Synthesis and Characterization of High-Purity, High-Entropy Diboride Ceramic Powders by a Liquid Phase Method

A nano-dual-phase powder with ultra-fine grain size was synthesized by the liquid precursor method at 1200 °C. A series of single-phase high-entropy ceramic powders ((Ti, Zr, Hf, Nb)B₂, (Ti, Zr, Hf, Nb, Ta)B₂, (Ti, Zr, Hf, Nb, Mo)B₂, (Ti, Zr, Hf, Nb, Ta, Mo)B₂) with high purity (C content less than 0.9 wt% and O content less than 0.7 wt%) and ultrafine (average grain sizes of 340-570 nm) were successfully synthesized at 1800 °C. The sample of (TiZrHfNbTa)B₂ exhibited a hexagonal close-packed (HCP) structure, and the metal elements were uniformly distributed at the nanoscale, microscale, and macroscale. This method did not apply to the preparation of all high-entropy ceramic powders and was unfavorable for the formation of single-phase high-entropy borides when the size difference factor exceeded 3.9%. The present work provides a guide for the development of ceramic-based composites through precursor impregnation pyrolysis.