ZnO薄膜的常压MOCVD生长及掺杂研究
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摘要
氧化锌(ZnO)是一种重要的化合物半导体光电材料，它具有良好的物理特性：直接带隙能带结构、室温禁带宽度3.37eV、激子束缚能60meV，是制备紫外发光二极管、特别是制备室温紫外半导体激光器的优选材料。可是性能良好的p型ZnO材料的制备问题一直以来成为实现ZnO基发光器件突破的瓶颈。近几年来，尽管国际上p型ZnO薄膜的制备取得了重要进展，但是可实用的ZnO发光器件仍没有制备成功。特别是在用金属有机化学气相沉积(MOCVD)法生长ZnO薄膜及其p型掺杂方面，还需要更多的研究，否则ZnO基发光器件将难以产业化。在这样的背景下，本论文开展ZnO薄膜的MOCVD生长及其掺杂性质研究。
本论文主要是采用自制常压MOCVD系统，以去离子水(H_2O)和二乙基锌(DEZn)为源材料，在蓝宝石(0001)衬底上进行ZnO薄膜的制备、掺杂等相关内容研究。在课题研究过程中，本文主要获得了以下一些有意义和有创新性的研究结果：
1、首次提出了在外延层生长过程中引入少量腐蚀性气体来提高ZnO薄膜的晶体质量。研究实验结果表明，在外延层生长过程中引入少量的H_2和NH_3都有利于提高ZnO的晶体质量，但是引入H_2将会影响ZnO薄膜的表面形貌和电学性能，而引入少量的NH_3后，ZnO薄膜的表面形貌、晶体质量、室温电子迁移率、低温10K下的激子发光及其声子伴线均变好，其(0002)和几何倾斜对称(10-12)面的双晶X射线衍射(DCXRD)Omega(ω)摇摆曲线半峰宽(FWHM)分别为132弧秒(＂)和235弧秒(＂)。金相显微镜结果显示ZnO薄膜中的平均晶粒尺寸直径大小20μm，为当前文献中MOCVD法生长ZnO薄膜的最大值，本文的这一实验结果也正好体现了用常压MOCVD方法生长ZnO薄膜能获得大的晶粒尺寸特点。
2、研究了高温缓冲层厚度、外延层的生长速率以及富Zn环境对ZnO薄膜生长的影响，优化了生长工艺参数。在保持较高的晶体质量前提下，得到了生长速率为4.2μm／h的ZnO单晶薄膜。据我们所知，这一生长速率是目前文献用MOCVD生长ZnO薄膜的最大报道值，较快生长速率和较高结晶质量对今后ZnO薄膜的规模化生产是十分有利的。
3、采用常压MOCVD方法在蓝宝石(0001)衬底上成功地制备出高质量的、高可见光透过率的、低电阻率的Al掺杂型ZnO透明导电薄膜(AZO)，其(0002)和(10-12)面DCXRD的ω摇摆曲线FWHM分别为289＂和406＂。据我们所知，这是首次报道AZO薄膜有几何倾斜对称(10-12)面DCXRD的ω摇摆曲线结果。本文制备出的AZO透明导电薄膜的可见光透过率超过90％，电阻率在9.72×10~(-4)Ω．cm范围内。这些参数与目前文献报道所制备的AZO薄膜最好的结果相当。
4、利用常压MOCVD技术以氨气(NH_3)作为掺杂源进行ZnO薄膜的p型掺杂研究，对NH_3掺杂温度、NH_3掺杂方式以及NH_3掺杂流量等重要影响参数进行了探讨。在优化的条件下，通过NH_3掺杂最终获得了p型ZnO薄膜。金相显微镜和DCXRD测试结果表明，该p型ZnO薄膜具有平整的薄膜表面和好的结晶性能，其(0002)和(10-12)面的的ω摇摆曲线FWHM分别为246＂和368＂。光致发光(PL：Photoluminescence)测试结果表明，该p型ZnO薄膜的10K低温和室温PL中都能观察到非常强的与N替代O受主相关的发光峰。室温霍尔测量结果表明：p型ZnO薄膜的空穴浓度约为10~(16)～10~(17)cm~(-3)，迁移率为3～10cm~2／V.S。该p型ZnO薄膜为研制ZnO同质p-n结奠定了良好的基础。
5、采用常压MOCVD方法在蓝宝石衬底上用Al和N做掺杂剂生长了具有p-n结构的ZnO同质结外延材料。采用Ti／Au和Ni／Au合金分别做n型和p型ZnO薄膜的欧姆接触，制备出ZnO同质p-n结芯片。在室温下，该ZnO同质p-n结具有典型的二极管整流Ⅰ-Ⅴ特性，开启电压约为5 V(正向电流10μA时)，反向电压高达20V(反向电流10μA时)。这一结果要明显优于文献报道的结果。据我们所知，20V的反向电压是目前报道ZnO同质p-n结的最大值。对本文所制备的ZnO同质p-n结的稳定性测试实验结果表明：本文用NH_3做掺杂源获得的p型ZnO的性能稳定。
本文以上研究结果从材料生长手段常压MOCVD系统的角度来说，均属国际首次。本文相关研究结果已在《Journal of Crystal Growth》、《Journal of Luminescence》以及《Materials Science and Engineering B》等国际杂志上公开发表。其中在《Materials Science and Engineering B》杂志上发表的论文按被国际读者下载次数排序，成为该杂志2006年第一季度最热门的25篇论文之一，列第15位。
本论文得到下列课题的支持：国家863纳米专项课题(合同号：No．2003AA302160)和信息产业部电子发展基金(2004-125号)。
