ZnO：Al透明导电薄膜和ZnO发光器件的制备及特性研究
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摘要
氧化锌(ZnO)是一种宽禁带(3.37 eV)Ⅱ-Ⅵ族化合物半导体材料，具有较大的激子束缚能(60 meV)，理论上更容易在室温下实现高效率的受激发射，由于ZnO在结构、电学和光学等方面有诸多优点，加上ZnO薄膜的制作方法很多，在透明电极、压敏电阻、太阳能电池窗口、表面声波器件、气体传感器、发光二极管等领域应用潜力巨大。本文采用磁控溅射法生长Al掺杂ZnO透明导电薄膜(AZO)，研究了掺H_2对AZO薄膜透明导电特性的影响；采用超声喷雾热分解法(USP)，通过氮-铟共掺杂制备了p型ZnO薄膜，在此基础上制备了ZnO同质结及异质结电致发光器件；采用脉冲激光沉积法(PLD)，通过GaAs衬底As扩散获得p型ZnO薄膜，并进一步尝试着制备了ZnO发光器件。具体研究内容如下：
(1)采用磁控溅射法，以AZO(2wt.％Al_2O_3)为靶材，在玻璃衬底上生长AZO薄膜。研究了背景Ar气氛中掺H_2对AZO薄膜结构、光学、电学等特性的影响，发现嵌入Zn-O键中的氢原子存在饱和阶段，在此阶段H_2可以改善AZO薄膜的光学、电学等特性。在低温100℃、H_2气流量1.0 sccm条件下成功制备出电阻率为4.15×10~(-4)Ωcm、可见光区域平均透射率为93％的优质AZO透明导电薄膜，与无H_2条件下制备的AZO薄膜相比较，电阻率降低到未掺H样品的1／4，实现了高质量AZO透明导电薄膜的低温制备。
(2)采用超声喷雾热分解法，以In(NO_3)_3和CH_3COONH_4为掺杂源，通过氮-铟共掺杂制备了p型ZnO薄膜。在此基础上，成功的进行了ZnO同质结发光器件的制备，室温条件下测得的电致发光谱(EL)由一个较宽的蓝绿光发光带(中心位于～2.44 eV)和一个较弱的蓝紫光右肩峰(中心位于～2.9 eV)组成。为了进一步提高器件发光效率，本论文还制备了ZnMgO／ZnO／ZnMgO双异质结构发光器件，室温下观测到该器件明显的电致发光现象，发光谱由中心位于450 nm和520 nm两个独立的峰组成，属于ZnO缺陷深能级发光。
(3)采用脉冲激光沉积法，通过衬底As扩散成功制备了p-ZnO薄膜。并在此基础上，成功制作出p-ZnO／n~+-GaAs异质结发光器件，其电致发光谱由蓝绿光波段和红外光波段组成，分别与光致发光谱(PL)测试结果中ZnO的深能光致发光和GaAs的光致发光相对应。在异质结器件基础上，以AZO薄膜作为n型层，构成n-ZnO／p-ZnO／n~+-GaAs三层结构的发光器件。室温下观测到该器件有明显的电致发光现象，EL谱是由一个较宽的蓝绿光发光带(中心位于～2.5 eV)和一个较弱的蓝紫光右肩峰(中心位于～3.0 eV)组成。I-V特性测试结果呈现典型的p-n结整流特性，正向开启电压约为4.5 V，反向击穿电压约为9 V。
ZnO has recently become a very popular material due to its great potential foroptoelectronics applications. The large direct band gap of 3.3 eV, along with the large excitonbinding energy (60 meV) and many other advantages, make ZnO a strong candidate for thenext generation of ultraviolet light emitting and lasing devices operating at high temperaturesand in harsh environments. In this thesis, the Al-doped ZnO (AZO) films were prepared byreactive frequency magnetron sputtering in H_2 ambient, and the influence of H_2 flux on thetransparent and conductive properties of the AZO films was investingated. Moreover, ZnOhomojunction light-emitting diode was grown on single-crystal GaAs (100) substrate byultrasonic spray pyrolysis (USP) based on the success of N-In codoped p-type ZnO films.Furthermore, As-doped p-type ZnO films were prepared by pulsed laser deposition (PLD),and the ZnO based devices were fabricated and characterized. The details are as follows:
(1) To investigate the influence H_2 on the properties of AZO films, the AZO films weregrown on glass substrate by magnetron sputtering with AZO (98 wt.% ZnO 2 wt.% Al_2O_3)ceramic target in H_2 ambient. The resistivity of 4.15×10~(-4)Ω.cm and the average transmittanceof more than 93% in the visible range were obtained with the optimal H_2-flux of 1.0 sccm at arelatively lower temperature of 100℃. The method of further improving the electricalproperties of AZO films prepared at low growth temperature can be especially useful forsome low-melting point photoelectric devices and substrates.
