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As such they have the potential to revolutionize renewable energy production on Earth. While proven efficiencies have reached 1.1%, further improvements of photocatalyst technology depend on a better understanding of energy loss mechanisms on the individual particle level. Here, we conduct the first <jats:italic>in operando<\/jats:italic> photoelectrochemical measurements on individual micrometer\u2010sized Al\u2010doped SrTiO<jats:sub>3<\/jats:sub>\/Rh<jats:sub>2\u2013y<\/jats:sub>Cr<jats:sub>y<\/jats:sub>O<jats:sub>3<\/jats:sub> photocatalyst particles. We find that the photocatalyst particles behave mainly as water oxidation photoanodes reaching up to 0.5\u00a0mA cm<jats:sup>\u22122<\/jats:sup> at 0.8\u00a0V versus RHE and a photovoltage of \u223c1.00 V under 4.7\u00a0mW cm<jats:sup>\u22122<\/jats:sup> ultraviolet illumination. This proves that charge separation in the unbiased Al:SrTiO<jats:sub>3<\/jats:sub>\/Rh<jats:sub>2\u2013y<\/jats:sub>Cr<jats:sub>y<\/jats:sub>O<jats:sub>3<\/jats:sub> catalyst is driven by a junction at the n\u2010semiconductor\u2010liquid contact. While O<jats:sub>2<\/jats:sub> is detected symmetrically around photocatalyst particles, uneven H<jats:sub>2<\/jats:sub> evolution profiles reflect an irregular Rh<jats:sub>2\u2013y<\/jats:sub>Cr<jats:sub>y<\/jats:sub>O<jats:sub>3<\/jats:sub> cocatalyst distribution. Additionally, the H<jats:sub>2<\/jats:sub> evolution activity varies significantly between different photocatalyst particles. This suggests that performance gains are possible by better controlling catalyst composition on the microscale.<\/jats:p>","DOI":"10.1002\/anie.202516520","type":"journal-article","created":{"date-parts":[[2025,8,26]],"date-time":"2025-08-26T05:26:02Z","timestamp":1756185962000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":7,"title":["Probing Photoelectrochemical Hydrogen and Oxygen Evolution at Individual Al:SrTiO<sub>3<\/sub>\/Rh<sub>2\u2013y<\/sub>Cr<sub>y<\/sub>O<sub>3<\/sub> Photocatalyst Particles"],"prefix":"10.1002","volume":"64","author":[{"given":"Gaukhar","family":"Askarova","sequence":"first","affiliation":[{"name":"Department of Chemistry and Biochemistry Queens College  Flushing CUNY NY 11367 USA"},{"name":"The Graduate Center of CUNY  New York NY 10016 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chengcan","family":"Xiao","sequence":"additional","affiliation":[{"name":"Department of 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