Oxidation and reduction behavior of Ni and NiO layers sputter deposited onto yttrium-stabilized zirconia single crystals

Thin single-crystal yttrium-stabilized zirconia (YSZ) substrate was prepared by indentation fracture and mechanical polishing. The specimen was analyzed in detail by transmission electron microscopy (TEM). The (110) edge surface was faceted, in contrast to the smooth (001) edge surface, and the facet surfaces were identified as {111}-type planes. Good cross-sectional TEM specimens comprised of crystalline Ni and NiO layers deposited on YSZ edge surface could be prepared by sputtering of a Ni support grid using Ar+ ion milling and subsequent re-deposiotion on the smooth (001) fracture surface of the YSZ specimen. The epitaxial growth of a pure Ni layer on the YSZ edge planes occurred during ion milling in vacuum. However, subsequent ion milling of the specimen after exposure in air for several minutes resulted in the formation of a NiO layer on top of the first Ni layer. Reduction of the NiO layer was confirmed by electron energy-loss spectroscopy after annealing at 973 K in a vacuum of 1.2 × 10−5 Pa. This Ni layer was re-oxidized upon annealing in air at 1073 K for 1 h. The deposition behavior of the Ni and NiO layers was discussed on the basis of the surface oxidation of Ni layer.