UV to IR Continuous Photocatalytic Gas‐Phase CO2 Hydrogenation Over Ni‐Doped Molybdenum Oxysulfide: An Experimental and Mechanistic Study

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Abstract
The reduction of CO2 toward CO and CH4 over Ni‐loaded MoS2‐like layered nanomaterials is investigated. The mild hydrothermal synthesis induced the formation of a molybdenum oxysulfide (MoOxSy) phase, enriched with sulfur defects and multiple Mo oxidation states that favor the insertion of Ni2+ cations via photo‐assisted precipitation. The photocatalytic tests under LED irradiation at different wavelengths from 365 to 940 nm at 250°C rendered 1% CO2 conversion and continuous CO production up to 0.6 mmol/(gcat h). The incorporation of Ni into the MoOxSy structure boosted the continuous production of CO up to 5.1 mmol/(gcat h) with a CO2 conversion of 3.5%. In situ spectroscopic techniques and DFT simulations showed the O‐incorporated MoS2 structure, in addition to Ni clusters as a supported metal catalyst. The mechanistic study of the CO2 reduction reaction over the catalysts revealed that the reverse water–gas shift reaction is favored due to the preferential formation of carboxylic species.

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