Zinc Oxide (ZnO) is one kind of important compound semiconductor photoelectric materials. It has a bandgap of 3.37 eV at room temperature (RT) and a large exciton binding energy of 60 meV, which provides an attractive prospect to highly efficient UV light emitters, light emitting diodes (LEDs) and low-threshold excitonic laser diodes (LDs). The greatest obstacle to harvest these advantages in real devices is posed by the realization of low resistant and reliable p-type ZnO. Although massive progress in growth of p type ZnO films has been made in recent years, the applicable ZnO light emitting devices have not been fabricated yet. Especially, it needs more research in the growth of ZnO and p-ZnO films by metal organic chemistry vapor deposition (MOCVD), otherwise it will be difficult to realize the bulk production of ZnO. Under such background, the first object of the dissertation is to grow device-quality ZnO films and the doping of ZnO so that pave the way for high performance ZnO light emitting devices.
In this thesis, a home-built vertical atmospheric pressure-MOCVD(AP-MOCVD) system was used for the growth of the undoped ZnO, Al doped ZnO and NH_3 doped ZnO films using 6N-purity diethylZinc (DEZn) as Zn precursor, deionized water (H_2O) as O-precursors, 7N-purity nitrogen as the carrier gas, and two inch c-plane sapphire(c-Al_2O_3) as the substrate. Finally, the realization of ZnO thin film with p-type conductivity makes it successfully to fabricate of ZnO p-n homojunction. New results are as follows:
1. A method was proposed to enhance the crystal quality of ZnO films by adding a small corrosive gas into the growth ambient of AP-MOCVD system. The effects of adding small H_2 and NH_3 gas into the growth ambient on the film properties have been studied. Experimental results showed that compared to the effect of small H_2, it was more effective on the improvements of the surface morphology, crystalline structure, and optical quality of ZnO epilayers by adding small NH_3 gas into the growth ambient. The full widths at half maximum (FWHMs) of the (0002) and (10-12) double crystal X-ray diffraction (DCXRD)ω-rocking curves of the ZnO film grown by adding NH_3 gas into the growth ambient were 152 arcsec and 253 arcsec, respectively, indicating the small mosaicity and low dislocation density of the film. It was very effective on the improvement of surface morphology of ZnO films by adding NH_3 gas into the growth ambient, which eventually leaded to a smooth surface with larger hexagonal grains (20μm). To the best of our knowledge, this is largest grain size report of ZnO film grown on c-Al_2O_3 by MOCVD, which was also just to manifest the characteristic of obtaining the big crystal grain size by APMOCVD.
