Metal molybdate (AMoO4; Ca and Ba) fine particles were synthesized successfully in a simple way using the mechanochemical method under ambient conditions, without surfactants or any capping agents. The effect of milling time on phase formation and morphology was investigated. The functional group and phase formation analyses were carried out using Fourier transform infrared (FT-IR), Raman spectroscopy and X-ray diffraction (XRD) methods. XRD revealed that all samples were of a pure tetragonal scheelite structure. FT-IR and Raman analysis exhibited a Mo-O stretching peak of molecular [MoO4]2-, which related to the scheelite structure. Difference in growth mechanism and morphology was observed significantly in CaMoO4 and BaMoO4 particles. The primary CaMoO4 nanocrystalline was formed in its initial state at 80–100nm, and tended to aggregate into a peach-like shaped morphology with increasing milling time, while a space shuttle-like morphology formed directly via an oriented attachment mechanism for the BaMoO4 particle. A possible mechanism for the formation of metal molybdate, with a different milling time, was discussed in detail. It is interesting that this work was able to present a simple way of synthesizing complex oxide materials on a large scale.
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