Al_xZn_(1-x)O薄膜光电性能的研究与应用
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摘要
ZnO是一种被广泛关注的宽禁带半导体，在室温下，其禁带宽度为3.37eV，能量对应于光谱中的近紫外波段，可用来对该波段的辐射进行探测；激子束缚能60meV，可用于制备室温下的短波长激光器件；热稳定性和化学稳定性高且抗辐射能力强，制备的器件适用范围广且寿命长。ZnO在掺入低浓度Al离子时可以形成良好的替位式半导体，制备出高性能的透明导电氧化物薄膜（TCO）；在掺入高浓度Al离子时可以形成合金半导体，调控其光学禁带宽度，制备出可对日盲区紫外辐射进行探测的功能薄膜。基于不同的Al离子浓度，ZnO基薄膜材料能在民用与军事方面实现特殊的功能，发挥不同的作用。
基于此，本论文在ZnO中掺入不同浓度的Al离子，并在优化的工艺条件下，分别实现了电阻率为3.8×10-4Ωcm，可见光区透过率达到90%的ZnO:Al（AZO）透明导电薄膜；以及光学禁带宽度为4.41eV，对应吸收截止波长281nm的Al0.3Zn0.7O日盲紫外光电阴极薄膜的制备。深入分析了材料的结构与性能，对基础理论进行了探讨，并对这两种薄膜材料各自功能的实现机制进行了详细论述。本论文的主要内容如下：
首先，探索了提高透明导电氧化物薄膜AZO结晶质量的制备方法，得到了优化的掺杂浓度与制备条件。实现了高效Al替位掺杂，降低了了电子迁移过程中的散射几率，从而提高了电子迁移率，实现了AZO薄膜高的电导率和可见光透过率。通过系统的分析表征，得到了其光电性能参数，以及薄膜的内部结构、缺陷状态、薄膜组分等信息。验证了其相对于ZnO薄膜而言高的迁移率（32cm2/Vs）；证实了锌空位（VZn）在薄膜中的大量存在。采用不同气氛中的原位退火处理，验证了反位取代缺陷OZn为产生光致发光(PL)谱中绿光发光峰的主要原因。
其次，基于Burstein-Moss效应的理论基础，提出了实现日盲紫外探测光电阴极薄膜的方法，并成功制备出了该Al0.3Zn0.7O薄膜。利用高浓度Al离子产生的大量电子，并且根据ZnO导带底较窄、有效态密度较小、对数量较多的电子无法完全容纳的特点，迫使电子占据导带底以上的电子态，实现了费米能级进入导带的简并状态。这种状态同时实现了光学带隙的展宽和表面功函数的减小。对Al_(0.3)Zn_(0.7)O阴极薄膜的研究结果表明，该薄膜处于无定型细微结晶的状态，表面平整度很高，且自身具有抑制氧吸附的能力。其光学禁带宽度约为4.41eV，对应的吸收边为281nm，符合日盲紫外探测的波长范围。光电子能谱证实了其价带和导带的展宽量，开尔文探针测试标定了其表面势垒的大小。这些结果表明该薄膜符合作为日盲紫外光电阴极材料的条件。利用上述两种薄膜共同构造了日盲紫外探测器，并采用了特有的Cs激活方式对薄膜进行修饰。该探测器对254nm的紫外辐射有很高的光暗响应比，对波长更长的辐射则没有响应，证实了电子在光辐射作用下直接从价带跃迁到导带的响应过程。在0.5mW/cm~2的辐射功率和80V偏压下，得到的光暗电流比约为10~3。在周期性光暗变换状态下，该探测器的响应特性十分清晰，证明了器件的重复使用性。同时，光谱响应也证实了该探测器的响应波段与日盲紫外相符。Cs激活使薄膜表面吸附一层Cs原子，利用其自身功函数低的特点（~1.8eV），进一步降低薄膜表面处的功函数，使电子发射时需要越过的势垒高度变低，增大量子效率。通过对探测器I-V曲线的理论推导和拟合，得到了电子发射的类型。最后探究了真空度、激活以及外置偏压对表面势垒的影响，为整个体系的进一步研究打下了基础。
ZnO is a wide-band-gap semiconductor that has been widely investigated. At roomtemperature, its band gap is3.37eV which corresponds with the energy of nearultraviolet (UV) band in light spectrum. So it can be used to fabricate detectors for theradiation of this band. The exciton binding energy of ZnO is60meV, which makes itcapable to be used to fabricate laser devices of short-wavelength at room temperature.Moreover, ZnO is stable under thermal and chemical environment, and has goodradiation-resistant ability. Thus, it enables ZnO with much more applicability and longlifetime in applications. ZnO can be used to form a well-grown n-type semiconductorafter being doped into Al ions with low concentration, which is able to preparetransparent conductive oxidation (TCO) thin film. Meanwhile, after being heavilyincorporated with Al ions, ZnO could form an alloy semiconductor. And this processcould modulate the optical band gap of this semiconductor to the suitable value forsolar-blind UV detecting. Based on the different concentration of Al ions, ZnO-basedmaterials can be used in both civil and military area with special functions.
