稀土掺杂的硅铝酸盐和掺Tm_2O_3微球的发光特性研究
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摘要
长余辉发光材料的研究已有百年历史,经历了硫化物长余辉发光材料和氧化物发光材料两代,第二代长余辉发光材料可以说是一种绿色材料,其应用也十分广泛。
我们首先对长余辉发光材料的基本概念,常用的制备方法,出现的几种能量传输机理模型进行了概述,然后对长余辉发光材料的研究现状进行了总结,并阐述了自己的研究思路。介绍了实验的详细方法和样品的性能测试手段。
利用高温固相法合成了xSrO-yAl2O3-zSiO2(x,y,z=1,2,3):Eu3+,Dy3+系列陶瓷结构长余辉发光材料,利用X射线衍射(XRD),荧光光谱,余辉衰减曲线等手段对样品的性能进行了研究。发现样品中的Sr/Al和Al/Si对样品的发光性能都有影响,但是Sr/Al的比值对样品的影响要远大于Al/Si比对样品的影响。随着Sr/Al的比值逐渐增大,样品受到365nm激发产生的发射谱的主峰位逐渐变小,在Sr/Al的比值相同的地方还会出现阶梯状平台;同时样品的激发谱主峰也由原来的单一峰位变成多峰位。而样品的性能随Al/Si比的变化则呈现无规律状态。
另外,我们还研究了掺杂Tm3+的高折射率TiBa玻璃微球和掺杂Er3+/Yb3+的硅酸盐玻璃微粒,分别使用633nm和976nm激光对样品进行激发。测量了TiBa玻璃以及该材料微球的发光,绘出了荧光发射强度随泵浦光功率的变化曲线并进行了拟合,证实其发光为双光子吸收发光;在微球的荧光光谱上发现了很强的形貌共振峰;利用Mie理论公式对共振峰间隔进行了计算,实验结果与计算结果相符。测量了掺Er3+/Yb3+的硅酸盐玻璃微粒的荧光光谱,绘制了荧光发射强度随泵浦光功率的变化曲线并进行了拟合,并证实其发光也是双光子吸收发光。
One hundred years ago, people began to investigate the long afterglow phosphors, which experience two eras--the first one is sulfide long afterglow phosphors, the second one is oxygenation long afterglow materials. The oxygenation long afterglow phosphors are green materials. It can be used in many fields.
We gave the basic ideas of long afterglow phosphors, the preparation methods in common use and several models of the energy transferring mechanism, and Summarized the investigation of these materials. We expounded our thoughts of work. Introduced our experimental means and the methods of capability research.
We prepared xSrO-yAl2O3-zSiO2(x,y,z=1,2,3):Eu3+,Dy3+ series long afterglow phosphors by traditional solid state method. In this paper, by means of some analytical methods such as XRD, the luminescent spectra and decay curves, the structure and luminescent properties of the phosphors were characterized. It was found that the ratio of the Sr/Al and the ratio of Al/Si had something to do with the luminescent properties of the samples. But the Sr/Al ratio had more influence on samples than the ratio of Al/Si. The peak of the spectrum excitated by 365nm decreased with the larger of the ratio of the Sr/Al. And there would be a flat roof when the ratio of the Sr/Al was the same. At the same time, the peak in the excitation spectra was changed from one to two or even more. The changes of the properties of samples as the ratio of the Al/Si did not obey the rule.
In addition, we studied high refractive index TiBa glass microspheres doped with Tm2O3 and the Er3+/Yb3+-codoped silicate glass micro-particle. The emission spectra of the TiBa matrix glass and the TiBa glass microspheres under 633nm excitation were measured. The dependences of the emission intensities of the Tm3+-codoped microsphere and matrix glass on the laser power excited with 633nm were researched. It’s proved that the emission of the sample was two-photon excitation. The observed resonances could be assigned by the well-known Lorenz-Mie formalism. The emission spectra of the Er3+/Yb3+-codoped silicate glass micro-particle under 976nm excitation were measured. The dependences of the emission intensities of the Er3+/Yb3+-codoped micro-particle on the laser power excited with 976nm were researched. It’s proved that the emission of the sample was two-photon excitation too.
