以光辅助MOCVD法生长高质量高温超导体YBa_2Cu_3O_（6.9）膜的初步研究
摘要
高温超导材料YBa2Cu3O6.9(简称YBCO),作为一种新型的重要材料,它有着极其广泛且重要的应用价值,如在大电流方面,可应用于超导发电机(此类发电机发电量远超过传统发电机,但体积更小,重量很轻)。另如在小电流方面,可应用于超导微波滤波器(抗波段干扰能力强,灵敏度高)。若超导发电机研发成功,可给人类带来一次新的能源革命;而超导微波滤波器则可对当前微波滤波器通讯的高速发展提供关键性的技术帮助。近年来美国与日本等国皆在其研发方面投入了巨大的人力物力。在大电流方面他们已经取得了很高的成果。
在本论文里论述了利用光辅助MOCVD法生长高质量的c轴向YBCO膜。通过优化生长温度,压强、气流,源的挥发速率等条件,可以在较高的膜的生长速率下,得到高晶体质量的YBCO厚膜,以供超导微波滤波器实用的需求。而后本论文在1英寸的LAO(100)衬底上对生长大面积YBCO单面厚膜作了初步但很有帮助的研究(为供超导微波滤波器的实际应用,YBCO膜的直径最少为2英寸)。
In this thesis, the growth of purely c-axis oriented YBa2Cu3O6.9 (YBCO) films by photo-assisted MOCVD was discussed. Thin YBCO films (less than 1μm) grown on LaAlO3(100) [LAO(100)] with high crystalline quality was successfully fabricated by a photo-assisted MOCVD system disigned by ourselves. Tests of one thin film sample with thickness of about 0.4μm indicated it is c-axis oriented, with no visible grain boundary in its sectional SEM mcrograph. This means this YBCO film is single-crystal like. On the otherhand, this film has high superconducting quality also. Its superconducting critical temperature (Tc) is 90K, and its superconducting critical current density (Jc) is 1.33MA/cm2 (77K, 0T). Then, thick YBCO films with thickness above 2μm were also succesfully prepared. As shown by both SEM micrographs and XRD 2θ-scanning plots. These thick YBCO-films have similar high crystslline quality as that for the thin YBCO films. As high quality, large area YBCO films are practically needed for the application of these films to the fabrication of superconducting microwave filters, optimization of the processing conditions for the growth of thick YBCO films was done in this thesis.
Firstly, substrate temperature window (Ts window) for the growth of purely c-axis YBCO films with high crystalline qulity was more precisely examined by using the photo-assisted MOCVD system on our lab. Secondly, an appropriate Ts of 820℃was chosen for the gowth of YBCO thick films. During the growth of these YBCO films, the influence of changing airflow and reactor pressure to film growth rate was discovered. From our primary study Finally, the optimized growth conditions indicated above were chosen for the preparation of YBCO thick films. The fastest growth rate of films with high crystalline quality was obtained by changing the evaporation rate of the Y and Cu precursors. The best respective evaporation rate along with the best proportion of Y and Cu precursors concusumed in the films growth were then found for the growth of YBCO thick films with high crystalline quality.
Besides, high crystalline quality, c-axis oriented YBCO thick films on 1-inch single sided LAO(100) wafers have also been successfully fabricated by the same system. XRD and SEM tests for evenly cut small pieces of a 1 inch YBCO film fabricated indicates. The YBCO film prepared over the entire 1" are as of high crystalline quality, c-axis oriented YBCO thick films. However, as now there is only gas inlet (indined above the surface of the substrate), and the susceptor was not rotated yet, it would be understanble that there would be a large variation in thickness over the 1" area of the YBCO thick films prepared. The thickness here ranges from 1.2 to 2.6μm. There is only piece among the 13 cut pieces from this 1" YBCO film which showes there are few grain boundaries in it. The cause of this phenomenon is discussed. In this thesis, the advantages of the photo-assited MOCD techniques employed for the deposition of YBCO films was also been discussed.
在本论文里论述了利用光辅助MOCVD法生长高质量的c轴向YBCO膜。通过优化生长温度,压强、气流,源的挥发速率等条件,可以在较高的膜的生长速率下,得到高晶体质量的YBCO厚膜,以供超导微波滤波器实用的需求。而后本论文在1英寸的LAO(100)衬底上对生长大面积YBCO单面厚膜作了初步但很有帮助的研究(为供超导微波滤波器的实际应用,YBCO膜的直径最少为2英寸)。
In this thesis, the growth of purely c-axis oriented YBa2Cu3O6.9 (YBCO) films by photo-assisted MOCVD was discussed. Thin YBCO films (less than 1μm) grown on LaAlO3(100) [LAO(100)] with high crystalline quality was successfully fabricated by a photo-assisted MOCVD system disigned by ourselves. Tests of one thin film sample with thickness of about 0.4μm indicated it is c-axis oriented, with no visible grain boundary in its sectional SEM mcrograph. This means this YBCO film is single-crystal like. On the otherhand, this film has high superconducting quality also. Its superconducting critical temperature (Tc) is 90K, and its superconducting critical current density (Jc) is 1.33MA/cm2 (77K, 0T). Then, thick YBCO films with thickness above 2μm were also succesfully prepared. As shown by both SEM micrographs and XRD 2θ-scanning plots. These thick YBCO-films have similar high crystslline quality as that for the thin YBCO films. As high quality, large area YBCO films are practically needed for the application of these films to the fabrication of superconducting microwave filters, optimization of the processing conditions for the growth of thick YBCO films was done in this thesis.
