In this study, we present a novel dissolution-precipitation approach for the synthesis of rhabdophane-type GdPO4·nH2O nanostructures using amorphous calcium phosphate (ACP) as a precursor. It was shown that in aqueous medium in the presence of Gd3+ ions ACP can be successfully converted to GdPO4·nH2O. We systematically investigated the effects of synthesis duration, P-to-Gd molar ratio in the reaction mixture, synthesis temperature, and hydrothermal reactor filling volume on the phase composition and morphology of the obtained products. The samples were analyzed using powder X-ray diffraction (XRD), thermogravimetry and differential scanning calorimetry (TG-DSC), Fourier-transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). Furthermore, the assessment of the specific surface area (SBET) and magnetic properties of the selected samples was performed. The GdPO4·nH2O particles prepared under certain synthesis conditions were characterized by notably high SBET values reaching up to 157 m2g⁻1.
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