Study on hydrogen reduction mechanism of MoO3 using Ti–Mo core–shell powder

In this study, the hydrogen reduction mechanism of MoO3 was analyzed in detail using Ti–Mo core–shell powder manufactured through a milling and reduction process. MoO3 and Ti powders were ball-milled to refine the MoO3 powder and coat it onto the Ti powder to fabricated core-shell structure. Subsequently, the milled powder was heat-treated at 600°C in a hydrogen atmosphere to reduce MoO3 to nano-sized Mo. In addition, the reduction behavior of MoO3 was analyzed by varing the reduction times to 1, 10, 30 min and 1, 3, 5 h. Phase analysis was conducted using X-ray diffraction, and oxidation state analysis was conducted using X-ray photoelectron spectroscopy. Morphology analysis was performed using scanning electron microscopy, and elemental analysis was conducted using electron probe micro-analysis. It was confirmed that Mo9O26 and Mo4O11 intermediate phases were formed sequentially as MoO3 was reduced to MoO2, and Mo9O26 had a plate shape with a thickness of sub-70 nm, and Mo4O11 exhibited a thickness of sub-300 nm. Especially, the Mo2O3 intermediate phase, previously studied only theoretically, was experimentally confirmed for the first time in the reduction process from MoO2 to Mo. Furthermore, the analysis of Mo-oxide intermediate phases was explained by the structural characteristics of the core–shell. The shell of Mo oxide was thick and dense, making it difficult for the vapor phase necessary for CVT reduction to penetrate and diffuse into the shell. As a result, the rapid CVT reduction occurred outside the shell, while relatively slower reduction occurred inside the shell where intermediate phases were observed.