ZnO：Al透明导电薄膜的磁控溅射制备及其特性研究
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摘要
本文采用直流磁控溅射技术在玻璃衬底上制备ZnO:Al透明导电薄膜,研究了衬底温度、溅射功率、退火气氛等工艺参数对薄膜性能的影响,并对薄膜其影响机制进行了探讨。在此基础上,以实现高质量ZnO:Al薄膜的低温沉积为目标,采用在溅射气氛中引入H2和ZnO:Al靶、Zn靶两靶共溅射两种方法制备ZnO:Al薄膜来改善低温沉积下的电学性质。得出以下主要结果：
(1)采用直流(DC)磁控溅射技术,以ZnO:Al陶瓷靶(ZnOwt%:Al2O3wt%=98:2)为靶材,在玻璃衬底上制备高透明和高导电的ZnO:Al薄膜。所制备的ZnO:Al薄膜均为具有(002)面择优取向的六角纤锌矿结构且c轴垂直于衬底,薄膜的晶粒尺寸均在18-32nm之间。
(2)衬底温度、溅射功率和退火气氛等因素对薄膜的结构、光学及电学性能均有很大的影响。衬底温度为400℃、溅射功率为120 W时,ZnO:Al薄膜的结晶性能最好。所有的ZnO:Al薄膜在可见光区域均表现出了良好的透过性能。随着衬底温度的升高,薄膜电阻率下降,当衬底温度为500℃时,ZnO:Al薄膜的电阻率降到最低,在真空、Ar气等气氛下退火后,ZnO:Al薄膜电阻率降低,而在O2,N2和空气等气氛下退火后,ZnO:Al薄膜电阻率增加。
(3)采用在溅射气氛中通入H2、衬底温度为200℃的低温条件下制备ZnO:Al薄膜。随着溅射气氛中H2流量的增加,薄膜的晶粒尺寸减小,载流子浓度上升,电阻率下降；薄膜在400-900 nm范围内透过率均保持的90%以上,体现出良好的光透性能。
(4)首次采用ZnO:Al靶和Zn靶两靶共溅射的方法,研究了Zn靶功率和衬底温度对薄膜性能的影响。随着Zn靶的溅射功率的增加,ZnO:Al薄膜的晶面间距增大,载流子浓度升高,而电阻率随之下降,这主要由于Zn填隙浓度增加造成。还发现在两靶共溅射模式下,随着衬底温度的升高,ZnO:Al薄膜的结构性能、光透过性能学和电导性能均有所改善。
In this paper ZnO:Al transparent conductive fims were deposited on glass substrate by using DC magnetron sputtering technique. The effects of substrate temperature, sputtering power and annealing atmosphere on the film structure, optical and electrical properties have been studied systemically, and the mechanisms of electrical property are discussed. In addition, in order to realize high quanity ZnO:Al films deposition at low temperature, H-doping and ZnO:Al target, Zn target co-sputtering methods are applied to grow ZnO:Al films, the influence of H2 flows, the power on Zn target and substrate temperature on ZnO:Al films properties were investigated in details separately. The main results obtained as follows:
(1) ZnO:Al thin films have been deposited on glass substrate applying ZnO:Al ceramic target by DC magnetron sputtering. All the ZnO:Al films with the preferential orientation of (002) plane are polycrystalline and possess hexagonal wurtzite structure with their crystallographic c-axis perpendicular to the substrate. The grain size of the films is between 18-32 nm.
(2) Substrate temperature, sputtering power and annealing atmosphere have great influences on structure, optical and electrical properties of ZnO:Al films. The crystalline quality of ZnO:Al film is best when the film was prepared under 120 W of sputtering power and 400℃of substrate temperature. All the films show good transmittance during the visible region. Resistivity decrease with the increasing of substrate temperature; the resistivity drops to the lowest, when the film was prepared at 500℃; after annealing in vacuum and Ar, the resistivity drop, but after annealing in O2, N2 and air, the resistivity rise.
(3) To realize high quanity ZnO:Al films deposition at low temperature, The effects of H2 flows in the sputtering atmosphere on the properties of ZnO:Al films are studied. As the H2 flow incresing, grain size decreases, carrier concentration increases and resistivity drops. The transmittance of ZnO:Al films is above 90% from 400-900 nm, indicating excellent optical property.
(4) The influence of power on Zn target and substrate temperature on the properties of ZnO:Al films is studied by using ZnO:Al target, Zn target co-sputtering. With the increasing of the power on Zn target, the content of Zn element rise and the crystalline distance increases, which may be result of the the increasement of the concentration of Zn interstitial, carrier concentration goes up and resistivity drops correspondingly. With the increasing of substrate temperature, the structure, transmittance and resistivity have been improved.
