稀土磷酸盐K_2LnZr(PO_4)_3(Ln=Gd,Y)基量子剪裁荧光粉
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摘要
近几十年来,为了适应无汞荧光灯和等离子平板显示(PDP)技术的发展,探寻新型量子剪裁荧光粉作为研究开发高量子效率真空紫外发光材料的一种新途径逐渐受到广泛的关注。稀土磷酸盐基质在VUV区有较强的吸收,且合成温度低、制备方法简单、物理化学性质稳定、热稳定性好、溶解度低和透光性好,是高效真空紫外荧光粉比较理想的基质。稀土元素由于其独特的电子层结构及物理化学性质而被广泛的应用于传统发光材料的改性和新材料的开发研究中。本论文以不同稀土离子掺杂的稀土磷酸盐K2LnZr(PO4)3(Ln=Gd,Y)作为研究对象,对于基质中不同离子对之间的能量传递过程和可见光量子剪裁现象做了初步的探索研究。内容主要包括以下几个方面：
(1)采用高温固相法制备了K2Gd1-xZr(PO4)3：Eux3+(0.02≤x≤0.1),并研究了其在紫外(UV)和真空紫外(VUV)区域的光致发光特性,结果表明：在Eu3+掺杂的K2GdZr(PO4)3体系中可以观察到基于Gd3+-Eu3+离子对间能量传递的量子剪裁下转换现象。在186 nm(Gd3+离子6GJ能级)激发下,该量子剪裁过程通过Gd3+离子到Eu3+离子的两步能量传递过程即交叉弛豫过程(第一步)及剩余激发能的直接传递过程(第二步)实现,并发射出两个可见的红光光子。Gd3+,Eu3+之间能量传递的量子效率可以达到155%。K2GdZr(PO4)3：Eu3+是一种有潜力的量子剪裁发光材料。
(2)利用高温固相法合成了K2YZr(PO4)3和K2Y1-xZr(PO4)3：xPr3+(0.01≤x≤0.05),通过对K2YZr(PO4)3：Pr3+系列样品在UV-VUV激发下的发射光谱和激发光谱的分析测试,在Pr3+离子掺杂的K2YZr(PO4)3荧光粉中观察到了一种新的光子级联发射现象,这在234 nm和147 nm激发下的发射光谱中得到了验证。该双光子级联发射过程中的第一步光子发射位于407 nm,对应Pr3+离子的1S0→1I6跃迁,属于自旋允许的4f5d→4f2跃迁,第二步发射的光子在610 nm附近,归属于3P0→3H6跃迁,为自旋禁戒的4f2→4f2跃迁。实验结果表明,在K2YZr(PO4)3：Pr3+中即使Pr3+离子1S0能级的能量高于4f15d1能级,双光子级联发射过程仍有可能实现。
(3)采用高温固相法成功合成了新型的K2YZr(PO4)3：Pr3+,Mn2+量子剪裁荧光粉,并研究了其在UV-VUV激发下的光谱性能并讨论了可见光量子剪裁过程,结果表明归属于Mn2+离子6A1g→4Eg-4A1g跃迁的光子能量与Pr3+离子1S0→1I6跃迁发射的能量相匹配,因此当Mn2+离子作为共激活剂离子掺入K2YZr(PO4)3基质中后,能够将Pr3+离子级联发射过程中第一步发射的对应于1S0→1I6,3PJ跃迁的光子转换成为Mn2+离子的红光发射,而这一过程是通过Pr→Mn之间的能量传递实现的。通过对系列样品量子效率的计算得出最佳量子效率可以达到126.3%左右。
(4)对K2GdZr(PO4)3：Er3+,Tb3+荧光粉中量子剪裁效应的研究以及量子效率的计算结果表明,Er3+-Gd3+-Tb3+体系中三个发光中心之间可以通过合作能量的过程实现可见光量子剪裁,在这个能量传递过程中Gd3+起到了“中介”的作用,而Er3+→Gd3+之间能量传递过程的有效性决定了量子剪裁效应存在的可能性。该可见光量子剪裁荧光粉的最佳量子效率为110%。
(5)研究了K2GdZr(PO4)3基质中Dy3+→Tb3+之间的能量传递过程,结果表明通过Dy3+→Tb3+之间非常有效的能量传递,Tb3+离子5D4→7F5跃迁发射增强,此过程中Tb3+通过两步能量传递实现了双光子发射。此外Gd3+→Tb3+和Gd3+→Dy3+间的能量传递也被观察到。
此外,考虑到实际应用的问题,为了探寻更多的能够实现高效量子剪裁发光的离子及离子对,本论文中还对其它稀土离子和离子对间的能量传递过程进行了研究,虽然结果不是很理想,但是依然为今后进一步的研究工作提供了参考。
Recently, for the development of non-mercury fluorescent tubes and plasma display panels (PDP) technology, new quantum cutting (two-photon luminescent) phosphors are required for the investigation of high efficient luminescent materials under VUV excitation. Rare-earth orthophosphates have stronger absorption in the range of the VUV and are more easily implemented. Besides, they have many advantages, such as high physical-chemical stability, low synthesis temperature and solubility, transparent, etc. Therefore, rare-earth orthophosphates could be ideal hosts for high luminescence efficiency VUV phosphors. Rare-earth (RE) ions are proper activators due to their abundant energy levels and physical-chemical properties. In the present work, the phenomena of energy transfer between different ion pairs and visible quantum cutting in rare-earth orthophosphate K2LnZr(PO4)3 (Ln= Gd, Y) doped with different rare-earth ions have been investigated. The content of this paper includes:
