The molybdenum bimetallic interstitial carbides Fe3Mo3C and Co3Mo3C have been synthesized by temperature-programmed reaction (TPR) between the molybdenum bimetallic interstitial nitrides Fe3Mo3N and Co3Mo3N and a flowing mixture of CH4 and H2 diluted in Ar. These compounds have been characterized by X-ray diffraction, laser Raman spectroscopy, elemental analysis, energy dispersive analysis of X rays, thermal analysis (in air) and scanning electron microscopy (field emission). Their structures have been refined from X-ray powder diffraction data. These carbides crystallize in the cubic system, space group Fd
m
[a
= 11.11376(6) and 11.0697(3)
Å for Fe and Co compounds, respectively].
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