Na掺杂ZnO性能研究
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摘要
ZnO是一种宽禁带直接带隙半导体,其禁带宽度为3.37eV。由于ZnO的高激子束缚能(60meV)而备受关注。同时,由于ZnO单晶及薄膜制备工艺的不断完善,使得ZnO在各个领域都有广泛的应用,如发光二极管、透明导电薄膜、紫外探测器及气敏材料等。由于ZnO掺杂的不对称性,使得n型ZnO非常容易通过本征缺陷或故意掺杂获得,但是,至目前为止,高质量稳定的p型ZnO的制备仍然比较困难。ZnO中的p型掺杂剂通常为I族及V族元素,其中,Na作为有效p型掺杂而受到广泛关注。理论计算显示Na掺杂可以在ZnO中形成浅受主能级,同时由于Na与Zn的离子半径相近,形成的受主掺杂Na_Zn引起的晶格畸变较小。在实验方面,Na掺杂ZnO相关的报道越来越多,也不乏p型ZnO及ZnO基同质结的实现。叶志镇教授课题组是最早开展Na掺杂ZnO研究的课题组之一,并取得了相当的成果。本文的工作在此基础上开展,通过PLD、热扩散及离子注入等方法对Na掺杂ZnO的制备和性质进行研究。本论文工作主要包含以下内容：
1.采用PLD工艺,在石英衬底上制备了多层结构的Naδ掺杂p型ZnO薄膜。实验中以NaF陶瓷靶材为Na源,研究了衬底温度及氧气压强对Na δ掺杂ZnO薄膜电学性能的影响。并获得了最佳的p型Na掺杂ZnO薄膜,其载流子浓度为7.9x10~(17)cm~(-3),电阻率为29.8Ωcm,霍尔迁移率为0.263cm2/Vs。此方面的工作为p型ZnO薄膜掺杂提供了新的思路。
2.以本征ZnO薄膜为衬底,通过热扩散制备了Na掺杂p型ZnO薄膜。其中,如1所述,Na源层通过PLD法获得。在此基础上,获得最佳的p型Na掺杂ZnO薄膜的载流子浓度为1.94×10~(15) cm~(-3),电阻率7.54Ωcm,霍尔迁移率为7.54cm2/Vs。通过霍尔及XPS结果分析,热扩散温度及时间是影响Na掺杂ZnO薄膜电学性能的主要因素。同时,我们制备的ZnO基同质结显示出良好的整流效应,进一步证实了通过热扩散方法掺杂的ZnO薄膜确实为p型ZnO。
3.通过三重Na离子注入,在ZnO单晶中实现了厚度约300nm的均匀Na掺杂ZnO层。低温PL显示,经过850℃,6min的快速热处理后,ZnO中位于3.352eV(I_10)的发光峰得到显著增强,我们认为其与Na受主相关。同时,我们制备的ZnO基同质结显示出良好的整流效应,证实了通过此方法制备的薄膜为p型ZnO薄膜。此外,我们还研究了单次Na离子注入对单晶ZnO影响。
4.我们采用离子注入工艺制备了Na掺杂的ZnO纳米阵列,并研究了退火温度对其光学性能的影响。实验发现通过在600-800℃下的退火处理可对ZnO中的辐射缺陷进行有效修复。同时,经过800℃退火后,ZnO薄膜的低温PL谱中显示了位于3.352eV(I10)的发光峰,其与Na受主NaZn目关。此外,随着退火温度的升高,I6-8发光峰强度下降,而I3发光峰强度升高,说明更多的中性施主在高温下产生了电离。
5.经过Ne离子注入的ZnO纳米阵列的光致发光谱中具有精细结构的紫光发光峰。其精细结构间隔为72meV,对应于ZnO中纵光学声子能量。通过拟合计算获得的黄昆因子为1.98,其电子声子耦合能量低于绿光发光带而高于DAP。激活能为160meV,我们以为,这与离子注入过程中引入的受主缺陷相关。
ZnO is an attractive wide-band-gap semiconductor with a direct band gap of3.37eV at room temperature. The large exciton binding energy (60meV) and well-developed bulk, film growth processes promise its optoelectronic applications, such as light emitting diodes (LEDs), transparent conductive layer, photodetector and gas sensor. Due to the asymmetric doping limitations, n-type ZnO can be easily obtained via intrinsic or extrinisic dopants, whereas it has thus-far proven very difficult to obtain high quality and stable p-type ZnO. Recently, Na has been considered as an effective p type dopant in ZnO. There has been many reports on p-type Na-doped ZnO using various methods. Theoretical studies indicate that Na doping produces shallow acceptor state and small relaxation for Nazn.Moreover, p-type ZnO thin film and ZnO-based p-n homoj unction fabricated by various methods prove Na as an effective p-type dopant in ZnO. In this thesis we focus on growth and characterization of Na doped p type ZnO obtained by pulsed laser deposition (PLD), diffusion and ion implantation methods. The thesis includes:
1. Na δ-doped p-type ZnO thin films were fabricated on quartz substrates with the structure of ZnO/Na (δ-layer) multi-layers by PLD. NaF ceramic target was used as Na source. The effects of oxygen pressure and substrate temperature on the electrical properties of δ-doped ZnO thin films were discussed. An optimized result with a resistivity of29.8Ωcm, Hall mobility of0.263cm2/Vs, and hole concentration of7.9×1017cm-3was achieved, and electrically stable over several months. The work is of interest for developing a novel method to realize p-type ZnO thin films doping with Na.
