近紫外光LED芯片用荧光粉的制备与性能研究
摘要
本文制备了几种适合近紫外光LED芯片激发的荧光粉。试验了最佳合成条件以及杂质的最佳浓度,测试了样品的激发光谱和发射光谱,研究了样品的发光性质及其形貌。主要内容如下：
(1)利用高温固相法合成了红色荧光粉Sr2SiO4:Sm3+。样品具有3组发射峰,主峰值分别位于570nm,606nm和653nm,其中最强峰位于606nm。激发光谱为从350到420nm的宽带,可以被近紫外光和紫光有效激发。当Sm3+浓度为6%,电荷补偿剂为Cl-时,样品的发光强度最大。
(2)利用燃烧法制备了红色荧光粉SrIn2O4:Eu3+。样品的最强发射峰位于613nm,对应于Eu3+的5D0→7F2跃迁。随着激活剂Eu3+浓度的增加,样品的发光强度逐渐增大。样品的主激发峰位于397和469nm,分别与紫外光和蓝光LED的辐射相符合。它由许多微小的晶粒组成,晶粒的平均直径小于500nm。
(3)利用凝胶燃烧法合成了绿色荧光粉Ca2Si04:Eu2+。样品呈现出峰值位于501nm的宽带发光,它可以被350-400nm的UVLED芯片有效激发,并且制备温度较低(1000℃),颗粒平均尺寸较小(小于1μm)。Eu2+的最佳浓度为3%。
(4)利用高温固相法合成了蓝色荧光粉Sr5Si04Cl6:Eu2+。样品的激发峰值位于360nm,适合UVLED芯片的激发。样品在360nm的紫外光激发下呈宽带发射,峰值位于454nm,属于Eu2+的4f(?)5d→4f(?)能级跃迁。样品的最佳制备温度为750℃,Eu2+的最佳浓度为2%。
In this paper, several kinds of phosphor used for near-ultraviolet LED were fabricated. The optimal synthesis temperature and the concentration of impurity were tested. The emission and excitation spectra were measured. The luminescence properties and appearances of samples were researched. The chief contents are given as follows:
(1) The red phosphor Sr2SiO4:Sm3+ was synthesized by high temperature solid state reaction. The sample has three groups of emission peaks. The main emission peaks are located at 570nm,606nm and 653nm and the strongest one appears at 606nm. Its excitation spectrum extends from 350 to 420nm which indicates that this phosphor can be excited effectively by near-ultraviolet and violet light. When the concentration of Sm3+ is 6% and the charge compensator is Cl-, the strongest emission is obtained.
(2) The red phosphor SrIn2O4:Eu3+ was synthesized by combustion. The emission spectrum shows the most intense peak is located at 613nm, which corresponds to the 5D0→7F2 transition of Eu3+. The emission enhances while the concentration of Eu3+ increases. The phosphor has two main excitation peaks located at 397 and 469nm, which match the emission of UV and blue LED respectively. The obtained phosphor consists of many crystalline granules, whose average diameter is less than 500nm.
(3) The green phosphor Ca2SiO4:Eu2+ was synthesized by a Sol-gel combustion method. The emission spectrum of Sample shows a broad band with a peak around 501nm. The phosphor can be excited efficiently by UVLED chip whose emission peak locates at 350-400nm. Moreover, the Sample has lower preparation temperature (1000℃) and smaller average grain size(less than 1μm). The best concentration of Eu2+ is 3%.
(4) The blue phosphor Sr5SiO4Cl6:Eu2+ was synthesized by high temperature solid state reaction. The excitation peak is located at 360nm, so the phosphor can be excited efficiently by UVLED chip. The phosphor excited by 360nm has a broad emission band with a peak at 454 nm, which corresponds to the 4f65d→4f7 transition of Eu2+. The best reaction temperature is 750℃and the best concentration of Eu2+ is 2%.
