Zirconium carbide, hafnium carbide and their ternary carbide nanoparticles by an in situ polymerization route

Abstract

An in situ polymerizable complex method to produce zirconium carbide, hafnium carbide and their ternary carbides at a relatively low temperature (1300 °C) using simple and mainly nontoxic starting reagents is presented. In this aqueous process, citric acid (CA) was used to chelate the metal ion and ethylene glycol (EG) to form a polymerized complex resin. We suggest that, based on the results of FT-IR and ¹³C NMR spectroscopies, a very stable metal–CA chelate complex formed in the starting solution, which was thermally stable upon gelation even up to 350 °C. Immobilization of the metal ion in a rigid polymer can largely guarantee the in situ charring, resulting in carbon adjacent to the metal oxide in the pyrolysed product. The contiguous carbon and metal oxide led to in situ reaction (1100 °C) with a minimum of diffusion, which involved the formation of large numbers of metastable phases. Afterwards, well-defined binary and ternary carbide nanoparticles (∼100 nm) were formed through localized particle coarsening by Ostwald ripening.