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In the present work, iron–sillenite (Bi₂₅FeO₄₀) was synthesized using a simple solid-state reaction method and characterized. The effects of the synthesis conditions on the phase purity of Bi₂O₃/Fe₃O₄, morphological features, and possible application as an XRD/MRI dual-contrast agent were investigated. For the synthesis, the stoichiometric amounts of Bi₂O₃ and Fe₃O₄ were mixed and subsequently milled in a planetary ball mill for 10 min with a speed of 300 rpm. The milled mixture was calcined at various temperatures (550 <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><mrow><mo>°</mo></mrow></semantics></math></inline-formula>C, 700 <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><mrow><mo>°</mo></mrow></semantics></math></inline-formula>C, 750 <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><mrow><mo>°</mo></mrow></semantics></math></inline-formula>C, 800 <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><mrow><mo>°</mo></mrow></semantics></math></inline-formula>C, and 850 <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><mrow><mo>°</mo></mrow></semantics></math></inline-formula>C) for 1 h in air at a heating rate of 5 °C/min. For phase identification, powder X-ray diffraction (XRD) analysis was performed and infrared (FTIR) spectra were recorded. The surface morphology of synthesized samples was studied by field-emission scanning electron microscopy (FE-SEM). For the radiopacity measurements, iron–sillenite specimens were synthesized at different temperatures and mixed with different amounts of BaSO₄ and Laponite solution. It was demonstrated that iron–sillenite Bi₂₅FeO₄₀ possessed sufficient radiopacity and could be a potential candidate to meet the requirements of its application as an XRD/MRI dual-contrast agent.