Solution‐Based Synthesis of Submicrometer ZrB ₂ and ZrB ₂ –TaB ₂

Zirconium diboride and a zirconium diboride/tantalum diboride mixture were synthesized by solution‐based processing. Zirconium n ‐propoxide was refluxed with 2,4‐pentanedione to form zirconium diketonate. This compound hydrolyzed in a controllable fashion to form a zirconia precursor. Boria and carbon precursors were formed via solution additions of phenol–formaldehyde and boric acid, respectively. Tantalum oxide precursors were formed similarly as zirconia precursors, in which tantalum ethoxide was used. Solutions were concentrated, dried, pyrolyzed (800°–1100°C, 2 h, flowing argon), and exposed to carbothermal reduction heat treatments (1150°–1800°C, 2 h, flowing argon). Spherical particles of 200–600 nm for pure ZrB 2 and ZrB 2 –TaB 2 mixtures were formed.