(1)利用高温固相法合成了红色荧光粉Sr2SiO4:Sm3+。样品具有3组发射峰,主峰值分别位于570nm,606nm和653nm,其中最强峰位于606nm。激发光谱为从350到420nm的宽带,可以被近紫外光和紫光有效激发。当Sm3+浓度为6%,电荷补偿剂为Cl-时,样品的发光强度最大。
(2)利用燃烧法制备了红色荧光粉SrIn2O4:Eu3+。样品的最强发射峰位于613nm,对应于Eu3+的5D0→7F2跃迁。随着激活剂Eu3+浓度的增加,样品的发光强度逐渐增大。样品的主激发峰位于397和469nm,分别与紫外光和蓝光LED的辐射相符合。它由许多微小的晶粒组成,晶粒的平均直径小于500nm。
(3)利用凝胶燃烧法合成了绿色荧光粉Ca2Si04:Eu2+。样品呈现出峰值位于501nm的宽带发光,它可以被350-400nm的UVLED芯片有效激发,并且制备温度较低(1000℃),颗粒平均尺寸较小(小于1μm)。Eu2+的最佳浓度为3%。
(4)利用高温固相法合成了蓝色荧光粉Sr5Si04Cl6:Eu2+。样品的激发峰值位于360nm,适合UVLED芯片的激发。样品在360nm的紫外光激发下呈宽带发射,峰值位于454nm,属于Eu2+的4f(?)5d→4f(?)能级跃迁。样品的最佳制备温度为750℃,Eu2+的最佳浓度为2%。
In this paper, several kinds of phosphor used for near-ultraviolet LED were fabricated. The optimal synthesis temperature and the concentration of impurity were tested. The emission and excitation spectra were measured. The luminescence properties and appearances of samples were researched. The chief contents are given as follows:
(1) The red phosphor Sr2SiO4:Sm3+ was synthesized by high temperature solid state reaction. The sample has three groups of emission peaks. The main emission peaks are located at 570nm,606nm and 653nm and the strongest one appears at 606nm. Its excitation spectrum extends from 350 to 420nm which indicates that this phosphor can be excited effectively by near-ultraviolet and violet light. When the concentration of Sm3+ is 6% and the charge compensator is Cl-, the strongest emission is obtained.
(2) The red phosphor SrIn2O4:Eu3+ was synthesized by combustion. The emission spectrum shows the most intense peak is located at 613nm, which corresponds to the 5D0→7F2 transition of Eu3+. The emission enhances while the concentration of Eu3+ increases. The phosphor has two main excitation peaks located at 397 and 469nm, which match the emission of UV and blue LED respectively. The obtained phosphor consists of many crystalline granules, whose average diameter is less than 500nm.
(3) The green phosphor Ca2SiO4:Eu2+ was synthesized by a Sol-gel combustion method. The emission spectrum of Sample shows a broad band with a peak around 501nm. The phosphor can be excited efficiently by UVLED chip whose emission peak locates at 350-400nm. Moreover, the Sample has lower preparation temperature (1000℃) and smaller average grain size(less than 1μm). The best concentration of Eu2+ is 3%.
(4) The blue phosphor Sr5SiO4Cl6:Eu2+ was synthesized by high temperature solid state reaction. The excitation peak is located at 360nm, so the phosphor can be excited efficiently by UVLED chip. The phosphor excited by 360nm has a broad emission band with a peak at 454 nm, which corresponds to the 4f65d→4f7 transition of Eu2+. The best reaction temperature is 750℃and the best concentration of Eu2+ is 2%.
引文
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[24]Jong Su Kim, Kwon Taek Lim, Yong Seok Jeong, et al. Full-color Ba3MgSi2O8:Eu2+, Mn2+ phosphors for white-light-emitting diodes[J]. Solid State Communications,2005,135:21-24.
[25]Honghua Huang, Bing Yan. In situ sol-gel composition of multicomponent hybrid precursor to hexagon-like Zn2SiO4:Tb3+ microcrystalline phosphors with different silicate sources[J]. Applied Surface Science,2006,252:2967-2972.
[26]Yutaka Ito, Akira Komeno, Kazuyoshi Uematsu, et al. Luminescence properties of long-persistence silicate phosphors[J]. Journal of Alloys and Compounds,2006,408-412:907-910.
[27]Sho Abe, Kazuyoshi Uematsu, Kenji Toda, et al. Luminescent properties of red long persistence phosphors, BaMg2Si207:Eu2+, Mn2+[J]. Journal of Alloys and Compounds,2006,408-412:911-914.
[28]Yoshihiro Nishisu, Mikio Kobayashi, Hitoshi Ohya, et al. Preparation of Eu-doped alkaline-earth silicate phosphor particles by using liquid-phase synthesis method[J]. Journal of Alloys and Compounds,2006,408-412:898-902.
[29]Hongmei Yang, Jianxin Shi, Menglian Gong, et al. Synthesis and photoluminescence of Eu3+-or Tb3+-doped Mg2SiO4 nanoparticles prepared by a combined novel approach[J]. Journal of Luminescence,2006,118:257-264.
[30]Akira Komeno, Kazuyoshi Uematsu, Kenji Toda, et al. VUV properties of Eu-doped alkaline earth magnesium silicate[J]. Journal of Alloys and Compounds,2006,408-412:871-874.
[31]J.S. Kim, S.W. Mho, Y.H. Park, et al. White-light-emitting Eu2+ and Mn2+-codoped silicate phosphors synthesized through combustion process[J]. Solid State Communications,2005,136: 504-507.
[32]雷炳富,刘应亮,唐功本等.一种新的橙红色长余辉荧光材料Y2O2S:Sm3+.高等学校化学学报,2003,24：(2),208-210.
