We have tried synthesis of molybdenum hydroxide using MoCl5 aqueous water solution by simple electrodeposition on nickel foam as negative or working electrode. After deposition we got brown/black product on nickel foam. Since material is amorphous (checked XRD), we are not able to find its form (Mo(OH)2 or Mo(OH)4). please guide us and provide some references to investigate the deposited product. Thank you so much.
Dear Umesh T. Nakate thanks for sharing this very interesting chemical prpblem with the RG community. Unfortunately it is not easy for me to give you a really qualified answer. In any case your electrodeposition reaction to form molybdenum hydroxides seems problematic to me. The first problem is, that MoCl5 is certainly not a suitable as precursor for this experiment. MoCl5 is known to be highly hygroscopic. It decomposes rapidly in contact with water under formation of oxychlorides and ill-defined hydrolysis products. Yet another problem is that molybdenum hydroxides are not just simple molecular compounds such as Mo(OH)5, Mo(OH)4, or Mo(OH)2. To the best of my knowledge, the compound Mo(OH)5 does not exist at all. Instead, they should be formulated as hydrated oxides. In the lower oxidation states (+2, +3), they can also form complicated cluster molecules. I think you should better skip the MoCl5 and try more stable and water-soluble precursors such as ammonium molybdate. For a potentially useful literature reference please have a look at the following article:
Electrodeposition of molybdenum oxides from weakly alkaline ammonia-molybdate electrolytes
http://www.bcc.bas.bg/bcc_volumes/Volume_43_Number_1_2011/Volume_43_Number_1_2011_PDF/2011-43-1_9.pdf
(please see attached pdf file)
I hope this helps. Good luck with your work and best wishes, Frank Edelmann
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