2. Na-diffused p-type ZnO thin films have been realized via pulsed laser deposition using NaF ceramic target followed by rapid thermal process in nitrogen. An optimized result with a resistivity of426.7Ω·cm, Hall mobility of7.54cm2/Vs, and hole concentration of1.94×1015cm-3was achieved, and electrically stable over several months. Hall-effect measurements supported by X-ray photoelectron spectroscopy indicated that diffusion temperature and diffusion time played a key role in optimizing the p-type conduction of Na-diffused ZnO thin films. Furthermore, ZnO-based p-n homoj unction was obtained by fabrication of a Na-diffused p-type ZnO layer on an undoped n-type ZnO layer.
3. Three-folder Na+ion implantation is applied to form a plant region of Na doped ZnO. Low temperature PL shows that a well-resolved bound exciton line at3.352eV with a linewidth of～8meV emerges from the850℃,6min annealed sample and is likely related to the formation of NaZn acceptor. ZnO-based p-n homojunction was obtained by three-folder Na+implanted layer. Also one time Na+implanted single crystal ZnO was studied.
4. The effects of annealing temperature on excitonic emissions from Na+ion implanted ZnO nanorods are studied and annealing at between600and800℃can effectively repair the implantation as evidenced by the enhanced excitonic emissions. A well-resolved bound exciton line at3.352eV with a linewidth of～2meV emerges from the800℃annealed sample and is likely related to the formation of NaZn acceptor. When the annealing temperature is increased, the intensity of the I6-8line decreases while that of I3increases, suggesting enhanced ionization of neutral donors at elevated temperature.
5. Unusual vibronic fine structures of the～3.0eV violet emission from ion-implanted ZnO nanorods has been investigated by photoluminescence (PL). A set of equally separated peaks with energy spacing of72meV, which corresponds to the longitudinal optical (LO) phonon energy of ZnO, were well resolved in the low temperature PL spectra. The overall emission band can be perfectly described by LO phonon-assisted transition with the Huang-Rhys factor of1.98, indicating intermediate electron-phonon coupling. The thermal quenching of PL gives rise to activation energy of～160meV, which is attributed to the energy level of acceptor-like defects introduced by implantation.
1.采用PLD工艺,在石英衬底上制备了多层结构的Naδ掺杂p型ZnO薄膜。实验中以NaF陶瓷靶材为Na源,研究了衬底温度及氧气压强对Na δ掺杂ZnO薄膜电学性能的影响。并获得了最佳的p型Na掺杂ZnO薄膜,其载流子浓度为7.9x10~(17)cm~(-3),电阻率为29.8Ωcm,霍尔迁移率为0.263cm2/Vs。此方面的工作为p型ZnO薄膜掺杂提供了新的思路。
2.以本征ZnO薄膜为衬底,通过热扩散制备了Na掺杂p型ZnO薄膜。其中,如1所述,Na源层通过PLD法获得。在此基础上,获得最佳的p型Na掺杂ZnO薄膜的载流子浓度为1.94×10~(15) cm~(-3),电阻率7.54Ωcm,霍尔迁移率为7.54cm2/Vs。通过霍尔及XPS结果分析,热扩散温度及时间是影响Na掺杂ZnO薄膜电学性能的主要因素。同时,我们制备的ZnO基同质结显示出良好的整流效应,进一步证实了通过热扩散方法掺杂的ZnO薄膜确实为p型ZnO。
3.通过三重Na离子注入,在ZnO单晶中实现了厚度约300nm的均匀Na掺杂ZnO层。低温PL显示,经过850℃,6min的快速热处理后,ZnO中位于3.352eV(I_10)的发光峰得到显著增强,我们认为其与Na受主相关。同时,我们制备的ZnO基同质结显示出良好的整流效应,证实了通过此方法制备的薄膜为p型ZnO薄膜。此外,我们还研究了单次Na离子注入对单晶ZnO影响。
4.我们采用离子注入工艺制备了Na掺杂的ZnO纳米阵列,并研究了退火温度对其光学性能的影响。实验发现通过在600-800℃下的退火处理可对ZnO中的辐射缺陷进行有效修复。同时,经过800℃退火后,ZnO薄膜的低温PL谱中显示了位于3.352eV(I10)的发光峰,其与Na受主NaZn目关。此外,随着退火温度的升高,I6-8发光峰强度下降,而I3发光峰强度升高,说明更多的中性施主在高温下产生了电离。
5.经过Ne离子注入的ZnO纳米阵列的光致发光谱中具有精细结构的紫光发光峰。其精细结构间隔为72meV,对应于ZnO中纵光学声子能量。通过拟合计算获得的黄昆因子为1.98,其电子声子耦合能量低于绿光发光带而高于DAP。激活能为160meV,我们以为,这与离子注入过程中引入的受主缺陷相关。
