La0.90Dy0.05Nb2O7 nanosheets were achieved by exfoliating a layered compound HLa0.90Dy0.05Nb2O7.Multilayer films composed of the exfoliated nanosheets were prepared by a layer-by-layer deposition technology, which were subsequently heat-treated at 450℃ and exposed under ultraviolet light to obtain the polymer-free nanosheet films, respectively.The resulting La0.90Dy0.0sNb2O7 nanosheet suspension and its films exhibit intense emission by the host excitation and negligibly low emission by the direct Dy3+ excitation, whereas the photoluminescence emissions of the bulk precursors are largely dominated by the direct Dy3+ excitation rather than the host excitation.