Through a polyethylene-glycol-assisted hydrothermal method, a series of potassium fluoride (KF)–Yttrium (III) fluoride (YF3) system materials have been synthesized. By controlling the reactant ratios of KF: rare earth ions (RE3+), the hydrothermal temperatures, and the pH values of the prepared solutions, the final products can evolve among the orthorhombic phase of YF3 and/or the tetragonal phase of potassium triyttrium decafluoride (KY3F10) and/or the cubic phase of potassium yttrium tetrafluoride (KYF4). The final products are characterized by the x-ray diffraction (XRD) patterns, the field-emission scanning electron microscopy (FE-SEM) images, the energy-dispersive spectroscopy (EDS) patterns, the photoluminescence (PL) spectra, and the luminescent dynamic decay curves. The XRD patterns of the samples suggest the phase evolution of the final products. The FE-SEM images and the EDS patterns prove that. Europium ion (Eu3+) acting as a probe, its PL spectra and the luminescent decay curves all put together prove the phase evolution of the final products. The research can be extended to study the other KF–REF3 system materials.

Based on a citric acid-assisted hydrothermal method, series of Ce3+/Tb3+ activated fluorides have been synthesized. By controlling the amount of KNO3, the final products evolve from the Ce3+/Tb3+ codoped orthorhombic phase GdF3 to the Ce3+/Tb3+ codoped cubic phase KGdF4. The concentration of Ce3+ has great effects on the crystalline phases and the morphologies of final products. The Ce3+ concentration dependent samples illustrate the appearance of the hexagonal phase solid solution CeF3–GdF3–TbF3 in the final products. When the Ce3+ concentration is 20 mol%, the sample Ce20 presents the hexagonal phase CeF3 but the diffraction peaks move to higher degree. The x-ray diffraction patterns suggest the phase evolution of final products, the field emission scanning electron microscopy images present the variation in morphology of samples, and the photoluminescence excitation and emission spectra as well as the luminescent dynamic curves illustrate the optical properties of samples.