稀土（Dy，Nd，Yb，Er）掺杂氧化铝发光特性和测温应用
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摘要
三价稀土离子有丰富的能级,其上转换发光在光学温度传感器、短波长激光器和白光模拟等领域展现了巨大的应用潜力。
首先,溶胶凝胶法制备氧化铝,选取乙酰丙酮、异丙醇、异丙醇铝、高纯水等化学原料按照特定的比例发生鳌合、水解反应生成基质材料氧化铝溶胶。在此基础上按照实验设计加入稀土硝酸盐Er(NO_3)_3、Yb(NO_3)_3、Nd(NO_3)_3和Dy(NO_3)_3等。将得到的稀土掺杂氧化铝凝胶经过干燥,制备出不同掺杂参数的镱铒钕共掺、镱镝共掺氧化铝系列样品,给出优化的工艺参数,如退火时间、退火温度等。
其次,用978nm半导体激光器作为泵浦源,常温下测量了Dy~(3+):Yb~(3+)共掺氧化铝样品在350-950nm区间的光致发光特性,讨论分析了主要发光峰的上转换机制。实验观测到6个较强的光致发光谱:378nm、408nm、527nm、544nm、663 nm和883nm。功率谱测量和上转换机制分析表明378nm和408nm上转换发光为三光子过程,而527nm是两光子和三光子共同作用过程, 544nm和663 nm主要为两光子过程。
再次,讨论了Yb~(3+):Er~(3+):Nd~(3+)共掺氧化铝温度传感材料的原理,并对813nm和887nm发射光谱跃迁机制及对应的能级结构进行了分析。当温度由375K升高到887K,钕离子在813nm和887nm的发射光谱随温度升高而增强,并且813nm光谱强度增强的速度明显超过887nm光谱,两光谱分别对应着~4F_(5/2)+~2H_(9/2)→~4I_(9/2)和~4F_(3/2)→~4I_(9/2)能级的跃迁,整个钕离子发射光谱的布局数是铒离子二次敏化过程。利用荧光强度比法对不同温度时两光谱强度进行处理,得到Yb~(3+):Er~(3+):Nd~(3+)共掺氧化铝温度传感材料灵敏度最高精度达到0.0015K~(-1)。
最后,对本论文工作进行了总结,并对掺杂稀土上转换发光材料的研究方向进行了展望。
The trivalent ions with abundant energy levels of rare earth elements exhibit considerable potential applications in optical temperature sensor, shortwave laser, biomedicine diagnostics and white-light illumination, etc, because of their up- conversion luminescence.
Firstly, the acetylacetone (AcAcH) was mixed with the Al(OC3H7)3 and PriOH solution chelating and hydrolyzing to be Al_2O_3 sol. Then, Nd~(3+), Er~(3+) ,Yb~(3+)andYb~(3+) ions were imported by addition of Nd(NO_3)_3·5H_2O, Er(NO_3)_3·5H_2O ,Yb(NO_3)_3·5H_2O and Yb(NO_3)_3·5H_2O with a particular molar ratio. The xerogel was obtained after drying of the co-doped sol at 373K for 8h to remove the solvent. The Nd~(3+): Er~(3+):Yb~(3+) co-doped Al_2O_3 was obtained after the xerogel was dried and heated. Finally, the technics parametres such as heating time and cooling temperature were performed. Secondly, the photoluminescence spectra of Yb~(3+):Dy~(3+) co-doped Al_2O_3 powder was measured in the range from 350nm to 950nm at room temperature, using a 978nm laser diode as an excitation source. The dominate up-conversion mechanisms, including energy transfer, cross relaxation and excited state absorption were discussed. The emissions of Dy~(3+) ions at 378nm, 408nm, 527nm, 544nm, 663 nm and 883nm observed. Through the measurement of the power spectra and the analysis of transition progress we know that emissions of Dy~(3+) ions at 378nm and 408nm are two photons progress, the emission at 527nm is two and three mixed photons progress, 544nm and 663 nm are totally two photons progress.
Thirdly, Nd~(3+):Er~(3+):Yb~(3+)co-doped Al_2O_3 powder have been prepared by nonaqueous sol-gel method. The two-stage sensitization processes for energy transfer among Yb~(3+), Er~(3+) and Nd~(3+) were discussed. Under a 978nm semiconductor laser excitation, the photoluminescence intensities at 813 and 887nm corresponding to the ~4F_(5/2)+~2H_(9/2)→~4I_(9/2) and ~4F_(3/2)→~4I_(9/2) transitions of Nd~(3+) ions enhance monotonously with the increasing temperature, and the fluorescence intensity ratio of the near-infrared emissions can be fitted the exponential function R=3.12exp(-1150/T) in the temperature range of 375-889K. The maximum sensitivity is 0.0015K~(-1) at 574.3K.