(1) K2Gd1-xZr(PO4)3:Eux3+(0.02≤x≤0.1) were prepared by solid-state reaction method and their photoluminescence properties were investigated in ultra-violet (UV) and vacuum ultra-violet (VUV) region. The phenomenon of visible quantum cutting through downconversion was observed for the Gd3+-Eu3+ couple in this Eu3+-doped K2GdZr(PO4)3 system. Visible quantum cutting, the emission of two visible light photons per absorbed VUV photon, occured upon the 186 nm excitation of Gd3+ at the 6GJ level via two-step energy transfer from, Gd3+ to Eu3+ by cross relaxation and sequential transfer of the remaining excitation energy. The results revealed that the efficiency of the energy transfer process from Gd3+ to Eu3+ in the Eu3+-doped K2GdZr(PO4)3 system could reach to 155% and K2GdZr(PO4)3:Eu3+ was effective quantum cutting material.
(2) In present work, K2Y1-xZr(PO4)3:Prx3+(1 mol.%≤x=≤5 mol.%) samples were prepared by solid-state reaction method and their photoluminescence properties were investigated in ultra-violet (UV) and vacuum ultra-violet (VUV) region. The results indicate that, in Pr3+-doped K2YZr(PO4)3 phosphor, even if the 1S0 state is above the lowest 4f5d energy level, the photon cascade emission (PCE) process for Pr3+ still could occur under 147 nm and 234 nm (4f15d1 state) excitation.
(3) K2YZr(PO4)3:Pr3+, Mn2+ single-phase powder samples were prepared by solid-state reaction method and their photoluminescence (PL) properties were investigated in ultra-violet (UV) and vacuum ultra-violet (VUV) region. The results indicated that in Pr3+ singly doped K2YZr(PO4)3 sample, the first-step transition(1So→I6,3PJ around 405 nm) of Pr3+ is near the ultraviolet (UV) range, not useful for practical application. When Mn2+ was doped as a co-activator ion, the energy of 1So→I6,3PJ transition can be transferred synchronously from Pr3+ to Mn2+ and then emit a visible photon. The optimal quantum efficiency (QE) of this co-doped system K2YZr(PO4)3:Pr3+, Mn2+ reached to 126.3%, suggesting a novel type of practical visible quantum cutting phosphor in promising application.
(4) Tb3+, Er3+ co-doped K2GdZr(PO4)3 were prepared by solid-state reaction method and their photoluminescence (PL) properties were investigated in ultra-violet (UV) and vacuum ultra-violet (VUV) region. The results indicate that the energy transfers from Er3+ to Gd3+ and from Gd3+ to Tb3+ required for occurring of visible quantum cutting through downconversion were efficient. In this cooperative energy transfer process, Gd3+ was used as an intermediate of energy transfer between Er3+ and Tb3+. The optimal quantum efficiency (QE) of K2GdZr(PO4)3:Er3+, Tb3+ phosphor was estimated to be 110%.
(5) In this work, K2GdZr(PO4)3:Tb3+, Dy3+ samples were synthesized by high-temperature solid-state reaction method and their photoluminescence (PL) properties were investigated in ultra-violet (UV) and vacuum ultra-violet (VUV) region. The results indicated that the 5D4→7F5 emission of Tb3+ was enhanced observably by the efficient energy transfer from Dy3+. In this phosphor, Tb3+ emitted two green photons through a two-step energy transfer process. In addition, the energy transfer of Gd3+→Tb3+ and Gd3+→Dy3+ was also been observed, suggesting that the existence of Gd3+ is helpful for improving the luminescence intensity of this novel efficient green emitting phosphor.
