Transition metal carbide precursors have been made in the past by the reaction of alkoxides with polymeric materials to form gels and resins. A new route to transition metal carbide precursors has been developed using alkoxides polymerized with dicarboxylic acids. (Dicarboxylic acid precursors have the advantage of precipitating as powders that can be removed from solvents by filtration and that are not very air sensitive.) Precursors were pyrolyzed under inert or reducing conditions to form metal carbides.
The choice of ligand(s) determined the carbon content after pyrolysis. Unsaturated ligands tended to increase carbon content. Materials from oils to fine powders were produced by varying the stereochemistry of the ligands. The morphology of the pyrolyzed product mimicked that of the precipitated powder. Pyrolysis was typically carried out under Ar/H2 at 1200–1600°C. X-ray diffraction (XRD) was used to follow the incorporation of carbon into the lattice.