(2) N-In codoped p-type ZnO films were successfully prepared by ultrasonic spraypyrolysis using CH_3COONH_4 and In(NO_3)_3 as the doped source of nitrogen and indium.Based on the achievement of p-type ZnO films, ZnO homojunction light-emitting devicescomprised of N-In codoped p-type ZnO and unintentionally doped n-type ZnO film wereprepared on GaAs substrate with the same method. A electroluminescence emissionassociated with defects was observed from the ZnO homojunction under forward currentinjection at room temperature. The EL spectra consisted of a wide band centered at～2.4.4 eV(FWHM,～0.47 eV) and a weak right shoulder centered at～2.9 eV. Furthermore, Theheterojunction light-emitting diode with n-Zn_(0.8)Mg_(0.2)O/ZnO/p-Zn_(0.8)Mg_(0.2)O structure wasgrown. A distinct visible electroluminescence with a dominant emission peak centered at450 nm and an emission peak centered at～520 nm were observed at room temperature fromthe heterojunction structure under forward bias conditions. The origin of electroluminescence emission was supposed to be attributed to a radiative recombination through deep-leveldefects in the ZnO active layer.
(3) As diffusion p-type ZnO films were successfully prepare by pulsed laser deposition.Based on the achievement of p-type ZnO films, p-ZnO/n~+-GaAs heterojunction light emittingdevice was successfully fabricated by pulsed laser deposition. The electroluminescenceemission was in the blue and ultra red region, which was coincidence with thephotoluminescence spectra of deep-level emission from ZnO layer and GaAs layerrespectively. In addition, the ZnO light emitting device with n-ZnO/p-ZnO/n~+-GaAs structurewas grown by pulsed laser deposition. As-doped ZnO film by diffusion of As from thesubstrate was used for the p-type side and Al-doped ZnO film for the n-type side of the device.Distinct electroluminescence spectrum consists of a dominant emission peak at～2.5 eV and aweak shoulder centered at～3.0 eV was observed at room temperature. The I-V characteristicof the ZnO homojunction showed a good rectifying behavior with a turn-on voltage of～4.5 Vand a reverse breakdown voltage of～9 V.
(1)采用磁控溅射法，以AZO(2wt.％Al_2O_3)为靶材，在玻璃衬底上生长AZO薄膜。研究了背景Ar气氛中掺H_2对AZO薄膜结构、光学、电学等特性的影响，发现嵌入Zn-O键中的氢原子存在饱和阶段，在此阶段H_2可以改善AZO薄膜的光学、电学等特性。在低温100℃、H_2气流量1.0 sccm条件下成功制备出电阻率为4.15×10~(-4)Ωcm、可见光区域平均透射率为93％的优质AZO透明导电薄膜，与无H_2条件下制备的AZO薄膜相比较，电阻率降低到未掺H样品的1／4，实现了高质量AZO透明导电薄膜的低温制备。
(2)采用超声喷雾热分解法，以In(NO_3)_3和CH_3COONH_4为掺杂源，通过氮-铟共掺杂制备了p型ZnO薄膜。在此基础上，成功的进行了ZnO同质结发光器件的制备，室温条件下测得的电致发光谱(EL)由一个较宽的蓝绿光发光带(中心位于～2.44 eV)和一个较弱的蓝紫光右肩峰(中心位于～2.9 eV)组成。为了进一步提高器件发光效率，本论文还制备了ZnMgO／ZnO／ZnMgO双异质结构发光器件，室温下观测到该器件明显的电致发光现象，发光谱由中心位于450 nm和520 nm两个独立的峰组成，属于ZnO缺陷深能级发光。
(3)采用脉冲激光沉积法，通过衬底As扩散成功制备了p-ZnO薄膜。并在此基础上，成功制作出p-ZnO／n~+-GaAs异质结发光器件，其电致发光谱由蓝绿光波段和红外光波段组成，分别与光致发光谱(PL)测试结果中ZnO的深能光致发光和GaAs的光致发光相对应。在异质结器件基础上，以AZO薄膜作为n型层，构成n-ZnO／p-ZnO／n~+-GaAs三层结构的发光器件。室温下观测到该器件有明显的电致发光现象，EL谱是由一个较宽的蓝绿光发光带(中心位于～2.5 eV)和一个较弱的蓝紫光右肩峰(中心位于～3.0 eV)组成。I-V特性测试结果呈现典型的p-n结整流特性，正向开启电压约为4.5 V，反向击穿电压约为9 V。
