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Schaffer, Berhnard
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article
On the origin of nanochessboard superlattices in a-site-deficient ca-stabilized Nd2/3TiO3
Abstract
<p>A-site deficient Nd<sub>2/3</sub>TiO<sub>3</sub> ceramics stabilized with CaTiO<sub>3</sub>, with an overall composition of 0.9 Nd<sub>2/3</sub>TiO<sub>3</sub>-0.1 CaTiO<sub>3</sub>, were synthesized by the mixed oxide route. Synchrotron X-ray diffraction was used to identify the basic perovskite structure and revealed cross-type superlattice reflections. An incommensurate superlattice structure with dimensions of a ≈ b ≈ 20a<sub>p</sub> and c = 2a<sub>p</sub> (where a<sub>p</sub> is the cell parameter for the parent perovskite phase) was identified, giving rise to contrast features resembling a nanochessboard pattern in electron microscopy images. The superlattice was further characterized by aberration-corrected scanning transmission electron microscopy (STEM): atomically resolved lattice images were obtained along «100» orientations to visualize the A-site (Ca, Nd, and vacancies) and B-site (Ti) cation column intensities, in correlation with observations of the nanochessboard superlattice. Electron energy loss spectroscopy (EELS) was used to precisely determine the distribution of Nd and Ca across the structure, confirming the absence of long-range elemental segregation or phase separation across the nanochessboard superstructure. Closer inspection of the chemical maps in two orthogonal directions, however, suggests the presence of localized ordering of cations and vacancies. The chessboard pattern superlattice is thus likely to be caused by periodic octahedral tilt distortions of the O sublattice, possibly induced by these short-range chemical variations, as a result of a complex interplay between cation and vacancy ordering in three dimensions.</p>