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<p>Core–shell structured high entropy oxide (HEO)–high entropy alloy (HEA) nanoparticles were successfully synthesized via a one-step ultrasonic spray pyrolysis (USP) process at 800&#xa0;°C under a reducing hydrogen atmosphere. X-ray diffraction (XRD) analysis confirmed the coexistence of a rock salt–type HEO phase and a metallic FCC HEA phase. SEM observations revealed uniformly spherical particles with an average diameter of approximately 224&#xa0;nm, consistent with the droplet-templating mechanism of USP. Advanced TEM analyses, including HRTEM, SAED, and STEM-EDS mapping, demonstrated a well-defined inverted core–shell particle structure, where the multicationic HEO phase is concentrated in the core while the HEA phase forms the outer shell. Unlike conventional oxide-shell/metal-core systems, this study presents a reversed configuration achieved in a single processing step without post-treatment. The results highlight the capability of USP to simultaneously control phase formation and nanoscale architecture in complex multicomponent systems, providing a promising platform for future catalytic and energy-related applications.</p> Graphical Abstract <p></p>

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Single Step Synthesis of CoCuFeNiZn High Entropy Alloy-Shell / (CoCuFeNiZn)O High Entropy Oxide-Core Nanoparticles Via Ultrasonic Spray Pyrolysis

  • 期刊论文

  • 发表日期：

    2026年7月17日

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  • Burak Küçükelyas,
  • İhsan Çaha,
  • İnal Kaan Duygun,
  • Emircan Uysal,
  • Bora Derin,
  • Francis Leonard Deepak,
  • Deniz Uzunsoy,
  • Sebahattin Gürmen

摘要

Core–shell structured high entropy oxide (HEO)–high entropy alloy (HEA) nanoparticles were successfully synthesized via a one-step ultrasonic spray pyrolysis (USP) process at 800 °C under a reducing hydrogen atmosphere. X-ray diffraction (XRD) analysis confirmed the coexistence of a rock salt–type HEO phase and a metallic FCC HEA phase. SEM observations revealed uniformly spherical particles with an average diameter of approximately 224 nm, consistent with the droplet-templating mechanism of USP. Advanced TEM analyses, including HRTEM, SAED, and STEM-EDS mapping, demonstrated a well-defined inverted core–shell particle structure, where the multicationic HEO phase is concentrated in the core while the HEA phase forms the outer shell. Unlike conventional oxide-shell/metal-core systems, this study presents a reversed configuration achieved in a single processing step without post-treatment. The results highlight the capability of USP to simultaneously control phase formation and nanoscale architecture in complex multicomponent systems, providing a promising platform for future catalytic and energy-related applications.

Graphical Abstract