2. The effects of the thickness of high temperature buffer layer, the growth rate of epitaxial layer and the rich Zn environment on the properties of ZnO films grown by AP-MOCVD were investigated. By the optimized condition, the high growth rate of 4.2μm/h has been obtained, which is the highest value for ZnO films grown by MOCVD compared to literatures. It will be extremely advantageous to the next scale production of ZnO films due to the quick growth speed as well as the high crystallization quality.
3. The high quality, the high transmittance of visible light and low resistance of Al doped ZnO(AZO) films was successfully prepared by AP-MOCVD on Al_2O_3(0001) substrate. The FWHM of AZO (0002) plane DCXRD omega rocking curve is 289", and (10-12) plane is 406". This is the first report of AZO film having the skew symmetry (10-12) plane DCXRD rocking curve result. The transmittance of visible light of the AZO film surpasses 90%, and the resistivity was about 9.72×10~(-4)Ω.cm. These parameters were equal to the best results of the AZO reported by the present literatures.
4. The effects of the doped temperature, the doped mode and the doped flux of NH_3 on the properties of ZnO films grown by AP-MOCVD were investigated, which were considered to the important parameters. By the optimized condition, the p type ZnO has been obtained under the suitable doped temperature and flux. The experimental results of the metal-phase interference microscope and the DCXRD indicated that the p-ZnO film was the crystallization performance, as well as smooth surface. The FWHMs of the (0002) and (10-12) DCXRDω-rocking curves of p-ZnO were 246" and 368", respectively. The extremely strong DAP peak of the p-ZnO film could be observed in both the 10K PL and room temperature PL. The room temperature Hall measurement result indicated that the hole carrier concentration of p-ZnO film was 10~(16)～10~(17)cm~(-3), and the mobility of hole was 3～10cm~2/V.S.
5. With the use of Ti/Au and the Ni/Au alloy as n and p type ZnO thin film ohm contact, respectively, ZnO homojunction has been fabricated by AP-MOCVD on the sapphire substrate by using the Al and N as the doping of the n and p type ZnO thin film, respectively. A typical ZnO homojunction shows rectifying behavior with a turn-on voltage of about 5 V, and the reverse voltage reaches as high as 20V, which obviously preceded the result reported by Japanese and the American researchers. To the best of our knowledge, this is best report of ZnO homojunction of the 20V reverse voltage according to literature. By the stabile test experiment of ZnO homojunction, it indicated that the p type ZnO doped with N was reliable.
From the material growth method angle of AP-MOCVD system, the above results are the first reported.
This work was supported by the 863 project (contract No. 2003AA302160) and China foundation for development of electronic information technology (contract No. 2004-125).
