Carbon-coated hydroxyapatite nanorods (HAp–C) were first synthesized using bovine bones from Urumqi as the carbon source. Ti3+-doped TiO2 (Ti3+–TiO2) was obtained via thermal reduction using NaBH4. Ti3+–TiO2 was hydrothermally deposited onto the surface of HAp–C, resulting in Ti3+–TiO2/HAp–C formation. The photocatalytic N2/H2O ammonia synthesis performance of the prepared materials was investigated while analyzing their structure. HAp–C, a stable carbon material derived from bones, exhibits considerable photoluminescence under ultraviolet light. It serves as a substrate for the Ti3+–TiO2 catalyst, reducing particle agglomeration and enhancing the photogenerated electron transfer rate. The presence of HAp–C further enhances the activation of Ti3+–TiO2/HAp–C for N2 adsorption and considerably increases its visible-light absorption compared to pure Ti3+–TiO2. The 85%–Ti3+–TiO2/HAp–C photocatalyst yielded 850.13 mol/(L·g cat.) of ammonia after 4 h of reaction during the photocatalytic N2/H2O ammonia synthesis, representing a 2.93-fold increase over the ammonia yield of pure Ti3+–TiO2 under identical conditions.
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