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The solid-state synthesis and structural characterisation of perovskite BaSn 1- x  Sc  x  O 3- δ  ( x = 0.0, 0.1, 0.2, 0.3, 0.4) and its corresponding hydrated ceramics are reported. Powder and neutron X-ray diffractions reveal the presence of cubic perovskites (space group Pm 3 m ) with an increasing cell parameter as a function of scandium concentration along with some indication of phase segregation. 119 Sn and 45 Sc solid-state NMR spectroscopy data highlight the existence of oxygen vacancies in the dry materials, and their filling upon hydrothermal treatment with D 2 O. It also indicates that the Sn 4+ and Sc 3+ local distribution at the B-site of the perovskite is inhomogeneous and suggests that the oxygen vacancies are located in the scandium dopant coordination shell at low concentrations ( x ≤ 0.2) and in the tin coordination shell at high concentrations ( x ≥ 0.3). 17 O NMR spectra on 17 O enriched BaSn 1- x  Sc  x  O 3- δ  materials show the existence of Sn-O-Sn, Sn-O-Sc and Sc-O-Sc bridging oxygen environments. A further room temperature neutron powder diffraction study on deuterated BaSn 0.6 Sc 0.4 O 3- δ  refines the deuteron position at the 24k crystallographic site ( x , y , 0) with x = 0.579(3) and y = 0.217(3) which leads to an O-D bond distance of 0.96(1) Å and suggests tilting of the proton towards the next nearest oxygen. Proton conduction was found to dominate in wet argon below 700 °C with total conductivity values in the range 1.8 × 10 -4 to 1.1 × 10 -3 S cm -1 between 300 and 600 °C. Electron holes govern the conduction process in dry oxidizing conditions, whilst in wet oxygen they compete with protonic defects leading to a wide mixed conduction region in the 200 to 600 °C temperature region, and a suppression of the conductivity at higher temperature.

journal of materials chemistry. a

Crystal structure and proton conductivity of BaSn0.6Sc0.4O3−δ: insights from neutron powder diffraction and solid-state NMR spectroscopy