The up-conversion of Er3+/Yb3+ co-doped transparent glass-ceramics 50SiO2-10AlF3-5TiO2-30BaF2-4LaF3-0.5ErF3-0.5YbF3 containing Ba2LaF7 nanocrystals under the changing of heat treatment temperature and time were investigated. The Ba2LaF7 nanocrystals precipitated from the glass matrix was confirmed by X-ray diffraction (XRD). The structural investigation carried out by XRD and transmission electron microscopy (TEM) evidenced the formation of cubic Ba2LaF7 nanocrystals with crystal size of about 14 nm. Comparing with the samples before heat treatment, the high efficiency up-conversion emission of Er3+/Yb3+ co-doped samples was observed in the glass-ceramics under 980 nm laser diode excitation. The increase in red emission intensity bands was stronger than the green bands when the crystal size increased. The mechanism for the up-conversion process in the glass-ceramics and the reasons for the increase of Er3+/Yb3+ co-doped up-conversion intensity after heat treatment were discussed.