新型电子俘获型红外转可见硅酸盐光转换材料发光性能的研究
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摘要
电子俘获型光转换材料(Electron trapping materials)具有光转换特性，在发光学领域也被称为光激励材料。这种材料自1986年由美国的Lindmayer首次提出以来便一直受到广泛的关注。在红外探测、光存储、红外光转换以及X射线成像等方面有其广泛的应用前景。光激励材料在受到光辐射后，电子（或空穴）可以被陷阱俘获而处于一种相对稳定的状态。当用红外光或者其他形式的光再次照射材料时，陷阱中的电子（或空穴）就能够释放出来形成光激励发光(photostimulated luminescence)。目前，可以商业化的红外转可见光转换材料主要是碱土金属硫化物系列，这种材料具有光激励发光初始强度高，光激励光存储量大等诸多优点。但是，硫化物的致命缺陷就是化学性质不稳定。最重要的是硫化物分解后会产生有毒物质，对环境造成严重的污染。针对这些问题，寻找一种化学性质稳定的光激励材料已经成为目前光激励材料研究的焦点。
硅酸盐有较好的化学稳定性，且耐高温、抗腐蚀。目前被广泛的用作稀土发光材料的基体材料。其中，Sr_3SiO_5: Eu~(2+)是一类传统的LED(light emitting diodes)用荧光粉，可以有效的吸收紫外光和蓝绿光发出以580nm为中心的黄光。本论文以Sr_3SiO_5: Eu~(2+)为研究对象，通过掺入另一种共激活剂的方式引入陷阱以提高其光激励发光性能。主要的研究成果如下：
1)研究了镧系共激活剂(La、Ce、Pr、Nd、Sm、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu)对材料Sr_(2.99)SiO_5:0.01Eu~(2+)的光激励发光性能的影响。我们发现：和其他共激活剂相比，Tm~(3+)掺杂的样品具有非常好的光激励发光性能。其光激励初始强度、光激励光存储量等性能都有不同程度的提高。其原因是因为掺杂Tm~(3+)的样品产生了一个新的陷阱（陷阱B），这个陷阱可以很大程度的提高材料的光激励发光性能；
2)系统的研究了不同浓度Tm~(3+)掺杂下Sr_(2.99)SiO_5:0.01Eu~(2+)光激励发光性能的变化。经研究我们发现：当Tm~(3+)的掺杂浓度为0.0004时，材料的光激励发光初始强度和光激励光存储量性能均达到了最佳。其中，光激励发光初始强度是未掺杂样品的33倍，光激励光存储量是未掺杂样品的2倍。充分的显示出该材料在红外探测等方面的广阔应用前景。当Tm~(3+)掺杂浓度为0.0004时，材料中陷阱B的数量也同样达到最大值。这说明陷阱B的数量与材料的光激励发光性能有着很强的对应关系；
3)研究了Sr_(2.9896)SiO_5:0.01Eu~(2+),0.0004Tm~(3+)中的陷阱A和陷阱B中电子的迁移规律。经过对数据的整理和分析，我们得出如下结论：陷阱A和B都可以分成两类，其本质区别是它们距离发光中心Eu~(2+)的远近不同。第一类陷阱距离Eu~(2+)较近，陷阱中的电子很容易与Eu~(2+)的基态能级发生电荷迁移效应。在热激励的条件下，陷阱中的电子仍然可以转化成光子形成发光，而在光激励的条件下则很容易发生无辐射跃迁。第二类陷阱是距离Eu~(2+)较远的陷阱，这类陷阱中的电子无论在热激励还是光激励条件下都可以转化成光子形成发光。不同之处在于，第二类陷阱A中电子在光激励条件下释放速率缓慢不能形成较强的光激励发光，而第二类陷阱B中的电子在光激励的条件下则可以快速的释放形成较强的光激励发光。与此同时，我们还发现在长余辉衰减过程中，陷阱A释放出的电子可以被陷阱B再次俘获。这就是陷阱B的电子再俘获效应；
4)探索性的研究了Ba元素对材料Sr_(2.9896)SiO_5:0.01Eu~(2+),0.0004Tm~(3+)的荧光发光、长余辉发光以及光激励发光性能的影响。材料的荧光发射、长余辉发射和光激励发射峰位都随着Ba元素的逐渐添加而发生红移。这是因为Ba元素的掺入改变了基体材料的晶格参数而造成发光中心Eu~(2+)的5d能级下降，材料的发射峰位发生红移。Ba元素逐渐掺入后，材料的长余辉和光激励发光性能都明显下降。材料中原来的陷阱A和陷阱B在加入Ba元素后都被破坏，产生了一种新的陷阱（陷阱A-B），而这种新陷阱中的电子无论对长余辉发光还是光激励发光都没有促进作用。
Electron trapping materials (ETM) have the property of photoconversion, and itis called the photostimulated luminescence materials in the field of luminescence.This kind of material has been always focused on extensively since it was firstmentioned by Lindmayer from USA in1986. It has extensive application prospect oninfrared detection, optical storage, infrared conversion and X-ray imaging. While thephotostimulated luminescence materials are irradiated by light, the electron (or hole)is captured by trap being in a comparative stable state. As it is stimulated by infraredlight or others, the electron (or hole) is released to produce photostimulatedluminescence (PSL). At present, the commercial ETM is main alkaline sulfides, whohave many advantages such as intense initial PSL intensity, high PSL light storagecapacity. However, the fatal disadvantage of alkaline sulfides is their poor chemicalstability. The more import is that the toxic substance will arise once the sulfides breakdown, and it will cause serious circumstance pollution. To solve this problem,searching an ETM with good chemical stability is the focus for study on ETM.
