以强碱性阴离子交换树脂为沉淀剂, 采用离子交换法制备了ZrO₂∶Eu ³⁺纳米晶. 通过XRD, TEM,HRTEM和EDS等对晶体的结构、形貌及化学成分进行了表征, 利用3D荧光光谱、激发光谱和发射光谱研究了Eu³⁺在ZrO₂纳米晶中的发光性质. 结果表明, 焙烧温度在800℃以下所得的ZrO₂∶Eu ³⁺纳米晶主要为四方结构, 晶粒尺寸约为5-20 nm, 随着焙烧温度的升高, 样品的晶结构发生了细微变化, 从900℃开始出现了少量单斜晶. 由ZrO₂∶Eu ³⁺的3D荧光光谱确定了其最佳监测波长和发射波长, 在394 nm波长光的激发下观察到纳米ZrO₂ 中Eu³⁺的590 nm (⁵D₀ →⁷F₁) 和606 nm (⁵D₀→⁷F₂) 特征发射谱, 随着相结构细微的变化, 发射光谱的形状及强度均发生变化, 说明ZrO₂∶Eu ³⁺纳米晶的发光性质对其结构非常敏感.

Eu³⁺ doped luminescent nano–materials have become a research focus due to their outstanding physical and chemical properties in light–emitting, magnetism, thermology, catalysis and chemical activity etc.. Furthermore, the relationship between crystal structure and energy levels transition of these nano–materials can be easily obtained by measuring the spectra of doped Eu³⁺. Among luminescence nano–materials, ZrO₂ nano–crystal as a potential one has been attracted great attention in its higher refractive, good optical transparency and relatively low phonon energy. By now certain materials doped RE ion in the matrix ZrO₂ for ZrO₂∶Er³⁺–Y³⁺, ZrO₂∶Pr³⁺ and ZrO₂∶(Pr³⁺, Sm³⁺) etc., and mesoporous ZrO₂ nano–crystals doped Eu³⁺ by hydrothermal way have been reported. In present study, the ZrO₂∶Eu³⁺ nano–crystal was prepared with high purity and uniform composition by ion exchange method using strong OH⁻ as a precipitant. Its composition, morphology and structure were characterized by XRD, TEM, HRTEM and EDS. The experimental results show that it has a tetragonal crystal structure and its average grain size is 5—20 nm after calcined at 800 ℃ . It is found that the microstructure of ZrO₂∶Eu³⁺ changes slightly with the increase of calcining temperature till a small amount of monoclinic phase forms after calcined at higher than 900  ℃. The luminescent properteof Eu³⁺ in the ZrO₂ nano–crystal were measured by 3D emission and excitation spectra. The characteristic emissin bands of 590 nm (⁵D₀ →⁷F₁) and 606 nm (⁵D₀ →⁷F₂) of Eu³⁺ were observed at an excitation spectrum of λ_ex=394 nm. The luminescent properties of ZrO₂∶Eu ³⁺ are very sensitive to its microstructure change since slight changes in the ZrO₂∶Eu ³⁺ microstructure cause the changes in the shape and intensity of its emission spectra.