ZnO has recently become a very popular material due to its great potential foroptoelectronics applications. The large direct band gap of 3.3 eV, along with the large excitonbinding energy (60 meV) and many other advantages, make ZnO a strong candidate for thenext generation of ultraviolet light emitting and lasing devices operating at high temperaturesand in harsh environments. In this thesis, the Al-doped ZnO (AZO) films were prepared byreactive frequency magnetron sputtering in H_2 ambient, and the influence of H_2 flux on thetransparent and conductive properties of the AZO films was investingated. Moreover, ZnOhomojunction light-emitting diode was grown on single-crystal GaAs (100) substrate byultrasonic spray pyrolysis (USP) based on the success of N-In codoped p-type ZnO films.Furthermore, As-doped p-type ZnO films were prepared by pulsed laser deposition (PLD),and the ZnO based devices were fabricated and characterized. The details are as follows:
(1) To investigate the influence H_2 on the properties of AZO films, the AZO films weregrown on glass substrate by magnetron sputtering with AZO (98 wt.% ZnO 2 wt.% Al_2O_3)ceramic target in H_2 ambient. The resistivity of 4.15×10~(-4)Ω.cm and the average transmittanceof more than 93% in the visible range were obtained with the optimal H_2-flux of 1.0 sccm at arelatively lower temperature of 100℃. The method of further improving the electricalproperties of AZO films prepared at low growth temperature can be especially useful forsome low-melting point photoelectric devices and substrates.
(2) N-In codoped p-type ZnO films were successfully prepared by ultrasonic spraypyrolysis using CH_3COONH_4 and In(NO_3)_3 as the doped source of nitrogen and indium.Based on the achievement of p-type ZnO films, ZnO homojunction light-emitting devicescomprised of N-In codoped p-type ZnO and unintentionally doped n-type ZnO film wereprepared on GaAs substrate with the same method. A electroluminescence emissionassociated with defects was observed from the ZnO homojunction under forward currentinjection at room temperature. The EL spectra consisted of a wide band centered at～2.4.4 eV(FWHM,～0.47 eV) and a weak right shoulder centered at～2.9 eV. Furthermore, Theheterojunction light-emitting diode with n-Zn_(0.8)Mg_(0.2)O/ZnO/p-Zn_(0.8)Mg_(0.2)O structure wasgrown. A distinct visible electroluminescence with a dominant emission peak centered at450 nm and an emission peak centered at～520 nm were observed at room temperature fromthe heterojunction structure under forward bias conditions. The origin of electroluminescence emission was supposed to be attributed to a radiative recombination through deep-leveldefects in the ZnO active layer.
(3) As diffusion p-type ZnO films were successfully prepare by pulsed laser deposition.Based on the achievement of p-type ZnO films, p-ZnO/n~+-GaAs heterojunction light emittingdevice was successfully fabricated by pulsed laser deposition. The electroluminescenceemission was in the blue and ultra red region, which was coincidence with thephotoluminescence spectra of deep-level emission from ZnO layer and GaAs layerrespectively. In addition, the ZnO light emitting device with n-ZnO/p-ZnO/n~+-GaAs structurewas grown by pulsed laser deposition. As-doped ZnO film by diffusion of As from thesubstrate was used for the p-type side and Al-doped ZnO film for the n-type side of the device.Distinct electroluminescence spectrum consists of a dominant emission peak at～2.5 eV and aweak shoulder centered at～3.0 eV was observed at room temperature. The I-V characteristicof the ZnO homojunction showed a good rectifying behavior with a turn-on voltage of～4.5 Vand a reverse breakdown voltage of～9 V.
引文
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