我们首先对长余辉发光材料的基本概念,常用的制备方法,出现的几种能量传输机理模型进行了概述,然后对长余辉发光材料的研究现状进行了总结,并阐述了自己的研究思路。介绍了实验的详细方法和样品的性能测试手段。
利用高温固相法合成了xSrO-yAl2O3-zSiO2(x,y,z=1,2,3):Eu3+,Dy3+系列陶瓷结构长余辉发光材料,利用X射线衍射(XRD),荧光光谱,余辉衰减曲线等手段对样品的性能进行了研究。发现样品中的Sr/Al和Al/Si对样品的发光性能都有影响,但是Sr/Al的比值对样品的影响要远大于Al/Si比对样品的影响。随着Sr/Al的比值逐渐增大,样品受到365nm激发产生的发射谱的主峰位逐渐变小,在Sr/Al的比值相同的地方还会出现阶梯状平台;同时样品的激发谱主峰也由原来的单一峰位变成多峰位。而样品的性能随Al/Si比的变化则呈现无规律状态。
另外,我们还研究了掺杂Tm3+的高折射率TiBa玻璃微球和掺杂Er3+/Yb3+的硅酸盐玻璃微粒,分别使用633nm和976nm激光对样品进行激发。测量了TiBa玻璃以及该材料微球的发光,绘出了荧光发射强度随泵浦光功率的变化曲线并进行了拟合,证实其发光为双光子吸收发光;在微球的荧光光谱上发现了很强的形貌共振峰;利用Mie理论公式对共振峰间隔进行了计算,实验结果与计算结果相符。测量了掺Er3+/Yb3+的硅酸盐玻璃微粒的荧光光谱,绘制了荧光发射强度随泵浦光功率的变化曲线并进行了拟合,并证实其发光也是双光子吸收发光。
One hundred years ago, people began to investigate the long afterglow phosphors, which experience two eras--the first one is sulfide long afterglow phosphors, the second one is oxygenation long afterglow materials. The oxygenation long afterglow phosphors are green materials. It can be used in many fields.
We gave the basic ideas of long afterglow phosphors, the preparation methods in common use and several models of the energy transferring mechanism, and Summarized the investigation of these materials. We expounded our thoughts of work. Introduced our experimental means and the methods of capability research.
We prepared xSrO-yAl2O3-zSiO2(x,y,z=1,2,3):Eu3+,Dy3+ series long afterglow phosphors by traditional solid state method. In this paper, by means of some analytical methods such as XRD, the luminescent spectra and decay curves, the structure and luminescent properties of the phosphors were characterized. It was found that the ratio of the Sr/Al and the ratio of Al/Si had something to do with the luminescent properties of the samples. But the Sr/Al ratio had more influence on samples than the ratio of Al/Si. The peak of the spectrum excitated by 365nm decreased with the larger of the ratio of the Sr/Al. And there would be a flat roof when the ratio of the Sr/Al was the same. At the same time, the peak in the excitation spectra was changed from one to two or even more. The changes of the properties of samples as the ratio of the Al/Si did not obey the rule.
In addition, we studied high refractive index TiBa glass microspheres doped with Tm2O3 and the Er3+/Yb3+-codoped silicate glass micro-particle. The emission spectra of the TiBa matrix glass and the TiBa glass microspheres under 633nm excitation were measured. The dependences of the emission intensities of the Tm3+-codoped microsphere and matrix glass on the laser power excited with 633nm were researched. It’s proved that the emission of the sample was two-photon excitation. The observed resonances could be assigned by the well-known Lorenz-Mie formalism. The emission spectra of the Er3+/Yb3+-codoped silicate glass micro-particle under 976nm excitation were measured. The dependences of the emission intensities of the Er3+/Yb3+-codoped micro-particle on the laser power excited with 976nm were researched. It’s proved that the emission of the sample was two-photon excitation too.
