稀土掺杂氧化物荧光粉末的水热制备及荧光性能研究
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摘要
稀土荧光粉由于在三基色节能灯、阴极射线管、场发射显示器和等离子体平板显示等技术领域的巨大应用前景而备受关注。然而,目前主要使用的荧光粉是稀土掺杂的以硫氧化物为基质的荧光材料,硫氧化物在使用过程中热稳定性差且容易污染空气,而以氧化物为基质的荧光粉具有良好的热稳定性、使用过程中无有害气体产生、以及发光性能较好的优点。因此,在提高以氧化物为基质的稀土荧光粉发光性能的同时,降低生产成本对其商业化生产具有重大的意义。
本论文提出用水热法制备Y_2O_3:Eu~(3+),Gd_2O_3:Eu~(3+)和Y_2O_3:Tb~(3+),Gd_2O_3:Tb~(3+),寻找最佳的稀土元素(Eu~(3+)和Tb~(3+))掺杂量,并在此基础上引入金属离子(Li~+,Mg~(2+),Al~(3+))利用共掺杂效应改良,提高荧光粉的发光强度以确定合适掺杂金属离子及最佳掺杂含量,制备出一系列新型荧光粉。得出的主要结论如下:
第一、利用水热法制备了红色荧光粉Y_2O_3:Eu~(3+)和Gd_2O_3:Eu~(3+),在Y~(3+)与Eu~(3+)摩尔比为20:1,Gd~(3+)与Eu~(3+)摩尔比为30:1时荧光粉Y_2O_3:Eu~(3+)和Gd_2O_3:Eu~(3+)具有最强的发光强度。为了进一步增强荧光粉的发光强度,在此基础上引入金属离子(Li~+, Mg~(2+), Al~(3+)),制备了红色荧光粉Y_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+))和Gd_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+))。其中Y~(3+):Eu~(3+):Li~+为20:1:1时发光强度最大,比Y_2O_3:Eu~(3+)的发光强度提高了1.06倍;Gd~(3+):Eu~(3+):Li~+为30:1:0.5时发光强度最大,比Gd_2O_3:Eu~(3+)的发光强度提高了2.42倍;Gd~(3+):Eu~(3+):Mg~(2+)为30:1:1时发光强度最大,比Gd_2O_3:Eu~(3+)的发光强度提高了1.27倍。掺杂Al~(3+)后,反而降低了Y_2O_3:Eu~(3+)和Gd_2O_3:Eu~(3+)的发光强度,说明金属Li~+比较适合做Y_2O_3:Eu~(3+)荧光粉的共掺杂离子,而Li~+与Mg~(2+)离子比较适合做Gd_2O_3:Eu~(3+)荧光粉的共掺杂离子。
第二、利用水热法制备了绿色荧光粉Y_2O_3:Tb~(3+)和Gd_2O_3:Tb~(3+),在Y~(3+)与Tb~(3+)摩尔比为20:1,Gd~(3+)与Tb~(3+)摩尔比为30:1时荧光粉Y_2O_3:Tb~(3+)和Gd_2O_3:Tb~(3+)具有最强的发光强度。为了进一步增强荧光粉的发光强度,在此基础上引入金属离子(Li~+, Mg~(2+), Al~(3+)),制备了绿色荧光粉Y_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+))和Gd_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+))。其中Y~(3+):Tb~(3+):Li~+为20:1:1时发光强度最大,比Y_2O_3:Tb~(3+)的发光强度提高了1.16倍;Y~(3+):Tb~(3+):Mg~(2+)为20:1:10时发光强度最大,比Y_2O_3:Tb~(3+)的发光强度提高了1.04倍;Gd~(3+):Tb~(3+):Li~+为30:1:1时发光强度最大,比Gd_2O_3:Tb~(3+)的发光强度提高了1.51倍。Gd~(3+):Tb~(3+):Mg~(2+)为30:1:5时发光强度最大,比Gd_2O_3:Tb~(3+)的发光强度提高了1.11倍。掺杂Al~(3+)后,Y_2O_3:Tb~(3+)和Gd_2O_3:Tb~(3+)发光强度反而降低了。说明Li~+与Mg~(2+)比较适合做Y_2O_3:Tb~(3+)和Gd_2O_3:Tb~(3+)的改良离子。
第三、利用水热法,制备了红色荧光粉Y_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+))及Gd_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+))和绿色荧光粉Y_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+))及Gd_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+))。XRD检测均属于立方结构,不同掺杂离子或同一掺杂离子不同掺杂量对材料的结晶性能和形貌有很大影响。
总之,本论文利用水热法,分别以Y_2O_3和Gd_2O_3为基质,稀土掺杂离子(Eu~(3+), Tb~(3+))作激活剂制备了红色和绿色荧光粉,金属离子的引入不同程度的改变了它们的发光强度,实验表明最终确定金属离子Li~+,Mg~(2+)是比较适合的掺杂离子,所掺杂改良的红粉Y_2O_3:Eu~(3+),Gd_2O_3:Eu~(3+)和绿粉Y_2O_3:Tb~(3+),Gd_2O_3:Tb~(3+)均是发光性能不错的荧光粉。
Due to the potential applications in the tricolor energy-saving lamps, cathode ray tube, field emission display and plasma display panel and so on, phosphors based on the rare earth elements (RE) doped materials have attracted enormous interests. However, the mainly used phosphors are the photoluminescence material based on the sulfide. Sulfide based phosphors have many disadvantages such as: poor thermal stability and generation of contamination gas. Even though the RE based phosphors have good photoluminescence properties, the cost is too high. Therefore, it is of great importance to reduce the environment pollution and lower the cost as well as to improve the photoluminescence properties of RE based phosphors.
