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6 April 1990 Processing And Patterning Of Thin Film Superconductors Formed By Metallo-Organic Deposition
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Proceedings Volume 1189, Rapid Isothermal Processing; (1990)
Event: 1989 Microelectronic Integrated Processing Conferences, 1989, Santa Clara, United States
Thin film superconductors of Y-Ba-Cu and Yb-Ba-Cu were formed by the pyrolysis of neodecanoate solutions of Y, Yb, Ba and Cu which had been deposited onto <100> SrTiO3 substrates [1]. Rapid thermal annealing, in oxygen, of the as-deposited films produced high T films having superconducting onset temperatures above 90 K and zero resistance at 8g K. Scanning Electron Microscopy (SEM) revealed enhancements in grain growth, compared to furnace annealed films, by a factor of 4. X-ray diffraction analysis showed preferred epitaxial grain growth with the c-axis of the films oriented both perpendicular and parallel to the substrate surface. Separate Rutherford Backscattering Spectrometry (RBS) channeling experiments confirmed the formation of preferred epitaxial grain growth. Film composition was determined by RBS and Inductively Coupled Plasma Emission Spectrometry (ICPES). Selective patterning was accomplished by focused beam exposure of the metal neodecanoate films [2-4]. The exposure rendered the neodecanoate film locally insoluble in xylene, thus permitting selective area patterning prior to pyrolysis. Electron, ion and laser beams were used to pattern films on <100> SrTiO3. The finest lines, approximately 5 #m in width and 26 nm thick, were patterned using electron beams whose lines had superconducting onsets above 90 K and zero resistance at 69 K after rapid thermal annealing. Both ion beam and laser patterning had similar superconducting onsets and zero resistance. Neodecanoates of Y, Yb, Ba, and Cu were formed, as previously described [5], by reacting the metal acetates of these materials with either ammonium neodecanoate or tetramethyl ammonium neodecanoate. The carboxylates formed from these reactions were then dissolved in a solution of xylene and pyridine. The individual chemical constituents were combined to produce solutions, Ln:Ba:Cu, in the ratio 1:2:4. Here, Ln is a rare-earth element. Details of the preparation of the metal carboxylates may be found elsewhere [6]. Thin films of Y-Ba-Cu and Yb-Ba-Cu were deposited onto <100> SrTiO by flooding the substrates with the appropriate neodecanoate solutions, then spin drying them at 2000 rpm for 30 s. The substrates were heated rapidly to 500°C for 5 min in an air oven to pyrolize the metallo organics to their oxides. This process produces thin films about 200 nm thick. The spin coating process was repeated 3-6 times if thicker films were desired. X-ray diffraction analysis of films pyrolized at 500°C shoed the presence of only microcrystallites. Room temperature resistivities of lx10 0-cm were measured for these films. No superconducting behavior was observed. After the 500°C pyrolysis the films were further processed by RTA in flowing oxygen. The substrates were placed upon oxidized silicon wafers, rapidly heated to 850°C for 60 s using infrared radiation produced by a bank of quartz lamps then allowed to cool to room temperature. A second rapid annealing was then performed at 920°C for 30 s in oxygen. Thin film superconductors formed in the manner described above were very uniform in structure and thickness across the surface of the film. The grains are approximately 1 #m wide and 2 #m long, a factor of 4 larger than the grains found in furnace annealed films formed by MOD [5].
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Adolph L. Micheli, Joseph V. Mantese, and Aboud H. Hamdi "Processing And Patterning Of Thin Film Superconductors Formed By Metallo-Organic Deposition", Proc. SPIE 1189, Rapid Isothermal Processing, (6 April 1990);

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