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采用干法(稀土氧化物与无水HF气体高温反应)合成Nd∶LiYF4(Nd∶YLF)多晶料。通过X射线衍射仪对多晶料的物相结构进行表征,确定了多晶料合成最佳工艺参数。发现稀土氟化物原料中氧化物杂质的存在对生长晶体有很大影响,直接采用未经处理的氟化物原料生长晶体,会在晶体表面出现白色包裹物。因此,在HF气氛下,经1 200℃热处理才能去除残留在氟化物原料中的氧化物杂质,保证生长晶体的质量。实验确定了生长YLF晶体的最佳组分配比是LiF与YF3的摩尔比为53∶47。以最佳组分配比,采用提拉法生长了Nd∶YLF晶体。结果表明:以最佳组分配比生长的Nd∶YLF晶体具有高的纯度和光学性能;在808nm二极管激光器泵浦下,位于1 047和1 053nm处的发射峰(4 F3/2→4 I11/2)均有较强的荧光发射。
Nd: LiYF4 (Nd: YLF) polycrystalline material was synthesized by dry method (reaction of rare earth oxide and anhydrous HF gas at high temperature). The phase structure of polycrystalline material was characterized by X-ray diffractometer, and the optimum process parameters for polycrystalline material synthesis were determined. It is found that the presence of oxide impurities in the rare earth fluoride raw materials has a great impact on the growth of the crystal. The green crystal grows directly from the raw fluoride raw material and a white inclusion appears on the crystal surface. Therefore, in the HF atmosphere, after the heat treatment at 1200 ℃ in order to remove oxide impurities remaining in the fluoride raw material, to ensure the quality of crystal growth. The optimum ratio of YFF crystal to YF3 is 53:47 LiF to YF3. Nd:YLF crystal was grown by Czochralski method with the best composition ratio. The results show that the Nd: YLF crystal grown with the best composition ratio has high purity and optical properties. The emission peaks at 1047 and 1053 nm (4 F3 / 2 → 4 I11 / 2) have strong fluorescence emission.