In the thesis, a novel synthesis route of Y_2O_3:Eu~(3+), Gd_2O_3:Eu~(3+) and Y_2O_3:Tb~(3+), Gd_2O_3:Tb~(3+) phosphor was proposed. By adjusting the experimental conditions, the optimum doping amount of activator ions (Eu~(3+) and Tb~(3+)) was achieved. Furthermore, metals ions (Li~+, Mg~(2+), Al~(3+)) were co-doped into the phosphors to improve the photoluminescence properties of the as-prepared phosphors, make sure which the best doping ions and theirs the best doping amounts. The major results achieved in the thesis are given as follows:
Firstly, red phosphors Y_2O_3:Eu~(3+)and Gd_2O_3:Eu~(3+) were prepared by a simple hydrothermal process followed by a post-annealing process. Y_2O_3:Eu~(3+) phosphor achieves the strongest emission intensity as the molar ratio of Y~(3+) to Eu~(3+) is 20:1. Gd_2O_3:Eu~(3+) phosphor achieves the strongest emission intensity as the molar ratio of Gd~(3+) to Eu~(3+) is 30:1. In order to further enhance the emission intensity, metals ions (Li~+, Mg~(2+), Al~(3+)) were doped and red phosphors Y_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) and Gd_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) were prepared. The result showed that red phosphor Y_2O_3:Eu~(3+):Li~+ achieves the strongest emission intensity as the molar ratio of Y~(3+):Eu~(3+):Li~+ is 20:1:1, and the emission intensity is 1.06 times as high as that of the Y_2O_3:Eu~(3+) phosphor. Gd_2O_3:Eu~(3+):Li~+ achieves the strongest emission intensity as the molar ratio of Gd~(3+):Eu~(3+):Li~+ is 30:1:0.5, and the emission intensity is 2.42 times as high as that of the Gd_2O_3:Eu~(3+) phosphor. Gd_2O_3:Eu~(3+):Mg~(2+) achieves the strongest emission intensity as the molar ratio of Gd~(3+):Eu~(3+):Mg~(2+) is 30:1:1, and the emission intensity is 1.27 times as high as that of the Gd_2O_3:Eu~(3+) phosphor. For the phosphors doped with Al~(3+), the emission intensity of Y_2O_3:Eu~(3+) and Gd_2O_3:Eu~(3+) decreased. The result shows that Li~+ ions are suitable dopants for the improvement of photoluminescence properties of Y_2O_3:Eu~(3+), while Li~+ and Mg~(2+) ions are suitable dopants for the improvement of photoluminescence properties of Gd_2O_3:Eu~(3+).
