doi:10.1039/d1na00021gengSanz-Marco, ArturoHueso, José L.Sebastián, VíctorNielsen, DavidMossin, SusanneHolgado, Juan P.Bueno-Alejo, Carlos J.Balas, FranciscoSantamaría, JesúsLED-driven controlled deposition of Ni onto TiO2 for visible-light expanded conversion of carbon dioxide into C1-C2 alkanesART-2021-125873Photocatalytic gas-phase hydrogenation of CO2into alkanes was achieved over TiO2-supported Ni nanoparticles under LED irradiation at 365 nm, 460 nm and white light. The photocatalysts were prepared using photo-assisted deposition of Ni salts under LED irradiation at 365 nm onto TiO2P25 nanoparticles in methanol as a hole scavenger. This procedure yielded 2 nm Ni particles decorating the surface of TiO2with a nickel mass content of about 2%. Before the photocatalytic runs, Ni/TiO2was submitted to thermal reduction at 400 °C in a 10% H2atmosphere which induced O-defective TiO2-xsubstrates. The formation of oxygen vacancies, Ti3+centers and metallic Ni sites upon photocatalytic CO2hydrogenation was confirmed byoperandoEPR analysis.In situXPS under reaction conditions suggested a strong metal-support interaction and the co-existence of zero and divalent Ni states. These photoactive species enhanced the photo-assisted reduction of CO2below 300 °C to yield CO, CH4and C2H6as final products.2021http://zaguan.unizar.es/record/15064110.1039/d1na00021ghttp://zaguan.unizar.es/record/150641oai:zaguan.unizar.es:150641info:eu-repo/grantAgreement/ES/MICINN/CTQ2016-77144-RNanoscale Advances 3, 13 (2021), 3788-3798byhttps://creativecommons.org/licenses/by/4.0/deed.esinfo:eu-repo/semantics/openAccess