铝酸钙、硫氧化钇基质长余辉发光材料的制备及发光性能表征
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摘要
本论文首先阐述了长余辉发光材料的发展历史及研究现状,针对蓝色和红色长余辉发光材料初始亮度低、余辉时间短的缺点,主要进行了以下几个方面的工作:
(1)采用高温固相法制备了CaAl_2O_4:Eu~(2+), Nd~(3+)蓝色长余辉发光材料。系统考察了煅烧温度、保温时间、稀土离子掺杂浓度、助熔剂用量对样品发光性能的影响。
(2)研究了Ca/Al对CaAl_2O_4:Eu~(2+), Nd~(3+)发光性能的影响。所得样品的激发峰峰位随着Ca/Al比值的递减而逐渐向短波方向移动,即发生了蓝移现象,而发射峰峰位仍为440 nm。Eu~(2+)在CaA12O4中的余辉效果较佳,这是由于基质组份配比的变化引起了基质晶格结构的改变,稀土离子在基质中形成的陷阱浓度和陷阱深度随之改变,从而造成了余辉时间的不同。
(3)研究了溶剂热法、共沉淀法、低热固相前驱体法对CaAl_2O_4:Eu~(2+), Nd~(3+)长余辉发光材料发光性能的影响。荧光测试结果表明,主激发波长随样品粒径的减小逐渐向短波方向移动,即发生了明显的蓝移现象;相反,主发射波长向长波方向移动,即发生了红移现象。对比不同方法所得样品的余辉衰减数据,高温固相法仍是制备铝酸钙长余辉发光材料的主要途径。
(4)在CaAl_2O_4: Eu~(2+), Nd~(3+)体系中共掺杂非稀土氧化物以期改善其发光性能。余辉测试结果表明,在体系中共掺杂Mn~(4+)时,样品的长余辉特性得到了明显改善,并对CaAl_2O_4:Eu~(2+), Nd~(3+)长余辉发光机理进行了初步探讨。
(5) Y_2O_2S:Eu~(3+), Ti~(4+), Mg~(2+)红色长余辉发光材料的制备及发光性能表征。考察了煅烧温度、煅烧气氛、保温时间、稀土离子掺杂浓度对样品发光性能的影响,并初步探讨了其发光机理。在此基础上考察了其它镧系稀土离子对体系发光性能的影响。余辉测试结果表明,在体系中共掺杂Ce~(3+)、Pr~(3+)、Tb~(3+)时发生了余辉猝灭,使得体系均没有长余辉发光现象,并探讨了其原因。
(6)制备出未见报道的Y_2O_2S:Gd~(3+), Lu~(3+), Ti~(4+), Mg~(2+)橘黄色长余辉发光材料,探讨了Gd~(3+)、Lu~(3+)在长余辉发光过程中各自所起的作用。
In this paper, the current situation and development of phosphors were summarized firstly. In order to increase the initial intensity and reduce the decay rate of the blue and red long afterglow phosphors, we studied the following aspects:
(1) Synthesis and characterization of blue long afterglow phosphor CaAl_2O_4: Eu~(2+), Nd~(3+) by high-temperature solid-state method. The influences of synthesis temperature, holding time, rare earth ions doping concentration and the concentration of H3BO3 on luminescence properties were systematic studied.
(2) The influences of the element ratio of Ca/Al on luminescence properties of CaAl_2O_4: Eu~(2+), Nd~(3+) phosphor were studied. The excitation spectra had a obvious blueshift and emission spectra was still 440 nm as the ratio of Ca/Al become small. The different matrix structure lead to the different trap depth and trap level that is why Eu~(2+) had better luminescence properties in stoichiometric CaAl_2O_4.
(3) The influences of hydrothermal, precipitation and low-heating solid-state precursor method on luminescence properties of CaAl_2O_4-based phosphor were studied. The spectral studies on nanosized CaAl_2O_4: Eu~(2+), Nd~(3+) indicated that the excitation spectra had a obvious blueshift and the emission spectra had a slightly redshift as comparisons with bulk samples. Comparison the afterglow decay data of the obtained samples which synthesis by different methods, high-temperature solid-state method is still the primary methods in synthesis of luminous materials.
(4) CaAl_2O_4: Eu~(2+), Nd~(3+) co-doped with non-rare earth oxides in order to increase the initial intensity and reduce the decay rate. The afterglow decay curve measurements result indicated that CaAl_2O_4: Eu~(2+), Nd~(3+) co-doped with Mn~(4+), had the better properties. We were also discussed luminescent mechanism of CaAl_2O_4: Eu~(2+), Nd~(3+).
(5) Synthesis and characterization of red long afterglow phosphor Y_2O_2S: Eu~(3+), Ti~(4+), Mg~(2+). The influences of synthesis temperature, calcinations atmosphere, holding time and rare earth ions doping concentration on luminescence properties were studied, and the luminescent mechanism of Y_2O_2S: Eu~(3+), Ti~(4+), Mg~(2+) was also discussed. Based on the above experiments, the influences of other lanthanide rare earth ions on luminescence properties were studied. The samples had no long afterglow properties when co-doped with Ce~(3+)、Pr~(3+) and Tb~(3+), and discussed the reasons.
(6) There is no report about the yellowish-orange long afterglow phosphor Y_2O_2S: Gd~(3+), Lu~(3+), Ti~(4+), Mg~(2+) so far as I know. The detailed research was conducted to investigate the influence of Gd~(3+) and Lu~(3+) on the luminescent properties of Y_2O_2S: Ti~(4+), Mg~(2+).