Secondly, green phosphors Y_2O_3:Tb~(3+)and Gd_2O_3:Tb~(3+) were prepared by a simple hydrothermal process followed by a post-annealing process. Y_2O_3:Tb~(3+) phosphor achieves the strongest emission intensity as the molar ratio of Y~(3+) to Tb~(3+) is 20:1. Gd_2O_3:Tb~(3+) phosphor achieves the strongest emission intensity as the molar ratio of Gd~(3+) to Tb~(3+) is 30:1. In order to further enhance the emission intensity, metals ions (Li~+, Mg~(2+), Al~(3+)) were doped and green phosphors Y_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) and Gd_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) were prepared. The result showed that green phosphor Y_2O_3:Tb~(3+):Li~+ achieves the strongest emission intensity as the molar ratio of Y~(3+):Tb~(3+):Li~+ is 20:1:1, and the emission intensity is 1.16 times as high as that of the Y_2O_3:Tb~(3+) phosphor. Y_2O_3:Tb~(3+):Mg~(2+) achieves the strongest emission intensity as the molar ratio of Y~(3+):Tb~(3+):Mg~(2+) is 20:1:10, and emission intensity is 1.04 times as high as that of the Y_2O_3:Tb~(3+) phosphor. Gd_2O_3:Tb~(3+):Li~+ achieves the strongest emission intensity as the molar ratio of Gd~(3+):Tb~(3+):Li~+ is 30:1:1, and the emission intensity is 1.51 times as high as that of the Gd_2O_3:Tb~(3+) phosphor. Gd_2O_3:Tb~(3+):Mg~(2+) achieves the strongest emission intensity as molar ratio of Gd~(3+):Tb~(3+):Mg~(2+) is 30:1:5, and the emission intensity is 1.11 times as high as that of the Gd_2O_3:Tb~(3+) phosphor. For the phosphors doped with Al~(3+), the emission intensity of Y_2O_3:Tb~(3+) and Gd_2O_3:Tb~(3+) decreased. The result shows that Li~+ and Mg~(2+) ions are suitable dopants for the improvement of photoluminescence properties of Y_2O_3:Tb~(3+) and Gd_2O_3:Tb~(3+).
Thirdly, red phosphors Y_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) and Gd_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) and green phosphors Y_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) and Gd_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) were prepared by a hydrothermal process. The results of XRD showed that all prepared phosphors with a cubic crystal structure. Different doping ions or same doping ions with different doping amounts have great effect on the structural properties of the as-prepared phosphors.
In conclusion, phosphors Y_2O_3:Eu~(3+)and Gd_2O_3:Tb~(3+) were prepared by hydrothermal method. It is found that the doping metals ions (Li~+, Mg~(2+), Al~(3+)) may improve the photoluminescence properties and the thermal stability. Finally, the result shows that phosphors: Li~+ doped red phosphors Y_2O_3:Eu~(3+) and Gd_2O_3:Eu~(3+), Mg~(2+) doped red phosphors Gd_2O_3:Eu~(3+); Li~+ and Mg~(2+) doped Y_2O_3:Tb~(3+) and Gd_2O_3:Tb~(3+) show better photoluminescence properties.
本论文提出用水热法制备Y_2O_3:Eu~(3+),Gd_2O_3:Eu~(3+)和Y_2O_3:Tb~(3+),Gd_2O_3:Tb~(3+),寻找最佳的稀土元素(Eu~(3+)和Tb~(3+))掺杂量,并在此基础上引入金属离子(Li~+,Mg~(2+),Al~(3+))利用共掺杂效应改良,提高荧光粉的发光强度以确定合适掺杂金属离子及最佳掺杂含量,制备出一系列新型荧光粉。得出的主要结论如下:
第一、利用水热法制备了红色荧光粉Y_2O_3:Eu~(3+)和Gd_2O_3:Eu~(3+),在Y~(3+)与Eu~(3+)摩尔比为20:1,Gd~(3+)与Eu~(3+)摩尔比为30:1时荧光粉Y_2O_3:Eu~(3+)和Gd_2O_3:Eu~(3+)具有最强的发光强度。为了进一步增强荧光粉的发光强度,在此基础上引入金属离子(Li~+, Mg~(2+), Al~(3+)),制备了红色荧光粉Y_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+))和Gd_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+))。其中Y~(3+):Eu~(3+):Li~+为20:1:1时发光强度最大,比Y_2O_3:Eu~(3+)的发光强度提高了1.06倍;Gd~(3+):Eu~(3+):Li~+为30:1:0.5时发光强度最大,比Gd_2O_3:Eu~(3+)的发光强度提高了2.42倍;Gd~(3+):Eu~(3+):Mg~(2+)为30:1:1时发光强度最大,比Gd_2O_3:Eu~(3+)的发光强度提高了1.27倍。掺杂Al~(3+)后,反而降低了Y_2O_3:Eu~(3+)和Gd_2O_3:Eu~(3+)的发光强度,说明金属Li~+比较适合做Y_2O_3:Eu~(3+)荧光粉的共掺杂离子,而Li~+与Mg~(2+)离子比较适合做Gd_2O_3:Eu~(3+)荧光粉的共掺杂离子。
