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ZnO薄膜的水溶液法制备及Li~+、柠檬酸钠对ZnO生长的影响

Preparation of ZnO Films by Aqueous Solution and the Influence of Li~+、 Citrate on the Growth of ZnO Films

作者: 专业:凝聚态物理 导师:张庆瑜 年度:2010  院校: 大连理工大学

Keywords

        ZnO是新一代的Ⅱ-Ⅵ族宽带隙半导体材料,具有纤锌矿晶体结构,室温下禁带宽度为3.37eV,激子束缚能为60meV,理论上可以实现室温下的受激发射,被认为是未来紫外发光器件的理想材料。ZnO薄膜具有良好的透明导电性,压电性,光电性,压敏性,因此具有广泛的应用前景。自从1997年Tang等人报道了ZnO薄膜的近紫外受激发射现象以来,ZnO再次成为当今半导体材料研究领域的热点。本文采用两步水溶液法,分别在处理过的蓝宝石衬底和硅衬底上成功的制备了ZnO薄膜,利用X射线衍射仪,PL光谱仪,反射光谱,SEM等测量手段对薄膜的结构,光学性能,表面形貌进行了分析,探讨了基片处理对ZnO薄膜生长的影响以及添加剂对ZnO薄膜生长的影响。论文分为以下两个部分:1.采用两步水溶液法,在经过酸煮,氮化,氧化处理的Al203(0001)基片上分别通过磁控溅射法和脉冲激光沉积方法预先生长ZnO种子层,再在此基础上通过水溶液的方法生长ZnO薄膜。XRD和Φ扫描结果表明,样品具有高c轴择优取向,并且与蓝宝石基片之间具有良好的外延关系。基片的处理方法,如酸煮,氮化,氧化能够影响薄膜的生长,种子层的结晶质量决定了ZnO薄膜的结晶质量。PL光谱显示,通过水溶液方法制备的ZnO薄膜的光量子效率接近单晶发光效率的80%。XRD,Φ扫描,SEM结果表明,通过脉冲激光沉积方法生长ZnO种子层比通过磁控溅射方法生长种子层,可以使薄膜的结晶质量有较大的提高,外延特性更强,薄膜表面更加平整,粗糙度更小,晶粒尺寸更大。2.采用两步水溶液法,在磁控溅射生长的ZnO种子层的Si(100)衬底上,通过水溶液生长方法制备了ZnO薄膜,研究了Li+和柠檬酸钠对ZnO薄膜生长的影响。扫描电镜结果显示,Li+能极大地改善ZnO薄膜的成膜特性,使薄膜更加均匀、连续、致密;溶液中添加柠檬酸钠制备的ZnO薄膜,晶粒尺寸没有出现明显的变化,PL光谱的发光强度较高,但薄膜生长速率显著降低,说明柠檬酸根离子有抑制ZnO生长的作用。
    ZnO is a newⅡ-Ⅵwide band gap semiconductor with a hexagonal wurtzite structure. ZnO has the band gap energy of 3.37eV at 300K and a large exciton binding energy (60meV), which makes it the promising materials for UV light-emitting devices. ZnO films also have some other potential applications such as transparent conductors, UV photodetectors, piezoelectric devices and gas sensors, etc. The renewed interest of ZnO film is fueled since room temperature lasing was reported by Tang et al.In this paper, high quality of ZnO films were deposited on silicon and pre-treated sapphire substrates successfully by a two-step aqueous solution routes. X-ray diffraction, room temperature photoluminescence (PL), reflection spectrum and scanning electron microscopy(SEM) were applied to analyze the microstructure, optical properties, surface morphology of the ZnO films. The results are summarized as follow:1. High quality ZnO films are grown on ZnO-buffered c-plane sapphire substrates at a low temperature of 70℃by a two-step aqueous solution process. The ZnO buffer was deposited on the pre-treated sapphire substrate by RF reactive magnetron sputtering or pulsed laser deposition(PLD). The treatment methods of sapphire include the acid etching, nitridation and oxidation. XRD scan and phi-scan results show the films are highly (001) textured and have epitaxial relationship with the substrates. Sapphire treatment, such as acid etching, nitridation and oxidation can influence the nucleation of the film growth, and the buffer layer determines the crystalline quality of the ZnO films. The maximum PL quantum efficiency of ZnO films grown with hydrothermal method is found to be about 80% of single-crystal ZnO.2. ZnO thin films are prepared on ZnO-buffered Si(100) substrates by a two-step aqueous process.We studied the influence of Li+and trisodium citrate on the growth of ZnO films. SEM results show that the Li+ions in the solution play the role to smooth the morphology of ZnO films, resulting in the films to be uniform, continuous and compact. For the films grown in the solution with citrates, the grain size of ZnO is not changed obviously, but the growth rates of the films are reduced considerably and the PL intensity is enhanced. The reduction of the growth rate can be attributed to the citrates inhibiting ZnO from the growth.
        