Firstly, substrate temperature window (Ts window) for the growth of purely c-axis YBCO films with high crystalline qulity was more precisely examined by using the photo-assisted MOCVD system on our lab. Secondly, an appropriate Ts of 820℃was chosen for the gowth of YBCO thick films. During the growth of these YBCO films, the influence of changing airflow and reactor pressure to film growth rate was discovered. From our primary study Finally, the optimized growth conditions indicated above were chosen for the preparation of YBCO thick films. The fastest growth rate of films with high crystalline quality was obtained by changing the evaporation rate of the Y and Cu precursors. The best respective evaporation rate along with the best proportion of Y and Cu precursors concusumed in the films growth were then found for the growth of YBCO thick films with high crystalline quality.
Besides, high crystalline quality, c-axis oriented YBCO thick films on 1-inch single sided LAO(100) wafers have also been successfully fabricated by the same system. XRD and SEM tests for evenly cut small pieces of a 1 inch YBCO film fabricated indicates. The YBCO film prepared over the entire 1" are as of high crystalline quality, c-axis oriented YBCO thick films. However, as now there is only gas inlet (indined above the surface of the substrate), and the susceptor was not rotated yet, it would be understanble that there would be a large variation in thickness over the 1" area of the YBCO thick films prepared. The thickness here ranges from 1.2 to 2.6μm. There is only piece among the 13 cut pieces from this 1" YBCO film which showes there are few grain boundaries in it. The cause of this phenomenon is discussed. In this thesis, the advantages of the photo-assited MOCD techniques employed for the deposition of YBCO films was also been discussed.
引文
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[32] 唐士兵 “金属有机化学气相沉积(MOCVD)前体物的制备.表征及热力学性质研究” 吉林大学化学学院本科论文 P23-26(2006)
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[38] J. Geerk, G. Linker and O. Meyer. “Epitaxial growth and properties of YBaCuO thin films” Materials Science Reports, 4(1989)No.5,6: 193
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[2] de Bruynt Ouboter, R., “Superconductivity:discoveries during the early years of low temperature research at Leiden,” IEEE trans. On Magnetic, Vol. MAG-23(1987)371.
[3] Pippard, A. B., “Early superconductivity research (except Leiden),” IEEE Trans. on Magnetics, Vol. MAG-23( 1987)371.
[4] Bednorz,J.G., K.A.Müller, “Possible high Tc superconductivity in the Ba-La-Cu-O compound system, ” Z.furPhys.Vol.64(1986)189.
[5] M.K.Wu, J.R.Ashburn, C.J.Torng, P.H.Hor, R.L.Meng,L.Gao, Z.J.Huang, Y.Q.Wang, C.W.Chu,“Superconductivity at 93K in a new mixed-phase Y-Ba-Cu-O Compound system at ambient pressure,” Phys. Rev.Lett.Vol. 58(1987)908.
[6] Sheng,Z.Z., A.M.Hermann, “Bulk superconductivity at 120K in the Tl-Ca/Ba-Cu-O system,” Nature, 332(1988)138
[7] Chu,C.W., L.Gao, F.Chen, Z.J.Huang, R.L.Meng and Y.Y.Xue, “Superconductivit above 150K in HgBa2Ca2Cu3O8+ at high pressure ” Nature, 365(1993)323
[8] 林良真 张金龙 李传义 夏平畴 杨乾声 “超导电性及其应用” 北京工业大学出版社 1998.12 第一版 P304-358
[9] M. Gurvitch, M. A. Washington, H. A. Huggins. “High Quality Refractory Josephson Tunnel Junction Utilizing Thin Aluminum Layers” Appl.phys.Lett. 42(1983)472
[10] K. K. Likharev, O. A. Mukhanov, V. K Semenov, “Resistive Single Flux Quantum Logic for The Josephson-Junction Digital Technolgy”, pp.1103-08, in SOUID 85, H D Hahlbohm, H Liibbig, Eds. Walter de Gruyter, Berlin, 1985
[11] H.K.Onnes, Commun. Phys. Lab. Uuiv. Leiden, 1395,1914
[12] H.K.Onnes "Report on the researches made in the Leiden Cryogenic Laboratory between the Second and Third International Congress of Refrigeration," Communs. Phys. Lab., Univ. Leiden Suppl. 34b (1913) 55
[13] Meissner, W., and R.Ochsenfeld, " Ein neuer Effect bei Eintritt der Supraleitf?higkeit, " Naturwissenschaften, 21(1933)787.
