APCVD法生长ZnO单晶和薄膜
摘要
ZnO是宽禁带直接带隙、六方纤锌矿结构半导体材料,室温下禁带宽度为3.37eV,激子结合能达60meV,具有优良的光电性能、压电性能、磁学性能、化学稳定性和生物无毒性。ZnO基材料被认为是制备紫外探测器、传感器、声表面波器件、薄膜晶体管、短波长激光和发光二极管等器件的理想候选材料,这使得ZnO基器件成为近些年持续研究的热点之一。然而,缺乏高质量、低成本、适合商业应用的ZnO晶体和薄膜是制约其相关器件发展的一个关键因素。为解决此问题,本论文尝试了在自组装的结构简单、造价低廉的常压化学气相沉积(APCVD)系统中生长ZnO,并研究了不同生长条件对ZnO的结构和光学性能的影响,得到了较高质量的ZnO单晶体、微纳结构薄膜和连续薄膜。主要研究内容如下：
1.用APCVD系统调控生长ZnO晶体。研究了不同生长温度(800-900℃)、不同衬底(石英、Si、Al2O3和Au、Pt、ZnO缓冲层)、不同HCl和NH3比值(0-∞)、不同H2O浓度(温度为60-90℃)、不同衬底位置(距中心5-35cm)对ZnO晶体生长的影响,初步得到了调控晶体生长的关键因素。
2.用APCVD系统在Al2O3衬底上生长ZnO单晶体。通过优化实验条件既可得到具有规则六角外形、显露(0001)晶面的ZnO单晶体,也可得到高密度定向生长的六角ZnO晶体。光学图片、SEM、XRD、Raman光谱和PL光谱结果表明ZnO晶体具有严格的纤锌矿结构、极高的纯度和优良的光学特性。发现用APCVD系统在Al2O3衬底上生长ZnO晶体的横向生长速率大于纵向速率,并通过三次连续生长实验进行了证实,继而深入探讨了其横向外延机理。
3.用APCVD系统在ZnO/Al2O3衬底上生长ZnO纳米结构薄膜。采用ZnO同质缓冲层可以最大限度减小晶格失配、提高晶体的成核密度和均匀性,分别得到了大面积的纳米墙状和纳米孔状ZnO薄膜。其中,纳米墙薄膜的各单片晶体之间具有互成120。夹角的排布规律,而纳米孔薄膜的小孔内径和整体分布极为均匀。研究了纳米墙、纳米孔ZnO薄膜的相关性能和生长机理。
4.用APCVD在ZnO/Al2O3衬底上生长了ZnO连续薄膜,并对其表面进行了优化。初步研究了ZnO连续薄膜的晶体结构和生长机理。
Zinc oxide (ZnO) is one of the wide direct bandgap semiconductors with wurtzite structure, which has a band gap of3.37eV and free exciton binding eneygy of60meV at room temperature. With the excellent photoelectricity, piezoelectric, magnetic, chemical stability and biologic safe properties, ZnO is also one of the candidates for UV photoelectric detectors, sensors, surface acoustic wave devices, short-wave lasers and light emitting diodes, and so on. These make ZnO to be a research hot point in recent years. However, a main handicap of the development of ZnO-based devices is lacking of high quality, low cost and suitable commerce using ZnO crystal and film. To solve this problem, in this thesis, a home made, simplified and low-cost atmosphere pressure chemical vapor depositon (APCVD) syatem was utilized to grow ZnO crystals and films. The special adjusting effects of different factors on the morphology and the optical properties of ZnO was researched, and the high quality ZnO crystals and films were finally gained. The main researching points are listed as follows:
1. Adjusting ZnO growth in the APCVD system. This thesis includs the different effects of growth temperatures (800-900℃), substrates (quatz, Si, Al2O3and Au, Pt, ZnO buffer layers), ratio of HCl and NH3(0-∞), concertations of H2O vapor (water temperature60-90℃) and the growth locations (5-35cm from center). The key effects of these factor on ZnO crystal growth are discovered.
2. Growth ZnO single crystals on Al2O3substrates in the APCVD system. After adjusting the experimental parameters, hexagonal (0001)-facet ZnO single crystals and high density hexagonal ZnO crystals were respectively achieved. The optical images, X-ray diffusion patterns, Raman and PL spectra showed the wurtzite structure, high element purity and charming optical properties of the ZnO crystal. The lateral growth rate is faster than the vertical rate of ZnO crystals on Al2O3substrate, which was testified by a three-time continuous growth experiment. The mechanism of lateral epitaxy mode was also deeply discussed
3. Growth ZnO nanostructured film on ZnO/Al2O3substrate in the APCVD system. The ZnO buffer layers were adopted to reduce the lattice mismatch and enhance the density and uniformity of ZnO nuclei, and large-area nanowall and nanoporous ZnO films were respectively gained. The nano sheets of nano-wall film presented120°assembly angles, and the inner-diameters and the distribution of the nano porous were uniform. The properties and growth mechanisms of the two films were also discussed.