This dissertation presents the realization of ZnO:Al (AZO) transparent conductivethin film with resistivity about3.8×10~(-4)Ω cm and transmittance about90%in the visibleregion, and Al_(0.3)Zn_(0.7)O thin film whose optical band gap is4.41eV and thecorresponding cutoff wavelength is281nm, based on the different Al concentration andoptimum preparation parameters. After specific study on the structure, characteristics,and theoretical fundament of these two types of functional film, the details are discussedin this thesis, which are as follows:
Firstly, we investigated the approaches to improve the crystalline quality of AZOtransparent conductive thin film, and summarized the optimum dopant concentrationand deposition conditions. Under the optimized parameters, we obtained AZO thin filmwith efficient Al substitution and less scattering probability. So that films with highconductivity and transmittance were achieved. Specific and systematic characterizationof AZO thin film was performed, and the structure, defect state, and composition of itwere attained. AZO film with relatively high mobility (32cm~2/Vs) comparing with common ZnO thin films was obtained. The non-ignorable existence of Zn vacancy (VZn)has also been verified. The antisite defect OZnwas identified to be responsible for thegreen emission band in photoluminescence (PL) spectrum, after annealing process hadbeen carried out in different ambience.
Secondly, we prepared the Al_(0.3)Zn_(0.7)O thin film which was fit for the detecting ofsolar-blind UV. Fabricate the solar-blind UV detector using this film as photocathode,based on Burstein-Moss theory. Massive electrons were generated due to highAl-incorporated concentration. Owing to the narrow conduction-band minimum andinsufficient effective state density in conduction band of ZnO, it does not have enoughstates to hold a large number of electrons beneath conduction band, and excess electronswould occupy states in conduction band, which shifted the Fermi level upwards,accordingly. This condition did not only enlarge the optical band gap, but also decreasethe surface work function of film. This Al_(0.3)Zn_(0.7)O thin film was verified to be inamorphous nanoscaled polycrystalline structure, have a smooth surface, and have theability to suppress surface adsorption. The optical band gap of this film is estimated tobe4.41eV and it only absorbs illumination whose wavelength is shorter than281nm.X-ray Photoelectron spectroscopy was used to estimate the enlargement values inconduction band and valence band, respectively. Kelvin probe microscope result labeledthe surface barrier height. These results proved the capability of Al_(0.3)Zn_(0.7)O thin film asphotocathode layer for solar-blind detecting. A photodetector was fabricated based onthis Al_(0.3)Zn_(0.7)O thin film as photocathode layer after being activated by Cs, and variousmeasurements of this photodetector were carried out to verify its solar-blind detectingability. This detector only responded to the illumination of254nm, but the illuminationwith longer wavelength, which revealed the direct transition process of electrons fromvalence band. UV/dark contrast nearly3orders of magnitude has been achieved of thisdetector, under254nm UV illumination of0.5mW/cm~2and80V bias. Current variationunder periodical exposal of254nm illumination indicated repeatability of this detector.Spectral response result proved that the detecting range of this detector fitted well withthe solar-blind band. Cs activation was utilized to decrease surface workfunction owingto its small work function (~1.8eV), which would incease the emission efficiency offilm. Through the deduction and fitting of I-V curve, we found out the essence ofemission and put forward the relationship between surface barrier height with vacuum level and activation process. The results told that the decrease of surface barrier heightbetween10~(-6)Pa and10~(-3)Pa was about0.042eV, and the surface barrier height performeda0.165eV decrease after Cs activation.
