白光LED用多钼酸盐红色荧光材料的发光性能研究
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摘要
白光发光二极管(White light emitting diode,简称WLED)是一种新型的固态照明,具有高效节能、寿命超长、绿色环保且体积小、响应快、结构简单等优点,被誉为二十一世纪的绿色光源。目前实现白光LED的最有效方法就是荧光体转换。但所开发的白光LED用红色荧光粉的发光效率较低,不能满足要求,因此需要研制新型高效的白光LED用红色荧光材料。
本文采用传统的高温固相法,以钼酸盐为基质材料,掺杂稀土Eu~(3+)离子制备了多种可被近紫外光有效激发的红色荧光粉:碱金属阳离子Li~+、K~+掺杂的Na_5Eu(MoO_4)_4体系;含氧酸根阴离子(PO_4)~(3-)、(SO_4)~(2-)、(ClO_3)~-掺杂的Na_5Eu(MoO_4)_4并在此基础上考虑电价平衡掺杂,在体系中引入Li~+离子、Cl~-离子; LiGd_(1-x_Eu_x(MoO_4)_2体系和LiGd_(0.6-x)Y_xEu_(0.4)(MoO_4)_2体系。并研究了反应条件和掺杂浓度对各体系样品的结构和发光性能的影响。
为分析不同掺杂离子、不同电荷补偿掺杂和不同基质对样品的晶体结构和荧光性能的影响,对样品进行了X -射线衍射(XRD)、扫描电镜(SEM)、激发和发射光谱等表征。XRD结果表明所得不同离子掺杂Na_5Eu(MoO_4)_4体系的样品均属于四方晶系的类白钨矿(Scheelite - like)结构。不同离子掺杂的LiGd(MoO_4)_2体系的样品均为四方晶系的白钨矿(Scheelite)结构。两个体系样品的空间群均为I41/a。SEM照片显示采取有效掺杂有助于改善样品的结晶效果,修饰样品的形貌。在395 nm近紫外光激发下,所有样品Eu~(3+)的5D0 - 7F2(615 nm)跃迁发射的红光强度均高于商用红粉Y_2O_2S: Eu~(3+)的发射强度。
本文关于不同掺杂离子,不同基质掺杂对稀土Eu~(3+)离子激活的钼酸盐的晶体结构和发光性能进行了基础性研究,可为白光LED用新型红色发光材料的设计开发提供有价值的理论基础。
In the 21st, white light-emitting diodes (WLEDs), as the promising solid-state lighting sources to replace the conventional incandescent and fluorescent lamps, have attracted much attention due to their high reliability, long lifetime, low energy consumption and environment-friendly characteristics. The most effective approach to obtain WLED is phosphor - converted. However, the current red-emitting phosphor used for WLED reveals a rather low red emission under near-UV light excitation. Hence, it is necessary to search new red phosphors that can be efficiently excited around near-UV light.
In this paper, a series of red phosphors containing (Na,M)_5Eu(MoO_4)_4 [M = Li, K], Na_5Eu(MoO_4)_(4-x)M_y [M = (PO_4)~(3-),(SO_4)~(2-),(ClO_3)~-], Na_5Eu(MoO_4)_(4-x)(PO_4)_xLi_x, Na_5Eu(MoO_4)_(4-x)(ClO_3)_xCl_x and LiGd_(1-x)Eu_x(MoO_4)_2, LiGd_(0.6-x)Y_xEu_(0.4)(MoO_4)_2 were prepared by conventional solid-state reaction. The influence of reaction conditions, doping concentration on the system structure and luminescence properties was investigated.
In order to analyze the effects of different doped ions and different substrates on the characteristics of system, XRD, SEM, excitation and emission spectra were carried out. XRD proves that the different doping Na_5Eu(MoO_4)_4 system samples belong to a tetragonal scheelite-like structure. The different doping LiGd(MoO_4)_2 system samples pertain to a tetragonal scheelite-structure. Samples of the two systems are space group I41/a. SEM photographs show that the effective doping can improve the crystallization effect and modify the morphology of the samples. With near-UV 395 nm light, the excitation and emission spectra of all phosphors exhibit superior red emission to the commercial red phosphor Y2O2S: Eu~(3+).
In this work, the influence of reaction conditions, doping concentration on the system structure and luminescence properties of Eu~(3+) doped molybdates were investigated, which expected to give the valuable reference to explore novel red phosphors for WLED.
