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We demonstrate a low-temperature reduction method for exhibiting fine control over the oxidation state of substitutional Mn ions in strontium titanate (SrTiO 3 ) bulk powder. We employ NaBH 4  as the chemical reductant that causes significant changes in the oxidation state and oxygen vacancy complexation with Mn 2+  dopants at temperatures <350°C where lattice reduction is negligible. At higher reduction temperatures, we also observe the formation of Ti 3+  in the lattice by diffuse-reflectance and low-temperature electron paramagnetic resonance (EPR) spectroscopy. In addition to Mn 2+ , Mn 4+ , and the Mn 2+  complex with an oxygen vacancy, we also observe a sharp resonance in the EPR spectrum of heavily reduced Mn-doped SrTiO 3 . This sharp signal is tentatively assigned to surface superoxide ion that is formed by the surface electron transfer reaction between Ti 3+  and O 2 . The ability to control the relative amounts of various paramagnetic defects in SrTiO 3  provides many possibilities to study in a model system the impact of tunable dopant-defect interactions for spin-based electronic applications or visible-light photocatalysis.

Reversible Control of the Mn Oxidation State in SrTiO3 Bulk Powders