Method for producing an active layer of an electrode for electrochemical reduction reactions

A process for the preparation of a catalytic material of an electrode for electrochemical reduction reactions, said material comprising an active phase based on at least one metal from group VIb and an electroconductive support, which process is carried out according to at least the following stages:

• a) a stage of bringing said support into contact with at least one solution containing at least one precursor of at least one metal from group VIb;
• b) optionally a stage of bringing the support into contact with an organic additive, it being understood that stage b) is obligatory when said precursor of at least one metal from group VIb according to stage a) is chosen from polyoxometallates corresponding to the formula (HhXxMmOy)q− in which H is hydrogen, X is an element chosen from phosphorus (P), silicon (Si), boron (B), nickel (Ni) and cobalt (Co), M is one or more metal(s) chosen from molybdenum (Mo), tungsten (W), nickel (Ni), cobalt (Co) and iron (Fe), 0 being oxygen, h being an integer between 0 and 12, x=0, m being an integer equal to 5, 6, 7, 8, 9, 10, 11, 12 and 18, y being an integer between 17 and 72 and q being an integer between 1 and 20, it being understood that M is not a nickel atom, a cobalt atom or an iron atom alone.
• stages 1) and 2), if both carried out, being carried out in any order or simultaneously;
• c) a drying stage on conclusion of stage a), optionally of the sequence of stages a) and b) or b) and a), at a temperature of less than 250° C., without a subsequent calcination stage;
• d) a stage of sulfurization of the material obtained on conclusion of stage c) at a temperature of between 100° C. and 600° C.