ZnO薄膜的水溶液法制备及Li~+、柠檬酸钠对ZnO生长的影响

摘要4-5
Abstract5
引言8-9
1. ZnO的材料特性9-17
    1.1 ZnO的基本性质9-10
    1.2 ZnO的光学性质10-11
    1.3 ZnO电学性质11
    1.4 ZnO的其他性质及应用11-12
        1.4.1 ZnO的压电特性11
        1.4.2 ZnO的压敏特性11-12
        1.4.3 ZnO的稀磁特性12
        1.4.4 纳米ZnO的应用12
    1.5 薄膜制备技术概论12-17
        1.5.1 脉冲激光沉积(Pulsed Laser Deposition,PLD)12-13
        1.5.2 分子束外延(MBE)13-14
        1.5.3 金属有机化学气相沉积(MOCVD)14-15
        1.5.4 磁控溅射法(Magnetron Sputtering)15
        1.5.5 溶胶-凝胶法(Sol-Gel)15
        1.5.6 喷涂热分解法(Spray Pyrolysis)15-16
        1.5.7 电子束反应蒸镀法(Reactive Electron Beam Evaporation)16
        1.5.8 水热法(Hydrothermal Synthesis)16-17
2 ZnO薄膜的制备方法及分析方法17-29
    2.1 反应磁控溅射法制备ZnO种子层17-19
        2.1.1 反应磁控溅射的基本原理17-19
        2.1.2 磁控溅射设备简介19
    2.2 脉冲激光沉积制备ZnO种子层19-22
        2.2.1 脉冲激光沉积的基本原理19-21
        2.2.2 实验设备简介21-22
    2.3 水溶液法制备ZnO薄膜22-23
        2.3.1 水溶液法生长ZnO的原理22
        2.3.2 水溶液法的实验条件22-23
    2.4 ZnO薄膜的表征方法23-29
        2.4.1 X射线衍射技术(XRD)23-24
        2.4.2 光致发光光谱(PL)24-25
        2.4.3 扫描电子显微镜(SEM)25-26
        2.4.4 透射光谱26-29
3 ZnO薄膜的水溶液制备与分析29-48
    3.1 磁控溅射制备ZnO种子层对ZnO薄膜的影响29-38
        3.1.1 实验部分29-30
            (1) 实验试剂29
            (2) 实验方案设计29-30
        3.1.2 结果与讨论30-38
    3.2 脉冲激光沉积ZnO种子层对ZnO薄膜的影响38-47
        3.2.1 实验部分38-39
        3.2.2 结果与讨论39-47
    3.3 本章小结47-48
4 添加剂对ZnO薄膜生长的影响48-59
    4.1 Li~+对ZnO薄膜生长的影响48-50
        4.1.1 实验方案设计48
        4.1.2 ZnO薄膜的制备48
        4.1.3 ZnO薄膜的表征与分析48-50
    4.2 柠檬酸钠对ZnO薄膜生长的影响50-58
        4.2.1 实验方案设计51
        4.2.2 ZnO薄膜的制备51
        4.2.3 ZnO薄膜的表征和分析51-58
    4.3 本章小结58-59
结论59-60
参考文献60-63
攻读硕士学位期间发表学术论文情况63-64
致谢64-66
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