第二、利用水热法制备了绿色荧光粉Y_2O_3:Tb~(3+)和Gd_2O_3:Tb~(3+),在Y~(3+)与Tb~(3+)摩尔比为20:1,Gd~(3+)与Tb~(3+)摩尔比为30:1时荧光粉Y_2O_3:Tb~(3+)和Gd_2O_3:Tb~(3+)具有最强的发光强度。为了进一步增强荧光粉的发光强度,在此基础上引入金属离子(Li~+, Mg~(2+), Al~(3+)),制备了绿色荧光粉Y_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+))和Gd_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+))。其中Y~(3+):Tb~(3+):Li~+为20:1:1时发光强度最大,比Y_2O_3:Tb~(3+)的发光强度提高了1.16倍;Y~(3+):Tb~(3+):Mg~(2+)为20:1:10时发光强度最大,比Y_2O_3:Tb~(3+)的发光强度提高了1.04倍;Gd~(3+):Tb~(3+):Li~+为30:1:1时发光强度最大,比Gd_2O_3:Tb~(3+)的发光强度提高了1.51倍。Gd~(3+):Tb~(3+):Mg~(2+)为30:1:5时发光强度最大,比Gd_2O_3:Tb~(3+)的发光强度提高了1.11倍。掺杂Al~(3+)后,Y_2O_3:Tb~(3+)和Gd_2O_3:Tb~(3+)发光强度反而降低了。说明Li~+与Mg~(2+)比较适合做Y_2O_3:Tb~(3+)和Gd_2O_3:Tb~(3+)的改良离子。
第三、利用水热法,制备了红色荧光粉Y_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+))及Gd_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+))和绿色荧光粉Y_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+))及Gd_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+))。XRD检测均属于立方结构,不同掺杂离子或同一掺杂离子不同掺杂量对材料的结晶性能和形貌有很大影响。
总之,本论文利用水热法,分别以Y_2O_3和Gd_2O_3为基质,稀土掺杂离子(Eu~(3+), Tb~(3+))作激活剂制备了红色和绿色荧光粉,金属离子的引入不同程度的改变了它们的发光强度,实验表明最终确定金属离子Li~+,Mg~(2+)是比较适合的掺杂离子,所掺杂改良的红粉Y_2O_3:Eu~(3+),Gd_2O_3:Eu~(3+)和绿粉Y_2O_3:Tb~(3+),Gd_2O_3:Tb~(3+)均是发光性能不错的荧光粉。
Due to the potential applications in the tricolor energy-saving lamps, cathode ray tube, field emission display and plasma display panel and so on, phosphors based on the rare earth elements (RE) doped materials have attracted enormous interests. However, the mainly used phosphors are the photoluminescence material based on the sulfide. Sulfide based phosphors have many disadvantages such as: poor thermal stability and generation of contamination gas. Even though the RE based phosphors have good photoluminescence properties, the cost is too high. Therefore, it is of great importance to reduce the environment pollution and lower the cost as well as to improve the photoluminescence properties of RE based phosphors.
In the thesis, a novel synthesis route of Y_2O_3:Eu~(3+), Gd_2O_3:Eu~(3+) and Y_2O_3:Tb~(3+), Gd_2O_3:Tb~(3+) phosphor was proposed. By adjusting the experimental conditions, the optimum doping amount of activator ions (Eu~(3+) and Tb~(3+)) was achieved. Furthermore, metals ions (Li~+, Mg~(2+), Al~(3+)) were co-doped into the phosphors to improve the photoluminescence properties of the as-prepared phosphors, make sure which the best doping ions and theirs the best doping amounts. The major results achieved in the thesis are given as follows:
Firstly, red phosphors Y_2O_3:Eu~(3+)and Gd_2O_3:Eu~(3+) were prepared by a simple hydrothermal process followed by a post-annealing process. Y_2O_3:Eu~(3+) phosphor achieves the strongest emission intensity as the molar ratio of Y~(3+) to Eu~(3+) is 20:1. Gd_2O_3:Eu~(3+) phosphor achieves the strongest emission intensity as the molar ratio of Gd~(3+) to Eu~(3+) is 30:1. In order to further enhance the emission intensity, metals ions (Li~+, Mg~(2+), Al~(3+)) were doped and red phosphors Y_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) and Gd_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) were prepared. The result showed that red phosphor Y_2O_3:Eu~(3+):Li~+ achieves the strongest emission intensity as the molar ratio of Y~(3+):Eu~(3+):Li~+ is 20:1:1, and the emission intensity is 1.06 times as high as that of the Y_2O_3:Eu~(3+) phosphor. Gd_2O_3:Eu~(3+):Li~+ achieves the strongest emission intensity as the molar ratio of Gd~(3+):Eu~(3+):Li~+ is 30:1:0.5, and the emission intensity is 2.42 times as high as that of the Gd_2O_3:Eu~(3+) phosphor. Gd_2O_3:Eu~(3+):Mg~(2+) achieves the strongest emission intensity as the molar ratio of Gd~(3+):Eu~(3+):Mg~(2+) is 30:1:1, and the emission intensity is 1.27 times as high as that of the Gd_2O_3:Eu~(3+) phosphor. For the phosphors doped with Al~(3+), the emission intensity of Y_2O_3:Eu~(3+) and Gd_2O_3:Eu~(3+) decreased. The result shows that Li~+ ions are suitable dopants for the improvement of photoluminescence properties of Y_2O_3:Eu~(3+), while Li~+ and Mg~(2+) ions are suitable dopants for the improvement of photoluminescence properties of Gd_2O_3:Eu~(3+).
