Low-temperature synthesis of HfC/HfO2 nanocomposites from a commercial single-source precursor

A liquid-phase polymer-to-ceramic approach is reported for the synthesis of hafnium carbide (HfC)/hafnium oxide (HfO₂) composite particles from a commercial precursor. Typically, HfC ceramics have been obtained by sintering of fine powders, which usually results in large particle size and high porosity during densification. In this study a single-source liquid precursor was first cured at low temperature and then pyrolyzed at varying conditions to achieve HfC ceramics. The chemical structure of the liquid and cured precursors, and the resulting HfC ceramics was studied using various analytical techniques. The nuclear magnetic resonance and Fourier transform infrared spectroscopy indicated the presence of partially hydrated hafnium oxychloride (Hf–O–Cl·nH₂O) in the precursor. Scanning electron microscopy of the resulting HfC crystals showed a size distribution in the range of approx. 600–700 nm. The X-ray diffraction of the pyrolyzed samples confirmed the formation of crystalline HfC along with monoclinic-HfO₂ and free carbon phase. The formation of HfO₂ in the ceramics was significantly reduced by controlling the low-temperature curing temperature. Pyrolysis at various temperatures showed that HfC formation occurred even at 1000°C. These results show that the reported precursor could be promising for the direct synthesis of ultrahigh temperature HfC ceramics and for precursor infiltration pyrolysis of reinforced ceramic matrix composites.