脉冲激光沉积法生长掺杂ZnO基薄膜及其相关器件研究
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摘要
氧化锌(ZnO)是一种新型的氧化物半导体材料,具有直接带隙的能带结构,室温下的禁带宽度为3.37 eV,激子束缚能高达60 meV,在下一代短波长光电器件如蓝紫光发光二极管(LEDs)和激光器(LDs)等方面具有潜在应用前景。要实现ZnO在这些光电子器件中的广泛应用,首先必须得到性能良好的n型和p型材料。ZnO的n型掺杂主要集中在Ⅲ族元素(如Al、Ga、In),而理论研究表明F也是ZnO的一种良好的n型掺杂剂,但关于F掺杂ZnO体系的研究工作进展缓慢,因此本论文开展了F掺杂ZnO透明导电薄膜方面的研究。另一方面,对于ZnO的p型掺杂,由于其存在非对称掺杂局限性使性能良好且稳定的p型ZnO薄膜难以实现,是制约其在光电器件得到应用的最大瓶颈。此外,当前国际上对于何种元素是ZnO最佳受主的问题仍然没有统一的定论。因此本论文的重要内容之一是探求合适的p型掺杂元素和掺杂技术,并结合理论和实验进一步探讨其掺杂机理。本论文的主要工作包括如下内容：
1.利用脉冲激光沉积技术制备了F掺杂ZnO透明导电薄膜,系统地研究了氧偏压对薄膜性能的影响。当氧偏压为0.1 Pa时,薄膜的电学性能最佳：电阻率4.83×10-4Qcm,载流子浓度5.43×1020cm-3和Hall迁移率23.8 cm2V-1s-1,可见光内的平均透过率约90%,在1500 nm处透过率约60%；并以此为基础制备了顶栅结构的全透明ZnO薄膜晶体管,以ZnO薄膜为沟道层,ZnO:F透明导电薄膜作为栅极、源极和漏极的电极材料,栅极绝缘层是Ta2O5薄膜。
2.采用脉冲激光沉积技术实现Li-F共掺杂ZnO薄膜p型导电的转变,研究了衬底温度对薄膜性能的影响。当衬底温度为550℃时,薄膜具有最好的p型导电性能：电阻率23.45Ωcm,空穴浓度7.57×1017 cm-3和Hall迁移率0.35cm2V-1s-1。进一步利用基于密度泛函理论的第一性原理对ZnO:(Li,F)体系进行了理论计算,探索Li-F共掺杂技术实现p型ZnO的机理。
3.用脉冲激光沉积法成功制备出了Ag掺杂p型ZnMgO薄膜,详细地研究了衬底温度对薄膜性能的影响。XPS分析表明薄膜中Ag以Ag+形式存在并占据Zn格点位置；当衬底温度为400℃时,薄膜呈现最好的p型导电性能：电阻率24.96Ωcm,空穴浓度7.89×1017cm-3和Hall迁移率0.32 cm2V-1s-1,且p型导电性具有良好的稳定性；并对ZnMgO:Ag和ZnO:Ag薄膜进行了对比研究,结果发现引入Mg之后的ZnMgO:Ag薄膜不仅可以使本征施主态能级加深,同时能有效抑制氧空位的形成,导致本征施主态对受主的补偿作用降低,有利于薄膜p型掺杂的实现。
Zinc oxide (ZnO), as a novel oxide semiconductor with a direct band-gap structure, has been considered as a very promising material for the next-generation short-wavelength optoelectronic devices, such as light-emitting diodes (LEDs) and laser diodes (LDs) due to a wide band-gap of 3.37 eV and a large excition binding energy of 60 meV. To realize these device applications, an imperative issue is to fabrication both high-qulity n-and p-type ZnO. Most of the previous studies related to ZnO-based transparent conducting thin films were carried out using metallic cation dopants such as Group IIIA (e.g., Al, Ga, and In). However, fluorine can be a promising n-type anion doping candidate. To the best of our knowledge, research on F-doped ZnO thin films is very limited. Therefore, we carried out some investigation on fluorine-doped ZnO transparent conducting thin films. On the other hand, it has proven to be difficulty in obtain high-quality, reproducible, and stable p-type doping in ZnO caused by the asymmetric doping limitation, which is the bottleneck of realizing such optoelectronic applications. Also, the optimal choice of acceptor species in ZnO remains to be determined. In this regard, the main work was focused on pursuing the appropriate doping species and doping techniques in p-type ZnO thin films in this dissertation, in an attempt to better understand the p-type doping mechanism by a combinatorial theory and experimental studies. The main work included:
1. Highly transparent and conducting fluorine-doped ZnO thin films were prepared on glass substrates by pulsed laser deposition. The effects of oxygen pressure on the structural, electrical and optical properties of the films were investigated and discussed in detail. The minimum resistivity of 4.83x10"4Ω-cm. with a carrier concentration of 5.43×1020cm-3 and a Hall mobility of 23.8 cm2V"'s"', were obtained for fluorine-doped ZnO film prepared at the optimal oxygen pressure of 0.1 Pa. The average optical transmittance in the entire visible wavelength region was higher than 90%and the transmittance in 1500 nm was about 60%. In addition, a top-gated transparent ZnO-based thin-film transistor with a ZnO layer as the channel. Ta2O5 as the gate insulator and F-doped ZnO film as the gate/source/drain electrodes has been prepared.
