The co-ammonolysis of V(NMe) and Si(NHMe) with ammonia in THF and in the presence of ammonium triflate ([NH][CFSO]) leads to the formation of monolithic gels. Pyrolysing these gels produces mesoporous composite materials containing nanocrystalline VN and amorphous silicon imidonitride. Elemental mapping indicated a thorough distribution of VN with no evidence of large cluster segregation. Whilst not active for ammonia synthesis, the silicon nitride based materials were found to possess activity for the CO-free production of H from methane, which makes them candidates for applications in which the presence of low levels of CO in H feedstreams is detrimental.
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