采用高温熔融法制备了Yb3+/Er3+掺杂的氟氧化物发光微晶玻璃，确定了最佳熔化温度(1 100 ℃)和退火温度(440 ℃，480 ℃)。测定得到基质玻璃的透过率为85%，掺入稀土后，透过率有所下降，并出现了稀土离子的特征吸收峰。980 nm半导体激光器(LD)激发下样品的上转换发射光谱存在4个明显的发射峰，分别为410,532,546和656 nm，对应于2H9/2→4I15/2,2H11/2→4I15/2,4S3/2→4I15/2和4F9/2→4I15/2跃迁。研究了不同Yb3+/Er3+(摩尔分数)和Er3+浓度对上转换发光强度的影响，当Yb3+∶Er3+=4∶1、 Er3+摩尔分数为15%时，上转换发光强度达到最高。根据发光强度与泵浦功率之间的关系，确定了上转换发射均为双光子过程。讨论了Yb3+,Er3+离子间的能量传递，建立了上转换发光机制。

Yb3+/Er3+codoped oxyfluoride glass ceramics were prepared by the high temperature melting method, and a suitable fusing temperature(1 100 ℃) and annealing temperatures(440 ℃, 480 ℃) of the rareearthdoped glass ceramics were determined. Experiments show that the transmittance of the host glass is 85%, but the transmittance drops evidently and there are characteristic absorption peaks of rareearth ions when the host glass is doped with Yb3+/Er3+ ions. With 980 nm laser diode(LD) excitation, the purple emission peak at 410 nm, green emission peak at 532 nm and 546 nm and red emission peak at 656 nm corresponding to 2H9/2→4I15/2, 2H11/2→4I15/2, 4S3/2→4I15/2 and 4F9/2→4I15/2 transitions of Er3+, respectively, were simultaneously observed at room temperature. The effects of Yb3+/Er3+ in mol concentration ratio and different concentrations of Er3+ ion on the intensity of upconversion luminescence was studied. The experiments show that the upconversion luminescence intensity is up to maximum value when the concentration ratio of Yb3+/Er3+ is 4∶1 and concentration of Er3+ ion is 15% in mol concentration. According to the relationship between the pump power and luminous intensity, the four upconversion luminescences are verified to be the twophoton process. Energy transfer was used in discussing the upconversion mechanism and the pertinent upconversion mechanism was proposed.