4. Growth ZnO continuous film on ZnO/Al2O3substrate in the APCVD system. The crystal structure and growth mechanism of ZnO continuous film were discussed.
1.用APCVD系统调控生长ZnO晶体。研究了不同生长温度(800-900℃)、不同衬底(石英、Si、Al2O3和Au、Pt、ZnO缓冲层)、不同HCl和NH3比值(0-∞)、不同H2O浓度(温度为60-90℃)、不同衬底位置(距中心5-35cm)对ZnO晶体生长的影响,初步得到了调控晶体生长的关键因素。
2.用APCVD系统在Al2O3衬底上生长ZnO单晶体。通过优化实验条件既可得到具有规则六角外形、显露(0001)晶面的ZnO单晶体,也可得到高密度定向生长的六角ZnO晶体。光学图片、SEM、XRD、Raman光谱和PL光谱结果表明ZnO晶体具有严格的纤锌矿结构、极高的纯度和优良的光学特性。发现用APCVD系统在Al2O3衬底上生长ZnO晶体的横向生长速率大于纵向速率,并通过三次连续生长实验进行了证实,继而深入探讨了其横向外延机理。
3.用APCVD系统在ZnO/Al2O3衬底上生长ZnO纳米结构薄膜。采用ZnO同质缓冲层可以最大限度减小晶格失配、提高晶体的成核密度和均匀性,分别得到了大面积的纳米墙状和纳米孔状ZnO薄膜。其中,纳米墙薄膜的各单片晶体之间具有互成120。夹角的排布规律,而纳米孔薄膜的小孔内径和整体分布极为均匀。研究了纳米墙、纳米孔ZnO薄膜的相关性能和生长机理。
4.用APCVD在ZnO/Al2O3衬底上生长了ZnO连续薄膜,并对其表面进行了优化。初步研究了ZnO连续薄膜的晶体结构和生长机理。
Zinc oxide (ZnO) is one of the wide direct bandgap semiconductors with wurtzite structure, which has a band gap of3.37eV and free exciton binding eneygy of60meV at room temperature. With the excellent photoelectricity, piezoelectric, magnetic, chemical stability and biologic safe properties, ZnO is also one of the candidates for UV photoelectric detectors, sensors, surface acoustic wave devices, short-wave lasers and light emitting diodes, and so on. These make ZnO to be a research hot point in recent years. However, a main handicap of the development of ZnO-based devices is lacking of high quality, low cost and suitable commerce using ZnO crystal and film. To solve this problem, in this thesis, a home made, simplified and low-cost atmosphere pressure chemical vapor depositon (APCVD) syatem was utilized to grow ZnO crystals and films. The special adjusting effects of different factors on the morphology and the optical properties of ZnO was researched, and the high quality ZnO crystals and films were finally gained. The main researching points are listed as follows:
1. Adjusting ZnO growth in the APCVD system. This thesis includs the different effects of growth temperatures (800-900℃), substrates (quatz, Si, Al2O3and Au, Pt, ZnO buffer layers), ratio of HCl and NH3(0-∞), concertations of H2O vapor (water temperature60-90℃) and the growth locations (5-35cm from center). The key effects of these factor on ZnO crystal growth are discovered.
2. Growth ZnO single crystals on Al2O3substrates in the APCVD system. After adjusting the experimental parameters, hexagonal (0001)-facet ZnO single crystals and high density hexagonal ZnO crystals were respectively achieved. The optical images, X-ray diffusion patterns, Raman and PL spectra showed the wurtzite structure, high element purity and charming optical properties of the ZnO crystal. The lateral growth rate is faster than the vertical rate of ZnO crystals on Al2O3substrate, which was testified by a three-time continuous growth experiment. The mechanism of lateral epitaxy mode was also deeply discussed
3. Growth ZnO nanostructured film on ZnO/Al2O3substrate in the APCVD system. The ZnO buffer layers were adopted to reduce the lattice mismatch and enhance the density and uniformity of ZnO nuclei, and large-area nanowall and nanoporous ZnO films were respectively gained. The nano sheets of nano-wall film presented120°assembly angles, and the inner-diameters and the distribution of the nano porous were uniform. The properties and growth mechanisms of the two films were also discussed.
4. Growth ZnO continuous film on ZnO/Al2O3substrate in the APCVD system. The crystal structure and growth mechanism of ZnO continuous film were discussed.
引文
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[1]D. Ehrentraut, H. Sato, Y. Kagamitani, H. Sato, A. Yoshikawa, and T. Fukuda, "Solvothermal growth of ZnO," Progress in Crystal Growth and Characterization of Materials, vol.52, pp. 280-335,2006.
