Fabrication of nonstoichiometric metal oxides containing oxygen vacancies (OVs) has been an effective strategy to modulate their (photo)catalytic or (photo)electrochemical performances which are all affected by charge transfer at the interface and in the bulk. Considerable efforts are still needed to achieve tunability of OVs, as well as their quantitative characterization. Herein, a one‐step flame synthesis method is reported for the first time for fast fabrication of blue TiO2−x with controllable defect content and location. Temperature‐programmed oxidation (TPO) analysis is applied for the first time and found to be an excellent technique in both differentiating and quantifying OVs at the surface, grain boundary (GB), and bulk of TiO2−x. The results indicate that a moderate level of OVs can greatly enhance the charge transfer. Importantly, the OVs locked at GBs due to the thermal sintering of nanoparticles during the synthesis can facilitate the anchoring and reduction of Pt species.
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