Nd/Yb-co-doped YAG transparent ceramic nano-powder was prepared by a sol–gel combustion method. The structure, morphology and properties were characterized by thermogravimetric-differential thermal analysis, X-ray dif-fraction, transmission electron microscopy, infrared spectroscopy, absorption analysis and fluorescence spectroscopy, respectively. The results show that the mass loss of the powder calcinated at 900℃for 3 h is 49.56%. A well-cry-stallized Nd/Yb:YAG nano-powder with the superior sintering performance and high purity is obtained, and the morpho-logy of the particles with the average diameter in the range of 60–100 nms appears regular. The nano-powder exhibits an intense absorption at 808 nm, corresponding to the 4I9/2–4F7/2 transition of Nd3+ ions, which is suitable to absorb the wavelength of 808 nm from a laser diode source. The emission peak at 1046 nm of the Nd/Yb:YAG powder is more intense than that of Nd3+:YAG powder. It is indicated that the energy absorbed by Yb3+ ions from the laser diode source can be transmitted to Nd3+ ions based on the cross relaxation process of [(4F3/2)Nd, (2F7/2)Yb]→[(4I9/2)Nd, (2F5/2)Yb].
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