Metal organic chemical vapor deposition of superconducting YBa2Cu3O7-x thin films
The discovery of YBCO superconductors has stimulated a great deal of scientific and technological research into thin films of these materials. Because the MOCVD technique is known to produce high quality films in the III/V and II/VI material groups, our approach has been to apply the method to superconducting thin films. Thin films were grown in a vertical high speed (0–2000 rpm) rotating disk reactor. The source materials were metalβ-diketonates kept at temperatures in excess of 100° in order to obtain growth rates of 0.3 to 0.5μm/hr. The precursors were transported to the chamber with a nitrogen carrier and injected separately in order to avoid any gas phase reactions. The chamber pressure was maintained at 76 Torr with an oxygen partial pressure of 38 Torr. A resistance heater was used to keep the substrate temperature at 500° YBa2Cu3O7-x films were deposited simultaneously on a variety of substrates such as (100) MgO, (1-102) sapphire, (100) SrTiO3 and (100) YSZ. Full XPS spectra were collected for the binary oxides. The scans demonstrate the existence of Y2O3, BaO, and CuO with the correct valence state for the metallic species. Energy dispersive analysis of x-ray (EDAX) was used to determine film compositions by comparing EDAX spectral intensity to a known superconducting standard. Appropriate changes were made in the precursor flows to correct the stoichiometry. The as-grown films were dark brown and semi-transparent. Cross-sectional SEM photomicrographs revealed an ordered columnar structure. After annealing at 950–980° however, the films on (100) SrTiO3 appeared dull black and opaque. The surface morphology exhibited smooth large plate-like grains. X-ray data clearly display an orthorhombic phase, with c-axis perpendicular to the substrate surface. Four point resistance measurements for films on (100) SrTiO3 show the onset of superconductivity at 90 K with a complete loss of resistance at 88 K. This sharp (≤2K) transition shows the high quality of these MOCVD grown YBCO films and are the first reported results from a large area (2 × 50 mm substrates) commercial reactor.