Eu~(2+)、Mn~(2+)激活的六铝酸盐基发光材料的制备及其发光特性研究
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摘要
等离子平板显示(PDP)具有薄、轻、视角广、响应速度快、大画面尺寸、色彩饱和度高、对比度高等诸多优点,其超快的响应速度使得其在三维(3D)和高清晰显示上具有无可比拟的优势。真空紫外发光材料的品质是影响PDP显示效果的一个关键因素,其色纯度、衰减时间、发光效率、稳定性等直接影响到显示的质量。六铝酸盐基发光材料广泛的应用于PDP显示器件,尤其是BaMgAl10O17:Eu2+蓝色发光材料和BaAl12O19:Mn2+绿色发光材料,均呈现了良好的发光性能,但BaMgAl10O17:Eu2+蓝色发光材料的劣化问题和BaAl12O19:Mn2+绿色发光材料的亮度和衰减时间问题始终是限制它们在PDP显示,尤其是3D显示方面应用的关键因素。本论文针对BaMgAl10O17:Eu2+蓝色发光材料热劣化问题和BaAl12O19:Mn2+绿色发光材料的亮度问题,通过一系列热处理、掺杂以及合成纳米级发光材料,探索其中的真空紫外发光机理以及相关的改性方案。主要研究内容包括以下几个方面：
1、通过在空气、氮气、还原气氛下对BaMgAl10O17:Eu2+蓝色发光材料进行不同时间的热处理,对比其光衰情况,研究了缺陷在BaMgAl10O17Eu2+蓝色发光材料热劣化中所起到的作用；同时,利用电荷平衡理论讨论Eu3+离子的自还原现象,讨论了在氮气和还原气氛下合成的样品中Eu2+离子的格位占据情况,并研究了Eu2+离子在BaMgAl10O17:Eu2+蓝色发光材料中的占位情况与其对热稳定性的影响。
2、通过对BaMgAl10O17晶体结构进行解析,分析了BaMgAl10O17:Eu2+中缺陷的形成机理,通过Castep程序计算了掺杂对于BaMgAl10O17电子结构的影响；考虑到低电负性的元素的引入,可以有效的提高BaMgAl10O17:Eu2+镜面层的稳定性,在BaMgAl10O17:Eu2+中掺入了S,研究了S的离子半径与电负性对于BaMgAl10O17:Eu2+发光以及热稳定性的影响,在BaMgAl10O17:Eu2+,Mn2+中引入Si3N4性,研究了Si3N4的掺入对于BaMgAl10O17Eu2+,Mn2+发光、热稳定性的影响,以及BaMgAl10O17Eu2+,Mn2+中能量传递机理。
3、利用溶胶凝胶法,探讨改变溶胶凝胶法中的预烧温度、反应时间、升温速率等因素对于制备微纳米BaMgAI10O17Eu2+样品的影响,并研究其生长过程；通过比较纳米样品和块体样品热处理前后在254nm紫外和147nm真空紫外下的发光差异,讨论了纳米样品和块体样品的发光性能差异,缺陷对于纳米样品热稳定性的影响以及纳米发光材料在3D-PDP显示器件方面的应用前景。
4、通过对BaAl12O190.1Mn2+晶体结构进行解析,分析了BaAl12O190.1Mn2+中缺陷的形成机理,针对BaAl12O190.1Mn2+中的缺陷形成机理,考虑低电负性元素对于镜面层的改性作用,在BaAl12O190.1Mn2+中掺入了S和Si3N4,研究了S和Si3N4的离子半径与电负性对于BaAl12O190.1Mn2+发光性能以及对于衰减时间的影响；研究了缺陷在能量传递机理以及衰减时间中所起到的作用。
上述研究表明,缺陷在BaMgAl10O17Eu2+蓝色发光材料的热劣化机理中扮演了重要角色,S和Si-N掺杂的BaMgAl10O17Eu2+和BaAl12O190.1Mn2+分别表现了高的发光亮度、好的热稳定性以及短的衰减时间,有望于应用于无汞荧光灯或3D-PDP,而类四方体形貌的BaMgAl10O17Eu2+蓝色发光材料也有希望应用于3D-PDP。
Due to its thin panel, a slight weight, an extensive visual angle, a large screen size, high-speed response with emissive, high contrast, more saturated colors etc, Plasma display panels (PDPs) were widely used in displays, especially in3D and high definition displays for its characteristics of higher response speed. The quality of Vacuum ultraviolet (VUV) luminescent materials is the key point of PDPs such as luminescence efficiency, color purity, decay time and stability play important role on the quality of displays. Phosphors based on hexaaluminates were widely used as PDP commercial materials, especially the blue phosphor BaMgAl10O17:Eu2+and green phosphor BaAl12O19:Mn2+, both of which exhibit excellent luminescent properties. However, there still some un-solved problems restrict its application in PDP, especially in3D displays, such as the degradation of BaMgAl10O17:Eu2+, the luminescent intensity and decay time of BaAl12O19:Mn2+. In this literature, BaMgAl10O17:Eu2+and BaAl12O19:Mn2+were choosed as the research object, and some experimental work were did for develop the luminescent mechanisms of these two phosphors in Vacuum ultraviolet and to improve its luminescent properties, such as some thermal processes, doping some other ions and synthesize nano phosphors. The main works were contained as below:
1. Blue phosphor BaMgAl10O17:Eu2+was annealed in air, nitrogen and reduction atmosphere for different times, the luminance degradation was evaluated, and the influence of defects in the thermal degradation was discussed; meanwhile, the self-reduction of Eu3+in BaMgAl10O17:Eu2+was discussed by theory of charge balance, and the influence of Eu2+sites in BaMgAl10O17:Eu2+on the photoluminescence and thermal properties were discussed in detailed.
