Thermodynamic assessment of an equiatomic FeNiCoCrMn precursor for a spinel high-entropy oxide produced via mechano-oxidation with structure–radiation interaction correlation

Spinel high-entropy oxides (HEOs) can stabilize multiple transition-metal cations within a single lattice, yet their radiation-interaction behavior is scarcely explored. Here, a (FeNiCoCrMn)3O4 spinel HEO was produced via an alloy-to-oxide route: 40 h mechanical alloying of equiatomic FeNiCoCrMn powders followed by mechano-oxidation (1000 °C/3 h) and high-energy grinding. HEA-derived thermodynamic metrics were used to rationalize the stability of the equiatomic metallic precursor prior to mechano-oxidation, rather than to directly predict the formation of the final oxide phase. XRD evidenced progressive amorphization of the HEA and its conversion to a crystalline spinel oxide, while SEM–EDS confirmed homogeneous elemental distribution. XPS indicated a defect-rich, multivalent surface (Co2+/Co3+, Cr3+/Cr6+, Fe3+, mixed Mn states, Ni2+) with lattice oxygen and vacancy-related components. Moreover, the spinel oxide showed higher linear attenuation coefficients than 316L stainless steel, Inconel-718, and several lightweight Al-based entropy alloys, yielding lower HVL values, especially at low energies. Zeff exhibited the expected energy dependence and exceeded Al-dominant alloys across the spectrum. EBF/EABF at 1 and 40 mfp displayed Compton-region peaks and strong depth effects, consistent with attenuation behavior. It can be concluded that a (FeNiCoCrMn)3O4 spinel high-entropy oxide, produced via an alloy-to-oxide transformation route, exhibits structurally stable and compositionally homogeneous characteristics together with favorable gamma-ray attenuation behavior.