NaYF4∶Yb, Er/rGO and SiO2-coated NaYF4∶Yb, Er/rGO nanocomposites can be prepared through “one-pot” and directly mixing preparation routes. Various measurement results show that the NaYF4∶Yb, Er in the nanocomposites exhibits a cubic α-type structure and nanoparticle-like morphology with a diameter range of 30～70 nm; the rGO layers are well-dispersed in the nanocomposites, and whereas the rGO obtained from “one-pot” preparation renders relatively better dispersion. Raman spectra demonstrate that there exists a surface coupling action between the two kinds of nanomaterials, and with the increase in the relative rGO content, such action becomes stronger. UC fluorescence measurement results reveal that the rGO has significantly quenching effect and optical-limiting performance on the UC fluorescence, particularly on the red-emission of the NaYF4∶Yb, Er or SiO2-coated NaYF4∶Yb, Er nanoparticles. The red-emission intensity gradually decreases with an increase in the rGO content, but the green-emission shows less change. It should be stressed that in comparison with NaYF4∶Yb, Er/rGO, with a similar rGO content, the red-emission intensity of SiO2-coated NaYF4∶Yb, Er/rGO decreases much obviously due to a stronger light-absorption caused by part rGO aggregation.