Silicates have good chemical stability, thermostability and resistance to corrosion.It is used as the host of rare earth luminescence material extensively now. Sr_3SiO_5:Eu~(2+)is a traditional LED (light emitting diodes) phosphor, which can absorb UV-lightand blue-green light to emit in yellow peaked at580nm. In this paper, we research theSr_3SiO_5: Eu~(2+)in the form of co-doping another coactivator to enhance the PSLproperty. The key results of researching are as follows:
1) We have researched the effect on the PSL properties by co-doping thecoactivators in lanthanide (La、Ce、Pr、Nd、Sm、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu) into Sr_(2.99)SiO_5:0.01Eu~(2+). It is found that the sample co-doping Tm~(3+)hasthe best PSL property. The initial PSL intensity and PSL light storage capacity isimproved at different extent. The reason is that a new trap (trap B) is arised in thesample co-doping Tm~(3+), and the trap could greatly enhance the PSL property ofmaterial.
2) We have researched the variation of PSL properties of Sr_(2.99)SiO_5:0.01Eu~(2+)withdifferent level of co-doping Tm~(3+). The initial PSL intensity and PSL light storagecapacity of ETM reached the maximum at the Tm~(3+)concentration of0.0004. Theinitial PSL intensity is33times of the Tm~(3+)free sample and the PSL light storagecapacity is2times of the Tm~(3+)free sample. It is shown that this kind of ETM hasbroad application prospect in the field of infrared detection. The quantity of trapB also reaches the maximum when the Tm~(3+)concentration is0.0004, it is impliedthat the intense relationship between the PSL property and the quantity of trap B.
3) The rules for electron transition of trap A and trap B in Sr_(2.9896)SiO_5:0.01Eu~(2+),0.0004Tm~(3+)have been studied. During the arrangement and analysis of data, it isconcluded that there are tow kinds of trap A and B, and the essential difference isthe distance between them and luminescence centre Eu~(2+). The first kind of trap isnear from Eu~(2+), the electron in trap is easy to perform charge transition betweenthe electron and Eu~(2+)ground level. In the condition of thermostimulation, theelectron in trap could convert to photon emitting thermoluminescence yet,nevertheless, with photostimulation, the electron in trap will cause non-irradiationtransition. The second kind trap is far from Eu~(2+), and the electron in trap willconvert to photon in the stimulation of thermal or luminescence. The electron inthe second kind of trap A will release slowly without intense PSL, and theelectron in the second kind of trap B will release rapidly to produce intense PSL.Meanwhile, it is found that the electron released from trap A could be retrappedby trap B in the process of phosphorescence decay. It is the effect of electronretrapping by trap B.