基于此，本论文在ZnO中掺入不同浓度的Al离子，并在优化的工艺条件下，分别实现了电阻率为3.8×10-4Ωcm，可见光区透过率达到90%的ZnO:Al（AZO）透明导电薄膜；以及光学禁带宽度为4.41eV，对应吸收截止波长281nm的Al0.3Zn0.7O日盲紫外光电阴极薄膜的制备。深入分析了材料的结构与性能，对基础理论进行了探讨，并对这两种薄膜材料各自功能的实现机制进行了详细论述。本论文的主要内容如下：
首先，探索了提高透明导电氧化物薄膜AZO结晶质量的制备方法，得到了优化的掺杂浓度与制备条件。实现了高效Al替位掺杂，降低了了电子迁移过程中的散射几率，从而提高了电子迁移率，实现了AZO薄膜高的电导率和可见光透过率。通过系统的分析表征，得到了其光电性能参数，以及薄膜的内部结构、缺陷状态、薄膜组分等信息。验证了其相对于ZnO薄膜而言高的迁移率（32cm2/Vs）；证实了锌空位（VZn）在薄膜中的大量存在。采用不同气氛中的原位退火处理，验证了反位取代缺陷OZn为产生光致发光(PL)谱中绿光发光峰的主要原因。
其次，基于Burstein-Moss效应的理论基础，提出了实现日盲紫外探测光电阴极薄膜的方法，并成功制备出了该Al0.3Zn0.7O薄膜。利用高浓度Al离子产生的大量电子，并且根据ZnO导带底较窄、有效态密度较小、对数量较多的电子无法完全容纳的特点，迫使电子占据导带底以上的电子态，实现了费米能级进入导带的简并状态。这种状态同时实现了光学带隙的展宽和表面功函数的减小。对Al_(0.3)Zn_(0.7)O阴极薄膜的研究结果表明，该薄膜处于无定型细微结晶的状态，表面平整度很高，且自身具有抑制氧吸附的能力。其光学禁带宽度约为4.41eV，对应的吸收边为281nm，符合日盲紫外探测的波长范围。光电子能谱证实了其价带和导带的展宽量，开尔文探针测试标定了其表面势垒的大小。这些结果表明该薄膜符合作为日盲紫外光电阴极材料的条件。利用上述两种薄膜共同构造了日盲紫外探测器，并采用了特有的Cs激活方式对薄膜进行修饰。该探测器对254nm的紫外辐射有很高的光暗响应比，对波长更长的辐射则没有响应，证实了电子在光辐射作用下直接从价带跃迁到导带的响应过程。在0.5mW/cm~2的辐射功率和80V偏压下，得到的光暗电流比约为10~3。在周期性光暗变换状态下，该探测器的响应特性十分清晰，证明了器件的重复使用性。同时，光谱响应也证实了该探测器的响应波段与日盲紫外相符。Cs激活使薄膜表面吸附一层Cs原子，利用其自身功函数低的特点（~1.8eV），进一步降低薄膜表面处的功函数，使电子发射时需要越过的势垒高度变低，增大量子效率。通过对探测器I-V曲线的理论推导和拟合，得到了电子发射的类型。最后探究了真空度、激活以及外置偏压对表面势垒的影响，为整个体系的进一步研究打下了基础。
ZnO is a wide-band-gap semiconductor that has been widely investigated. At roomtemperature, its band gap is3.37eV which corresponds with the energy of nearultraviolet (UV) band in light spectrum. So it can be used to fabricate detectors for theradiation of this band. The exciton binding energy of ZnO is60meV, which makes itcapable to be used to fabricate laser devices of short-wavelength at room temperature.Moreover, ZnO is stable under thermal and chemical environment, and has goodradiation-resistant ability. Thus, it enables ZnO with much more applicability and longlifetime in applications. ZnO can be used to form a well-grown n-type semiconductorafter being doped into Al ions with low concentration, which is able to preparetransparent conductive oxidation (TCO) thin film. Meanwhile, after being heavilyincorporated with Al ions, ZnO could form an alloy semiconductor. And this processcould modulate the optical band gap of this semiconductor to the suitable value forsolar-blind UV detecting. Based on the different concentration of Al ions, ZnO-basedmaterials can be used in both civil and military area with special functions.
