LB法制备ZnO和Mg_xZn_（1-x）O薄膜及其光学性能研究
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摘要
采用LB技术在石英衬底上制备出ZnO薄膜以及MgxZn1-xO薄膜,研究了ZnO及MgxZn1-xO薄膜的成膜条件和拉膜条件,并对制备的ZnO及MgxZn1-xO薄膜进行了X射线衍射分析(XRD)、紫外-可见光谱(UV-Vis)分析及原子力显微镜(AFM)的表征。对不同层数及不同Mg掺杂量对MgxZn1-xO光学性能的影响进行了探讨。通过LB膜技术,确定了较佳的亚相浓度,滑障速度,铺展液的静置时间,铺展量;在适宜的转移膜压、基片向上提拉速度、向下浸入速度,可获得转移比在1.0附近,性能稳定的硬脂酸/ZnO复合LB膜。在此基础上确定了亚相浓度,滑障速度,铺展液的静置时间,铺展量等较佳的MgxZn1-xO薄膜的成膜条件;转移膜压,基片向上提拉速度,向下浸入速度等拉膜条件,获得转移比在1.0附近,性能稳定的硬脂酸/MgxZn1-xO复合LB膜。
通过热处理,获得了ZnO和MgxZn1-xO粉体及超薄膜。采用X射线衍射(XRD)检测其结晶状态,并通过紫外-可见光谱(UV-Vis)对复合LB膜的层间重叠情况进行了考查。ZnO及MgxZn1-xO复合LB膜及超薄膜的表面形貌及粒子覆盖度等信息,则通过原子力显微镜(AFM)进行了检测。采用PL光谱研究了不同层数和Mg掺杂量对ZnO及MgxZn1-xO薄膜光学性能的影响。掺入Mg后,薄膜的结晶质量提高。随着Mg的掺杂量x的增加,MgxZn1-xO薄膜的紫外发射强度增大;当x≥0.4时,紫外发射峰强度减小。在Mg掺杂量一定的情况下,随着提拉层数的提高,紫外发射峰的强度也会随之增加。
The ZnO thin film and MgxZn1-xO thin films at the air/water interface have been transferred onto quartz substrates by Langmuir-Blodgett technique. Effects of different conditions of forming and preparing thin films were investigated. ZnO thin films and MgxZn1-xO thin films were then studied by XRD, UV–Vis spectroscope, atomic force microscope (AFM). ZnO and MgxZn1-xO thin films with different layer number and with different content of Mg-doping were studied on the test of optical properties.
Through LB technique, favourable subphase concentration, barrier speed, temperature of the subphase, still time, pH value and spreading volume were confirmed. Then surface pressure, lifting speed upward and downward were investigated to form stable stearic acid/ZnO composite LB films with transfer ratio at 1.0. Favourable subphase concentration, barrier speed, temperature of the subphase, still time, pH value and spreading volume were confirmed. Then surface pressure, lifting speed upward and downward were investigated to form stable stearic acid/MgxZn1-xO composite LB films with transfer ratio at 1.0.
Through heat treatment, ZnO and MgxZn1-xO powders and ultra-thin films were obtained. X-ray diffraction (XRD) was used to detect the crystalline state, and UV - visible spectrum (UV-Vis) was used to investigate overlap state of the composite LB film. The surface morphology and particle coverage information of ZnO and MgxZn1-xO composite LB film and ultra-thin films were determined by atomic force microscope (AFM).PL spectra were used to investigate the effects of different layer numbers and the content Mg-doping ZnO and MgxZn1-xO thin film on optical properties. After Mg was doped, the crystallization quality of thin film increased. With the amount of Mg doping x increased, MgxZn1-xO thin films of UV emission intensity increased. When x value is no less than 0.4, the UV emission intensity decreases instead. When Mg-doping content is certain, with the improvement of layer numbers, the intensity of UV emission peak will also increase.
