Holmium, ytterbium co-doped potassium lutecium tungstate crystal (Ho,Yb:KLu(WO4)2, abbreviated Ho,Yb:KLuW) and erbium, ytterbium co-doped potassium lutecium tungstate crystal (Er,Yb:KLu(WO4)2, abbreviated Er,Yb:KLuW) are two kinds of new solid laser materials which are very apt to LD pump.In this paper, Ho,Yb:KLuW and Er,Yb:KLuW were grown by Top Seeded Solvent Growth (TSSG) method, using K2W2O7 as flux. The properties of crystals were researched based on the study of the choice of the growing method, the raw material pre-processing, the growth technology, the annealing technology, structure and spectrum. X-ray powder diffraction analysis were given to the crystals. Two kinds of crystals belong to monoclinic system with space group C2/c. The lattice parameters of the crystals were a=10.562(A|°), b=10.244(A|°), c=7.480(A|°),β=130.60°and a=10.567(A|°), b=10.238(A|°), c=7.482(A|°),β=130.65°. respectively. The infrared spectrum and Raman spectrum of the crystals were measured. The absorption peaks of the vibration modes were analysed and vibrational frequencies of vibratory activity were assigned. The absorption spectrum and fluorescence spectrum of the crystals were obtained. The peaks of Ho,Yb:KLuW crystal at 952nm, 981nm were found stronger and broader from the absorption spectrum, and the peaks of Er,Yb:KLuW crystal were at 931nm and 979nm. The emitting wavelength of Ho,Yb:KLuW crystal was at 2043nm, and the peaks of Er,Yb:KLuW crystal at 1541nm and 1547nm were found stronger, both of them were propitious to InGaAs semiconductor laser pump.
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