Mechanochemical Defect Engineering of Nb<sub>2</sub>O<sub>5</sub>: Influence of LiBH<sub>4</sub> and NaBH<sub>4</sub> Reduction on Structure and Photocatalysis

Partial reduction of transition metal oxides via defect engineering is a promising strategy to enhance their electronic and photocatalytic properties. In this study, we systematically explored the mechanochemical reduction of Nb<sub>2</sub>O<sub>5</sub> using LiBH<sub>4...

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Bibliographic Details
Main Authors: Anna Michaely, Elias C. J. Gießelmann, Guido Kickelbick
Format: Article
Language:English
Published: MDPI AG 2025-05-01
Series:Solids
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Online Access:https://www.mdpi.com/2673-6497/6/2/26
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Summary:Partial reduction of transition metal oxides via defect engineering is a promising strategy to enhance their electronic and photocatalytic properties. In this study, we systematically explored the mechanochemical reduction of Nb<sub>2</sub>O<sub>5</sub> using LiBH<sub>4</sub> and NaBH<sub>4</sub> as reducing agents. Electron paramagnetic resonance (EPR) spectroscopy confirmed a successful partial reduction of the oxide, as seen by the presence of unpaired electrons. Interestingly, larger hydride concentrations did not necessarily enable a higher degree of reduction as large amounts of boron hydrides acted as a buffer material and thus hindered the effective transfer of mechanical energy. Powder X-ray diffraction (PXRD) and <sup>7</sup>Li solid-state NMR spectroscopy indicated the intercalation of Li<sup>+</sup> into the Nb<sub>2</sub>O<sub>5</sub> lattice. Raman spectroscopy further revealed the increased structural disorder, while optical measurements showed a decreased band gap compared with pristine Nb<sub>2</sub>O<sub>5</sub>. The partially reduced samples showed significantly enhanced photocatalytic performance for methylene blue degradation relative to the unmodified oxides.
ISSN:2673-6497