Alloy-to-oxide transformation of a spinel-structured (Fe30Cr30Mn20Ni10V10)3O4 high-entropy alloy-oxide via mechanical alloying: Synthesis, phase stability, multivalent surface states, and radiation attenuation behaviour

A spinel-structured high-entropy alloy-oxide (HEAO) with the nominal composition (Fe₃₀Cr₃₀Mn₂₀Ni₁₀V₁₀)₃O₄ was synthesized via mechanical alloying followed by thermo-mechanical oxidation X-ray diffraction indicated the formation of a predominantly spinel-type cubic oxide phase after oxidation, with the observed reflections being consistent with the Fd-3m spinel structure, while SEM-EDS mapping showed a homogeneous cation distribution at the examined scale. XPS analysis revealed mixed valence states of Fe²⁺/Fe³⁺, Cr³⁺/Cr⁴⁺, Mn³⁺/Mn⁴⁺, Ni²⁺/Ni³⁺, and V⁴⁺/V⁵⁺. Thermodynamic parameters supported phase stability, with ΔS_mix = 12.51 J K⁻¹·mol⁻¹ and Ω = 2.68. Gamma-ray attenuation properties were evaluated over 0.015-15 MeV. The linear attenuation coefficient decreased from 193.685 cm⁻¹ at 0.015 MeV to 0.309 cm⁻¹ at 1 MeV and stabilized near 0.137 cm⁻¹ at 15 MeV. Correspondingly, the half value layer increased from 0.004 cm to 5.068 cm across the same energy range. The effective atomic number decreased from 24.58 at 0.015 MeV to approximately 15.37 at 1 MeV, followed by a moderate increase to 17.71 at 15 MeV. Comparative analysis with commercial stainless steel, titanium alloys, nickel-based superalloys, ferro-boron systems, and lightweight entropy alloys demonstrated that the synthesized HEAO exhibits intermediate yet stable attenuation performance, positioning it between low-density Al-based systems and high-density Ni-rich alloys. It can be concluded that the alloy-to-oxide strategy enables the production of a structurally stable spinel HEAO with consistent and competitive gamma-ray attenuation behaviour across a broad photon energy spectrum.