| ZrO2∶Tb3+纳米晶的离子交换法制备及其发光特性 |
| Luminescence Properties of ZrO2∶Tb3+ Nanocrystals Prepared by Ion Exchange Method |
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| 摘要: 以强碱性阴离子交换树脂为交换介质，采用离子交换法制备了稀土Tb3+离子掺杂的ZrO2∶Tb3+纳米晶。通过XRD，TG-DSC，TEM，HRTEM等手段分析了样品制备过程的物相变化及晶粒形貌，用荧光光度计研究了样品的三维荧光光谱、激发光谱和发射光谱。结果表明：前驱沉淀物经800 ℃焙烧处理2 h，制备出近方型形貌，颗粒分散性好、尺寸约为40 nm的四方相ZrO2∶Tb3+纳米晶，当焙烧温度升高到900 ℃以上时样品出现了少量单斜晶相，而经800 ℃焙烧处理的纯ZrO2是以四方相和单斜相同时存在，说明稀土Tb3+离子的掺杂对ZrO2基质的四方晶相起到稳定作用。由ZrO2∶Tb3+的等角三维荧光光谱图显示Tb3+在ZrO2基质中的最佳激发波长为290 nm；在290 nm波长光的激发下观察到纳米ZrO2中Tb3+的发射峰位于491，545，582 nm分别对应于Tb3+的5D4→7F6、5D4→7F5、5D4→7F4能级跃迁，以491，545 nm的发射峰最强，其中经800 ℃焙烧处理的样品其5D4→7F6跃迁发射与5D4→7F5跃迁发射强度几乎相同，说明该法制备的纳米ZrO2∶Tb3+中5D4→7F6跃迁发射增强，使Tb3+发光的蓝色成分增加了。 |
| 关键词: ZrO2∶Tb3+纳米晶 离子交换法 发光特性 |
| 基金项目: |
| Abstract: ZrO2∶Tb3+ nanocrystals were prepared by ion exchange method in strong base media. The structure and morphology of products were characterized through XRD, TG-DSC, TEM and HRTEM after preparation. The luminescence properties of them were investigated with three dimension spectra, emission and excitation spectra. The results indicate that the ZrO2∶Tb3+ nanocrystals were in tetragonal phase with good dispersion, and the crystal size is about 40 nm after the precursor annealed at 800 ℃ for 2 h. As an annealing temperature above 900 ℃, some of the Tb3+-doped nanocrystals transfers to monoclinic phase, while under the annealing temperature of 800 ℃ the tetragonal and monoclinic phase co-exist for the pure ZrO2 sample, which indicates that the Tb3+ doping stabilized the tetragonal phase of ZrO2 matrix. The best excitation wavelength of ZrO2∶Tb3+ nanocrystal was 290 nm based on the analysis of the three dimension spectra. The characteristic emission bands of 491, 545 and 582 nm were corresponding to 5D4→7F6, 5D4→7F5 and 5D4→7F4 transitions of Tb3+ ion. The intensity of the 5D4→7F6 transition and the 5D4→7F5 transition is nearly the same under the annealing temperature of 800 ℃, showing an increase of the blue-green component from the 5D4→7F6 transition in the ZrO2∶Tb3+ nanocrystals prepared by the ion exchange method. |
| Keywords: ZrO2∶Tb3+ nanocrystal ion exchange method luminescence properties |
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| 莎 仁,李 霞,王喜贵.ZrO2∶Tb3+纳米晶的离子交换法制备及其发光特性[J].无机化学学报,2009,25(5):844-848. |
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