新型照明显示器件用氧氮化物荧光粉的性能研究
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摘要
随着人类社会的快速发展,作为人们生活基本需求之一的照明显示技术也表现出日新月异的变化。特别是在近些年,新一代的照明显示技术,如LED(发光二级管)和PDP(等离子平板显示技术)等,取得了突飞猛进的进展。相对于传统技术,LED和PDP技术有以下优点：能量转换效率高,对环境友好无(低)污染,图像质量高,性能稳定,可在全数字模式下工作等等,因此已经逐渐得到学界以及市场的广泛认可,是具有广阔发展前景的高新技术产业。
在照明及显示器件中,荧光材料是非常重要的组成部分,因为它承担了将光源发出的光转化成所需要色彩的作用,因此,荧光材料的品质直接决定了观察者的最终感受。正因为荧光材料具有如此重要的地位,伴随近年来照明显示技术的快速发展,对于荧光材料的研究也越来越受到重视。传统的荧光材料主要是氧化物、硫化物、含氧酸盐等,这些材料合成方法较为简单,并且由于已经经过长期的研究,在技术方面已经较为成熟。但是由于新一代光源(LED,等离子体等)的普及,这些传统材料在性能上已经逐渐难以满足需要。
作为一种优秀的荧光材料,它需要具有以下基本性质：光转化效率高、合适的激发和发射波长、化学及热稳定性好等,如果要应用于显示领域,荧光材料还需要具有快速的响应时间。正是由于在这些方面具有巨大的发展潜力,氧氮化物荧光材料在近些年逐渐兴起并取得了快速的发展。为了对氧氮化物荧光粉进行探索研究,本工作主要对硅基氧氮化物荧光材料——稀土离子激活的CaSi2O2N2的合成条件、发光性能、材料优化、能级分布等进行了研究和探讨,同时还研究了Si-N掺杂对于铝酸盐荧光粉荧光性能的影响。通过这些研究,希望能够在氧氮化物荧光粉性能的预估、优化以及Si-N键对荧光粉性能的作用机理上探索理论和实验依据,为今后荧光材料的研究开发提供一定的参考。
论文的第一章简单阐述了照明及显示技术的发展历程,并且通过介绍相关文献和技术,对传统荧光粉材料的结构特点、发光原理和性能、优点以及不足进行了说明,然后介绍了新型照明及显示技术的现状和需求,并在此基础上提出了本文的工作思路。
在第二章中,介绍了本工作的实验部分,主要包括：起始原料、材料合成设备、合成工艺流程、材料性能表征技术等。
论文的第三章包括两个部分：第一,阐述了Eu2+掺杂的CaSi2O2N2荧光材料的合成条件、晶体结构、从真空紫外波段到可见光区域的荧光性能等。通过研究表明：在真空紫外光谱中,材料的激发对应于基质的晶格吸收,然后会发生从晶格到发光中心Eu2+的能量转移并最终发射出来；在紫外或蓝光激发下,则在Eu2+离子自身发生从4f能级到5d能级的电子跃迁。由于发光来源于Eu2+离子中电子从5d能级向4f能级的跃迁,因此在任何波段的光源激发下,材料的发射光谱都是区间在绿光-黄光波段的宽带谱。第二,探讨了离子共掺对于CaSi2O2N2:Eu2+发光性能的影响以及产生影响的机理,内容包括共掺杂的元素选择、掺杂离子的配比含量、基质材料的氧氮比例调整、不同发光中心之间的能量传递、掺杂前后离子的价态变化等等。研究结果表明：1.在荧光材料中,稳定Eu离子的价态对材料的荧光性能有明显优化作用。当加入适当的共掺离子时,共掺离子能够影响材料中缺陷的存在状态,并与Eu2+形成更加稳定的缺陷组合,有效地稳定材料中的Eu2+离子,从而提高有效的发光中心浓度,大幅减少Eu2+和Eu3+离子之间的非辐射能量传递,进而优化荧光粉的荧光性能。本工作不仅在实验上观察到了这种价态稳定现象,并且从理论计算的角度也证明了这种稳定机理的存在。2.通过改变基质材料氧氮比例的方法,能够影响材料的色坐标、发光强度等荧光性能。
第四章对不同镧系离子在材料中的发光行为进行了表征和分析。对于在发光过程中镧系离子的电子跃迁方式进行了分析和归类,研究了不同镧系离子之间的能量传递现象。最终,根据对这些离子发光行为的系统分析,得到了镧系离子在CaSi2O2N2基质中的部分能级分布情况,并据此对材料中镧系离子的发光行为给出了一定程度的解释。
在第五章中,通过在CaAl2O4基质中掺杂Si-N键来部分取代Al-O键的方法,提高了荧光粉的发光强度和余辉性能。通过电子顺磁共振(EPR)的方法,证明掺杂Si-N倾向于取代Eu2+附近的Al-O,并且由于Si-N键具有较短的键长,导致引入的Si-N能够提高发光中心周围晶体骨架的刚性,减少热震动导致的非辐射跃迁能量损失,从而提高荧光粉的发光性能。
第六章中简单介绍了Tb3+和Ce3+离子激活的CaSiO3和Ca2SiO4基质荧光粉的荧光性能。
第七章则对全文进行了总结并对今后的工作进行展望。
The lighting technology is one of the most basic demands in daily life and therefore has been growing rapidly with the development of the society. In particular, the new lighting technologies, such as LEDs (light emitting diodes) and PDP (plasma flat-panel display technology), etc., have made rapid progress in recent years. Compared to traditional technologies, the LED and the PDP technologies have the following advantages:high energy conversion efficiency and environmental friendliness without (low) pollution, high image quality, stable performance in all-digital mode, and therefore has been admitted both in academic and market.