[33]宋春燕,王晓华,刘应亮等.新型橙红色长余辉发光材料Gd2O2S:Sm3+的合成[J].化学通报,2004,5：373-376
[34]于健,刘又年,陈立妙,黄可龙.Sm3+掺杂CaO-SiO2-B2O3发光玻璃的制备、表征及性质[J].无机化学学报,2006,22(2)：249-252.
[35]卢利平,张希艳,柏朝晖,米晓云,刘全生,王晓春.宽频谱红外上转换材料CaS:Eu, Sm的快速合成及表征[J].中国激光,2006,33(4)：561-564.
[36]F. S. Kao and Teng-Ming Chen. A Study on the Luminescent Properties of Praseodymium-Activated CaIn2O4 Phosphors[J]. Journal of Solid State Chemistry,2000,155:441-446.
[37]Feng-shih Kao and Teng-Ming Chen. A Study on the Luminescent Properties of Red-Emitting Praseodymium-Activated SrIn2O4 Phosphors[J]. Journal of Solid State Chemistry,2001,156:84-87.
[38]F. S. Kao and Teng-Ming Chen. A Study on the Luminescent Properties of new green-emitting terbium-activated CaIn2O4:xTb Phosphors[J]. Journal of Luminescence,2002,96:261-267
[39]A. Baszczuk, M. Jasiorski, M. Nyk, et al. Luminescence properties of europium activated SrIn2O4[J]. Journal of Alloys and Compounds,2005,394:88-92.
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[2]Niina Tatsuhito. GaP Red Light Emitting Diodes Produced by a Rotating Boat System of Liquid Phase Epitaxial Growth[J]. Journal of The Electrochemical Society,1977,124(8):1285-1289.
[3]Sugawara H, Ishikawa M, Hatakoshi G. High-efficiency InGaAlP/GaAs visible light-emitting diodes[J]. Applied Physics Letters,1991,58(10):1010-1012.
[4]Kish F A, Steranka F M, De Fevere D C, et al. Very high efficiency semiconductor wafer bonded transparent substrate (AlxGa1-x)0.5In0.5P/GaP light emitting diodes[J]. Applied Physics Letters,1994, 64(21):2839-2841.
[5]Yun Xu, Lianghui Chen, Yuzhang Li. Phosphor-conversion white light using InGaN ultraviolet laser diode[J]. Applied Physics Letters,2008,92:021129
[6]徐叙瑢,苏勉曾.《发光学与发光材料》.北京：化学工业出版社,2004,第1版：2.
[7]孙家跃,杜海燕,胡文祥.《固体发光材料》.北京：化学工业出版社,2003,第1版：2.
[8]李建宇.《稀土发光材料及其应用》.北京：化学工业出版社,2003,第1版：11-13.
[9]Jong Su Kim, Pyung Eun Jeon, Yun Hyung park, et al. White-light generation through ultraviolet-emitting diode and white-emitting phosphor[J]. Applied Physics Letters,2004,85(17):3696-3698
[10]Rong-Jun Xie, Naoto Hirosaki, Mamoru Mitomo, et al. Highly efficient white-light-emitting diodes fabricated with short-wavelength yellow oxynitride phosphors[J]. Applied Physics Letters,2006,88: 101104
[11]Weijia Ding, Jing Wang, Mei Zhang, et al. A novel orange phosphor of Eu2+-activated calcium chlorosilicate for white light-emitting diodes[J]. Journal of Solid State Chemistry,2006,179: 3582-3585.
[12]Zhengliang Wang, Hongbin Liang, Jing Wang, et al. Red-light-emitting diodes fabricated by near-ultraviolet InGaN chips with molybdate phosphors[J]. Applied Physics Letters,2006,89:071921
[13]Yu-Ho Won, Ho Seong Jang, Won Bin Im, et al. Tunable full-color-emitting La0.827Al11.9019.09: Eu2+,Mn2+ phosphor for application to warm white-light-emitting diodes[J]. Applied Physics Letters, 2006,89:231909.
[14]Chun-Kuei Chang and Teng-Ming Chen. Sr3B2O6:Ce3+,Eu2+:A potential single-phased white-emitting borate phosphor for ultraviolet light-emitting diodes [J]. Applied Physics Letters,2007,91:081902.
[15]O. Ozuna, G. A. Hirata, J. McKittrick. Luminescence enhancement in Eu3+-doped α-and γ-Al2O3 produced by pressure-assisted low-temperature combustion synthesis[J]. Applied Physics Letters, 2004,84(8):1296-1298
[16]D. Haranath, Harish Chander, Pooja Sharma, et al. Enhanced luminescence of Y3Al5O12:Ce3+ nanophosphor for white lightemitting diodes[J]. Applied Physics Letters,2006,89:173118.
