将Yb³⁺作为协助发光的敏化剂，Tb³⁺和Tm³⁺作为发光中心的激活剂分别加入到基质氟化钇钠中，通过水热合成法分别制成不同掺杂浓度的NaYF₄：Yb³⁺/Tb³⁺和NaYF₄：Yb³⁺/Tm³⁺双掺杂氟化物纳米发光材料，并通过扫描电子显微镜、X射线衍射以及荧光光谱等手段分别对NaYF₄：Yb³⁺/Tb³⁺和NaYF₄：Yb³⁺/Tm³⁺双掺杂氟化物材料纳米颗粒的形貌及其发光特性进行了研究.实验结果表明：系列样品的X射线衍射图谱衍射峰与标准卡片吻合得很好，实验浓度范围内Yb³⁺/Tb³⁺和Yb³⁺/Tm³⁺共掺没有改变NaYF₄的晶体结构.实验得到了该材料在980 nm激光激发下的上转换发光光谱并分析了该材料的上转换发光机理，NaYF₄：Yb³⁺/Tb³⁺在980 nm激光激发的情况下出现的蓝光，绿光以及红光，分别对应于⁵D₄→⁷F₆、⁵D₄→⁷F₅、⁵D₄→⁷F₁的辐射跃迁；NaYF₄：Yb³⁺/Tm³⁺在980 nm光源激发下出现强的480 nm的蓝光，对应的是¹G₄→³H₆的电子跃迁能级带，在660 nm强的红光发射谱带，对应的是¹G₄→³F₄能级跃迁辐射光.

NaYF₄:Yb³⁺/Tb³⁺ and NaYF₄:Yb³⁺/Tm³⁺ double doping fluoride nanomaterials with different doping concentrations were prepared by hydrothermal synthesis. In these materials, the Yb³⁺ was used as sensitizer to assist in luminous, Tb³⁺ and Tm³⁺ were added to the matrix sodium yttrium fluoride as activators of luminous center. The morphology and luminous properties of NaYF₄:Yb³⁺/Tb³⁺ and NaYF₄:Yb³⁺/Tm³⁺ nanoparticles were investigated by scanning electron microscope (SEM), X-ray diffraction andfluorescence spectrum. The X-ray diffraction patterns of the series of samples well match the NaYF₄ standard card. Upconversion luminescence spectra of materials under 980 nm laser excitation were obtained and the mechanism was also analyzed. Excited by 980 nm laser, the emission spectra of NaYF₄:Yb³⁺/Tb³⁺ including blue, green and red light, which correspond to the radiative transition of ⁵D₄→⁷F₆, ⁵D₄→⁷F₅, ⁵D₄→⁷F₁, respectively. The strong 480 nm emission can be seen in NaYF₄:Yb³⁺/Tm³⁺ excited by 980 nm laser, corresponding to the electron transition energy band of ¹G₄→³H₆. A strong red light emission band centered at 660 nm is corresponding to the ¹G₄→³F₄ energy level transition.