ZnO is an attractive wide-band-gap semiconductor with a direct band gap of3.37eV at room temperature. The large exciton binding energy (60meV) and well-developed bulk, film growth processes promise its optoelectronic applications, such as light emitting diodes (LEDs), transparent conductive layer, photodetector and gas sensor. Due to the asymmetric doping limitations, n-type ZnO can be easily obtained via intrinsic or extrinisic dopants, whereas it has thus-far proven very difficult to obtain high quality and stable p-type ZnO. Recently, Na has been considered as an effective p type dopant in ZnO. There has been many reports on p-type Na-doped ZnO using various methods. Theoretical studies indicate that Na doping produces shallow acceptor state and small relaxation for Nazn.Moreover, p-type ZnO thin film and ZnO-based p-n homoj unction fabricated by various methods prove Na as an effective p-type dopant in ZnO. In this thesis we focus on growth and characterization of Na doped p type ZnO obtained by pulsed laser deposition (PLD), diffusion and ion implantation methods. The thesis includes:
1. Na δ-doped p-type ZnO thin films were fabricated on quartz substrates with the structure of ZnO/Na (δ-layer) multi-layers by PLD. NaF ceramic target was used as Na source. The effects of oxygen pressure and substrate temperature on the electrical properties of δ-doped ZnO thin films were discussed. An optimized result with a resistivity of29.8Ωcm, Hall mobility of0.263cm2/Vs, and hole concentration of7.9×1017cm-3was achieved, and electrically stable over several months. The work is of interest for developing a novel method to realize p-type ZnO thin films doping with Na.
2. Na-diffused p-type ZnO thin films have been realized via pulsed laser deposition using NaF ceramic target followed by rapid thermal process in nitrogen. An optimized result with a resistivity of426.7Ω·cm, Hall mobility of7.54cm2/Vs, and hole concentration of1.94×1015cm-3was achieved, and electrically stable over several months. Hall-effect measurements supported by X-ray photoelectron spectroscopy indicated that diffusion temperature and diffusion time played a key role in optimizing the p-type conduction of Na-diffused ZnO thin films. Furthermore, ZnO-based p-n homoj unction was obtained by fabrication of a Na-diffused p-type ZnO layer on an undoped n-type ZnO layer.
3. Three-folder Na+ion implantation is applied to form a plant region of Na doped ZnO. Low temperature PL shows that a well-resolved bound exciton line at3.352eV with a linewidth of～8meV emerges from the850℃,6min annealed sample and is likely related to the formation of NaZn acceptor. ZnO-based p-n homojunction was obtained by three-folder Na+implanted layer. Also one time Na+implanted single crystal ZnO was studied.
4. The effects of annealing temperature on excitonic emissions from Na+ion implanted ZnO nanorods are studied and annealing at between600and800℃can effectively repair the implantation as evidenced by the enhanced excitonic emissions. A well-resolved bound exciton line at3.352eV with a linewidth of～2meV emerges from the800℃annealed sample and is likely related to the formation of NaZn acceptor. When the annealing temperature is increased, the intensity of the I6-8line decreases while that of I3increases, suggesting enhanced ionization of neutral donors at elevated temperature.
5. Unusual vibronic fine structures of the～3.0eV violet emission from ion-implanted ZnO nanorods has been investigated by photoluminescence (PL). A set of equally separated peaks with energy spacing of72meV, which corresponds to the longitudinal optical (LO) phonon energy of ZnO, were well resolved in the low temperature PL spectra. The overall emission band can be perfectly described by LO phonon-assisted transition with the Huang-Rhys factor of1.98, indicating intermediate electron-phonon coupling. The thermal quenching of PL gives rise to activation energy of～160meV, which is attributed to the energy level of acceptor-like defects introduced by implantation.
引文
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