4) The effect on the characteristics of photoluminescence (PL), phosphorescenceand PSL of Sr_(2.9896)SiO_5:0.01Eu~(2+),0.0004Tm~(3+)doped Ba has been researchedtentatively. The emission peaks of PL, phosphorescence and PSL are all redshifted gradually as the Ba content is increased. The reason is that the latticeparameter of material is changed to make the Eu~(2+)5d orbital decrease afterdoping Ba. The properties of phosphorescence and PSL of the material are decreased evidently as the Ba content is increased. The trap A and trap B inphosphors are both destroyed after doping Ba, and a new trap (trap A-B) isemerged. However, the new trap could not enhance the phosphorescence or thePSL at all.
硅酸盐有较好的化学稳定性，且耐高温、抗腐蚀。目前被广泛的用作稀土发光材料的基体材料。其中，Sr_3SiO_5: Eu~(2+)是一类传统的LED(light emitting diodes)用荧光粉，可以有效的吸收紫外光和蓝绿光发出以580nm为中心的黄光。本论文以Sr_3SiO_5: Eu~(2+)为研究对象，通过掺入另一种共激活剂的方式引入陷阱以提高其光激励发光性能。主要的研究成果如下：
1)研究了镧系共激活剂(La、Ce、Pr、Nd、Sm、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu)对材料Sr_(2.99)SiO_5:0.01Eu~(2+)的光激励发光性能的影响。我们发现：和其他共激活剂相比，Tm~(3+)掺杂的样品具有非常好的光激励发光性能。其光激励初始强度、光激励光存储量等性能都有不同程度的提高。其原因是因为掺杂Tm~(3+)的样品产生了一个新的陷阱（陷阱B），这个陷阱可以很大程度的提高材料的光激励发光性能；
2)系统的研究了不同浓度Tm~(3+)掺杂下Sr_(2.99)SiO_5:0.01Eu~(2+)光激励发光性能的变化。经研究我们发现：当Tm~(3+)的掺杂浓度为0.0004时，材料的光激励发光初始强度和光激励光存储量性能均达到了最佳。其中，光激励发光初始强度是未掺杂样品的33倍，光激励光存储量是未掺杂样品的2倍。充分的显示出该材料在红外探测等方面的广阔应用前景。当Tm~(3+)掺杂浓度为0.0004时，材料中陷阱B的数量也同样达到最大值。这说明陷阱B的数量与材料的光激励发光性能有着很强的对应关系；
3)研究了Sr_(2.9896)SiO_5:0.01Eu~(2+),0.0004Tm~(3+)中的陷阱A和陷阱B中电子的迁移规律。经过对数据的整理和分析，我们得出如下结论：陷阱A和B都可以分成两类，其本质区别是它们距离发光中心Eu~(2+)的远近不同。第一类陷阱距离Eu~(2+)较近，陷阱中的电子很容易与Eu~(2+)的基态能级发生电荷迁移效应。在热激励的条件下，陷阱中的电子仍然可以转化成光子形成发光，而在光激励的条件下则很容易发生无辐射跃迁。第二类陷阱是距离Eu~(2+)较远的陷阱，这类陷阱中的电子无论在热激励还是光激励条件下都可以转化成光子形成发光。不同之处在于，第二类陷阱A中电子在光激励条件下释放速率缓慢不能形成较强的光激励发光，而第二类陷阱B中的电子在光激励的条件下则可以快速的释放形成较强的光激励发光。与此同时，我们还发现在长余辉衰减过程中，陷阱A释放出的电子可以被陷阱B再次俘获。这就是陷阱B的电子再俘获效应；
4)探索性的研究了Ba元素对材料Sr_(2.9896)SiO_5:0.01Eu~(2+),0.0004Tm~(3+)的荧光发光、长余辉发光以及光激励发光性能的影响。材料的荧光发射、长余辉发射和光激励发射峰位都随着Ba元素的逐渐添加而发生红移。这是因为Ba元素的掺入改变了基体材料的晶格参数而造成发光中心Eu~(2+)的5d能级下降，材料的发射峰位发生红移。Ba元素逐渐掺入后，材料的长余辉和光激励发光性能都明显下降。材料中原来的陷阱A和陷阱B在加入Ba元素后都被破坏，产生了一种新的陷阱（陷阱A-B），而这种新陷阱中的电子无论对长余辉发光还是光激励发光都没有促进作用。
Electron trapping materials (ETM) have the property of photoconversion, and itis called the photostimulated luminescence materials in the field of luminescence.This kind of material has been always focused on extensively since it was firstmentioned by Lindmayer from USA in1986. It has extensive application prospect oninfrared detection, optical storage, infrared conversion and X-ray imaging. While thephotostimulated luminescence materials are irradiated by light, the electron (or hole)is captured by trap being in a comparative stable state. As it is stimulated by infraredlight or others, the electron (or hole) is released to produce photostimulatedluminescence (PSL). At present, the commercial ETM is main alkaline sulfides, whohave many advantages such as intense initial PSL intensity, high PSL light storagecapacity. However, the fatal disadvantage of alkaline sulfides is their poor chemicalstability. The more import is that the toxic substance will arise once the sulfides breakdown, and it will cause serious circumstance pollution. To solve this problem,searching an ETM with good chemical stability is the focus for study on ETM.