At last, the work of the thesis was summarized, and future research plans have been prospected for rare earth doped materials.
首先,溶胶凝胶法制备氧化铝,选取乙酰丙酮、异丙醇、异丙醇铝、高纯水等化学原料按照特定的比例发生鳌合、水解反应生成基质材料氧化铝溶胶。在此基础上按照实验设计加入稀土硝酸盐Er(NO_3)_3、Yb(NO_3)_3、Nd(NO_3)_3和Dy(NO_3)_3等。将得到的稀土掺杂氧化铝凝胶经过干燥,制备出不同掺杂参数的镱铒钕共掺、镱镝共掺氧化铝系列样品,给出优化的工艺参数,如退火时间、退火温度等。
其次,用978nm半导体激光器作为泵浦源,常温下测量了Dy~(3+):Yb~(3+)共掺氧化铝样品在350-950nm区间的光致发光特性,讨论分析了主要发光峰的上转换机制。实验观测到6个较强的光致发光谱:378nm、408nm、527nm、544nm、663 nm和883nm。功率谱测量和上转换机制分析表明378nm和408nm上转换发光为三光子过程,而527nm是两光子和三光子共同作用过程, 544nm和663 nm主要为两光子过程。
再次,讨论了Yb~(3+):Er~(3+):Nd~(3+)共掺氧化铝温度传感材料的原理,并对813nm和887nm发射光谱跃迁机制及对应的能级结构进行了分析。当温度由375K升高到887K,钕离子在813nm和887nm的发射光谱随温度升高而增强,并且813nm光谱强度增强的速度明显超过887nm光谱,两光谱分别对应着~4F_(5/2)+~2H_(9/2)→~4I_(9/2)和~4F_(3/2)→~4I_(9/2)能级的跃迁,整个钕离子发射光谱的布局数是铒离子二次敏化过程。利用荧光强度比法对不同温度时两光谱强度进行处理,得到Yb~(3+):Er~(3+):Nd~(3+)共掺氧化铝温度传感材料灵敏度最高精度达到0.0015K~(-1)。
最后,对本论文工作进行了总结,并对掺杂稀土上转换发光材料的研究方向进行了展望。
The trivalent ions with abundant energy levels of rare earth elements exhibit considerable potential applications in optical temperature sensor, shortwave laser, biomedicine diagnostics and white-light illumination, etc, because of their up- conversion luminescence.
Firstly, the acetylacetone (AcAcH) was mixed with the Al(OC3H7)3 and PriOH solution chelating and hydrolyzing to be Al_2O_3 sol. Then, Nd~(3+), Er~(3+) ,Yb~(3+)andYb~(3+) ions were imported by addition of Nd(NO_3)_3·5H_2O, Er(NO_3)_3·5H_2O ,Yb(NO_3)_3·5H_2O and Yb(NO_3)_3·5H_2O with a particular molar ratio. The xerogel was obtained after drying of the co-doped sol at 373K for 8h to remove the solvent. The Nd~(3+): Er~(3+):Yb~(3+) co-doped Al_2O_3 was obtained after the xerogel was dried and heated. Finally, the technics parametres such as heating time and cooling temperature were performed. Secondly, the photoluminescence spectra of Yb~(3+):Dy~(3+) co-doped Al_2O_3 powder was measured in the range from 350nm to 950nm at room temperature, using a 978nm laser diode as an excitation source. The dominate up-conversion mechanisms, including energy transfer, cross relaxation and excited state absorption were discussed. The emissions of Dy~(3+) ions at 378nm, 408nm, 527nm, 544nm, 663 nm and 883nm observed. Through the measurement of the power spectra and the analysis of transition progress we know that emissions of Dy~(3+) ions at 378nm and 408nm are two photons progress, the emission at 527nm is two and three mixed photons progress, 544nm and 663 nm are totally two photons progress.
Thirdly, Nd~(3+):Er~(3+):Yb~(3+)co-doped Al_2O_3 powder have been prepared by nonaqueous sol-gel method. The two-stage sensitization processes for energy transfer among Yb~(3+), Er~(3+) and Nd~(3+) were discussed. Under a 978nm semiconductor laser excitation, the photoluminescence intensities at 813 and 887nm corresponding to the ~4F_(5/2)+~2H_(9/2)→~4I_(9/2) and ~4F_(3/2)→~4I_(9/2) transitions of Nd~(3+) ions enhance monotonously with the increasing temperature, and the fluorescence intensity ratio of the near-infrared emissions can be fitted the exponential function R=3.12exp(-1150/T) in the temperature range of 375-889K. The maximum sensitivity is 0.0015K~(-1) at 574.3K.
At last, the work of the thesis was summarized, and future research plans have been prospected for rare earth doped materials.
引文
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