A series of zirconia-supported molybdenum oxide catalysts with different mo
lybdenum loadings prepared using conditions reported to generate "superacid
ity" have been evaluated for their performance as catalysts for methane oxi
dation. A marked dependence of Mo content on activity has been observed, wi
th the most active material being that with intermediate molybdenum content
. 5 wt% MoO3/ZrO2 compares favourably with ZrxCe1-xO2 for methane combustio
n. The presence of MoO3 is observed to stabilise the tetragonal polymorph o
f ZrO2 and, as Mo content is increased, dispersed MoO3 crystallites are for
med as evidenced by Raman spectroscopy. Temperature-programmed reduction st
udies evidence differences in the reduction behaviour of the materials as a
function of loading. The results indicate that molybdenum oxide supported
on monoclinic zirconia gives rise to the most active catalyst. It is tentat
ively suggested that the formation of a MoO3 monolayer during reaction may
be of importance.