Ultrafast Synthesis of High Entropy Oxide Nanoparticles by Flame Spray Pyrolysis

The synthesis of high entropy oxide (HEO) nanoparticles (NPs) possesses many challenges in terms of process complexity and cost, scalability, tailoring nanoparticle morphology, and rapid synthesis. Herein, we report the synthesis of novel single-phase solid solution (Mn, Fe, Ni, Cu, Zn)₃(O)₄ quinary HEO NPs produced by a flame spray pyrolysis route. The aberration-corrected scanning transmission electron microscopy (STEM) technique is utilized to investigate the spinel crystal structure of synthesized HEO NPs, and energy-dispersive X-ray spectroscopy analysis confirmed the high entropy configuration of five metal elements in their oxide form within a single HEO nanoparticle. Selected area electron diffraction, X-ray diffraction, and Raman spectroscopy analysis results are in accordance with STEM results, providing the key attributes of a spinel crystal structure of HEO NPs. X-ray photoelectron spectroscopy results provide the insightful understanding of chemical oxidation states of individual elements and their possible cation occupancy sites in the spinel-structured HEO NPs.