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Organic semiconductors have now joined the quorum of materials currently dominated by inorganic oxides, where for both families of compounds the bandgaps and energies can be adjusted synthetically to perform the Water Splitting Reaction. However, elaborated and tedious synthetic pathways are necessary to optimize the photophysical properties of organic semiconductors. This study reports here, that when pyrrole dissolved distilled water is exposed to high energy radiation, this leads to the formation of nanostructured spherical polypyrrole (Nano\u2010PPy) particles that are characterized as overoxidized polypyrrole. Electrochemical studies and Tauc's plot highlight the production of a semiconducting material with a bandgap of \u22481.8\u00a0eV with the conduction band at \u2248\u22120.5\u00a0V and a valence band at \u2248+1.3\u00a0V vs NHE. When suspended in water and under irradiation at wavelengths higher than 420\u00a0nm, Nano\u2010PPy materials lead to O<jats:sub>2<\/jats:sub> evolution, while electrons and protons can be recovered in the form of reduced quinone. Interestingly, upon intermittent visible irradiation and dark phases, a consumption of the evolved O<jats:sub>2<\/jats:sub> from oxidation of water is observed. This concomitant O<jats:sub>2<\/jats:sub> reduction is found to produce H<jats:sub>2<\/jats:sub>O<jats:sub>2<\/jats:sub>.<\/jats:p>","DOI":"10.1002\/smll.202407364","type":"journal-article","created":{"date-parts":[[2025,1,24]],"date-time":"2025-01-24T08:27:09Z","timestamp":1737707229000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":4,"title":["Semiconducting Overoxidized Polypyrrole Nano\u2010Particles for Photocatalytic Water Splitting"],"prefix":"10.1002","volume":"21","author":[{"given":"Xiaojiao","family":"Yuan","sequence":"first","affiliation":[{"name":"UMR 8000 CNRS Institut de Chimie Physique Universit\u00e9 Paris\u2010Saclay  Orsay 91405 France"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Girlie Eunice","family":"Lopez","sequence":"additional","affiliation":[{"name":"UMR 8000 CNRS Institut de Chimie Physique Universit\u00e9 Paris\u2010Saclay  Orsay 91405 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