In addition, from the aspect of practical application, it is necessary to seek for new rare-earth ions or ion pairs which can implement the high efficient quantum cutting process. It is unfortunately that there was no ideal result. However, these works still provide reference for the further researches.
(1)采用高温固相法制备了K2Gd1-xZr(PO4)3：Eux3+(0.02≤x≤0.1),并研究了其在紫外(UV)和真空紫外(VUV)区域的光致发光特性,结果表明：在Eu3+掺杂的K2GdZr(PO4)3体系中可以观察到基于Gd3+-Eu3+离子对间能量传递的量子剪裁下转换现象。在186 nm(Gd3+离子6GJ能级)激发下,该量子剪裁过程通过Gd3+离子到Eu3+离子的两步能量传递过程即交叉弛豫过程(第一步)及剩余激发能的直接传递过程(第二步)实现,并发射出两个可见的红光光子。Gd3+,Eu3+之间能量传递的量子效率可以达到155%。K2GdZr(PO4)3：Eu3+是一种有潜力的量子剪裁发光材料。
(2)利用高温固相法合成了K2YZr(PO4)3和K2Y1-xZr(PO4)3：xPr3+(0.01≤x≤0.05),通过对K2YZr(PO4)3：Pr3+系列样品在UV-VUV激发下的发射光谱和激发光谱的分析测试,在Pr3+离子掺杂的K2YZr(PO4)3荧光粉中观察到了一种新的光子级联发射现象,这在234 nm和147 nm激发下的发射光谱中得到了验证。该双光子级联发射过程中的第一步光子发射位于407 nm,对应Pr3+离子的1S0→1I6跃迁,属于自旋允许的4f5d→4f2跃迁,第二步发射的光子在610 nm附近,归属于3P0→3H6跃迁,为自旋禁戒的4f2→4f2跃迁。实验结果表明,在K2YZr(PO4)3：Pr3+中即使Pr3+离子1S0能级的能量高于4f15d1能级,双光子级联发射过程仍有可能实现。
(3)采用高温固相法成功合成了新型的K2YZr(PO4)3：Pr3+,Mn2+量子剪裁荧光粉,并研究了其在UV-VUV激发下的光谱性能并讨论了可见光量子剪裁过程,结果表明归属于Mn2+离子6A1g→4Eg-4A1g跃迁的光子能量与Pr3+离子1S0→1I6跃迁发射的能量相匹配,因此当Mn2+离子作为共激活剂离子掺入K2YZr(PO4)3基质中后,能够将Pr3+离子级联发射过程中第一步发射的对应于1S0→1I6,3PJ跃迁的光子转换成为Mn2+离子的红光发射,而这一过程是通过Pr→Mn之间的能量传递实现的。通过对系列样品量子效率的计算得出最佳量子效率可以达到126.3%左右。
(4)对K2GdZr(PO4)3：Er3+,Tb3+荧光粉中量子剪裁效应的研究以及量子效率的计算结果表明,Er3+-Gd3+-Tb3+体系中三个发光中心之间可以通过合作能量的过程实现可见光量子剪裁,在这个能量传递过程中Gd3+起到了“中介”的作用,而Er3+→Gd3+之间能量传递过程的有效性决定了量子剪裁效应存在的可能性。该可见光量子剪裁荧光粉的最佳量子效率为110%。
(5)研究了K2GdZr(PO4)3基质中Dy3+→Tb3+之间的能量传递过程,结果表明通过Dy3+→Tb3+之间非常有效的能量传递,Tb3+离子5D4→7F5跃迁发射增强,此过程中Tb3+通过两步能量传递实现了双光子发射。此外Gd3+→Tb3+和Gd3+→Dy3+间的能量传递也被观察到。
此外,考虑到实际应用的问题,为了探寻更多的能够实现高效量子剪裁发光的离子及离子对,本论文中还对其它稀土离子和离子对间的能量传递过程进行了研究,虽然结果不是很理想,但是依然为今后进一步的研究工作提供了参考。
Recently, for the development of non-mercury fluorescent tubes and plasma display panels (PDP) technology, new quantum cutting (two-photon luminescent) phosphors are required for the investigation of high efficient luminescent materials under VUV excitation. Rare-earth orthophosphates have stronger absorption in the range of the VUV and are more easily implemented. Besides, they have many advantages, such as high physical-chemical stability, low synthesis temperature and solubility, transparent, etc. Therefore, rare-earth orthophosphates could be ideal hosts for high luminescence efficiency VUV phosphors. Rare-earth (RE) ions are proper activators due to their abundant energy levels and physical-chemical properties. In the present work, the phenomena of energy transfer between different ion pairs and visible quantum cutting in rare-earth orthophosphate K2LnZr(PO4)3 (Ln= Gd, Y) doped with different rare-earth ions have been investigated. The content of this paper includes:
(1) K2Gd1-xZr(PO4)3:Eux3+(0.02≤x≤0.1) were prepared by solid-state reaction method and their photoluminescence properties were investigated in ultra-violet (UV) and vacuum ultra-violet (VUV) region. The phenomenon of visible quantum cutting through downconversion was observed for the Gd3+-Eu3+ couple in this Eu3+-doped K2GdZr(PO4)3 system. Visible quantum cutting, the emission of two visible light photons per absorbed VUV photon, occured upon the 186 nm excitation of Gd3+ at the 6GJ level via two-step energy transfer from, Gd3+ to Eu3+ by cross relaxation and sequential transfer of the remaining excitation energy. The results revealed that the efficiency of the energy transfer process from Gd3+ to Eu3+ in the Eu3+-doped K2GdZr(PO4)3 system could reach to 155% and K2GdZr(PO4)3:Eu3+ was effective quantum cutting material.
