Ho3+ and Yb3+ co-doped La7P3O18 up-conversion phosphors were prepared by a high-temperature solid-state process. XRD results reveal that the samples are mixtures of monoclinic structure La7P3O18 crystals with P21/n space group and minor LaPO4 crystals. UV—Vis DRS results indicate that La7P3O18 crystal is an indirect semiconductor with an optical band gap of 4.10 eV. After 980 nm laser excitation, the Ho3+ and Yb3+ co-doped La7P3O18 phosphors show the characteristic blue (486 nm), green (550 nm), and red (661 nm) luminescence peaks of Ho3+ ions. The peak at 661 nm dominates in the up-conversion luminescence spectra of samples. Meanwhile, with the increase of Ho3+ and Yb3+ doping content, the up-conversion luminescence intensity increases first and then decreases. By increasing the doping contents of Ho3+ and Yb3+ up to 1 at.% and 10 at.%, respectively, concentration quenching may appear by an electric quadrupole– electric quadrupole interaction process. The pumping power dependence of luminescence indicates that the green and red emissions of samples are excited by a two-photon absorption process. The color coordinates of Ho3+ and Yb3+ co-doped La7P3O18 crystals locate in the orange—red region.
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