通过热处理,获得了ZnO和MgxZn1-xO粉体及超薄膜。采用X射线衍射(XRD)检测其结晶状态,并通过紫外-可见光谱(UV-Vis)对复合LB膜的层间重叠情况进行了考查。ZnO及MgxZn1-xO复合LB膜及超薄膜的表面形貌及粒子覆盖度等信息,则通过原子力显微镜(AFM)进行了检测。采用PL光谱研究了不同层数和Mg掺杂量对ZnO及MgxZn1-xO薄膜光学性能的影响。掺入Mg后,薄膜的结晶质量提高。随着Mg的掺杂量x的增加,MgxZn1-xO薄膜的紫外发射强度增大;当x≥0.4时,紫外发射峰强度减小。在Mg掺杂量一定的情况下,随着提拉层数的提高,紫外发射峰的强度也会随之增加。
The ZnO thin film and MgxZn1-xO thin films at the air/water interface have been transferred onto quartz substrates by Langmuir-Blodgett technique. Effects of different conditions of forming and preparing thin films were investigated. ZnO thin films and MgxZn1-xO thin films were then studied by XRD, UV–Vis spectroscope, atomic force microscope (AFM). ZnO and MgxZn1-xO thin films with different layer number and with different content of Mg-doping were studied on the test of optical properties.
Through LB technique, favourable subphase concentration, barrier speed, temperature of the subphase, still time, pH value and spreading volume were confirmed. Then surface pressure, lifting speed upward and downward were investigated to form stable stearic acid/ZnO composite LB films with transfer ratio at 1.0. Favourable subphase concentration, barrier speed, temperature of the subphase, still time, pH value and spreading volume were confirmed. Then surface pressure, lifting speed upward and downward were investigated to form stable stearic acid/MgxZn1-xO composite LB films with transfer ratio at 1.0.
Through heat treatment, ZnO and MgxZn1-xO powders and ultra-thin films were obtained. X-ray diffraction (XRD) was used to detect the crystalline state, and UV - visible spectrum (UV-Vis) was used to investigate overlap state of the composite LB film. The surface morphology and particle coverage information of ZnO and MgxZn1-xO composite LB film and ultra-thin films were determined by atomic force microscope (AFM).PL spectra were used to investigate the effects of different layer numbers and the content Mg-doping ZnO and MgxZn1-xO thin film on optical properties. After Mg was doped, the crystallization quality of thin film increased. With the amount of Mg doping x increased, MgxZn1-xO thin films of UV emission intensity increased. When x value is no less than 0.4, the UV emission intensity decreases instead. When Mg-doping content is certain, with the improvement of layer numbers, the intensity of UV emission peak will also increase.
引文
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27李微,孙云,何青,刘芳芳,李凤岩,孪生对靶直流磁控溅射制备薄膜及其特性研究,人工晶体学报, 2006, 35(04): 761
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32 V. srikant, Valter Sergo and David R. Clarke. Epitaxial Aluminum-doped Zinc Oxide Thin Films on Sapphire:Ⅱ, Defect Equilibria and Electrical Properties. J. Am. Ceram. Soc. 1995, 78(7): 1935
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37 A. Ohtomo, R. Shiroki, I. Ohkubo, H. Koinuma, and M. Kawasaki, Thermal stability of supersaturated MgxZn1-xO alloy films and MgxZn1-xO/ZnO heterointerfaces, Appl.Phys. Lett. 1999, 75: 4088
38 T. Makino, Y. Segawa, M. Kawasaki, A. Ohtomo, R. Shiroki, K. Tamura, and H.Koinuma, Band gap engineers ng based on MgxZn1-xO and CdyZn1-yO ternary alloy films, Appl. Phys. Lett. 2001, 78: 1237
39 D. W. Ma, Z. Z. Ye, and L. L. Chen, Dependence of structural and optical properties of Zn1-xCdxO films on the Cd composition, Phys. Status Solids A. 2004, 201:2929
40 S. ChooPun,R. D. Vispute,W.Yang et. al ,Realization of band gap above 5.0eV in metastable cubie-Phase MgxZn1-xO alloy films,Applied Physics Letters,2002,80(9):1529-1531.
41 Chal-Hwan Choi,Seon-Hyo Kim,Effects of Post-annealing temperature onstructural,optical and electrical Properties of ZnO and Znl-xMgxO films by reactive RF magnetron sputtering,Journal of Cyrstal Growth,2005,283:170-179.
