氧化钒薄膜的制备及电学性质研究
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摘要
作为过渡金属元素，钒可以和氧以V_xO_y形式结合成多种氧化物。各种氧化钒薄膜以其优良的性能成为国内外功能材料研究的热点，具有广阔的应用前景。但由于钒的多价态，制备具有纯净化学计量比的氧化钒非常困难。本文利用真空蒸发—真空还原方法以高纯V_2O_5粉末为原料制备出纯度较高、结晶度好的几种主要的氧化钒薄膜(V_2O_5、VO_2(B)、VO_2(A)、V_2O_3)，通过控制各个工艺参数(薄膜衬底材料、薄膜厚度、真空度、衬底温度、蒸发电流、蒸发时间、退火时间、退火温度等)来探索最佳制备条件，并运用各种测试方法对薄膜性能进行分析，研究各工艺参数对氧化钒薄膜晶体结构、表面形貌、V离子价态及电学性质等方面的影响。经过多次实验取得了一定成果。本论文的研究工作如下：
1．研究了衬底温度和衬底材料对薄膜晶体结构和电阻温度系数的影响。发现衬底温度对退火后薄膜的晶粒生长影响不大。而单晶衬底利于氧化钒薄膜生长，且制备的薄膜较非晶衬底具有较高的电阻—温度系数。
2．研究了退火温度对氧化钒薄膜制备的影响。发现随退火温度升高，薄膜先后经历了单斜晶系VO_2(B)型→单斜晶系VO_2(A)型→四方晶系VO_2→V_2O_3的变化，并对VO_2薄膜进行深入研究。研究发现，三种VO_2薄膜中V均以V~(4+)为主，且VO_2(A)型薄膜中V~(4+)含量最高。薄膜电阻以退火温度460℃时为分界，低于460℃时，VO_2(B)型薄膜电阻和电阻温度系数随退火温度升高而增大，高于460℃时，四方晶系VO_2薄膜电阻及其电阻温度系数随退火温度升高呈现相反的趋势。在460℃时，薄膜的电阻温度系数最大，能达到3.2％／℃．经查新说明，使用这种工艺方法和条件制备各种氧化钒薄膜是本工作的创新。
Vanadium as a transition element can compose varial Vanadium oxides by V_xO_y with oxygen and Vanadium oxides have been widely studied because of their excellent characters. But Vanadium has so many valence that Vanadium Oxides with strict metric are not available. In this paper, good crystal thermal-sensitive Vanadium oxides (V_2O_5, VO_2(B), VO_2(A), V_2O_3) thin films are prepared from V_2O_5 powder by vacuum evaporation and vacuum annealing. We selected the best qualifications by experimenting with various fabricative parameters such as underlay material and temeprature, thin film thickness, vacuum degree, evaporation current, evaporation time, anealing hour, anealing temperature. The structural properties, surface morphology, electrical properties, and V ion valence state of VOx thin films were measured by tesing and analysed and some instructive results were got. The contents of the work are listed as following:
1. The effects on the crystal structure and the temperature coefficient of Vanadium oxide thin films were studied because of different underlay temperatures and materials. Rusults were found underlay temperature did not influence obviously the crystals' sizes of the thin films, but Vanadium oxide thin films on single-crystal underlay had better crystal structure and temperature coefficient of
1．研究了衬底温度和衬底材料对薄膜晶体结构和电阻温度系数的影响。发现衬底温度对退火后薄膜的晶粒生长影响不大。而单晶衬底利于氧化钒薄膜生长，且制备的薄膜较非晶衬底具有较高的电阻—温度系数。
2．研究了退火温度对氧化钒薄膜制备的影响。发现随退火温度升高，薄膜先后经历了单斜晶系VO_2(B)型→单斜晶系VO_2(A)型→四方晶系VO_2→V_2O_3的变化，并对VO_2薄膜进行深入研究。研究发现，三种VO_2薄膜中V均以V~(4+)为主，且VO_2(A)型薄膜中V~(4+)含量最高。薄膜电阻以退火温度460℃时为分界，低于460℃时，VO_2(B)型薄膜电阻和电阻温度系数随退火温度升高而增大，高于460℃时，四方晶系VO_2薄膜电阻及其电阻温度系数随退火温度升高呈现相反的趋势。在460℃时，薄膜的电阻温度系数最大，能达到3.2％／℃．经查新说明，使用这种工艺方法和条件制备各种氧化钒薄膜是本工作的创新。
Vanadium as a transition element can compose varial Vanadium oxides by V_xO_y with oxygen and Vanadium oxides have been widely studied because of their excellent characters. But Vanadium has so many valence that Vanadium Oxides with strict metric are not available. In this paper, good crystal thermal-sensitive Vanadium oxides (V_2O_5, VO_2(B), VO_2(A), V_2O_3) thin films are prepared from V_2O_5 powder by vacuum evaporation and vacuum annealing. We selected the best qualifications by experimenting with various fabricative parameters such as underlay material and temeprature, thin film thickness, vacuum degree, evaporation current, evaporation time, anealing hour, anealing temperature. The structural properties, surface morphology, electrical properties, and V ion valence state of VOx thin films were measured by tesing and analysed and some instructive results were got. The contents of the work are listed as following:
1. The effects on the crystal structure and the temperature coefficient of Vanadium oxide thin films were studied because of different underlay temperatures and materials. Rusults were found underlay temperature did not influence obviously the crystals' sizes of the thin films, but Vanadium oxide thin films on single-crystal underlay had better crystal structure and temperature coefficient of
引文
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[2] 申文等著．《无机化学丛书》第八卷．北京：科学出版社，1998．224
