掺铝掺硅氧化锌薄膜的制备工艺及其性能研究
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摘要
氧化锌铝(ZAO)透明导电薄膜具有可见光透过率高、红外反射率高、电阻率低等特点,在平板显示器、太阳能薄膜电池、热反射镜、薄膜玻璃等领域具有极其广泛的应用前景。
     本文采用预压成型加常压烧结的工艺方法,制备了ZAO陶瓷靶材,利用交流磁控溅射方法,采用ZAO陶瓷靶材制备了ZAO薄膜。研究了靶材中Al_2O_3含量对溅射靶材所制备的ZAO薄膜性能的影响,结果表明,当Al_2O_3含量为2.0wt%时,所制备的ZAO薄膜电学光学性能最优。
     本文中,利用四探针电阻测试仪测试了ZAO薄膜的电学性能;利用分光光度计和红外谱仪测试了ZAO薄膜的光学性能;利用扫描电镜、原子力显微镜和X射线衍射仪等设备测试了薄膜的表面形貌和结构。
     比较系统地研究了制备ZAO薄膜的工艺参数,即本底真空压力、靶电流密度、氧流量、基体温度和氩气压力等五个因素对ZAO薄膜性能的影响规律。在大量试验结果和综合分析的基础上确定优化工艺为:靶材中Al_2O_3含量为2.0wt%,本底真空压力2.0×10~(-3) Pa,纯氩溅射,靶电流密度6.67 mA/cm~2,基体温度250℃,氩气压力0.8 Pa;在上述优化工艺条件下沉积了厚度为127 nm的薄膜,方阻为32Ω/□,薄膜电阻率4.6×10~(-4)Ω·cm,可见光区平均透过率86%。性能已达到国际先进水平。
     研究了具有绒面结构的ZAO薄膜的光学性能和表面特征。通过分析氩气压力、基体温度和薄膜厚度对绒面结构的影响规律,得出了制备具有不同绒度和粗糙度的绒面ZAO薄膜的工艺参数。并制备出具有与已获实际应用的绒面FTO薄膜相比拟绒度的绒面ZAO薄膜。
     分析了薄膜厚度、基体温度和氩气压力对红外反射性能的影响规律。确定了制备具有高红外反射率的ZAO薄膜制备工艺。制备的ZAO薄膜的红外反射率大于80%。
     采用冷压预成型加常压烧结方法,制备了氧化锌硅(ZSO)陶瓷靶材。确定了制备ZSO靶材的优化工艺参数。并初步研究了基体温度和氩气压力对ZSO薄膜性能的影响。
Aluminum doped zinc oxide (ZAO) transparent conductive thin films with high transparency in visible wavelength range, high infrared reflection, and low resistivity will be widely used in many fields such as flat display panel, thin film solar cell, and heat reflection glass.
     In the work, ZAO ceramic targets were manufactured by a composite process of cold mould pressing and sintering. ZAO thin films were prepared by middle-frequency magnetron sputtering with the ZAO target. The effects of Al_2O_3 concentration in target on the electrical and optical properties of ZAO films were investigated. The results showed that ZAO film with optimum properties can be obtained by sputtering the ZAO ceramic target with Al_2O_3 concentration of 2.0wt%.
     Four-point probe tester was employed to measure electrical properties. UV-VIS and IR spectrometry were used to examine optical properties at different wavelength. Surface morphology and microstructure were characterized by scanning electronic microscopy (SEM), atomic force microscopy (AFM), and X-ray diffraction (XRD), respectively.
     The effects of the technological parameters for preparing ZAO film including base vacuum pressure, target current density, oxygen pressure, substrate temperature, and argon gas pressure on the properties of ZAO films were systematically studied. Based on a lot of experimental results and comprehensive analysis, the optimum technological parameters were determined as follows: substrate temperature: 250℃, target current density: 6.67 mA/cm~2, base vacuum pressure: 2.0×10~(-3) Pa,argon gas pressure:0.8 Pa without oxygen. Under the optimum preparation condition, the ZAO film with the best properties of average transmittance of 86% in visible range, sheet resistance of 32Ω/□, and resistivity of 4.6×10~(-4)Ω·cm at film thickness of 127 nm, which reach international level, was obtained.
     The optical properties and surface morphology characterization of milky ZAO films were studied. The technological parameters for preparing milky ZAO films with various hazes and surface roughnesses were obtained by analyzing the effects of argon gas pressure, substrate temperature, and film thickness on the surface structure of milky films. Meanwhile milky ZAO films with similar haze to milky FTO films, which was already used commercially, can be easily deposited.
     The influence of film thickness, substrate temperature, and argon gas pressure on the performance of infrared reflection was experimentally analyzed. The deposition parameters for the ZAO films with high infrared reflection of exceeding 80% were gotten.
     Dense Si-doped ZnO (ZSO) ceramic target could be also prepared by cold mould pressing plus sintering under optimized technological parameters. The influence of substrate temperature and argon gas pressure on the electrical and optical properties of ZSO films was preliminary investigated.
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