Pure β-KYF 4 nanocrystals codoped with Er 3+ /Yb 3+ and Tm 3+ /Yb 3+ were successfully synthesized via the thermal decomposition of trifluoroacetate precursors using oleic acid and octadecylene as coordinate solvents. The up-conversion optical properties of the β-KYF 4 nanocrystals with different lanthanide (Ln)-doped ions (Yb 3+ /Er 3+ , Yb 3+ /Tm 3+ ) were investigated. It is found that the colloidal dispersion of β-KYF 4 :Yb,Er/Tm nanocrystals display strong multiple up-conversion emission spanning from the deep UV-to-NIR region under 980 nm excitation. Pure β-KYF 4 nanocrystals codoped with Er 3+ /Yb 3+ and Tm 3+ /Yb 3+ can emit the bright eye-visible blue, green, yellow, and red emissions by adjusting concentration of Yb 3+ sensitizer ion and Er 3+ or Tm 3+ activator ions. Moreover, the UC luminescent colors can be tuned for the four colors from blue to green to yellow and finally to red emission in the average particle size, X-ray wavelength (0.15405 nm), the diffraction angle and full-width at half-maximum, respectively.The morphology and size of Yb 3+ ,Er 3+ /Tm 3+ codoped KYF 4 NCs are analyzed by TEM and HRTEM. Fig.2 shows the TEM images of KYF 4 :20% Yb 3+ /2% Er 3+ and KYF 4 :25% Yb 3+ /0.2% Tm 3+ NCs, respectively. It is shown that as-synthesized KYF 4 :Yb 3+ ,Er 3+ /Tm 3+ NCs contain smaller hexagonal nanorods particles and nanoplates with good monodispersity. From Fig. 2a,b the average grain size for KYF 4 :20% Yb/2% Er and KYF 4 :25% Yb/0.2% Tm NCs are calculated from random 100 nanoparticle to be 16nm, 18nm, respectively , which are in good consistent to XRD analysis result calculated by scherrer's formula. The lattice fringes are obviously observed in HR-TEM images of KYF 4 :Yb,Er/Tm ( Fig. 2c,d ), which indicated that as-synthesized KYF 4 NCs possessed highly crystallinity. The HRTEM images (Fig. 2c) of as-synthesized nanocrystals showed clear lattice fringes with a interplanar spacing of d = 0.33 nm, which corresponds to the (221) lattice plane of the hexagonal phase KYF 4 . In addition, the interplanar distances of 0.21nm was also observed by HR-TEM images in Fig. 2d, corresponding to the (600) lattice planes of the hexagonal phase KYF 4 , which was consistent with the XRD analysis. The corresponding elemental composition of KYF 4 codoped with 20% Yb 3+ /2% Er 3+ and 25% Yb 3+ /0.2% Tm 3+ NCs were obtained by the EDS analysis, as shown in Fig.2f.The EDS result for KYF 4 :20%Yb/2%Er (Fig. 2e) demonstrates that as-synthesizedNCs are mostly consist of K, Y, Yb, Er and F. The EDS result for KYF 4 :25% Yb/0.2% Tm as-synthesized NCs are mostly consist of K, Y, Yb, Tm and F. Based on