O. Solorzaferia et al., NOVEL LOW-TEMPERATURE SYNTHESIS OF SEMICONDUCTING TRANSITION-METAL CHALCOGENIDE ELECTROCATALYST FOR MULTIELECTRON CHARGE-TRANSFER - MOLECULAR-OXYGEN REDUCTION, Electrochimica acta, 39(11-12), 1994, pp. 1647-1653
Powder and thin layers (<0.5 mu m) of transition metal chalcogenide de
posited on various substrates (glass, gc, ito) were synthesized at 140
degrees C. The catalyst compound was obtained when reacting the corre
sponding transition metal carbonyl compounds and elemental selenium in
xylene solvent. Efficient reduction of molecular oxygen to water, in
0.5 M H2SO4 electrolyte, was obtained. This catalyst also showed semic
onducting behaviour. XPS-analysis and those results gained by Rutherfo
rd backscattering spectrometry (RBS) revealed that oxygen is incorpora
ted in this compound. Transmission electron microscopy (TEM) performed
on thin layers deposited on conducting glass or glassy carbon electro
des consisted of amorphous regions and nanocrystal domains with partic
le sizes ranging from 30 to 40 Angstrom. The probable stoichiometry of
the semiconducting catalyst compound resulted to be: (Ru1-xMox)(y)SeO
z where 0.02 < x < 0.04; 1 < y < 3 and z approximate to 2y after data
analysis obtained with XPS, RBS and TEM.