Silicates have good chemical stability, thermostability and resistance to corrosion.It is used as the host of rare earth luminescence material extensively now. Sr_3SiO_5:Eu~(2+)is a traditional LED (light emitting diodes) phosphor, which can absorb UV-lightand blue-green light to emit in yellow peaked at580nm. In this paper, we research theSr_3SiO_5: Eu~(2+)in the form of co-doping another coactivator to enhance the PSLproperty. The key results of researching are as follows:
1) We have researched the effect on the PSL properties by co-doping thecoactivators in lanthanide (La、Ce、Pr、Nd、Sm、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu) into Sr_(2.99)SiO_5:0.01Eu~(2+). It is found that the sample co-doping Tm~(3+)hasthe best PSL property. The initial PSL intensity and PSL light storage capacity isimproved at different extent. The reason is that a new trap (trap B) is arised in thesample co-doping Tm~(3+), and the trap could greatly enhance the PSL property ofmaterial.
2) We have researched the variation of PSL properties of Sr_(2.99)SiO_5:0.01Eu~(2+)withdifferent level of co-doping Tm~(3+). The initial PSL intensity and PSL light storagecapacity of ETM reached the maximum at the Tm~(3+)concentration of0.0004. Theinitial PSL intensity is33times of the Tm~(3+)free sample and the PSL light storagecapacity is2times of the Tm~(3+)free sample. It is shown that this kind of ETM hasbroad application prospect in the field of infrared detection. The quantity of trapB also reaches the maximum when the Tm~(3+)concentration is0.0004, it is impliedthat the intense relationship between the PSL property and the quantity of trap B.
3) The rules for electron transition of trap A and trap B in Sr_(2.9896)SiO_5:0.01Eu~(2+),0.0004Tm~(3+)have been studied. During the arrangement and analysis of data, it isconcluded that there are tow kinds of trap A and B, and the essential difference isthe distance between them and luminescence centre Eu~(2+). The first kind of trap isnear from Eu~(2+), the electron in trap is easy to perform charge transition betweenthe electron and Eu~(2+)ground level. In the condition of thermostimulation, theelectron in trap could convert to photon emitting thermoluminescence yet,nevertheless, with photostimulation, the electron in trap will cause non-irradiationtransition. The second kind trap is far from Eu~(2+), and the electron in trap willconvert to photon in the stimulation of thermal or luminescence. The electron inthe second kind of trap A will release slowly without intense PSL, and theelectron in the second kind of trap B will release rapidly to produce intense PSL.Meanwhile, it is found that the electron released from trap A could be retrappedby trap B in the process of phosphorescence decay. It is the effect of electronretrapping by trap B.
4) The effect on the characteristics of photoluminescence (PL), phosphorescenceand PSL of Sr_(2.9896)SiO_5:0.01Eu~(2+),0.0004Tm~(3+)doped Ba has been researchedtentatively. The emission peaks of PL, phosphorescence and PSL are all redshifted gradually as the Ba content is increased. The reason is that the latticeparameter of material is changed to make the Eu~(2+)5d orbital decrease afterdoping Ba. The properties of phosphorescence and PSL of the material are decreased evidently as the Ba content is increased. The trap A and trap B inphosphors are both destroyed after doping Ba, and a new trap (trap A-B) isemerged. However, the new trap could not enhance the phosphorescence or thePSL at all.
引文
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