引文
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4 Mastuzawa T, Aoki Y, Takeuchi N, Murayama Y. A new phosphorescent phosphor with high brightness,SrAl2O4:Eu2+,Dy3+.j.Electrochem.Soc.1996, 143(8):2670-2673
5 Qiu J, Miura K, Inouye H, Kondo, Y, Mitsuyu T, Hirao K. Femtosecond laser-induced three-dimensional bright and long-lasting phosphorescence inside calcium aluminosilicate glasses dope with rare earth ions. Appl.Phys.Lett,1998,73(13):1763-1765
6 Kowatari M, Koyama D, Satoh Y, Iinuma K, Uchida S. The temperature dependence of luminescence from a long-lasting phosphor exposed to ionizing radiation. Nuclear Instruments and Methods in Physics Research section A, 2003, 480(2&3):431-439
7 李建宇.稀土发光材料及其应用,化学工业出版社,2003:124
8 欧得华,黄慧民,邓淑华等.长余辉发光材料研究进展.江苏化工.2005,33(4):11
9 李晓云,陆天长.共沉淀法制备长余辉荧光粉,新型建筑材料,2001,4:43-44
10 Kutty T R N,Jannathan R.Mater Res Bull, 1990, 25:1355~1358
11 石林考.无机盐工业,1995,31(3):1~5
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16 Louis C, Bazzi R, Flores M A, etal Synthesis and characterization of Gd2O3:Eu3+ phosphor nanoparticles by a sol-lyophilization technique[J]. Joumal of Solid State Chemisry.2003,(173):335-341
17 Jia Weiyi, Yuan Huabiao, Lu Lizhu, etal. Phosph-orescent dynamics in SrAl2O4:Eu2+,Dy3+ single crystal fibers[J]. Lumin.1998,(76&77):424
18 Hoogenstraaten W. Philips Res. Repts, 1958, 13: 515-693
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27 P. Dorenbos, Systematic behaviour in trivalent lanthanide charge transfer energies. J. Phys.Condens. Matter.,2003,15:8417-8434
28 P. Dorenbos, Exchange and crystal field effects on the 4f(n-1)5d levels of Tb3+. J. Phys.Condens.Matter.2003,15:6249-6268
29 P. Dorenbos, Relation between Eu2+ and Ce3+ f?d-transition energies in inorganic compounds.J. Phys.Condens. Matter.2003,15:4797-4807
30 Thomas Aitasalo, et al. J. Lumin. 2001, 94/95: 59-63
31 Jia D, Yen W M. J. Lumin., 2003, 101: 115-121
32 刘正伟.新型长余辉发光材料的合成与性能研究.暨南大学硕士学位论文.2005:7-8
33 Jia D, Meltzer R.S, Yen W. M. Green phosphorescence of CaA12O4:Tb3+, Ce3+ through persistence energy transfer. Applied Physics Letters.2002, 80 (9): 1535—1537
34 Yamazaki M, Yamamoto Y, Nagahama S, Sawanobori N, Mizuguchi M. Longluminescent glass:Tb3+-activated ZnO-B2O-SiO2 glass. J. Non-crystalline Solids. 1998, 241(1):71-73
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2 肖志国. 蓄光型发光材料及其制品(第二版),化学工业出版社,2002:1
3 F. C. Palilla, A. K. Levine and M. R Tomkus. Fluorescent properties of alkaline of the type Mal2O4 actived by divalent europium. ,J. Electronchem. Soc.Solid State Science, 1968,115 :642
4 Mastuzawa T, Aoki Y, Takeuchi N, Murayama Y. A new phosphorescent phosphor with high brightness,SrAl2O4:Eu2+,Dy3+.j.Electrochem.Soc.1996, 143(8):2670-2673