This dissertation presents the realization of ZnO:Al (AZO) transparent conductivethin film with resistivity about3.8×10~(-4)Ω cm and transmittance about90%in the visibleregion, and Al_(0.3)Zn_(0.7)O thin film whose optical band gap is4.41eV and thecorresponding cutoff wavelength is281nm, based on the different Al concentration andoptimum preparation parameters. After specific study on the structure, characteristics,and theoretical fundament of these two types of functional film, the details are discussedin this thesis, which are as follows:
Firstly, we investigated the approaches to improve the crystalline quality of AZOtransparent conductive thin film, and summarized the optimum dopant concentrationand deposition conditions. Under the optimized parameters, we obtained AZO thin filmwith efficient Al substitution and less scattering probability. So that films with highconductivity and transmittance were achieved. Specific and systematic characterizationof AZO thin film was performed, and the structure, defect state, and composition of itwere attained. AZO film with relatively high mobility (32cm~2/Vs) comparing with common ZnO thin films was obtained. The non-ignorable existence of Zn vacancy (VZn)has also been verified. The antisite defect OZnwas identified to be responsible for thegreen emission band in photoluminescence (PL) spectrum, after annealing process hadbeen carried out in different ambience.
Secondly, we prepared the Al_(0.3)Zn_(0.7)O thin film which was fit for the detecting ofsolar-blind UV. Fabricate the solar-blind UV detector using this film as photocathode,based on Burstein-Moss theory. Massive electrons were generated due to highAl-incorporated concentration. Owing to the narrow conduction-band minimum andinsufficient effective state density in conduction band of ZnO, it does not have enoughstates to hold a large number of electrons beneath conduction band, and excess electronswould occupy states in conduction band, which shifted the Fermi level upwards,accordingly. This condition did not only enlarge the optical band gap, but also decreasethe surface work function of film. This Al_(0.3)Zn_(0.7)O thin film was verified to be inamorphous nanoscaled polycrystalline structure, have a smooth surface, and have theability to suppress surface adsorption. The optical band gap of this film is estimated tobe4.41eV and it only absorbs illumination whose wavelength is shorter than281nm.X-ray Photoelectron spectroscopy was used to estimate the enlargement values inconduction band and valence band, respectively. Kelvin probe microscope result labeledthe surface barrier height. These results proved the capability of Al_(0.3)Zn_(0.7)O thin film asphotocathode layer for solar-blind detecting. A photodetector was fabricated based onthis Al_(0.3)Zn_(0.7)O thin film as photocathode layer after being activated by Cs, and variousmeasurements of this photodetector were carried out to verify its solar-blind detectingability. This detector only responded to the illumination of254nm, but the illuminationwith longer wavelength, which revealed the direct transition process of electrons fromvalence band. UV/dark contrast nearly3orders of magnitude has been achieved of thisdetector, under254nm UV illumination of0.5mW/cm~2and80V bias. Current variationunder periodical exposal of254nm illumination indicated repeatability of this detector.Spectral response result proved that the detecting range of this detector fitted well withthe solar-blind band. Cs activation was utilized to decrease surface workfunction owingto its small work function (~1.8eV), which would incease the emission efficiency offilm. Through the deduction and fitting of I-V curve, we found out the essence ofemission and put forward the relationship between surface barrier height with vacuum level and activation process. The results told that the decrease of surface barrier heightbetween10~(-6)Pa and10~(-3)Pa was about0.042eV, and the surface barrier height performeda0.165eV decrease after Cs activation.
引文
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