[14] L.N.Cooper, "Bound Electron Pairs in a Degenerate Fermi Gas" Phys Rev 104 (1956)1189
[15]J.Bardeen, L.N.Cooper, J.R.Schrieffer. “Theory of Superconductivity” Phys Rev,108(1957)1175
[16] 沈致远著 盛克敏译 王家素校 “高温超导微波电路” 国防工业出版社 2000 年 1 月 P21 (原著为 1994 年版)
[17] Q.Zhong, P.C.Chou, Q.L.Li, G.S.Taraldsen, A.Ignatiev, “High-rate growth of purely a-axis oriented YBCO high-Tc thin films by photo-assisted MOCVD” Phys C 246(1995)288.
[18] J. Geerk, G. Linker and O. Meyer. “Epitaxial growth and properties of YBaCuO thin films” Materials Science Reports, 4 (1989) No.5,6: 193
[19] W. Prellier, Ph Lecoeur, and B, Mercey “Colossal-magnetoresistive manganite thin films” J. Phys: Condens. Matter 13(2001)915
[20] 陶伯万 “3英寸YBCO双面超导薄膜的外延生长和均匀性研究” 电子科技大学博士论文 2003.8 p16
[21] L. Méchin, G. Huot, and D. Bloyet Cofabrication of superconductingYBa2Cu3O7-δ and semiconducting devices on (100) Si substrates, Appl. Phys. Lett. 85 (2004) 3154
[22] V. F. Solovyov , H. J. Wiesmann, “Application of low-angle polishing for rapid assessment of the texture and morphology of thick film Y1Ba2Cu3O7 superconducting tapes” , Physica C 467 (2007) 186
[23] R. A. Hawsey , D. K. Christen, “Progress in research, development, and pre-commercial deployment of second generation HTS wires in the USA” , Phys. C 445-448(2006) 488
[24] A. Goyal, D.P.Norton, J.D. Budai, M. Paranthaman, E.D. Specht, D.M. Kroeger,D.K. Christen, Q.He, B. Saffian, F.A. List, D.F. Lee, P.M. Martin, C.E. Klabunde, E. Hatfield, V.K. Sikka, “High critical current density superconducting tapes by epitaxial deposition of YBa2Cu3Ox thick films on biaxially textured metal substrates”, Appl. Phys. Lett. 69(1996)1795.
[25] Y. Iijima, N. Tanabe, O. Kohno, Y. Ikeno, “In-plane aligned YBa2Cu3O7-x thin films deposited on polycrystalline metallic substrates”, Appl. Phys. Lett. 60(1992)769.
[26] Y. Shiohara , M. Yoshizumi , T. Izumi , Y. Yamada, “Current status and prospects of national project on coated conductors in Japan” , Phys. C 463-465(2007) 1
[27] Superconductivity for Electric Systems 2004 Annual Peer Review, Texas Center for Superconductivity and Advanced Materials(TcSAM), University of Houston
[28] H.M.Manasevit, “Single-crystal gallium arsenide on insulating substrates” Appl.Phys.Let., 12(1968) 156.
[29] H.M.Manasevit, W.I.Simpson, J.Electrochem.Sco.12(1968)156
[30] H.M.Manasevit, “The use of metalorganics in the preparation of semiconductor materials: Growth on insulating substrates” , J.Cryst.Growth,13/14(1972) 306.
[31] Hiskes, R., S.A.DiCarolis, R.D.Jacowitz, Z.Lu, R.S.Feigelson, R.K.Route, and J.L.Young, “Single source MOCVD of epitaxial oxide thin films,” J.Cryst.Growth, 128(1993) 781
[32] 唐士兵 “金属有机化学气相沉积(MOCVD)前体物的制备.表征及热力学性质研究” 吉林大学化学学院本科论文 P23-26(2006)
[33]R.Singh, P.Chou, F.Radpour A.J.NeLson, H.S.Ullal “Oxidation of tin on silicon substrate by rapid isothermal processing” J.Appl.Phys.66(1989)2381
[34]R.Singh, F.Radpour P.Chou, “Comparative study of dielectric formation by furnace and rapid isothermal processing” J.Vac.Sci.Technol.A7(1989)1456
[35] R. H. Hammond , R. Bormann. “Corelation between the in situ growth conditions of YBCO thin films and the thermodynamic stability criteria” Physica C 162-164(1989)703
[36]RJ.Cava,B .Batlogg,C .H .C hen,et al . “Oxygen stoichiometry, superconductivity and normal- state properties of YBa2Cu3O7- " Natuer, 329(1987)423.
[37] Y. Xu, D. Shi, S. McClellen, et al. “Deposition of epitaxial YBCO thin film on single domain YBCO substrate for the development of RF components”, IEEE Trans. Appl. Supercond., 11(2001)2865
[38] J. Geerk, G. Linker and O. Meyer. “Epitaxial growth and properties of YBaCuO thin films” Materials Science Reports, 4(1989)No.5,6: 193
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