CdIn_2O_4薄膜的制备及光电性能研究
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摘要
CdIn2O4(CIO)薄膜是一种n型三元金属氧化物薄膜材料,由于其优异的光电性能和广泛的应用前景而倍受人们的青睐,成为当前透明导电氧化物(TCO)薄膜研究领域的热点之一。目前,商业上制备透明导电薄膜最常用的方法是直流反应磁控溅射法,但利用这种方法制备高质量的CIO薄膜的报道较少,缺乏低成本、大面积商业化制备技术是制约CIO薄膜走向实际应用的障碍之一。为此,本文在综述国内外CIO薄膜的研究发展概况基础上,采用实验研究与理论分析相结合的方法,对CIO薄膜的制备工艺和光电性能进行了较深入的研究。
本文在JGP450型高真空磁控溅射台上,采用直流反应磁控溅射法制备了CIO薄膜,用AFM、XRD和XPS分析了样品的表面形貌、组织结构、化学态和元素价态。结果表明:制备的薄膜是多晶结构,表面粗糙度为1.6nm～2.4nm,晶粒尺寸约为13nm～35nm,晶界比较清晰;薄膜含有CIO相、In2O3相,部分样品还含有微量的CdO相;CIO薄膜包含了Cd、In、O和C元素,并处于缺氧状态。采用霍尔效应测试仪、紫外-可见双光束分光光度计等手段对不同条件下制备的薄膜的电学和光学性能进行了分析,实验结果表明,随着氧浓度的降低、基底温度的增加和溅射时间的适当延长,薄膜的导电性能得到提高;而随着氧浓度的升高、基底温度的增加、溅射时间适当延长薄膜的透光性能得到提高。在N2气氛中进行退火处理有利于提高CIO薄膜的结晶度和光电性能。
从大量的实验数据中,归纳出光电性能与制备条件之间的关系,推荐直流反应磁控溅射法制备CIO薄膜的最佳制备工艺条件为:氧浓度为4.29%,工作压强为3.1Pa,沉积温度为250℃,溅射功率为50W,溅射时间为45min,靶基距为7.5cm。此条件下获得的薄膜,电阻率为2.95×10-4?.cm;载流子浓度为3.508×1020cm-3;霍尔迁移率为60.32cm2/V.S,在可见光区域内,波长为628nm时薄膜的透光率高达91.7%。可见CIO薄膜有着非常良好的光电性能。
此外,本文还研究了CIO薄膜的Seebeck效应,并利用Swanepoel方法从透射光谱中计算出薄膜厚度、吸收系数、光学带隙以及吸收带尾局域态宽度,并进行了机理分析。
CdIn2O4(CIO)thin film,n-type ternary mental oxides thin film materials, has attracted much attention for its excellent optical and electrical properties and foreground for comprehensive application, and become a hot point in the research field of transparent conducting oxides(TCO) thin film. At present, the direct-current (DC) reactive magnetron sputtering method is widely used in preparing TCO thin film in business while few studies on high quality CIO thin film prepared in this method were reported. The key factor which has impeded application of CIO thin film in practice is the lack of low cost and large-area commercialized preparation technology. Therefore, in this paper, based on the review of the development of CIO thin film both at home and abroad, adopting the methods of experimental research and theoretical analysis, the preparing conditions and the optical and electrical properties of CIO thin film were studied deeply.
In this paper, CIO thin film was prepared by DC reactive magnetron sputtering method in JGP450 type high vacuum magnetron sputtering apparatus, the surface morphology and structure of the CIO thin film were analyzed by AFM, XRD and XPS. The results indicate that the CIO thin film is polycrystalline structure and its surface roughness is 1.6nm～2.4nm, with the crystalline size being 13nm～35nm and very clear grain boundary. The CIO thin film consists of CIO phase and In2O3 phase, some samples still contain minimal CdO phase as well, Cd、In、O and C elements are included in CIO thin film which is in oxygen-deficient state.
The optical and electrical properties of the CIO thin film prepared in different preparing conditions were analyzed by Hall testing apparatus and double-light ultraviolet and visible photometer and so on, experiment results show that the electrical property is improved with the decrease of oxygen concentration and the increase of substrate temperature and the proper prolongation of the time; while the optical property is improved with the increase of oxygen concentration and the increase of substrate temperature and the proper prolongation of the time. The optical and electrical properties and crystal degree of CIO thin film are improved after being annealed in N2.