Secondly, green phosphors Y_2O_3:Tb~(3+)and Gd_2O_3:Tb~(3+) were prepared by a simple hydrothermal process followed by a post-annealing process. Y_2O_3:Tb~(3+) phosphor achieves the strongest emission intensity as the molar ratio of Y~(3+) to Tb~(3+) is 20:1. Gd_2O_3:Tb~(3+) phosphor achieves the strongest emission intensity as the molar ratio of Gd~(3+) to Tb~(3+) is 30:1. In order to further enhance the emission intensity, metals ions (Li~+, Mg~(2+), Al~(3+)) were doped and green phosphors Y_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) and Gd_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) were prepared. The result showed that green phosphor Y_2O_3:Tb~(3+):Li~+ achieves the strongest emission intensity as the molar ratio of Y~(3+):Tb~(3+):Li~+ is 20:1:1, and the emission intensity is 1.16 times as high as that of the Y_2O_3:Tb~(3+) phosphor. Y_2O_3:Tb~(3+):Mg~(2+) achieves the strongest emission intensity as the molar ratio of Y~(3+):Tb~(3+):Mg~(2+) is 20:1:10, and emission intensity is 1.04 times as high as that of the Y_2O_3:Tb~(3+) phosphor. Gd_2O_3:Tb~(3+):Li~+ achieves the strongest emission intensity as the molar ratio of Gd~(3+):Tb~(3+):Li~+ is 30:1:1, and the emission intensity is 1.51 times as high as that of the Gd_2O_3:Tb~(3+) phosphor. Gd_2O_3:Tb~(3+):Mg~(2+) achieves the strongest emission intensity as molar ratio of Gd~(3+):Tb~(3+):Mg~(2+) is 30:1:5, and the emission intensity is 1.11 times as high as that of the Gd_2O_3:Tb~(3+) phosphor. For the phosphors doped with Al~(3+), the emission intensity of Y_2O_3:Tb~(3+) and Gd_2O_3:Tb~(3+) decreased. The result shows that Li~+ and Mg~(2+) ions are suitable dopants for the improvement of photoluminescence properties of Y_2O_3:Tb~(3+) and Gd_2O_3:Tb~(3+).
Thirdly, red phosphors Y_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) and Gd_2O_3:Eu~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) and green phosphors Y_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) and Gd_2O_3:Tb~(3+):M (M=Li~+, Mg~(2+), Al~(3+)) were prepared by a hydrothermal process. The results of XRD showed that all prepared phosphors with a cubic crystal structure. Different doping ions or same doping ions with different doping amounts have great effect on the structural properties of the as-prepared phosphors.
In conclusion, phosphors Y_2O_3:Eu~(3+)and Gd_2O_3:Tb~(3+) were prepared by hydrothermal method. It is found that the doping metals ions (Li~+, Mg~(2+), Al~(3+)) may improve the photoluminescence properties and the thermal stability. Finally, the result shows that phosphors: Li~+ doped red phosphors Y_2O_3:Eu~(3+) and Gd_2O_3:Eu~(3+), Mg~(2+) doped red phosphors Gd_2O_3:Eu~(3+); Li~+ and Mg~(2+) doped Y_2O_3:Tb~(3+) and Gd_2O_3:Tb~(3+) show better photoluminescence properties.
引文
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