The Deposition of Smooth Metallic Molybdenum from Aqueous Electrolytes Containing Molybdate Ions

"This paper details the electrodeposition of metallic molybdenum from an aqueous, acetateelectrolyte containing molybdate ions. The deposition is carried out in a highly concentrated (up to I 0 M) acetate bath in the presence of a very low concentration of bone glue (60 µg/L). The molybdenum metal deposits are up to 20 µm thick and adherent. The deposits were characterized by XRD and XPS analysis. The deposition process is very inefficient, as up to 99% of the current is used to generate hydrogen during electrolysis. The effect of acetate concentration, pH, additives and current on the deposition efficiency and physical properties of the molybdenum deposit were investigated and optimized to obtain smooth, adherent coatings.IntroductionMolybdenum has increased thermal and wear resistance properties that are often utilized in material coatings [I]. These coatings are most often manufactured by sintering, pressing or spraying molybdenum powder at elevated temperatures, as a substitute method for standard metallurgical practices, such as electroplating [2, 3]. The lack of reports describing molybdenum deposition is most likely due to the highly oxophilic nature of molybdenum and the stability of its oxides, especially in water. Previous attempts to electrochemically reduce molybdenum from molybdate (Mool·) ions to molybdenum metal have reported the production of either a poorly adherent mixed oxide [4-6], or a thin(< 0.1 µm) metallic film [7-9]. Thick metallic molybdenum is capable of being co-deposited with one of the iron-group metals (Ni [10], Co [11] and Fe [12]) to produce an alloy [13, 14]. These alloys, however, may not be suitable for applications requiring pure molybdenum as they usually contain less than 50% molybdenum (often less than 30%)."