The relationship between optical and electrical properties and preparing conditions was summarized from lots of experiment data. It is recommended that the optimal preparing conditions of CIO thin film by DC magnetron sputtering method are that
本文在JGP450型高真空磁控溅射台上,采用直流反应磁控溅射法制备了CIO薄膜,用AFM、XRD和XPS分析了样品的表面形貌、组织结构、化学态和元素价态。结果表明:制备的薄膜是多晶结构,表面粗糙度为1.6nm～2.4nm,晶粒尺寸约为13nm～35nm,晶界比较清晰;薄膜含有CIO相、In2O3相,部分样品还含有微量的CdO相;CIO薄膜包含了Cd、In、O和C元素,并处于缺氧状态。采用霍尔效应测试仪、紫外-可见双光束分光光度计等手段对不同条件下制备的薄膜的电学和光学性能进行了分析,实验结果表明,随着氧浓度的降低、基底温度的增加和溅射时间的适当延长,薄膜的导电性能得到提高;而随着氧浓度的升高、基底温度的增加、溅射时间适当延长薄膜的透光性能得到提高。在N2气氛中进行退火处理有利于提高CIO薄膜的结晶度和光电性能。
从大量的实验数据中,归纳出光电性能与制备条件之间的关系,推荐直流反应磁控溅射法制备CIO薄膜的最佳制备工艺条件为:氧浓度为4.29%,工作压强为3.1Pa,沉积温度为250℃,溅射功率为50W,溅射时间为45min,靶基距为7.5cm。此条件下获得的薄膜,电阻率为2.95×10-4?.cm;载流子浓度为3.508×1020cm-3;霍尔迁移率为60.32cm2/V.S,在可见光区域内,波长为628nm时薄膜的透光率高达91.7%。可见CIO薄膜有着非常良好的光电性能。
此外,本文还研究了CIO薄膜的Seebeck效应,并利用Swanepoel方法从透射光谱中计算出薄膜厚度、吸收系数、光学带隙以及吸收带尾局域态宽度,并进行了机理分析。
CdIn2O4(CIO)thin film,n-type ternary mental oxides thin film materials, has attracted much attention for its excellent optical and electrical properties and foreground for comprehensive application, and become a hot point in the research field of transparent conducting oxides(TCO) thin film. At present, the direct-current (DC) reactive magnetron sputtering method is widely used in preparing TCO thin film in business while few studies on high quality CIO thin film prepared in this method were reported. The key factor which has impeded application of CIO thin film in practice is the lack of low cost and large-area commercialized preparation technology. Therefore, in this paper, based on the review of the development of CIO thin film both at home and abroad, adopting the methods of experimental research and theoretical analysis, the preparing conditions and the optical and electrical properties of CIO thin film were studied deeply.
In this paper, CIO thin film was prepared by DC reactive magnetron sputtering method in JGP450 type high vacuum magnetron sputtering apparatus, the surface morphology and structure of the CIO thin film were analyzed by AFM, XRD and XPS. The results indicate that the CIO thin film is polycrystalline structure and its surface roughness is 1.6nm～2.4nm, with the crystalline size being 13nm～35nm and very clear grain boundary. The CIO thin film consists of CIO phase and In2O3 phase, some samples still contain minimal CdO phase as well, Cd、In、O and C elements are included in CIO thin film which is in oxygen-deficient state.
The optical and electrical properties of the CIO thin film prepared in different preparing conditions were analyzed by Hall testing apparatus and double-light ultraviolet and visible photometer and so on, experiment results show that the electrical property is improved with the decrease of oxygen concentration and the increase of substrate temperature and the proper prolongation of the time; while the optical property is improved with the increase of oxygen concentration and the increase of substrate temperature and the proper prolongation of the time. The optical and electrical properties and crystal degree of CIO thin film are improved after being annealed in N2.
The relationship between optical and electrical properties and preparing conditions was summarized from lots of experiment data. It is recommended that the optimal preparing conditions of CIO thin film by DC magnetron sputtering method are that
引文
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[2] 李世涛,乔学亮,陈建国, 透明导电薄膜的研究现状及应用, 激光与光电子学研究进展, 2003, 40(7):53-59
[3] 孟扬,沈杰,蒋益明等, 透明导电氧化物薄膜的新进展,光电子技术,2002.9 22(3):125-130
[4] 钱伯强,俞大畏,潘惠英, 用于液晶显示的透明导电膜, 无机材料学报, 1995.3, 10(1):125-128
[5] 王敏,蒙继龙,透明导电氧化物薄膜的研究进展, 表面技术, 2003,32(1):5-7
[6] 曹建, 曹学峰, 热处理气氛对 CdSn2O4 透明导电薄膜化学态结构和电导率的影响, 太阳能学报, 1997, 118(12):212-214
[7] Yanagi H, Inoue S, Ueda K, et.al. Electronic structure and optoelectronic properties of transparent p-type conducting CuAlO2.J Appl Phys, 2000, 88(7): 4159-4163.
[8] Ueda K,Hase T,Yanagi H,et al.Epitaxial growth of transparent p-type conducting CuGaO2 thin films on sapphire (001) substrates by pulsed laser deposition, J.Appl Phys,2001,89(3):1790-1793.
[9] Hiromichi Ohta, Masahiro Orita, and Masahiro Hirano. Electronic structure and optical properties of SrCu2O2. J.Appl.Phys, 91(5): 3074-3078
[10] 刘世友, 铟锡氧化物薄膜的生产现状与应用, 材料科学与工程, 17(2):98-100
[11] 方泽波, 朋兴平, 谭永胜等, ZnO:Tb 透明导电薄膜的制备及其特性研究, 稀有金属, 28(3): 502-504
[12] Xiangfeng Chu. Xingqin Liu, Jianjun Deng et al. The effect of Ln3+ (Ln=Y, Nd) on the conductivity and gas-sensing properties of CdIn2O4 semiconductor. Sensors and Actuators B, 2000, 67:290-293.
[13] Xiangfeng Chu. Xingqin Liu, Yanchun Song et al. Study on gas-sensing properties of Cd1-xAgxIn2O4 semiconductor materials, Sensors and Actuators B, 1999, 61: 19-22.
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