In lighting and display equipments, phosphors which convert the light from the light source into different colors are indispensable components. Moreover, the phosphors directly determine the quality of the observers'final experience. As phosphors have such an important position, they have gotten more and more attention along with the rapid development of the lighting technology. The conventional phosphors are mainly oxides, sulfides, oxysalts and so on. However, only a very limited number of present phosphors can meet the minimum requirements for the new generation of lighting and display technology. Therefore, to modify existing and explore new phosphor materials is extremely urgent.
A new class of inorganic phosphors, namely rare-earth-doped silicon oxynitrides, has attracted much attention in recent years due to their high chemical and thermal stability as well as their unusual luminescence properties. In order to research the oxynitrides, the present work studied the rare-earth ions activated CaSi2O2N2on the synthesis conditions, luminescent properties, optical optimization, and the energy level distribution. On the other hand, the influence of Si-N codoping in the aluminate phosphors has also been studied.
In Chapter Ⅰ, the development process of lighting and display technologies was briefly introduced, and a brief description about conventional and newly phosphors was given with relevant literatures and technologies.
In Chapter Ⅱ the experimental process of this work is described, including the starting materials, synthesis equipment, the synthesis process, material testing techniques.
Chapter Ⅲ consists of three parts.(1) The synthesis conditions, crystal structure, and the photoluminescence properties of Eu2+doped CaSi2O2N2were studied. The results show that in the VUV region, the excitation corresponds to the host absorption, and the energy transfer from host to activators exists. The excitation from ultraviolet to blue originates from the electronic transitions from the4f ground level to the5d levels of Eu2+. The light emission located in the green-yellow region and corresponds to the electronic transitions from the5d levels to the4f levels.(2) The photoluminescence properties of CaSi2O2N2:Eu2+may be greatly impact by Lanthanide3+ions. The optimization mechanism was studied in detail by the case of La3+doping. The La3+ions could stabilize Ca2+vacancies, inhibit the oxidization of Eu2+to Eu3+, and consequently increase the total number of activators. Meanwhile, new defect-energy levels were detected. These defects might capture electrons which were excited from Eu2+to the conductive band, and then detrap a considerable amount of the electrons back to the5d levels of Eu2+ions.(3) The influence of some other co-dopants was also discussed in the material.
In Chapter IV, The photoluminescence properties of different lanthanide ions in the material were characterized and analyzed systematically. Energy transitions attributed to electron transfers from4f to4f (ff), from4f to5d (fd), from5d to4f (df) and charge transfer (CT) transition were obtained and classified. Finally, an energy-level diagram of lanthanide-ions in CaSi2O2N2was proposed. The diagram matches perfectly with the experimental results and explains the luminescence properties of lanthanide-doped CaSi2O2N2phosphors.
In Chapter V, the impact on the photoluminescence and afterglow properties of CaAl2O4:Eu2+via Si-N co-doping was discussed. A small amount of Si-N was introduced into the conventional phosphor CaAl2O4:Eu2+, and obviously improved the photoluminescence intensity. It was proved that the Si-N bands preferred to replace the the Al-O near Eu2+though electron paramagnetic resonance (EPR) measurements. Since Si-N bond has a shorter bond length, they may improve the lattice rigidity around Eu2+. As a result, the energy loss caused by the lattice vibration may be reduced.
