In literature they 1st deposited CuFe2 alloy at 2mA current in Ethylene Glycol which was followed by anodization into CuFe2O4 in 1N KOH. But anodic potential is not given. And will I use 2 electrode system in 1st step?
You can use two electrode set up in both the cases. Please note that ethylene glycol (EG) will have a low electrical conductivity and therefore the potential drop will be large. Since you are going to deposit under galvanostatic condition, it may not be a problem. Place your anode closer to the cathode substrate and make sure that the electric field will be uniform. Three electrode set up with potentiostatic or pulsed potential may give a better control over the stoichiometry of the deposit. But, with EG solution this is not easy. You may have to add a little bit of water for better solubility of the copper and iron precursors. EG is used to avoid unwanted hydrogen evolution during the electrodeposition that is normally encountered using aqueous solutions. However, EG does not dissolve the salts that easily.
You can anodize the deposit either under potentiostatic or galvanostatic condition. You may need a potential larger than + 2.5 V in pH 14. Larger the potential faster will be the oxidation rate, and also the oxygen evolution rate. You can also apply a constant current density of +2 mA/cm2 for anodization.
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