[2]W. Palosz, "Vapor transport of ZnO in closed ampoules," Journal of Crystal Growth, vol.286, pp.42-49,2006.
[3]D. C. Reynolds, "High-quality, melt-grown ZnO single crystals," Journal of Applied Physics, vol. 95, p.4802,2004.
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[5]D. N. Montenegro, S. Agouram, M. C. Martinez-Tomas, C. Llorens, C. Reig, and V. Munoz-Sanjose, "Crystal growth of ZnO micro and nanostructures by PVT on c-sapphire and amorphous quartz substrates," Physics Procedia, vol.8, pp.121-125,2010.
[6]J. Zhu, R. Yao, C. Liu, I.-H. Lee, L. Zhu, J.-w. Ju, J. H. Baek, B. Lin, and Z. Fu, "Effect of total gas velocity on the growth of ZnO films by metal-organic chemical vapor deposition," Thin Solid Films, vol.514, pp.306-309,2006.
[7]X. Xu, C. Xu, J. Dai, J. Pan, and J. Hu, "Evolutions of defects and blue-green emissions in ZnO microwhiskers fabricated by vapor-phase transport," Journal of Physics and Chemistry of Solids, vol.73, pp.858-862,2012.
[8]M. R. Khanlary, V. Vahedi, and A. Reyhani, "Synthesis and Characterization of ZnO Nanowires by Thermal Oxidation of Zn Thin Films at Various Temperatures," Molecules, vol.17, pp. 5021-5029,2012.
[9]D. Calestani, F. Pattini, F. Bissoli, E. Gilioli, M. Villani, and A. Zappettini, "Solution-free and catalyst-free synthesis of ZnO-based nanostructured TCOs by PED and vapor phase growth techniques," Nanotechnology, vol.23, p.194008,2012.
[10]J. P. Biethan, V. P. Sirkeli, L. Considine, D. D. Nedeoglo, D. Pavlidis, and H. L. Hartnagel, "Photoluminescence study of ZnO nanostructures grown on silicon by MOCVD," Materials Science and Engineering: B, vol.177, pp.594-599,2012.
[11]Z. J. Chew, R. A. Brown, T. G. G. Maffeis, and L. Li, "Comparison of ZnO nanowires synthesized on various surfaces on a single substrate," Materials Letters, vol.72, pp.60-63, 2012.
[12]S. W. Shin, G. L. Agawane, I. Y. Kim, Y. B. Kwon, I. O. Jung, M. G. Gang, A. V. Moholkar, J.-H. Moon, J. H. Kim, and J. Y. Lee, "Low temperature epitaxial growth and characterization of Ga-doped ZnO thin films on Al2O3(0001) substrates prepared with different buffer layers," Applied Surface Science, vol.258, pp.5073-5079,2012.
[13]A. Hirsch, C. Wille, H. Bremers, U. Rossow, A. Hangleiter, F. Ludwig, and M. Schilling, "Imposed layer-by-layer growth of ZnO on GaN/sapphire substrates using pulsed laser interval deposition," Thin Solid Films, vol.519, pp.7683-7685,2011.
[14]T. Ngo-Duc, K. Singh, M. Meyyappan, and M. M. Oye, "Vertical ZnO nanowire growth on metal substrates," Nanotechnology, vol.23, p.194015,2012.
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[16]M. Kim, M. J. Shin, H. Jeon, H. S. Ahn, S. N. Yi, S.-C. Choi, S.-G. Lee, Y. M. Yu, and N. Sawaki, "Crystal Orientation of GaN Nanostructures Grown on A12O3 and Si(111) with a Zr Buffer Layer," Japanese Journal of Applied Physics, vol.51, p.01AF04,2012.
[17]A. Hongsingthong, I. Afdi Yunaz, S. Miyajima, and M. Konagai, "Preparation of ZnO thin films using MOCVD technique with D2O/H2O gas mixture for use as TCO in silicon-based thin film solar cells," Solar Energy Materials and Solar Cells, vol.95, pp.171-174,2011.
[18]G. A. Alimenti, M. E. Gschaider, J. C. Bazan, and M. L. Ferreira, "Theoretical and experimental study of the interaction of O2 and H2O with metallic zinc--discussion of the initial step of oxide formation," J Colloid Interface Sci, vol.276, pp.24-38,2004.
[19]M. Suchea, S. Christoulakis, M. Katharakis, G. Kiriakidis, N. Katsarakis, and E. Koudoumas, "Substrate temperature influence on the properties of nanostructured ZnO transparent ultrathin films grown by PLD," Applied Surface Science, vol.253, pp.8141-8145,2007.
[20]A. Redondo-Cubero, M. Vinnichenko, M. Krause, A. Mucklich, E. Munoz, A. Kolitsch, and R. Gago, "Sublattice-specific ordering of ZnO layers during the heteroepitaxial growth at different temperatures," Journal of Applied Physics, vol.110, p.113516,2011.
