In this study, ferrihydrite (Fhy) nanoparticles (NPles) synthesized by the radiation chemical method (RCM) from an iron nitrate alcohol solution were annealed in air at temperatures ranging from 100 to 1200 ºC. The effects of annealing temperature on the phase transformation and basic physicochemical properties of the annealed Fhy nanopowders (NPs) were investigated. Fhy NPles annealed at 400 ºC and above can be converted to hematite NPles. The X-ray diffraction (XRD) pattern of the RCM-synthesized product corresponded to two-line (2 L) Fhy NPles, with no additional peaks, confirming their chemical purity. Up to 200 ºC, no significant phase transformation of Fhy NPles was observed; at 300 ºC, Fhy transformed into maghemite, which further transformed into hematite at 400 ºC. TEM/HRTEM analysis showed the formation of mesoporous agglomerates consisting of amorphous-crystalline NPles approximately 2 nm in size in the Fhy S95 sample annealed at 95 ºC. Selected area electron diffraction (SAED) images indicated the presence of two crystalline phases in sample S95: FeO and zero-valence Fe. The specific surface area (SSA) of mesoporous Fhy NPles varied non-monotonically between 100 and 500 ºC, peaking at 53.2 m2/g at 300 ºC. X-ray photoelectron spectroscopy (XPS) analysis revealed a minor nitrogen impurity, likely from the initial iron nitrate precursor, and a significant amount of adsorbed carbon on the developed porous surface of Fhy NPles. The phase composition of annealed Fhy samples correlated with their photoluminescent (PL) spectra. In samples S400 and S500 containing hematite, a small ferromagnetic contribution emerged, disrupting the linear magnetization-field dependence observed in samples S0-S200. Thus, the properties of 2 L Fhy nanoparticles produced by the radiation chemical method can be modified through thermal annealing while maintaining their potential biomedical applications as nanocontainers for drug delivery and contrast agents.
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