In this paper, we propose a facile
and efficient strategy for synthesizing mesoporous BaSnO<sub>3</sub> with a surface area as large as 67 m<sup>2</sup>/g using a peroxo-precursor
decomposition procedure. As far as we know, this is the largest surface
area reported in literature for BaSnO<sub>3</sub> materials and may
have a potential to greatly promote the technological applications
of this kind of functional material in the area of chemical sensors,
NO<sub><i>x</i></sub> storage, and dye-sensitized solar
cells. The structure evolution of the mesoporous BaSnO<sub>3</sub> from the precursor was followed using a series of techniques. Infrared
analysis indicates large amount of protons and peroxo ligands are
contained in the peroxo-precursor. Although the crystal structure
of the precursor appears cubic according to the analysis of X-ray
diffraction data, Raman and Mössbauer spectroscopy results
show that the Sn atom is offset from the center of [SnO<sub>6</sub>] octahedron. After calcination at different temperatures, the precursor
gradually transforms into BaSnO<sub>3</sub> by release of water and
oxygen, and the distortion degree of [SnO<sub>6</sub>] octahedral
decreases. However, a number of oxygen vacancies are generated in
the calcined samples, which are further confirmed by the physical
property measurement system, and they would lower the local symmetry
to some content. The concentration of the oxygen vacancies reduces
simultaneously as the calcination temperature increases, and their
contributions to the total heat capacity of the sample are calculated
based on theoretical analysis of heat capacity data in the temperature
region below 10 K