,NH4Cl的浓度范围选取为0.02～0.04mol/L, SC(NH2)2的浓度范围选取为0.01-0.015mol/L, pH值范围选取为10-11,反应温度控制在85-90℃,沉积时间为20-30min,退火温度为400℃。且适当的超声震荡可使薄膜缺陷减少、厚度均匀和透射率提高等。在以上条件下,制备出大面积(20cm×20cm)的CdS薄膜,并测试了光导电特性。
其次,介绍了真空蒸发法制备CdS薄膜。经一系列实验并且用透射谱、XRD谱、SEM图等表征手段研究蒸发电流、沉积时间、退火处理等制备参数对CdS薄膜的透射率、结构和表面形貌的影响。当其他条件不变时,在蒸发电流小于100A的情况下,CdS薄膜沉积速率随着蒸发电流的增加而变快,同时薄膜的结晶性变好；当其他条件不变时,沉积时间在16min以内与CdS薄膜厚度的增长几乎是线性的；后期的退火处理,会使CdS粒子具有一定的能量,可以在一定范围内运动,随着退火处理温度的增加,粒子获得的动能更多,可移动的范围更大,能形成更大的粒子团,而且更加均匀,结晶性越好,400℃退火后的CdS薄膜结构、导电性及光学特性最佳。最后得到CdS薄膜的最佳制备条件为：蒸发电流：100A,退火温度：400℃,沉积时间：15min。
最后,用提拉法制备CdS/Cu2S双层膜。分别用化学水浴沉积法和真空蒸发法制备出的CdS薄膜浸渍到CuCl的溶液中,然后用提拉法制备出CdS/Cu2S双层膜。由真空蒸发法的CdS薄膜而制备的CdS/Cu2S双层膜的亮电阻及膜的均匀性等都优于由CBD法的CdS薄膜而制备的CdS/Cu2S双层膜。实验过程中发现,在未经退火处理的CdS薄膜上沉积Cu2S时,易脱落,退火处理高于500℃时,双层膜缺陷多。经测试CdS/Cu2S双层膜的光导电性优于CdS单层膜的。
Cadmium sulfide (CdS) is an excellent compound semiconductor photoelectric material, and showing potential application prospects in solar cells,optoelectronic devices,photocatalytic materials,nonlinear optical devices and so on.The large scale of CdS films research and application are especially important that study on it may boost the development of optoelectronic technology and its applications.
In this dissertation thesis the different spatial dimensions preparation of CdS were introduced. The recent advances and applications were reviewed.
Theoretical parts, first of all, it presented the desposition process and growth mechanism of CdS thin films prepared by the chemical bath deposition. Then introduced the laboratory equipment, operational processes, film deposition theory of CdS thin films prepared by vacuum evaporation,and detection means of characterize of CdS thin film.
Experimental parts, first of all, presented CdS thin films prepared by the chemical bath deposition. The growth behaviors of CBD-CdS thin films may be influenced by the experimental conditions, such as, the initial reaction solution concentration, deposition time, deposition temperature, ultrasonic vibration and the solution stirring speed. In these conditions factors, the initial reaction solution concentration and deposition temperature were the main conditions factors to determine the thickness of CdS thin films. In addition, post-annealing treatment had greatly affected on the structure, surface morphology and transmittance of CdS thin films. After comparing experimental groups and the characterization of CdS thin films by XRD spectra, SEM graph, Raman spectroscopy, transimission spectroscopy, fluorescence spectroscopy that we have obtained the optimum conditions to deposit CdS thin films in the CBD process. The optimum ranges were:CdCl2 concentration in the range of 0.01 to 0.02mol/L, NH4Cl concentration in the range of 0.02 to 0.04mol/L, SC(NH2)2 concentration in the range of 0.01 to 0.015mol/L, pH value in the range of 10 to 11, temperature in range of 85 to 90℃, deposition time general during from 20 to 30 min, annealing temperature 400℃, and appropriate ultrasonic vibration could benefict reduction film defects reduce the film defects, make thickness uniform and improve transmission rate, ect. In the conditions above, we prepared the large area (20cm×20cm) of CdS thin films, and tested the optical and electrical properties.
Secondly, it presented CdS thin films prepared by the vacuum evaporation. Analysis of preparation parameters include evaporation current, deposition time and annealing treatment influencing on the transmittance, structure and surface morphology of the CdS thin films by doing a series of experiment tests and using transmission spectroscopy, XRD spectra, Raman spectroscopy, SEM graph of characterization. When other conditions remained unchanged, the current less than 100A that deposition rate of the CdS thin films increased with the current becomed faster, while the crystallinity of films changed for the better. When other conditions remain unchanged, deposition time in less than 16min and the growth of CdS film thickness was almost linear. Post-annealing treatment would lead to CdS particles with a certain energy that could move within a certain range, as the annealing temperature increased, the particles gained more kinetic energy could be moved to larger and larger particles, and more uniform crystalline better. After annealing at 400℃, the structure, conductivity and optical properties of CdS thin films would be the best. So the optimum ranges were:evaporation current 100A, annealing temputer 400℃, deposition time 15min.
Finally, we prepared CdS/Cu2S bilayers by pulling method. Using the chemical bath deposition and vacuum evaporation prepared CdS thin films respectively, then dipping into a solution of CuCl and pulling out to be CdS/Cu2S bilayers. The light resistance and uniformity of CdS/Cu2S bilayers prepared by vacuum evaporation CdS thin films were excellent. In the experiment found that the CdS thin films without annealing and then depositing Cu2S was easy to fall off, annealing above 500℃the bilayer membrane deficit. After tested the photoelectric of CdS/Cu2S bilayers better than CdS monolayer.
引文
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