The simple co-precipitation method was used to prepare AgxFeO2 delafossite with non-stoichiometric silver concentration in the range of x = 0.05–1. The obtained material was investigated using X-ray powder diffraction and 57Fe Mössbauer spectroscopy at room temperature. The structural and hyperfine interaction parameters were recognized in relation with decreasing silver concentration. The study revealed that the delafossite structure of AgxFeO2 was maintained up to x = 0.9; as the range of silver concentration was decreased to 0.05 ≤ x ≤ 0.8, a mixture of AgFeO2, Fe2O3 or/and FeOOH was formed.
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