| Summary: | Black phosphorus nanomaterials (BPN) have been well developed in tumor therapy. However, lack of diagnostic function limits the development of BPN in biomedicine. Lanthanide-doped nanoparticles are considered as versatile materials for fluorescence or magnetic resonance imaging. Integration of BPN with lanthanide-doped nanoparticles was rarely reported owing to the complex synthesis processes and poor modification effect. Herein, we report a simple and general method for synthesizing BPN@NaReF<sub>4</sub> (Re: Gd or Y, Yb, Er) nanocomposite. TEM and XRD characterization confirm efficient combination of BPN and NaGdF<sub>4</sub> or NaYF<sub>4</sub>:Yb,Er (18.2 mol %) after one-step mixing. The FTIR and XPS spectra were used to prove the generation of PO<sub>4</sub><sup>3</sup><sup>−</sup>-Gd and P-Gd coordination bonds and clarify ligand exchange mechanism. The anchored nanoparticles on BPN were stable and become hydrophilic. The prepared BPN@NaGdF<sub>4</sub> exhibit the signals of photoacoustic and magnetic resonance imaging. The obtained BPN@NaYF<sub>4</sub>:Yb,Er (18.2 mol %) have the potential in fluorescence bioimaging. We believe that this work will expand the applications of BPN in diagnosis and therapy together.
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