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The preparation of single crystals and bicrystals of SrTiO 3 and their surface treatment have been investigated to facilitate their application to the substrates of high-T c superconducting thin films and devices. Bicrystals with different inter-crossing angles were used to elucidate the weak-link characteristics of grain boundary junctions formed in the epitaxial YBa 2 Cu 3 O 7-δ films on the bicrystal substrates. Wet etching by pH-controlled ammonium fluoride solutions enabled us to finish SrTiO 3 surfaces with atomically defined step-and-terrace structures. Atomically controlled two-dimensional layer-by-layer epitaxial growth was achieved by laser molecular beam epitaxy of oxide films on this atomically regulated surface.