Phase-pure spinel
Ni2FeS4 nanosheets with
a specific surface area of 80 m2 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 X-ray
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.