(1)采用直流(DC)磁控溅射技术,以ZnO:Al陶瓷靶(ZnOwt%:Al2O3wt%=98:2)为靶材,在玻璃衬底上制备高透明和高导电的ZnO:Al薄膜。所制备的ZnO:Al薄膜均为具有(002)面择优取向的六角纤锌矿结构且c轴垂直于衬底,薄膜的晶粒尺寸均在18-32nm之间。
(2)衬底温度、溅射功率和退火气氛等因素对薄膜的结构、光学及电学性能均有很大的影响。衬底温度为400℃、溅射功率为120 W时,ZnO:Al薄膜的结晶性能最好。所有的ZnO:Al薄膜在可见光区域均表现出了良好的透过性能。随着衬底温度的升高,薄膜电阻率下降,当衬底温度为500℃时,ZnO:Al薄膜的电阻率降到最低,在真空、Ar气等气氛下退火后,ZnO:Al薄膜电阻率降低,而在O2,N2和空气等气氛下退火后,ZnO:Al薄膜电阻率增加。
(3)采用在溅射气氛中通入H2、衬底温度为200℃的低温条件下制备ZnO:Al薄膜。随着溅射气氛中H2流量的增加,薄膜的晶粒尺寸减小,载流子浓度上升,电阻率下降；薄膜在400-900 nm范围内透过率均保持的90%以上,体现出良好的光透性能。
(4)首次采用ZnO:Al靶和Zn靶两靶共溅射的方法,研究了Zn靶功率和衬底温度对薄膜性能的影响。随着Zn靶的溅射功率的增加,ZnO:Al薄膜的晶面间距增大,载流子浓度升高,而电阻率随之下降,这主要由于Zn填隙浓度增加造成。还发现在两靶共溅射模式下,随着衬底温度的升高,ZnO:Al薄膜的结构性能、光透过性能学和电导性能均有所改善。
In this paper ZnO:Al transparent conductive fims were deposited on glass substrate by using DC magnetron sputtering technique. The effects of substrate temperature, sputtering power and annealing atmosphere on the film structure, optical and electrical properties have been studied systemically, and the mechanisms of electrical property are discussed. In addition, in order to realize high quanity ZnO:Al films deposition at low temperature, H-doping and ZnO:Al target, Zn target co-sputtering methods are applied to grow ZnO:Al films, the influence of H2 flows, the power on Zn target and substrate temperature on ZnO:Al films properties were investigated in details separately. The main results obtained as follows:
(1) ZnO:Al thin films have been deposited on glass substrate applying ZnO:Al ceramic target by DC magnetron sputtering. All the ZnO:Al films with the preferential orientation of (002) plane are polycrystalline and possess hexagonal wurtzite structure with their crystallographic c-axis perpendicular to the substrate. The grain size of the films is between 18-32 nm.
(2) Substrate temperature, sputtering power and annealing atmosphere have great influences on structure, optical and electrical properties of ZnO:Al films. The crystalline quality of ZnO:Al film is best when the film was prepared under 120 W of sputtering power and 400℃of substrate temperature. All the films show good transmittance during the visible region. Resistivity decrease with the increasing of substrate temperature; the resistivity drops to the lowest, when the film was prepared at 500℃; after annealing in vacuum and Ar, the resistivity drop, but after annealing in O2, N2 and air, the resistivity rise.
(3) To realize high quanity ZnO:Al films deposition at low temperature, The effects of H2 flows in the sputtering atmosphere on the properties of ZnO:Al films are studied. As the H2 flow incresing, grain size decreases, carrier concentration increases and resistivity drops. The transmittance of ZnO:Al films is above 90% from 400-900 nm, indicating excellent optical property.
(4) The influence of power on Zn target and substrate temperature on the properties of ZnO:Al films is studied by using ZnO:Al target, Zn target co-sputtering. With the increasing of the power on Zn target, the content of Zn element rise and the crystalline distance increases, which may be result of the the increasement of the concentration of Zn interstitial, carrier concentration goes up and resistivity drops correspondingly. With the increasing of substrate temperature, the structure, transmittance and resistivity have been improved.
引文
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[3]孙柏.PLD技术制备ZnO薄膜及其结构和发光性质的研究.[博士学位论文].合肥：中国科学技术大学,2007
[4]黄昆,谢希德.半导体物理学.北京：科学出版社,1958.236
[5]E.L. Papadopoulou, M. Varda, K. Kouroupis-Agalou, M. Androulidaki, E. Chikoidze, P. Galtier, G. Huyberechits, E. Aperathitis. Undoped and Al-ZnO films with tuned properties grown by pulsed laser deposition. Thin solid films,2008, (516): 8141
[6]Klaus Ellmer, Rainald Mientus. Carrier transport in polycrystalline ITO and ZnO:Al Ⅱ:the influence of grain barriors and boundaries. Thin Solid Films,2008, 516:4620
[7]M.Chen, Z.L.Pei, X.Wang, et al. Structural, electrical, and optical properties of transparent conductive oxide ZnO:Al films prepared by magnetron reactive sputtering. J. Vac. Sci. Technol,2001, A19(3):963
[8]Wei Li, Yun sun, Yaxin Wang, et al. Effects of substrate temperature on the properties of facing-target sputtered Al-doped ZnO films. Sol. Energy Mater. Sol. Cells,2007,91(8):659
[9]F. Couzinie-Devy, N. Barreau, J. Kessler. Dependence of ZnO:Al properties on the substrate to target position in RF sputtering. Thin solid films,2008, (516):7049
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