Due to the high temperature at combustion moment, the combustive reduction of MoO3 by Zn is normally accompanied with a great deal of zinc vaporization and the formation of undesired compound, Zn2Mo3O8. Experimental results showed that there was about 23 wt.% Zn loss at the combustion moment as a result of temperature rising. In the present research, preliminary mechanical activation was employed to control Zn loss during the combustion. It was shown that the decrease in zinc loss is associated with the intensity of structural disorder generated during mechanical milling. Zinc loss was calculated to be about 4 wt.% as the pre-milling time increased up to 30 min. X-ray diffraction, electron microscopic images (SEM and TEM), EDS mapping, and differential scanning calorimetry were used in this research to study the synthesis process. TEM results revealed that synthesized Mo particles were nanosized and under 50 nm on average.

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