本论文主要是采用自制常压MOCVD系统，以去离子水(H_2O)和二乙基锌(DEZn)为源材料，在蓝宝石(0001)衬底上进行ZnO薄膜的制备、掺杂等相关内容研究。在课题研究过程中，本文主要获得了以下一些有意义和有创新性的研究结果：
1、首次提出了在外延层生长过程中引入少量腐蚀性气体来提高ZnO薄膜的晶体质量。研究实验结果表明，在外延层生长过程中引入少量的H_2和NH_3都有利于提高ZnO的晶体质量，但是引入H_2将会影响ZnO薄膜的表面形貌和电学性能，而引入少量的NH_3后，ZnO薄膜的表面形貌、晶体质量、室温电子迁移率、低温10K下的激子发光及其声子伴线均变好，其(0002)和几何倾斜对称(10-12)面的双晶X射线衍射(DCXRD)Omega(ω)摇摆曲线半峰宽(FWHM)分别为132弧秒(＂)和235弧秒(＂)。金相显微镜结果显示ZnO薄膜中的平均晶粒尺寸直径大小20μm，为当前文献中MOCVD法生长ZnO薄膜的最大值，本文的这一实验结果也正好体现了用常压MOCVD方法生长ZnO薄膜能获得大的晶粒尺寸特点。
2、研究了高温缓冲层厚度、外延层的生长速率以及富Zn环境对ZnO薄膜生长的影响，优化了生长工艺参数。在保持较高的晶体质量前提下，得到了生长速率为4.2μm／h的ZnO单晶薄膜。据我们所知，这一生长速率是目前文献用MOCVD生长ZnO薄膜的最大报道值，较快生长速率和较高结晶质量对今后ZnO薄膜的规模化生产是十分有利的。
3、采用常压MOCVD方法在蓝宝石(0001)衬底上成功地制备出高质量的、高可见光透过率的、低电阻率的Al掺杂型ZnO透明导电薄膜(AZO)，其(0002)和(10-12)面DCXRD的ω摇摆曲线FWHM分别为289＂和406＂。据我们所知，这是首次报道AZO薄膜有几何倾斜对称(10-12)面DCXRD的ω摇摆曲线结果。本文制备出的AZO透明导电薄膜的可见光透过率超过90％，电阻率在9.72×10~(-4)Ω．cm范围内。这些参数与目前文献报道所制备的AZO薄膜最好的结果相当。
4、利用常压MOCVD技术以氨气(NH_3)作为掺杂源进行ZnO薄膜的p型掺杂研究，对NH_3掺杂温度、NH_3掺杂方式以及NH_3掺杂流量等重要影响参数进行了探讨。在优化的条件下，通过NH_3掺杂最终获得了p型ZnO薄膜。金相显微镜和DCXRD测试结果表明，该p型ZnO薄膜具有平整的薄膜表面和好的结晶性能，其(0002)和(10-12)面的的ω摇摆曲线FWHM分别为246＂和368＂。光致发光(PL：Photoluminescence)测试结果表明，该p型ZnO薄膜的10K低温和室温PL中都能观察到非常强的与N替代O受主相关的发光峰。室温霍尔测量结果表明：p型ZnO薄膜的空穴浓度约为10~(16)～10~(17)cm~(-3)，迁移率为3～10cm~2／V.S。该p型ZnO薄膜为研制ZnO同质p-n结奠定了良好的基础。
5、采用常压MOCVD方法在蓝宝石衬底上用Al和N做掺杂剂生长了具有p-n结构的ZnO同质结外延材料。采用Ti／Au和Ni／Au合金分别做n型和p型ZnO薄膜的欧姆接触，制备出ZnO同质p-n结芯片。在室温下，该ZnO同质p-n结具有典型的二极管整流Ⅰ-Ⅴ特性，开启电压约为5 V(正向电流10μA时)，反向电压高达20V(反向电流10μA时)。这一结果要明显优于文献报道的结果。据我们所知，20V的反向电压是目前报道ZnO同质p-n结的最大值。对本文所制备的ZnO同质p-n结的稳定性测试实验结果表明：本文用NH_3做掺杂源获得的p型ZnO的性能稳定。
本文以上研究结果从材料生长手段常压MOCVD系统的角度来说，均属国际首次。本文相关研究结果已在《Journal of Crystal Growth》、《Journal of Luminescence》以及《Materials Science and Engineering B》等国际杂志上公开发表。其中在《Materials Science and Engineering B》杂志上发表的论文按被国际读者下载次数排序，成为该杂志2006年第一季度最热门的25篇论文之一，列第15位。
本论文得到下列课题的支持：国家863纳米专项课题(合同号：No．2003AA302160)和信息产业部电子发展基金(2004-125号)。
Zinc Oxide (ZnO) is one kind of important compound semiconductor photoelectric materials. It has a bandgap of 3.37 eV at room temperature (RT) and a large exciton binding energy of 60 meV, which provides an attractive prospect to highly efficient UV light emitters, light emitting diodes (LEDs) and low-threshold excitonic laser diodes (LDs). The greatest obstacle to harvest these advantages in real devices is posed by the realization of low resistant and reliable p-type ZnO. Although massive progress in growth of p type ZnO films has been made in recent years, the applicable ZnO light emitting devices have not been fabricated yet. Especially, it needs more research in the growth of ZnO and p-ZnO films by metal organic chemistry vapor deposition (MOCVD), otherwise it will be difficult to realize the bulk production of ZnO. Under such background, the first object of the dissertation is to grow device-quality ZnO films and the doping of ZnO so that pave the way for high performance ZnO light emitting devices.