[3] Partlow D. P., Gukovich S. R., Radford K. C., et al. J. Appl. Phys.,1991, 70: 443
[4] Kimizuka Noboru, Ishii Motihiko, Kawada Isao et al. BEHAVIOR OF VANADIUM DIOXIDE SINGLE CRYSTALS SYNTHESIZED UNDER THE VARIOUS OXYGEN PARTIAL PRESSURES AT 1500 K, Journal of Solid State Chemistry, 1974, 9(1): 69
[5] M. L. Gray, W. J. Croft, K. Dwight et al. Effect of high pressure on the electronic properties of VO_2, J. of solid state chemistry, 1984, 54: 421
[6] J. przedmojsky, B. pura, W. Piekarczyk et al.. Phase transformation of twinned VO_2 crystals obtained by means of chemical transport method, Phys. Stat. Sol. (a), 1972, 11: K1
[7] Hans W. Verleur, A. S. Barker, C. N. Berglund et al. Optical properties of VO_2 between 0.25 and 5 eV, Physical Review, 1968, 172(3): 788
[8] W. Bruckner, W. Moldenhauer, H. Wich et al. The Range of homogeneity of VO_2 and the influence of the composition on the physical properties, Phys. Stat. Sol.(a), 1975, 29: 63
[9] D. B. Mcwhan, M. Marezio, J. P. Remeika et al. X-ray diffraction study of metallic VO_2, Phys. Rev. B, 1974, 10(2): 490
[10] Larry A, Ladd, William Paul, Solid State Communications, 1969, 7: 425
[11] Noboru Kimizuka, Motohiko Ishh, Isao Kawada et al. Behavior of vanadium dioxide single crystals synthesized under the various oxygen partial pressures at 1500K, J. of Solid state chemistry, 1974, 9: 69
[12] H. oppermann, W. Reichelt, U. Gerlach et al. The range of homogeneity of VO_2 and the influence of the composition on the physical properties, Phys. stat. sol. (a), 1975, 28: 439
[13] Ramakant Srivastava, L. L. Chase. Raman spectrum of semiconducting and metallic VO_2. Physical Review Letters, 1971, 27(11): 727-730
[14] F. C. Case. Simple resistance model fit to the oxidation of a vanadium film into VO_2, J. Vac. Sci. Technol. A, 1988, 6(1): 123
[15] F. C. Case. Modification in the phase transition properties of predeposited VO_2 films, J. Vac. Sci. Technol. A, 1984, 2(4): 1509
[16] J. Livage, G. Guzman, F. Beteille. Optical properties of Sol-Gel derived vanadium oxide films, J. of Sol-Gel Sci. and Technol.. 1997, 8: 857
[17] Songwei LU, Lisong Hou, Fuxi Gan. Preparation and optical properties of phase-change VO_2 thin films, J. of Mat. Sci.. 1993, 28: 2169
[18] P. Jin, M. Tazawa, K. Yoshimura et al.. Thermochromism of metal-doped VO_2 films deposited by dual-target sputtering, SPIE Vol. 2255, 1994: 415
[19] 吴召平，方平安．二氧化钒薄膜在α-Al_2O_3衬底上的外延生长及其金属半导体相变特性研究，无机材料学报，1999，14(5)：823
[20] A. Razavi, L. Bobyak, P. Fallon. The effects of biasing and annealing on the optical properties of radio-frequency sputtered VO_2, J. Vac. Sci. Technil. A, 1990, 8(3): 1391
[21] Yin DaChuan, Xu Niankan, Zhang Jingyu et al.. Vanadium dioxide films with good electrical switching property, J. Phys. D:Appl. Phys.,1996, 29: 1051
[22] S. -J. Jiang, C. -B. Ye, M. S. R. Khan et al.. Structural and compositional evolution during oxidation of vanadium coatings, SPIE Vol. 1272, 1990: 185
[23] 陈长虹、易新建、张静等．基于VO_2薄膜非致冷红外探测器性能研究，红外与毫米波学报，2001，20(2)：136
[24][68] 李华高，杨子文，刘爽．非致冷红外探测器用VO_2薄膜的制备，半导体光电，2001，22(1)：38
[25] 王宏臣、易新建、黄光等．一种制备氧化矾薄膜的新工艺，半导体光电，2003，24(4)：280
[26] E. Kusano, J. A. Theil et al. J. Vac. Sci. Technol. A, 1988, 6(3): 1663
[27] F. C. Case. J. Vac. Sci. Technol. A, 1987, 5(4): 1762
[28] A. Razavi, L. Bobyak, P. Fallon. The effects of biasing and annealing on the optical properties of radio-frequency sputtered VO_2, J. Vac. Sci. Technil. A, 1990, 8(3): 1391
[29] 崔敬忠，达道安，姜万顺．VO_2热致变色薄膜的结构和光电性能研究，物理学报，1998，47(3)：454
[30] Mitsuhiro Nagashima, Hideo Wada, Kunihiro tanikawa et al.. The electronic behaviors of oxygen-deficient VO_2 thin films in low temperature region, Jpn. J. appl. Phys., 1998, 37: 4433
[31] F. C. Case. J. Vac. Sci. Technol. A, 1987, 5(4): 1762
[32] K. D. Ufert. Phys. Stat. Sol. (a), 1977, 42: 187
[33] Leonov A. S., Podsvirov O. A.. Degradation of the phase transition in vanadium dioxide during electron bombardment and heat treatment, Soviet Technical Physocs Letters, 1984, 10(9): 440
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