Sol-gel法掺杂导电ZnO薄膜及其低温氮气热处理
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摘要
ZnO薄膜是一种直接宽带隙半导体材料,具有多种用途,可广泛的应用于太阳能电池、压电薄膜、光电器件、气敏器件和紫外探测器等方面。其特性可通过适当的掺杂来调剂。通过适量掺杂的ZnO透明导电薄膜具有优异的光电性能,能在太阳能电池、液晶显示器等多种电器设备中被用作透明导电电极。
本课题研究的主要目的是探索Sol-Gel法制备掺Al的ZnO透明导电薄膜在氮气中的稳定性和Sol-Gel法制备掺Li的ZnO透明导电薄膜的掺杂比和涂膜层数对薄膜导电率和透光率的影响。本文通过溶胶-凝胶法在载玻片上成功地制备出Al3+、Li+掺杂型ZnO薄膜。所用的溶胶以乙二醇甲醚为溶剂,醋酸锌为前驱体,单乙醇胺为稳定剂经加热搅拌制得;薄膜经烘干、预处理、氮气热处理后形成均匀透明的ZnO薄膜。
利用XRD、SEM、XPS、UV-VIS和四探针测试仪对薄膜的结构和光电特性进行了研究。结果表明,掺杂物、掺杂量、热处理温度、涂膜层数和热处理气氛对ZnO薄膜光电性能均有不同程度的影响。适当增加掺杂量能提高薄膜的电导率,过多的掺杂反而会降低电导率;不同的掺杂物对氮气中处理后的薄膜稳定性有较大影响,掺Al的薄膜稳定性很好,而Li的薄膜则较差;增加涂膜层数均能增加薄膜的厚度,并导致薄膜电导率的提高,同时也降低了薄膜的透射率;掺杂量和热处理气氛对薄膜在可见光范围内透射率影响不大;热处理气氛的不同直接影响了薄膜的导电性,在氮气中300℃可得到电导率高的薄膜。本实验制备的薄膜表面致密结构,晶粒大小均匀,方阻最低为270Ω/□,可见光透射率最大为83%。
溶胶-凝胶方法制备AZO薄膜的最佳工艺条件为:溶胶浓度0.6mol/L、掺杂Al量1at%、镀膜层数15层、预处理温度450℃、空气气氛热处理温度为550℃、氮气热处理温度为300℃;溶胶-凝胶方法制备LZO薄膜的最佳工艺条件为:溶胶浓度0.6mol/L、掺杂Li量2.3at%、镀膜层数10层、预处理温度450℃、空气气氛热处理温度为550℃、氮气热处理温度为300℃。
ZnO film, a semiconductor with wide direct band gap, has been actively studied because of its potential applications. It can be used in solar cell, piezoelectric device, photoelectric device, gas sensor and UV detector and the characteristics can be modulated by appropriate doping. The transparent ZnO conductive thin films doped with suitable dopants have excellent optical and electrical properties, and are applied widely as transparent and conductive oxide electrodes in various electrical and optical devices including liquid crystal display, solar cell and so on.
In this paper, the primary objective is researching the stability in N_2 of ZnO flims doped with Al by sol-gel and the influence of dopant concentration and the number of coating on the conductivity and transmittance of ZnO films doped with Li by sol-gel. ZnO thin films doped with Al~(3+),Li~+ were prepared on microslides by sol-gel method successfully. The sol was prepared with 2-methoxyethanol as solvent, Zincacetate as precursor and MEA as stabilizer. The mixture was heated, stirred to obtain the sol, and then homogenous transparent ZnO thin films were prepared from the sol by dipping, drying, pre-heat treatment in air and annealing in N_2 atmospheres.
XRD, SEM, XPS and Four-Point probe method were used to characterize the structure and optical and electrical properties of the ZnO thin films. The results showed that the kind of dopant, dopant concentration, temperature of pre-heat treatment, the number of coating and annealing atmosphere had influence in various extents on the photoelectric performance of the doped ZnO thin films. Increasing the dopant concentration could reduce resistivity of thin films, but over high dopant concentration would increase the resistivity. The difference of dopants has great influence on the stability of films annealed in N2; the stability of ZnO flims doped with Al is good but that doped with Li is bad. Increasing the number of coating could increase the thickness of thin films, which would reduce the resistivity and the transmittance within the range of visible light. The transmittance of thin films in the range of visible light was not impacted greatly by different dopant concentrations and annealing atmosphere. The different atmospheres can directly influence the electric conductivity. The film with low resistivity can be obtained by heat treatment in N2 at 300℃. In this experiment, the surface configuration of the films is compact, the sizes of crystal grain is uniform, the lowest sheet resistance is 270?/□and the maximum transmittance within the range of visible light is about 83%.