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2 Kamalasanan M N ,Chandra S. Sol-gel synthesis of ZnO thin films[J] . Thin solid films ,1996 ,288 :112 - 115.
3 Nagata T,Shimura T,Ashida A ,et al . Electrol - optic properties of ZnO:X (X=Li ,Mg) thin films[J ] . J Cryst Growth ,2002 ,237 -239 :533– 537
4 Konopny L, Berfeld M, Popovitz-Boro R, et al. Phase transitions and stabilization of the organized hybrid Langmuir-Blodgett films of alkanoic acids/CdS and PbS Q-particles. Adv Mater, 2001,13(8):580~584
5 M.H.Koch, A.J.Hartmann, R.N.Lamb, etal. Self-Texture in the initial stages of ZnO film growth. J?Phys.Chem.B, 1997,101(4):P8231.
6 H.S.Ku, H.Takashi, K.H.Ju,et al. Control of polarity of ZnO films grown by plasma-assisted molecular-beam epitaxy:Zn- and O-polar ZnO films on Ga-palor GaN templates.Appl.Phys.Lett.2000,77(22):p3571
7 Bagnall D M,Chen Y F,Zhu Z,et al. High temperature exeitonie stimulated emission from ZnO epitaxial layers.Appl Phys Lett.1998,73(8):1038
8 N.Riehl and O.Ortman, Purification and biochemical characterization of recombinant hirudin produced by Saccharomyces , J.Eleetrochem.1952,60:14
9 E.G.Bylander,Surface effects on the low-energy cathodoluminescence of zinc oxide J.Appl.Phys.1978,49:1188
10 K.Vanheusden,C.H.Seager,W.L.Warren,Correlation between photoluminescence and oxygen vacancies in ZnO phosphors , et al.,Appl. Phys. Lett.1996,68:403-405
11 A.Ghis,R.Meyer,R.Rambaud,Sealed vacuum devices: fluorescent microtip displays et al.,IEEE. Trans. Electron Device ED-38,1991:2320
12 P. Yu,Z. K. Tang,G. K. L. Wong,et al.,23nd Int. Conf. On the Physics of Semiconductors,World Scientific,Singapore,1996:1453
13 Z. K. Tang ,G. K. L. Wong,R. Yu,et al.,Room-temperature ultraviolet laser emission from self-assembled ZnO microcrystallite thin films Appl. Phys. Lett. 1998,72:3270-3272
14 D. M. Baganall ,et al., Structural, Morphological and Optical Properties of ZnO Thin Films Grown onγ-LiAlO2 Substrate by Pulsed Laser Deposition , Appl. Phys. Lett. 1997,70:2230-2232
15 R. F. Service,NANOTECHNOLOGY: Calls Rise for More Research on Toxicology of Nanomaterials Science,1997,276:895
16 Z. K. Tang,P. Yu,and G. K. L. Wong,Room-temperature stimulated emission of excitons in ZnO/(Mg, Zn) O superlattices , Nonlinear Optics,1997,18(2一4):355-359
17 P.Yu,Z. K. Tang,G. K. L. Wong et al.,Ultraviolet spontaneous and stimulated emissions from ZnO microcrystallite thin films at room temperature ,Phys. Low-Dim. Struct. 1998,1/2:243-247
18 M. Kaeasaki,A. Ohtomo,I.Ohkubo,et al.,Room-Temperature Ferromagnetism in Transparent Transition Metal-Doped Titanium Dioxide, Mat. Sci. &Eng. ,1998,B56:239-244
19 P.Yu,Z. K. Tang,G. K. L. Wong,et al.,Room-temperature gain spectra and lasing in microcrystalline ZnO thin films,J.Cryst. Growth,1998,184/185:601-605
20 A. Ohtomo,M. Kawasaki,Y.Sakurai ,et al.,Fabrication of alloys and superlattices based on ZnO towards ultraviolet laser ,Mat. Sci. &Eng.,1998,B54:24-28
21李剑光,叶志镇,硅基上直流反应磁控溅射沉积优质ZnO薄膜及其性能研究,第五届全国固体薄膜学术会议论文集,1997:256-257
22 Z. X. Fu,et al.,The effect of Zn buffer layer on growth and luminescence of ZnO films deposited on Si substrates. J. Cryst. Growth,1998,193:316-320
23 C. X. Guo,Z. X. Fu,and C. S. Shi,Ultraviolet super-radiation luminescence of sputtering ZnO film under cathode-ray excitation at room temperature, Chinese Phys. Lett.1999,16(2):146-148
24 W. L. Zhang, L. Chai, Q. R. Xing,Femtosecond degenerate four-wave-mixing in ZnO microcrystallite thin film, et al.,Chinese Phys.Lett.1999,16(10):728-731
25余旭浒,马瑾,计峰,王玉恒,张锡健,程传福,马洪磊,薄膜厚度对ZnO:Ga透明导电薄膜性能的影响.功能材料, 2005, 36(02): 241
26 P. Nunes, E. Fortunato, R. Martins. Influence of the post-treatment on the properties of ZnO thin films Thin Solid Films. 2001, 383: 277.