5 Qiu J, Miura K, Inouye H, Kondo, Y, Mitsuyu T, Hirao K. Femtosecond laser-induced three-dimensional bright and long-lasting phosphorescence inside calcium aluminosilicate glasses dope with rare earth ions. Appl.Phys.Lett,1998,73(13):1763-1765
6 Kowatari M, Koyama D, Satoh Y, Iinuma K, Uchida S. The temperature dependence of luminescence from a long-lasting phosphor exposed to ionizing radiation. Nuclear Instruments and Methods in Physics Research section A, 2003, 480(2&3):431-439
7 李建宇.稀土发光材料及其应用,化学工业出版社,2003:124
8 欧得华,黄慧民,邓淑华等.长余辉发光材料研究进展.江苏化工.2005,33(4):11
9 李晓云,陆天长.共沉淀法制备长余辉荧光粉,新型建筑材料,2001,4:43-44
10 Kutty T R N,Jannathan R.Mater Res Bull, 1990, 25:1355~1358
11 石林考.无机盐工业,1995,31(3):1~5
12 李沅英,戴德昌,蔡少华.微波热效应法合成Y2O2S:Eu3+荧光体.高等学校化学学报,1995,16:844-846
13 张迈生,杨燕生,区瑞明.CaS:Mn2+荧光体的微波辐射合成及发光特性,中山大学学报.1998,37(4):77-80
14 李强,高濂,严东生. YAG:Ce3+微粉的制备及光谱性能[J].无机材料学报.1997,12(4):575-578
15 Wen fu-shan, Chen Jie-sheng ,Moon Jong-ha, etal Hydrothermal Synthesis and luminescent properties of Sb3+ — doped Sr3(PO4)2[J]. Joumal of Solid State Chemistry.2004,(177):3114-3118
16 Louis C, Bazzi R, Flores M A, etal Synthesis and characterization of Gd2O3:Eu3+ phosphor nanoparticles by a sol-lyophilization technique[J]. Joumal of Solid State Chemisry.2003,(173):335-341
17 Jia Weiyi, Yuan Huabiao, Lu Lizhu, etal. Phosph-orescent dynamics in SrAl2O4:Eu2+,Dy3+ single crystal fibers[J]. Lumin.1998,(76&77):424
18 Hoogenstraaten W. Philips Res. Repts, 1958, 13: 515-693
19 Avouris Ph, Morgan T N. J. Chem. Phys,1981, 74: 4347-4355
20 Avouris Ph, Chang I F. J. Electron. Mater., 1981, 10: 887-899
21 Chang I F, Thioulouse P. J. Appl. Phys., 1982, 53: 5873-5875
22 施朝淑,戚泽明.长余辉(寿命)发光材料研究的最新进展.无机材料学报. 2004,19(5):964
23 Matsuzawa T,Aoki Y,Yakeuchi N,etal. J.Electrochem.Soc.1996,143:2670-2673
24 Zeming Qi ,Chaoshu Shi, Miao Liu, Dongfang Zhou, Xixian Luo, Jing Zhang, and Yaning Xie. The valence of rare earth ions in R2MgSi2O7:Eu,Dy(R=Ca,Sr) long-afterglow phosphors. phys.slat. sol. (a).2004,201(14): 3109-3112
25 P. Dorenbos, Locating lanthanide impurity levels in the forbidden band of host crystals. J. Lumin.2004,108:301-305
26 P. Dorenbos, The Eu3+ charge transfer energy and the relation with the band gap of compounds. 2005,111:89-103
27 P. Dorenbos, Systematic behaviour in trivalent lanthanide charge transfer energies. J. Phys.Condens. Matter.,2003,15:8417-8434
28 P. Dorenbos, Exchange and crystal field effects on the 4f(n-1)5d levels of Tb3+. J. Phys.Condens.Matter.2003,15:6249-6268
29 P. Dorenbos, Relation between Eu2+ and Ce3+ f?d-transition energies in inorganic compounds.J. Phys.Condens. Matter.2003,15:4797-4807
30 Thomas Aitasalo, et al. J. Lumin. 2001, 94/95: 59-63
31 Jia D, Yen W M. J. Lumin., 2003, 101: 115-121
32 刘正伟.新型长余辉发光材料的合成与性能研究.暨南大学硕士学位论文.2005:7-8
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