In this thesis, a home-built vertical atmospheric pressure-MOCVD(AP-MOCVD) system was used for the growth of the undoped ZnO, Al doped ZnO and NH_3 doped ZnO films using 6N-purity diethylZinc (DEZn) as Zn precursor, deionized water (H_2O) as O-precursors, 7N-purity nitrogen as the carrier gas, and two inch c-plane sapphire(c-Al_2O_3) as the substrate. Finally, the realization of ZnO thin film with p-type conductivity makes it successfully to fabricate of ZnO p-n homojunction. New results are as follows:
1. A method was proposed to enhance the crystal quality of ZnO films by adding a small corrosive gas into the growth ambient of AP-MOCVD system. The effects of adding small H_2 and NH_3 gas into the growth ambient on the film properties have been studied. Experimental results showed that compared to the effect of small H_2, it was more effective on the improvements of the surface morphology, crystalline structure, and optical quality of ZnO epilayers by adding small NH_3 gas into the growth ambient. The full widths at half maximum (FWHMs) of the (0002) and (10-12) double crystal X-ray diffraction (DCXRD)ω-rocking curves of the ZnO film grown by adding NH_3 gas into the growth ambient were 152 arcsec and 253 arcsec, respectively, indicating the small mosaicity and low dislocation density of the film. It was very effective on the improvement of surface morphology of ZnO films by adding NH_3 gas into the growth ambient, which eventually leaded to a smooth surface with larger hexagonal grains (20μm). To the best of our knowledge, this is largest grain size report of ZnO film grown on c-Al_2O_3 by MOCVD, which was also just to manifest the characteristic of obtaining the big crystal grain size by APMOCVD.
2. The effects of the thickness of high temperature buffer layer, the growth rate of epitaxial layer and the rich Zn environment on the properties of ZnO films grown by AP-MOCVD were investigated. By the optimized condition, the high growth rate of 4.2μm/h has been obtained, which is the highest value for ZnO films grown by MOCVD compared to literatures. It will be extremely advantageous to the next scale production of ZnO films due to the quick growth speed as well as the high crystallization quality.
3. The high quality, the high transmittance of visible light and low resistance of Al doped ZnO(AZO) films was successfully prepared by AP-MOCVD on Al_2O_3(0001) substrate. The FWHM of AZO (0002) plane DCXRD omega rocking curve is 289", and (10-12) plane is 406". This is the first report of AZO film having the skew symmetry (10-12) plane DCXRD rocking curve result. The transmittance of visible light of the AZO film surpasses 90%, and the resistivity was about 9.72×10~(-4)Ω.cm. These parameters were equal to the best results of the AZO reported by the present literatures.
4. The effects of the doped temperature, the doped mode and the doped flux of NH_3 on the properties of ZnO films grown by AP-MOCVD were investigated, which were considered to the important parameters. By the optimized condition, the p type ZnO has been obtained under the suitable doped temperature and flux. The experimental results of the metal-phase interference microscope and the DCXRD indicated that the p-ZnO film was the crystallization performance, as well as smooth surface. The FWHMs of the (0002) and (10-12) DCXRDω-rocking curves of p-ZnO were 246" and 368", respectively. The extremely strong DAP peak of the p-ZnO film could be observed in both the 10K PL and room temperature PL. The room temperature Hall measurement result indicated that the hole carrier concentration of p-ZnO film was 10~(16)～10~(17)cm~(-3), and the mobility of hole was 3～10cm~2/V.S.
5. With the use of Ti/Au and the Ni/Au alloy as n and p type ZnO thin film ohm contact, respectively, ZnO homojunction has been fabricated by AP-MOCVD on the sapphire substrate by using the Al and N as the doping of the n and p type ZnO thin film, respectively. A typical ZnO homojunction shows rectifying behavior with a turn-on voltage of about 5 V, and the reverse voltage reaches as high as 20V, which obviously preceded the result reported by Japanese and the American researchers. To the best of our knowledge, this is best report of ZnO homojunction of the 20V reverse voltage according to literature. By the stabile test experiment of ZnO homojunction, it indicated that the p type ZnO doped with N was reliable.
From the material growth method angle of AP-MOCVD system, the above results are the first reported.
This work was supported by the 863 project (contract No. 2003AA302160) and China foundation for development of electronic information technology (contract No. 2004-125).
引文
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