In Chapter VII, Tb3+and/or Ce3+activated CaSiO3and Ca2SiO4phosphors were synthesized and their photoluminescence properties were discussed.
Chapter VII consists of summary and future work outlook.
在照明及显示器件中,荧光材料是非常重要的组成部分,因为它承担了将光源发出的光转化成所需要色彩的作用,因此,荧光材料的品质直接决定了观察者的最终感受。正因为荧光材料具有如此重要的地位,伴随近年来照明显示技术的快速发展,对于荧光材料的研究也越来越受到重视。传统的荧光材料主要是氧化物、硫化物、含氧酸盐等,这些材料合成方法较为简单,并且由于已经经过长期的研究,在技术方面已经较为成熟。但是由于新一代光源(LED,等离子体等)的普及,这些传统材料在性能上已经逐渐难以满足需要。
作为一种优秀的荧光材料,它需要具有以下基本性质：光转化效率高、合适的激发和发射波长、化学及热稳定性好等,如果要应用于显示领域,荧光材料还需要具有快速的响应时间。正是由于在这些方面具有巨大的发展潜力,氧氮化物荧光材料在近些年逐渐兴起并取得了快速的发展。为了对氧氮化物荧光粉进行探索研究,本工作主要对硅基氧氮化物荧光材料——稀土离子激活的CaSi2O2N2的合成条件、发光性能、材料优化、能级分布等进行了研究和探讨,同时还研究了Si-N掺杂对于铝酸盐荧光粉荧光性能的影响。通过这些研究,希望能够在氧氮化物荧光粉性能的预估、优化以及Si-N键对荧光粉性能的作用机理上探索理论和实验依据,为今后荧光材料的研究开发提供一定的参考。
论文的第一章简单阐述了照明及显示技术的发展历程,并且通过介绍相关文献和技术,对传统荧光粉材料的结构特点、发光原理和性能、优点以及不足进行了说明,然后介绍了新型照明及显示技术的现状和需求,并在此基础上提出了本文的工作思路。
在第二章中,介绍了本工作的实验部分,主要包括：起始原料、材料合成设备、合成工艺流程、材料性能表征技术等。
论文的第三章包括两个部分：第一,阐述了Eu2+掺杂的CaSi2O2N2荧光材料的合成条件、晶体结构、从真空紫外波段到可见光区域的荧光性能等。通过研究表明：在真空紫外光谱中,材料的激发对应于基质的晶格吸收,然后会发生从晶格到发光中心Eu2+的能量转移并最终发射出来；在紫外或蓝光激发下,则在Eu2+离子自身发生从4f能级到5d能级的电子跃迁。由于发光来源于Eu2+离子中电子从5d能级向4f能级的跃迁,因此在任何波段的光源激发下,材料的发射光谱都是区间在绿光-黄光波段的宽带谱。第二,探讨了离子共掺对于CaSi2O2N2:Eu2+发光性能的影响以及产生影响的机理,内容包括共掺杂的元素选择、掺杂离子的配比含量、基质材料的氧氮比例调整、不同发光中心之间的能量传递、掺杂前后离子的价态变化等等。研究结果表明：1.在荧光材料中,稳定Eu离子的价态对材料的荧光性能有明显优化作用。当加入适当的共掺离子时,共掺离子能够影响材料中缺陷的存在状态,并与Eu2+形成更加稳定的缺陷组合,有效地稳定材料中的Eu2+离子,从而提高有效的发光中心浓度,大幅减少Eu2+和Eu3+离子之间的非辐射能量传递,进而优化荧光粉的荧光性能。本工作不仅在实验上观察到了这种价态稳定现象,并且从理论计算的角度也证明了这种稳定机理的存在。2.通过改变基质材料氧氮比例的方法,能够影响材料的色坐标、发光强度等荧光性能。
第四章对不同镧系离子在材料中的发光行为进行了表征和分析。对于在发光过程中镧系离子的电子跃迁方式进行了分析和归类,研究了不同镧系离子之间的能量传递现象。最终,根据对这些离子发光行为的系统分析,得到了镧系离子在CaSi2O2N2基质中的部分能级分布情况,并据此对材料中镧系离子的发光行为给出了一定程度的解释。
在第五章中,通过在CaAl2O4基质中掺杂Si-N键来部分取代Al-O键的方法,提高了荧光粉的发光强度和余辉性能。通过电子顺磁共振(EPR)的方法,证明掺杂Si-N倾向于取代Eu2+附近的Al-O,并且由于Si-N键具有较短的键长,导致引入的Si-N能够提高发光中心周围晶体骨架的刚性,减少热震动导致的非辐射跃迁能量损失,从而提高荧光粉的发光性能。
第六章中简单介绍了Tb3+和Ce3+离子激活的CaSiO3和Ca2SiO4基质荧光粉的荧光性能。
第七章则对全文进行了总结并对今后的工作进行展望。
The lighting technology is one of the most basic demands in daily life and therefore has been growing rapidly with the development of the society. In particular, the new lighting technologies, such as LEDs (light emitting diodes) and PDP (plasma flat-panel display technology), etc., have made rapid progress in recent years. Compared to traditional technologies, the LED and the PDP technologies have the following advantages:high energy conversion efficiency and environmental friendliness without (low) pollution, high image quality, stable performance in all-digital mode, and therefore has been admitted both in academic and market.