[17]Shi Shikao, Wang Jiye. Combustion synthesis of Eu3+ activated Y3Al5O12 phosphor nanoparticles[J]. Journal of Alloys and Compounds,2001,327:82-86.
[18]Zhiping Yang, Xu Li, Yong Yang, et al. The influence of different conditions on the luminescent properties of YAG:Ce phosphor formed by combustion[J]. Journal of Luminescence,2007,122-123: 707-709.
[19]Zhiping Yang, Xu Li, Xingmin LI, et al. Synthesis of red-emitting phosphors Ca1-xSrxS:Eu2+ used in white light emitting diodes by combustion[J]. Journal of the chinese ceramic society,2006,34(8): 966-969.
[20]Park Joung Kyu, Lim Mi Ae, Kim Chang Hae, et al. White light-emitting diodes of GaN-based Sr2SiO4:Eu2+ and the luminescent properties[J]. Applied Physics Letters,2003,82(5):683-685.
[21]N. Lakshminarasimhan and U. V. Varadaraju. White-Light Generation in Sr2SiO4:Eu2+, Ce3+ under Near-UV Excitation[J]. Journal of The Electrochemical Society,2005,152 (9):152-156.
[22]N. Taghavinia, G. Lerondel, H. Makino, et al. Blue-and red-emitting phosphor nanoparticles embedded in a porous matrix[J]. Thin Solid Films,2006,503:190-195.
[23]Junxi Wan, Zhenghua Wang, Xiangying Chen, et al. Controlled synthesis and relationship between luminescent properties and shape/crystal structure of Zn2SiO4:Mn2+ phosphor[J]. Journal of Luminescence,2006,121:32-38.
[24]Jong Su Kim, Kwon Taek Lim, Yong Seok Jeong, et al. Full-color Ba3MgSi2O8:Eu2+, Mn2+ phosphors for white-light-emitting diodes[J]. Solid State Communications,2005,135:21-24.
[25]Honghua Huang, Bing Yan. In situ sol-gel composition of multicomponent hybrid precursor to hexagon-like Zn2SiO4:Tb3+ microcrystalline phosphors with different silicate sources[J]. Applied Surface Science,2006,252:2967-2972.
[26]Yutaka Ito, Akira Komeno, Kazuyoshi Uematsu, et al. Luminescence properties of long-persistence silicate phosphors[J]. Journal of Alloys and Compounds,2006,408-412:907-910.
[27]Sho Abe, Kazuyoshi Uematsu, Kenji Toda, et al. Luminescent properties of red long persistence phosphors, BaMg2Si207:Eu2+, Mn2+[J]. Journal of Alloys and Compounds,2006,408-412:911-914.
[28]Yoshihiro Nishisu, Mikio Kobayashi, Hitoshi Ohya, et al. Preparation of Eu-doped alkaline-earth silicate phosphor particles by using liquid-phase synthesis method[J]. Journal of Alloys and Compounds,2006,408-412:898-902.
[29]Hongmei Yang, Jianxin Shi, Menglian Gong, et al. Synthesis and photoluminescence of Eu3+-or Tb3+-doped Mg2SiO4 nanoparticles prepared by a combined novel approach[J]. Journal of Luminescence,2006,118:257-264.
[30]Akira Komeno, Kazuyoshi Uematsu, Kenji Toda, et al. VUV properties of Eu-doped alkaline earth magnesium silicate[J]. Journal of Alloys and Compounds,2006,408-412:871-874.
[31]J.S. Kim, S.W. Mho, Y.H. Park, et al. White-light-emitting Eu2+ and Mn2+-codoped silicate phosphors synthesized through combustion process[J]. Solid State Communications,2005,136: 504-507.
[32]雷炳富,刘应亮,唐功本等.一种新的橙红色长余辉荧光材料Y2O2S:Sm3+.高等学校化学学报,2003,24：(2),208-210.
[33]宋春燕,王晓华,刘应亮等.新型橙红色长余辉发光材料Gd2O2S:Sm3+的合成[J].化学通报,2004,5：373-376
[34]于健,刘又年,陈立妙,黄可龙.Sm3+掺杂CaO-SiO2-B2O3发光玻璃的制备、表征及性质[J].无机化学学报,2006,22(2)：249-252.
[35]卢利平,张希艳,柏朝晖,米晓云,刘全生,王晓春.宽频谱红外上转换材料CaS:Eu, Sm的快速合成及表征[J].中国激光,2006,33(4)：561-564.
[36]F. S. Kao and Teng-Ming Chen. A Study on the Luminescent Properties of Praseodymium-Activated CaIn2O4 Phosphors[J]. Journal of Solid State Chemistry,2000,155:441-446.
[37]Feng-shih Kao and Teng-Ming Chen. A Study on the Luminescent Properties of Red-Emitting Praseodymium-Activated SrIn2O4 Phosphors[J]. Journal of Solid State Chemistry,2001,156:84-87.
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