Two-electron oxygen reduction reaction (2e⁻ ORR) to produce hydrogen peroxide (H₂O₂) presents an efficient, secure, and sustainable method. However, the competing four-electron pathway produces H₂O, yielding low H₂O₂ selectivity (~ 70%). In this work, a high-dimensional rod-like structure of niobium oxide (Nb₂O₅-HD) containing NbO₆ octahedra was synthesized using a hydrothermal method combined with a calcination strategy. Under 50 mA·cm⁻², the Faradaic efficiency (FE) of H₂O₂ reached 94%, with the H₂O₂ yield reaching as high as 874 mmol·g_cat⁻¹·h⁻¹. After 34 h of operation, FE was still 76%, and the stability is great. In situ Raman spectroscopy analysis and experiments revealed that the NbO₆ octahedra on Nb₂O₅-HD were the key factor for its excellent ORR activity and H₂O₂ FE. This inspires the development of high-performance ORR transition metal electrocatalysts.

Converting methanol to high-value formate through electrochemical methods can significantly reduce the energy consumption associated with conventional production processes. In this study, we directly synthesized iron-doped cobalt phosphate (Fe-CoPO) on nickel foam (NF) to achieve excellent activity for the methanol electro-oxidation reaction (MOR). Our results demonstrated that Fe-CoPO produced a current density of 100 mA·cm⁻² at a significantly low operating potential of 1.436 V (vs. reversible hydrogen electrode (RHE)) and operated steadily for 16 h at this current density with a Faradaic efficiency (FE) of 97%. Furthermore, Fe-CoPO maintained a high FE of 100% even at an extremely high current density of 300 mA·cm⁻² for 8 h. We found that the high MOR activity of Fe-CoPO results from electrochemical reconstruction to generate the Co^2+/3+–O bond. The heterogeneous interface between Fe and Co inhibits the formation of Co⁴⁺, which significantly enhances the MOR activity. Thus, this work not only provides insights into the mechanism of MOR over Co-based catalysts but also offers a novel direction for developing highly active MOR catalysts.