In lighting and display equipments, phosphors which convert the light from the light source into different colors are indispensable components. Moreover, the phosphors directly determine the quality of the observers'final experience. As phosphors have such an important position, they have gotten more and more attention along with the rapid development of the lighting technology. The conventional phosphors are mainly oxides, sulfides, oxysalts and so on. However, only a very limited number of present phosphors can meet the minimum requirements for the new generation of lighting and display technology. Therefore, to modify existing and explore new phosphor materials is extremely urgent.
A new class of inorganic phosphors, namely rare-earth-doped silicon oxynitrides, has attracted much attention in recent years due to their high chemical and thermal stability as well as their unusual luminescence properties. In order to research the oxynitrides, the present work studied the rare-earth ions activated CaSi2O2N2on the synthesis conditions, luminescent properties, optical optimization, and the energy level distribution. On the other hand, the influence of Si-N codoping in the aluminate phosphors has also been studied.
In Chapter Ⅰ, the development process of lighting and display technologies was briefly introduced, and a brief description about conventional and newly phosphors was given with relevant literatures and technologies.
In Chapter Ⅱ the experimental process of this work is described, including the starting materials, synthesis equipment, the synthesis process, material testing techniques.
Chapter Ⅲ consists of three parts.(1) The synthesis conditions, crystal structure, and the photoluminescence properties of Eu2+doped CaSi2O2N2were studied. The results show that in the VUV region, the excitation corresponds to the host absorption, and the energy transfer from host to activators exists. The excitation from ultraviolet to blue originates from the electronic transitions from the4f ground level to the5d levels of Eu2+. The light emission located in the green-yellow region and corresponds to the electronic transitions from the5d levels to the4f levels.(2) The photoluminescence properties of CaSi2O2N2:Eu2+may be greatly impact by Lanthanide3+ions. The optimization mechanism was studied in detail by the case of La3+doping. The La3+ions could stabilize Ca2+vacancies, inhibit the oxidization of Eu2+to Eu3+, and consequently increase the total number of activators. Meanwhile, new defect-energy levels were detected. These defects might capture electrons which were excited from Eu2+to the conductive band, and then detrap a considerable amount of the electrons back to the5d levels of Eu2+ions.(3) The influence of some other co-dopants was also discussed in the material.
In Chapter IV, The photoluminescence properties of different lanthanide ions in the material were characterized and analyzed systematically. Energy transitions attributed to electron transfers from4f to4f (ff), from4f to5d (fd), from5d to4f (df) and charge transfer (CT) transition were obtained and classified. Finally, an energy-level diagram of lanthanide-ions in CaSi2O2N2was proposed. The diagram matches perfectly with the experimental results and explains the luminescence properties of lanthanide-doped CaSi2O2N2phosphors.
In Chapter V, the impact on the photoluminescence and afterglow properties of CaAl2O4:Eu2+via Si-N co-doping was discussed. A small amount of Si-N was introduced into the conventional phosphor CaAl2O4:Eu2+, and obviously improved the photoluminescence intensity. It was proved that the Si-N bands preferred to replace the the Al-O near Eu2+though electron paramagnetic resonance (EPR) measurements. Since Si-N bond has a shorter bond length, they may improve the lattice rigidity around Eu2+. As a result, the energy loss caused by the lattice vibration may be reduced.
In Chapter VII, Tb3+and/or Ce3+activated CaSiO3and Ca2SiO4phosphors were synthesized and their photoluminescence properties were discussed.
Chapter VII consists of summary and future work outlook.
引文
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