(1)采用高温固相法制备了CaAl_2O_4:Eu~(2+), Nd~(3+)蓝色长余辉发光材料。系统考察了煅烧温度、保温时间、稀土离子掺杂浓度、助熔剂用量对样品发光性能的影响。
(2)研究了Ca/Al对CaAl_2O_4:Eu~(2+), Nd~(3+)发光性能的影响。所得样品的激发峰峰位随着Ca/Al比值的递减而逐渐向短波方向移动,即发生了蓝移现象,而发射峰峰位仍为440 nm。Eu~(2+)在CaA12O4中的余辉效果较佳,这是由于基质组份配比的变化引起了基质晶格结构的改变,稀土离子在基质中形成的陷阱浓度和陷阱深度随之改变,从而造成了余辉时间的不同。
(3)研究了溶剂热法、共沉淀法、低热固相前驱体法对CaAl_2O_4:Eu~(2+), Nd~(3+)长余辉发光材料发光性能的影响。荧光测试结果表明,主激发波长随样品粒径的减小逐渐向短波方向移动,即发生了明显的蓝移现象;相反,主发射波长向长波方向移动,即发生了红移现象。对比不同方法所得样品的余辉衰减数据,高温固相法仍是制备铝酸钙长余辉发光材料的主要途径。
(4)在CaAl_2O_4: Eu~(2+), Nd~(3+)体系中共掺杂非稀土氧化物以期改善其发光性能。余辉测试结果表明,在体系中共掺杂Mn~(4+)时,样品的长余辉特性得到了明显改善,并对CaAl_2O_4:Eu~(2+), Nd~(3+)长余辉发光机理进行了初步探讨。
(5) Y_2O_2S:Eu~(3+), Ti~(4+), Mg~(2+)红色长余辉发光材料的制备及发光性能表征。考察了煅烧温度、煅烧气氛、保温时间、稀土离子掺杂浓度对样品发光性能的影响,并初步探讨了其发光机理。在此基础上考察了其它镧系稀土离子对体系发光性能的影响。余辉测试结果表明,在体系中共掺杂Ce~(3+)、Pr~(3+)、Tb~(3+)时发生了余辉猝灭,使得体系均没有长余辉发光现象,并探讨了其原因。
(6)制备出未见报道的Y_2O_2S:Gd~(3+), Lu~(3+), Ti~(4+), Mg~(2+)橘黄色长余辉发光材料,探讨了Gd~(3+)、Lu~(3+)在长余辉发光过程中各自所起的作用。
In this paper, the current situation and development of phosphors were summarized firstly. In order to increase the initial intensity and reduce the decay rate of the blue and red long afterglow phosphors, we studied the following aspects:
(1) Synthesis and characterization of blue long afterglow phosphor CaAl_2O_4: Eu~(2+), Nd~(3+) by high-temperature solid-state method. The influences of synthesis temperature, holding time, rare earth ions doping concentration and the concentration of H3BO3 on luminescence properties were systematic studied.
(2) The influences of the element ratio of Ca/Al on luminescence properties of CaAl_2O_4: Eu~(2+), Nd~(3+) phosphor were studied. The excitation spectra had a obvious blueshift and emission spectra was still 440 nm as the ratio of Ca/Al become small. The different matrix structure lead to the different trap depth and trap level that is why Eu~(2+) had better luminescence properties in stoichiometric CaAl_2O_4.
(3) The influences of hydrothermal, precipitation and low-heating solid-state precursor method on luminescence properties of CaAl_2O_4-based phosphor were studied. The spectral studies on nanosized CaAl_2O_4: Eu~(2+), Nd~(3+) indicated that the excitation spectra had a obvious blueshift and the emission spectra had a slightly redshift as comparisons with bulk samples. Comparison the afterglow decay data of the obtained samples which synthesis by different methods, high-temperature solid-state method is still the primary methods in synthesis of luminous materials.
(4) CaAl_2O_4: Eu~(2+), Nd~(3+) co-doped with non-rare earth oxides in order to increase the initial intensity and reduce the decay rate. The afterglow decay curve measurements result indicated that CaAl_2O_4: Eu~(2+), Nd~(3+) co-doped with Mn~(4+), had the better properties. We were also discussed luminescent mechanism of CaAl_2O_4: Eu~(2+), Nd~(3+).
(5) Synthesis and characterization of red long afterglow phosphor Y_2O_2S: Eu~(3+), Ti~(4+), Mg~(2+). The influences of synthesis temperature, calcinations atmosphere, holding time and rare earth ions doping concentration on luminescence properties were studied, and the luminescent mechanism of Y_2O_2S: Eu~(3+), Ti~(4+), Mg~(2+) was also discussed. Based on the above experiments, the influences of other lanthanide rare earth ions on luminescence properties were studied. The samples had no long afterglow properties when co-doped with Ce~(3+)、Pr~(3+) and Tb~(3+), and discussed the reasons.
(6) There is no report about the yellowish-orange long afterglow phosphor Y_2O_2S: Gd~(3+), Lu~(3+), Ti~(4+), Mg~(2+) so far as I know. The detailed research was conducted to investigate the influence of Gd~(3+) and Lu~(3+) on the luminescent properties of Y_2O_2S: Ti~(4+), Mg~(2+).
引文
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