[21]H. W. Liang, Y. M. Lu, D. Z. Shen, J. F. Yan, B. H. Li, J. Y. Zhang, Y. C. Liu, and X. W. Fan, "Investigation of growth mode in ZnO thin films prepared at different temperature by plasma-molecular beam epitaxy," Journal of Crystal Growth, vol.278, pp.305-310,2005.
[I]B. Mohamad Fariza, J. Sasano, T. Shinagawa, H. Nakano, S. Watase, and M. Izaki, "Electrochemical Growth of (0001)-n-ZnO Film on (111)-p-Cu2O Film and the Characterization of the Heterojunction Diode," Journal of The Electrochemical Society, vol.158, p. D621,2011.
[2]J. D. Ye, S. T. Tan, S. Pannirselvam, S. F. Choy, X. W. Sun, G. Q. Lo, and K. L. Teo, "Surfactant effect of arsenic doping on modification of ZnO (0001) growth kinetics," Applied Physics Letters, vol.95, p.101905,2009.
[3]J. S. Park, J. H. Chang, T. Minegishi, H. J. Lee, S. H. Park, I. H. Im, T. Hanada, S. K. Hong, M. W. Cho, and T. Yao, "Growth of Polarity-Controlled ZnO Films on (0001) A12O3," Journal of Electronic Materials, vol.37, pp.736-742,2007.
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[17]Y.Khlebnikov, I. Khlebnikov, M.Parker, and T. S. Sudarshan, "Local epitaxy and lateral epitaxial overgrowth of SiC," Journal of Crystal Growth, vol.233,pp.112-120,2001.
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[19]V. Lebedev, V. Cimalla, F. M. Morales, J. G. Lozano, D. Gonzalez, C. Mauder, and O. Ambacher, "Effect of island coalescence on structural and electrical properties of InN thin films," Journal of Crystal Growth, vol.300, pp.50-56,2007.
[20]D. Kashchiev, "Toward a better description of the nucleation rate of crystals and crystalline monolayers," The Journal of Chemical Physics, vol.129, p.164701,2008.
[21]A. G. Vega-Poot, G. Rodriguez-Gattorno, O. E. Soberanis-Dominguez, R. T. Patino-Diaz, M. Espinosa-Pesqueira, and G. Oskam, "The nucleation kinetics of ZnO nanoparticles from ZnCl2in ethanol solutions," Nanoscale, vol.2, p.2710,2010.
[22]L. d Abbadie, T. T. Tan, C. C. Yang, and S. Li, "Nucleation and growth mechanisms of ZnO heterostructures controlled by temperature and pressure of CVD," Materials Science and Engineering: B, vol.167, pp.31-35,2010.
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[1]J. E. Jang, S. N. Cha, T. P. Butler, J. I. Sohn, J. W. Kim, Y. W. Jin, G. A. J. Amaratunga, J. E. Jung, and J. M. Kim, "A Characterization Study of a Nanowire-Network Transistor with Various Channel Layers," Advanced Materials, vol.21, pp.4139-4142,2009.
[2]Q. Li, J. Bian, J. Sun, J. Wang, Y. Luo, K. Sun, and D. Yu, "Controllable growth of well-aligned ZnO nanorod arrays by low-temperature wet chemical bath deposition method," Applied Surface Science, vol.256, pp.1698-1702,2010.
[3]Y. Shi, Z. Yang, H. Cao, and Z. Liu, "Controlled c-oriented ZnO nanorod arrays and m-plane ZnO thin film growth on Si substrate by a hydrothermal method," Journal of Crystal Growth, vol. 312, pp.568-572,2010.
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[5]D. Wang, J. Zhang, Y. n. Hu, G. Li, Z. Bi, X. a. Zhang, X. Bian, and X. Hou, "Fabrication and optical properties of spear-like ZnO nanostructures by chemical vapor deposition," Materials Letters, vol.63, pp.2157-2159,2009.
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[9]Y. Xi, J. Song, S. Xu, R. Yang, Z. Gao, C. Hu, and Z. L. Wang, "Growth of ZnO nanotube arrays and nanotube based piezoelectric nanogenerators," Journal of Materials Chemistry, vol.19, p. 9260,2009.
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[1]P. Atanasova, R. T. Weitz, P. Gerstel, V. Srot, P. Kopold, P. A. van Aken, M. Burghard, and J. Bill, "DNA-templated synthesis of ZnO thin layers and nanowires," Nanotechnology, vol.20, p. 365302,2009.
[2]K. V. Gurav, P. R. Deshmukh, and C. D. Lokhande, "LPG sensing properties of Pd-sensitized vertically aligned ZnO nanorods," Sensors and Actuators B: Chemical, vol.151, pp.365-369, 2011.
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