研究了Er3+掺杂的高氟浓度的透明氟氧化物玻璃陶瓷的微观结构和光谱性质。采用不同条件制备了两组初始组分为50SiO2-45PbF2-5PbO-1ErF3的样品,利用氟离子电极对实验样品的最终氟含量进行测定,表明了烧结过程中坩埚加盖可以有效地增加最终生成样品的氟含量。对样品进行了X射线衍射、透射电镜、吸收光谱以及上转换光谱的测试,结果显示,与低氟含量的先驱样品为非晶态不同,高氟含量的先驱样品中出现了β-PbF2结晶,高分辨透射电镜像表明该结晶为球形且颗粒尺寸大约在10~15nm。吸收光谱、J—O参数和上转换光谱进一步证明了高氟含量的先驱样品中Er3+存在于玻璃基质和β-PbF2微晶中。退火后,玻璃基质中的Er3+进入了PbF2微晶中,显示了比退火前强的上转换发光强度。
The microstructure and spectral properties of Er3+ doped transparent oxyfluoride glass ceramics with high fluorine content were reported.Two samples with the same initial contents(50SiO2-45PbF2-5PbO-1ErF3)were prepared under the different preparation parameters.The final fluorine contents were detected by a fluoride ion selective electrode.The results shows that the final fluorine contents increase by covering crucibles with corundum lid during melt.The samples were characterized by X-ray diffraction,transmission electron microscopy(TEM),absorption spectra and upconversion luminescence spectra.The results show that PbF2 crystals were precipitated in the sample with high fluorine content before heat treatment.And the PbF2 crystals precipitated inside the glass matrix are spherical with diameters of approximately 10-15 nm in size from the high resolution TEM micrograph.The absorption spectra,J—O parameters and the upconversion spectra show that the Er3+ ions were located in crystalline and vitreous mixed states.It is different from the sample with low fluorine content which is completely amorphous.After heat treatment,Er3+ ions that remain in the glassy phase entered into fluoride nanocrystals in the sample with high fluorine content.The fluorine environment decreases non-radiative transfer which eases the upconversion processes.Hence,the upconversion luminescence intensity of Er3+ ions in the high fluorine content sample after heat treatment is much stronger than that in the precursor sample.