2. The crystal structure of BaMgAl10O17was carefully discussed, and the formation of lattice defects was also discussed, the band structure was calculated by computer simulation via Castep; considering the lower electronegativity elements can improve the the stability properties of conduction layer, the influence of doped S such as its ion radius and electronegativity on the photoluminescence and thermal properties were discussed; the influence of doped Si3N4on the photoluminescence and thermal properties were discussed based on its ion radius and electronegativity, and the energy transfer between Eu2+and Mn2+was also discussed.
3. Nano meter blue phosphor BaMgAl10O17:Eu2+was synthesized via sol-gel method, its growth process was investigated by change the burning temperature, reaction time and heating rate etc; the difference of photoluminescence between nano and bulk BaMgAl10O17:Eu2+phosphor under254nm and147nm excitation were evaluated, and the influence of defects on the photoluminescence and thermal properties were investigated, its potential application in3D-PDP was also evaluated.
4. The crystal structure of BaAl12O19and the formation of lattice defects were studied; S and Si3N4were introduced in to BaAl12O19:0.1Mn2+, considering the lower electronegativity elements can improve the the stability properties of conduction layer, the change of photoluminescence properties and decay time were investigated based on the ion radius and electronegativity of S and Si3N4, the influence of defects in the energy transfer also investigated.
These works indicated that defect play an important role in the thermal degradation of BaMgAl10O17:Eu2+; S and Si-N doped BaMgAl10O17:Eu2+and BaAl12O19:0.1Mn2+exhibits better intensity, good thermal stability and shorter decay time respectively, which have potential application in mercury free fluorescent lamp or3D-PDP; the cubic like sharp BaMgAl10O17:Eu2+phosphor also have potential application in3D-PDP.
1、通过在空气、氮气、还原气氛下对BaMgAl10O17:Eu2+蓝色发光材料进行不同时间的热处理,对比其光衰情况,研究了缺陷在BaMgAl10O17Eu2+蓝色发光材料热劣化中所起到的作用；同时,利用电荷平衡理论讨论Eu3+离子的自还原现象,讨论了在氮气和还原气氛下合成的样品中Eu2+离子的格位占据情况,并研究了Eu2+离子在BaMgAl10O17:Eu2+蓝色发光材料中的占位情况与其对热稳定性的影响。
2、通过对BaMgAl10O17晶体结构进行解析,分析了BaMgAl10O17:Eu2+中缺陷的形成机理,通过Castep程序计算了掺杂对于BaMgAl10O17电子结构的影响；考虑到低电负性的元素的引入,可以有效的提高BaMgAl10O17:Eu2+镜面层的稳定性,在BaMgAl10O17:Eu2+中掺入了S,研究了S的离子半径与电负性对于BaMgAl10O17:Eu2+发光以及热稳定性的影响,在BaMgAl10O17:Eu2+,Mn2+中引入Si3N4性,研究了Si3N4的掺入对于BaMgAl10O17Eu2+,Mn2+发光、热稳定性的影响,以及BaMgAl10O17Eu2+,Mn2+中能量传递机理。
3、利用溶胶凝胶法,探讨改变溶胶凝胶法中的预烧温度、反应时间、升温速率等因素对于制备微纳米BaMgAI10O17Eu2+样品的影响,并研究其生长过程；通过比较纳米样品和块体样品热处理前后在254nm紫外和147nm真空紫外下的发光差异,讨论了纳米样品和块体样品的发光性能差异,缺陷对于纳米样品热稳定性的影响以及纳米发光材料在3D-PDP显示器件方面的应用前景。
4、通过对BaAl12O190.1Mn2+晶体结构进行解析,分析了BaAl12O190.1Mn2+中缺陷的形成机理,针对BaAl12O190.1Mn2+中的缺陷形成机理,考虑低电负性元素对于镜面层的改性作用,在BaAl12O190.1Mn2+中掺入了S和Si3N4,研究了S和Si3N4的离子半径与电负性对于BaAl12O190.1Mn2+发光性能以及对于衰减时间的影响；研究了缺陷在能量传递机理以及衰减时间中所起到的作用。
上述研究表明,缺陷在BaMgAl10O17Eu2+蓝色发光材料的热劣化机理中扮演了重要角色,S和Si-N掺杂的BaMgAl10O17Eu2+和BaAl12O190.1Mn2+分别表现了高的发光亮度、好的热稳定性以及短的衰减时间,有望于应用于无汞荧光灯或3D-PDP,而类四方体形貌的BaMgAl10O17Eu2+蓝色发光材料也有希望应用于3D-PDP。