27李微,孙云,何青,刘芳芳,李凤岩,孪生对靶直流磁控溅射制备薄膜及其特性研究,人工晶体学报, 2006, 35(04): 761
28倪星元,吴永刚,吴广明,张慧琴,金哲民,氧化锌透明导电薄膜的制备及其特性材料研究,材料研究学报, 1999, 13(03): 331
29 K wang, Joo Kim and Young Ran Park. Large and abrupt optical band gap variation in In-doped ZnO. Appl. Phys. Lett. 2001, 78(4): 475
30 Suzuki, T. Matsushita, N. Wada, et al. Transparent Conducting AI-Doped ZnO Films Prepared by Pulsed Laser Deposition. Jpn. J. Appl. Phys. Part 2, 1996, 35: L56
31郝晓涛,马瑾,田茂华,王卿璞,马洪磊,叶丽娜,陈峰,柔性衬底铝掺杂氧化锌透明导电膜的特性研究,功能材料与器件学报, 2002, 8(01): 8
32 V. srikant, Valter Sergo and David R. Clarke. Epitaxial Aluminum-doped Zinc Oxide Thin Films on Sapphire:Ⅱ, Defect Equilibria and Electrical Properties. J. Am. Ceram. Soc. 1995, 78(7): 1935
33 NF Cooray, K Kushiya, A Fujimaki, D Okumura et al. Optimization of Al-doped ZnO window layers for large-area CuInGaSe-2 based modules by RF/DC/DC multiple magnetron sputtering, Jpn. J. Appl. Phys. 2000, 39: L555.
34陆峰,徐成海,曹洪涛,裴志亮,孙超,闻立时,透明导电纳米薄膜的性能分析,真空科学与技术, 2003, 23(01): 9
35陈汉鸿,叶志镇.ZnO薄膜的掺杂和转型的研究进展。半导体学报, 2001,38(2):37-39
36赵磊,磁控溅射制备掺杂氧化锌薄膜晶体结构与光电性能研究,材料研究学报, 2008, 28(2): 946-956
37 A. Ohtomo, R. Shiroki, I. Ohkubo, H. Koinuma, and M. Kawasaki, Thermal stability of supersaturated MgxZn1-xO alloy films and MgxZn1-xO/ZnO heterointerfaces, Appl.Phys. Lett. 1999, 75: 4088
38 T. Makino, Y. Segawa, M. Kawasaki, A. Ohtomo, R. Shiroki, K. Tamura, and H.Koinuma, Band gap engineers ng based on MgxZn1-xO and CdyZn1-yO ternary alloy films, Appl. Phys. Lett. 2001, 78: 1237
39 D. W. Ma, Z. Z. Ye, and L. L. Chen, Dependence of structural and optical properties of Zn1-xCdxO films on the Cd composition, Phys. Status Solids A. 2004, 201:2929
40 S. ChooPun,R. D. Vispute,W.Yang et. al ,Realization of band gap above 5.0eV in metastable cubie-Phase MgxZn1-xO alloy films,Applied Physics Letters,2002,80(9):1529-1531.
41 Chal-Hwan Choi,Seon-Hyo Kim,Effects of Post-annealing temperature onstructural,optical and electrical Properties of ZnO and Znl-xMgxO films by reactive RF magnetron sputtering,Journal of Cyrstal Growth,2005,283:170-179.
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