(2) In present work, K2Y1-xZr(PO4)3:Prx3+(1 mol.%≤x=≤5 mol.%) samples were prepared by solid-state reaction method and their photoluminescence properties were investigated in ultra-violet (UV) and vacuum ultra-violet (VUV) region. The results indicate that, in Pr3+-doped K2YZr(PO4)3 phosphor, even if the 1S0 state is above the lowest 4f5d energy level, the photon cascade emission (PCE) process for Pr3+ still could occur under 147 nm and 234 nm (4f15d1 state) excitation.
(3) K2YZr(PO4)3:Pr3+, Mn2+ single-phase powder samples were prepared by solid-state reaction method and their photoluminescence (PL) properties were investigated in ultra-violet (UV) and vacuum ultra-violet (VUV) region. The results indicated that in Pr3+ singly doped K2YZr(PO4)3 sample, the first-step transition(1So→I6,3PJ around 405 nm) of Pr3+ is near the ultraviolet (UV) range, not useful for practical application. When Mn2+ was doped as a co-activator ion, the energy of 1So→I6,3PJ transition can be transferred synchronously from Pr3+ to Mn2+ and then emit a visible photon. The optimal quantum efficiency (QE) of this co-doped system K2YZr(PO4)3:Pr3+, Mn2+ reached to 126.3%, suggesting a novel type of practical visible quantum cutting phosphor in promising application.
(4) Tb3+, Er3+ co-doped K2GdZr(PO4)3 were prepared by solid-state reaction method and their photoluminescence (PL) properties were investigated in ultra-violet (UV) and vacuum ultra-violet (VUV) region. The results indicate that the energy transfers from Er3+ to Gd3+ and from Gd3+ to Tb3+ required for occurring of visible quantum cutting through downconversion were efficient. In this cooperative energy transfer process, Gd3+ was used as an intermediate of energy transfer between Er3+ and Tb3+. The optimal quantum efficiency (QE) of K2GdZr(PO4)3:Er3+, Tb3+ phosphor was estimated to be 110%.
(5) In this work, K2GdZr(PO4)3:Tb3+, Dy3+ samples were synthesized by high-temperature solid-state reaction method and their photoluminescence (PL) properties were investigated in ultra-violet (UV) and vacuum ultra-violet (VUV) region. The results indicated that the 5D4→7F5 emission of Tb3+ was enhanced observably by the efficient energy transfer from Dy3+. In this phosphor, Tb3+ emitted two green photons through a two-step energy transfer process. In addition, the energy transfer of Gd3+→Tb3+ and Gd3+→Dy3+ was also been observed, suggesting that the existence of Gd3+ is helpful for improving the luminescence intensity of this novel efficient green emitting phosphor.
In addition, from the aspect of practical application, it is necessary to seek for new rare-earth ions or ion pairs which can implement the high efficient quantum cutting process. It is unfortunately that there was no ideal result. However, these works still provide reference for the further researches.
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