Due to its thin panel, a slight weight, an extensive visual angle, a large screen size, high-speed response with emissive, high contrast, more saturated colors etc, Plasma display panels (PDPs) were widely used in displays, especially in3D and high definition displays for its characteristics of higher response speed. The quality of Vacuum ultraviolet (VUV) luminescent materials is the key point of PDPs such as luminescence efficiency, color purity, decay time and stability play important role on the quality of displays. Phosphors based on hexaaluminates were widely used as PDP commercial materials, especially the blue phosphor BaMgAl10O17:Eu2+and green phosphor BaAl12O19:Mn2+, both of which exhibit excellent luminescent properties. However, there still some un-solved problems restrict its application in PDP, especially in3D displays, such as the degradation of BaMgAl10O17:Eu2+, the luminescent intensity and decay time of BaAl12O19:Mn2+. In this literature, BaMgAl10O17:Eu2+and BaAl12O19:Mn2+were choosed as the research object, and some experimental work were did for develop the luminescent mechanisms of these two phosphors in Vacuum ultraviolet and to improve its luminescent properties, such as some thermal processes, doping some other ions and synthesize nano phosphors. The main works were contained as below:
1. Blue phosphor BaMgAl10O17:Eu2+was annealed in air, nitrogen and reduction atmosphere for different times, the luminance degradation was evaluated, and the influence of defects in the thermal degradation was discussed; meanwhile, the self-reduction of Eu3+in BaMgAl10O17:Eu2+was discussed by theory of charge balance, and the influence of Eu2+sites in BaMgAl10O17:Eu2+on the photoluminescence and thermal properties were discussed in detailed.
2. The crystal structure of BaMgAl10O17was carefully discussed, and the formation of lattice defects was also discussed, the band structure was calculated by computer simulation via Castep; considering the lower electronegativity elements can improve the the stability properties of conduction layer, the influence of doped S such as its ion radius and electronegativity on the photoluminescence and thermal properties were discussed; the influence of doped Si3N4on the photoluminescence and thermal properties were discussed based on its ion radius and electronegativity, and the energy transfer between Eu2+and Mn2+was also discussed.
3. Nano meter blue phosphor BaMgAl10O17:Eu2+was synthesized via sol-gel method, its growth process was investigated by change the burning temperature, reaction time and heating rate etc; the difference of photoluminescence between nano and bulk BaMgAl10O17:Eu2+phosphor under254nm and147nm excitation were evaluated, and the influence of defects on the photoluminescence and thermal properties were investigated, its potential application in3D-PDP was also evaluated.
4. The crystal structure of BaAl12O19and the formation of lattice defects were studied; S and Si3N4were introduced in to BaAl12O19:0.1Mn2+, considering the lower electronegativity elements can improve the the stability properties of conduction layer, the change of photoluminescence properties and decay time were investigated based on the ion radius and electronegativity of S and Si3N4, the influence of defects in the energy transfer also investigated.
These works indicated that defect play an important role in the thermal degradation of BaMgAl10O17:Eu2+; S and Si-N doped BaMgAl10O17:Eu2+and BaAl12O19:0.1Mn2+exhibits better intensity, good thermal stability and shorter decay time respectively, which have potential application in mercury free fluorescent lamp or3D-PDP; the cubic like sharp BaMgAl10O17:Eu2+phosphor also have potential application in3D-PDP.
引文
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