The optimum technological parameters for AZO and LZO thin film by sol-gel are as follows: the sol concentration is 0.6 mol/L; the dopant concentrations of Al and Li are 1at% and 2.3at%, respectively; the number of coating is 15 and 10, respectively; the pre-heat treatment temperature is 450℃and the annealing temperature is 550℃in air, 300℃in N_2.
本课题研究的主要目的是探索Sol-Gel法制备掺Al的ZnO透明导电薄膜在氮气中的稳定性和Sol-Gel法制备掺Li的ZnO透明导电薄膜的掺杂比和涂膜层数对薄膜导电率和透光率的影响。本文通过溶胶-凝胶法在载玻片上成功地制备出Al3+、Li+掺杂型ZnO薄膜。所用的溶胶以乙二醇甲醚为溶剂,醋酸锌为前驱体,单乙醇胺为稳定剂经加热搅拌制得;薄膜经烘干、预处理、氮气热处理后形成均匀透明的ZnO薄膜。
利用XRD、SEM、XPS、UV-VIS和四探针测试仪对薄膜的结构和光电特性进行了研究。结果表明,掺杂物、掺杂量、热处理温度、涂膜层数和热处理气氛对ZnO薄膜光电性能均有不同程度的影响。适当增加掺杂量能提高薄膜的电导率,过多的掺杂反而会降低电导率;不同的掺杂物对氮气中处理后的薄膜稳定性有较大影响,掺Al的薄膜稳定性很好,而Li的薄膜则较差;增加涂膜层数均能增加薄膜的厚度,并导致薄膜电导率的提高,同时也降低了薄膜的透射率;掺杂量和热处理气氛对薄膜在可见光范围内透射率影响不大;热处理气氛的不同直接影响了薄膜的导电性,在氮气中300℃可得到电导率高的薄膜。本实验制备的薄膜表面致密结构,晶粒大小均匀,方阻最低为270Ω/□,可见光透射率最大为83%。
溶胶-凝胶方法制备AZO薄膜的最佳工艺条件为:溶胶浓度0.6mol/L、掺杂Al量1at%、镀膜层数15层、预处理温度450℃、空气气氛热处理温度为550℃、氮气热处理温度为300℃;溶胶-凝胶方法制备LZO薄膜的最佳工艺条件为:溶胶浓度0.6mol/L、掺杂Li量2.3at%、镀膜层数10层、预处理温度450℃、空气气氛热处理温度为550℃、氮气热处理温度为300℃。
ZnO film, a semiconductor with wide direct band gap, has been actively studied because of its potential applications. It can be used in solar cell, piezoelectric device, photoelectric device, gas sensor and UV detector and the characteristics can be modulated by appropriate doping. The transparent ZnO conductive thin films doped with suitable dopants have excellent optical and electrical properties, and are applied widely as transparent and conductive oxide electrodes in various electrical and optical devices including liquid crystal display, solar cell and so on.
In this paper, the primary objective is researching the stability in N_2 of ZnO flims doped with Al by sol-gel and the influence of dopant concentration and the number of coating on the conductivity and transmittance of ZnO films doped with Li by sol-gel. ZnO thin films doped with Al~(3+),Li~+ were prepared on microslides by sol-gel method successfully. The sol was prepared with 2-methoxyethanol as solvent, Zincacetate as precursor and MEA as stabilizer. The mixture was heated, stirred to obtain the sol, and then homogenous transparent ZnO thin films were prepared from the sol by dipping, drying, pre-heat treatment in air and annealing in N_2 atmospheres.
XRD, SEM, XPS and Four-Point probe method were used to characterize the structure and optical and electrical properties of the ZnO thin films. The results showed that the kind of dopant, dopant concentration, temperature of pre-heat treatment, the number of coating and annealing atmosphere had influence in various extents on the photoelectric performance of the doped ZnO thin films. Increasing the dopant concentration could reduce resistivity of thin films, but over high dopant concentration would increase the resistivity. The difference of dopants has great influence on the stability of films annealed in N2; the stability of ZnO flims doped with Al is good but that doped with Li is bad. Increasing the number of coating could increase the thickness of thin films, which would reduce the resistivity and the transmittance within the range of visible light. The transmittance of thin films in the range of visible light was not impacted greatly by different dopant concentrations and annealing atmosphere. The different atmospheres can directly influence the electric conductivity. The film with low resistivity can be obtained by heat treatment in N2 at 300℃. In this experiment, the surface configuration of the films is compact, the sizes of crystal grain is uniform, the lowest sheet resistance is 270?/□and the maximum transmittance within the range of visible light is about 83%.
The optimum technological parameters for AZO and LZO thin film by sol-gel are as follows: the sol concentration is 0.6 mol/L; the dopant concentrations of Al and Li are 1at% and 2.3at%, respectively; the number of coating is 15 and 10, respectively; the pre-heat treatment temperature is 450℃and the annealing temperature is 550℃in air, 300℃in N_2.
引文
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