Because of their high mixing entropies, multi-component alloys can exhibit enhanced catalytic activity compared to traditional catalysts in various chemical reactions, including hydrogenation, oxidation, and reduction processes. In this work, new AgCoCuFeNi high entropy alloy nanoparticles were synthesized by the hydrogen reduction-assisted ultrasonic spray pyrolysis method. The aim was to investigate the effects of processing parameters (reaction temperature, precursor solution concentration, and residence time) on the microstructure, composition, and crystallinity of the high entropy alloy nanoparticles. The characterization was performed with scanning electron microscope, energy-dispersive X-ray spectroscopy, and X-ray diffraction. The syntheses performed at 600, 700, 800, and 900 ◦C, resulted in smaller and smoother spherical particles with a near-equiatomic elemental composition as the temperature increased to 900 ◦C.With 0.25, 0.1, and 0.05 M precursor solutions, narrower size distribution and uniform AgCoCuFeNi nanoparticles were produced by reducing the solution concentration to 0.05 M. A near-equiatomic elemental composition was only obtained at 0.25 and 0.05 M. Increasing the residence time from 5.3 to 23.8 s resulted in an unclear particle microstructure. None of the five metal elements were formed in the large tubular reactor. X-ray diffraction revealed that various crystal phase structures were obtained in the synthesized AgCoCuFeNi particles.
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