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Molybdenum carbide (β-Mo 2 C) supported on carbon spheres was prepared via a carbothermal hydrogen reduction (CHR) method from delaminated nanosheets of molybdenum(vi) oxide (d-MoO 3 /C). The carburization process was followed by combined in situ XANES/XRD analysis revealing the formation of molybdenum oxycarbide Mo 2 C x O y as an intermediate phase during the transformation of d-MoO 3 /C to β-Mo 2 C/C. It was found that Mo 2 C x O y could not be completely carburized to β-Mo 2 C under a He atmosphere at 750 °C, instead a reduction in H 2 is required. The β-Mo 2 C/C obtained showed activity and stability for the dry reforming of methane at 800 °C and 8 bar. In situ XANES/XRD evaluation of the catalyst under DRM reaction conditions combined with high resolution TEM analysis revealed the evolution of β-Mo 2 C/C to Mo 2 C x O y /C. Notably, the gradual oxidation of β-Mo 2 C/C to Mo 2 C x O y /C correlates directly with the increased activity of the competing reverse water gas shift reaction.

nanoscale

Molybdenum carbide and oxycarbide from carbon-supported MoO<sub>3</sub> nanosheets: phase evolution and DRM catalytic activity assessed by TEM and <i>in situ</i> XANES/XRD methods

Molybdenum carbide and oxycarbide from carbon-supported MoO3 nanosheets: phase evolution and DRM catalytic activity assessed by TEM and in situ XANES/XRD methods

Molybdenum carbide and oxycarbide from carbon-supported MoO₃ nanosheets: phase evolution and DRM catalytic activity assessed by TEM and in situ XANES/XRD methods