Fast Microwave Synthesis of Phase-Pure Ni2FeS4 Thiospinel Nanosheets for Application in Electrochemical CO2 Reduction

Phase-pure spinel Ni2FeS4 nanosheets with a specific surface area of 80 m(2) g(-1) were successfully prepared via fast and energy-saving microwave-assisted nonaqueous sol-gel synthesis, starting from metal acetylacetonates and benzyl mercaptan as the sulfur source. Synthesized nanosheets were characterized thoroughly by X-ray diffraction including Rietveld refinement, X-ray photoelectron spectroscopy, energy-dispersive Xray spectroscopy, electron microscopy, nitrogen and water vapor physisorption measurements, and thermogravimetric analysis coupled with mass spectrometry. Such noble metal free Ni2FeS4 nanosheets were successfully applied as electrocatalyst for the aqueous carbon dioxide reduction reaction, yielding selectively the syngas components hydrogen and carbon monoxide.

Automated summary

Phase-pure spinel Ni2FeS4 nanosheets with specific surface area of 80 m²/g were successfully prepared via fast and energy-saving microwave-assisted nonaqueous sol-gel synthesis. These nanosheets were applied as electrocatalyst for aqueous carbon dioxide reduction reaction, selectively yielding syngas components hydrogen and carbon monoxide.