2. We realized the p-type ZnO thin films via Li-F codoping technique prepared by pulsed laser deposition. The effects of substrate temperature on the structural and electrical properties of the films were investigated in detail. An acceptable p-type conduction, with a resistivity of 23.45Ωcm. a Hall mobility of 0.35 cm3v-1s-1, and a hole concentration of 7.57x1017 cm-3 at room temperature, has been obtained for the Li-F codoped ZnO thin films grown at 550℃The possible formation mechanism of the p-type conduction in Li-F codoped ZnO has been proposed by first-principles calculations based on density functional theory.
3. We reported on p-type Ag-doped ZnMgO thin films prepared on quartz substrates by pulsed laser deposition. The effects of substrate temperature on the structural, electrical and optical properties of the films were investigated in detail. XPS measurement confirmed that Ag principally occupies Zn site in the state of Ag+ ion and acts as an acceptor. An acceptable p-type conduction, with a resistivity of 24.96Ωcm. a Hall mobility of 0.32 cm2v-1s-1.and hole concentration of 7.89x1017 cm-3 at room temperature, was obtained for the film grown at the optimal substrate temperature of 400℃Meanwhile, a comparative study of p-type ZnO.Ag and ZnMgO:Ag films showed that the incorporation of Mg can result in the increase of the activation energy of the intrinsic donors and the suppression of charge-compensating oxygen-related defects, thus reduce the charge compensation effect of intrinsic defects, which is favorable to the realization of p-type ZnO thin films.
1.利用脉冲激光沉积技术制备了F掺杂ZnO透明导电薄膜,系统地研究了氧偏压对薄膜性能的影响。当氧偏压为0.1 Pa时,薄膜的电学性能最佳：电阻率4.83×10-4Qcm,载流子浓度5.43×1020cm-3和Hall迁移率23.8 cm2V-1s-1,可见光内的平均透过率约90%,在1500 nm处透过率约60%；并以此为基础制备了顶栅结构的全透明ZnO薄膜晶体管,以ZnO薄膜为沟道层,ZnO:F透明导电薄膜作为栅极、源极和漏极的电极材料,栅极绝缘层是Ta2O5薄膜。
2.采用脉冲激光沉积技术实现Li-F共掺杂ZnO薄膜p型导电的转变,研究了衬底温度对薄膜性能的影响。当衬底温度为550℃时,薄膜具有最好的p型导电性能：电阻率23.45Ωcm,空穴浓度7.57×1017 cm-3和Hall迁移率0.35cm2V-1s-1。进一步利用基于密度泛函理论的第一性原理对ZnO:(Li,F)体系进行了理论计算,探索Li-F共掺杂技术实现p型ZnO的机理。
3.用脉冲激光沉积法成功制备出了Ag掺杂p型ZnMgO薄膜,详细地研究了衬底温度对薄膜性能的影响。XPS分析表明薄膜中Ag以Ag+形式存在并占据Zn格点位置；当衬底温度为400℃时,薄膜呈现最好的p型导电性能：电阻率24.96Ωcm,空穴浓度7.89×1017cm-3和Hall迁移率0.32 cm2V-1s-1,且p型导电性具有良好的稳定性；并对ZnMgO:Ag和ZnO:Ag薄膜进行了对比研究,结果发现引入Mg之后的ZnMgO:Ag薄膜不仅可以使本征施主态能级加深,同时能有效抑制氧空位的形成,导致本征施主态对受主的补偿作用降低,有利于薄膜p型掺杂的实现。
Zinc oxide (ZnO), as a novel oxide semiconductor with a direct band-gap structure, has been considered as a very promising material for the next-generation short-wavelength optoelectronic devices, such as light-emitting diodes (LEDs) and laser diodes (LDs) due to a wide band-gap of 3.37 eV and a large excition binding energy of 60 meV. To realize these device applications, an imperative issue is to fabrication both high-qulity n-and p-type ZnO. Most of the previous studies related to ZnO-based transparent conducting thin films were carried out using metallic cation dopants such as Group IIIA (e.g., Al, Ga, and In). However, fluorine can be a promising n-type anion doping candidate. To the best of our knowledge, research on F-doped ZnO thin films is very limited. Therefore, we carried out some investigation on fluorine-doped ZnO transparent conducting thin films. On the other hand, it has proven to be difficulty in obtain high-quality, reproducible, and stable p-type doping in ZnO caused by the asymmetric doping limitation, which is the bottleneck of realizing such optoelectronic applications. Also, the optimal choice of acceptor species in ZnO remains to be determined. In this regard, the main work was focused on pursuing the appropriate doping species and doping techniques in p-type ZnO thin films in this dissertation, in an attempt to better understand the p-type doping mechanism by a combinatorial theory and experimental studies. The main work included:
1. Highly transparent and conducting fluorine-doped ZnO thin films were prepared on glass substrates by pulsed laser deposition. The effects of oxygen pressure on the structural, electrical and optical properties of the films were investigated and discussed in detail. The minimum resistivity of 4.83x10"4Ω-cm. with a carrier concentration of 5.43×1020cm-3 and a Hall mobility of 23.8 cm2V"'s"', were obtained for fluorine-doped ZnO film prepared at the optimal oxygen pressure of 0.1 Pa. The average optical transmittance in the entire visible wavelength region was higher than 90%and the transmittance in 1500 nm was about 60%. In addition, a top-gated transparent ZnO-based thin-film transistor with a ZnO layer as the channel. Ta2O5 as the gate insulator and F-doped ZnO film as the gate/source/drain electrodes has been prepared.
2. We realized the p-type ZnO thin films via Li-F codoping technique prepared by pulsed laser deposition. The effects of substrate temperature on the structural and electrical properties of the films were investigated in detail. An acceptable p-type conduction, with a resistivity of 23.45Ωcm. a Hall mobility of 0.35 cm3v-1s-1, and a hole concentration of 7.57x1017 cm-3 at room temperature, has been obtained for the Li-F codoped ZnO thin films grown at 550℃The possible formation mechanism of the p-type conduction in Li-F codoped ZnO has been proposed by first-principles calculations based on density functional theory.
3. We reported on p-type Ag-doped ZnMgO thin films prepared on quartz substrates by pulsed laser deposition. The effects of substrate temperature on the structural, electrical and optical properties of the films were investigated in detail. XPS measurement confirmed that Ag principally occupies Zn site in the state of Ag+ ion and acts as an acceptor. An acceptable p-type conduction, with a resistivity of 24.96Ωcm. a Hall mobility of 0.32 cm2v-1s-1.and hole concentration of 7.89x1017 cm-3 at room temperature, was obtained for the film grown at the optimal substrate temperature of 400℃Meanwhile, a comparative study of p-type ZnO.Ag and ZnMgO:Ag films showed that the incorporation of Mg can result in the increase of the activation energy of the intrinsic donors and the suppression of charge-compensating oxygen-related defects, thus reduce the charge compensation effect of intrinsic defects, which is favorable to the realization of p-type ZnO thin films.
引文
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