本文采用传统的高温固相法,以钼酸盐为基质材料,掺杂稀土Eu~(3+)离子制备了多种可被近紫外光有效激发的红色荧光粉:碱金属阳离子Li~+、K~+掺杂的Na_5Eu(MoO_4)_4体系;含氧酸根阴离子(PO_4)~(3-)、(SO_4)~(2-)、(ClO_3)~-掺杂的Na_5Eu(MoO_4)_4并在此基础上考虑电价平衡掺杂,在体系中引入Li~+离子、Cl~-离子; LiGd_(1-x_Eu_x(MoO_4)_2体系和LiGd_(0.6-x)Y_xEu_(0.4)(MoO_4)_2体系。并研究了反应条件和掺杂浓度对各体系样品的结构和发光性能的影响。
为分析不同掺杂离子、不同电荷补偿掺杂和不同基质对样品的晶体结构和荧光性能的影响,对样品进行了X -射线衍射(XRD)、扫描电镜(SEM)、激发和发射光谱等表征。XRD结果表明所得不同离子掺杂Na_5Eu(MoO_4)_4体系的样品均属于四方晶系的类白钨矿(Scheelite - like)结构。不同离子掺杂的LiGd(MoO_4)_2体系的样品均为四方晶系的白钨矿(Scheelite)结构。两个体系样品的空间群均为I41/a。SEM照片显示采取有效掺杂有助于改善样品的结晶效果,修饰样品的形貌。在395 nm近紫外光激发下,所有样品Eu~(3+)的5D0 - 7F2(615 nm)跃迁发射的红光强度均高于商用红粉Y_2O_2S: Eu~(3+)的发射强度。
本文关于不同掺杂离子,不同基质掺杂对稀土Eu~(3+)离子激活的钼酸盐的晶体结构和发光性能进行了基础性研究,可为白光LED用新型红色发光材料的设计开发提供有价值的理论基础。
In the 21st, white light-emitting diodes (WLEDs), as the promising solid-state lighting sources to replace the conventional incandescent and fluorescent lamps, have attracted much attention due to their high reliability, long lifetime, low energy consumption and environment-friendly characteristics. The most effective approach to obtain WLED is phosphor - converted. However, the current red-emitting phosphor used for WLED reveals a rather low red emission under near-UV light excitation. Hence, it is necessary to search new red phosphors that can be efficiently excited around near-UV light.
In this paper, a series of red phosphors containing (Na,M)_5Eu(MoO_4)_4 [M = Li, K], Na_5Eu(MoO_4)_(4-x)M_y [M = (PO_4)~(3-),(SO_4)~(2-),(ClO_3)~-], Na_5Eu(MoO_4)_(4-x)(PO_4)_xLi_x, Na_5Eu(MoO_4)_(4-x)(ClO_3)_xCl_x and LiGd_(1-x)Eu_x(MoO_4)_2, LiGd_(0.6-x)Y_xEu_(0.4)(MoO_4)_2 were prepared by conventional solid-state reaction. The influence of reaction conditions, doping concentration on the system structure and luminescence properties was investigated.
In order to analyze the effects of different doped ions and different substrates on the characteristics of system, XRD, SEM, excitation and emission spectra were carried out. XRD proves that the different doping Na_5Eu(MoO_4)_4 system samples belong to a tetragonal scheelite-like structure. The different doping LiGd(MoO_4)_2 system samples pertain to a tetragonal scheelite-structure. Samples of the two systems are space group I41/a. SEM photographs show that the effective doping can improve the crystallization effect and modify the morphology of the samples. With near-UV 395 nm light, the excitation and emission spectra of all phosphors exhibit superior red emission to the commercial red phosphor Y2O2S: Eu~(3+).
In this work, the influence of reaction conditions, doping concentration on the system structure and luminescence properties of Eu~(3+) doped molybdates were investigated, which expected to give the valuable reference to explore novel red phosphors for WLED.
引文
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[2]刘行仁.白光LED固态照明光转换荧光体[J].发光学报, 2007, 28(3): 291 - 301.
[3] Qin C X, Huang Y L, Chen G Q, et al. Luminescence properties of a red phosphor europium tungsten oxide Eu2WO6[J]. Materials Letters, 2009 63: 1162 - 1164.
[4] Sivakumar V, Varadaraju U V. Intense red phosphor for white LEDs based on blue GaN LEDs[J]. Journal of The Electrochemical Society, 2006, 153(3): H54 - H57.
[5] Hu Y S, Zhuang W D, Ye H Q, et al. A novel red phosphor for white light emitting diodes[J]. Journal of Alloys and Compounds, 2005, 390: 226 - 229.
[6] Liu J, Lian H Z, Shi C H. Improved optical photoluminescence by charge compensation in the phosphor system CaMoO4: Eu3+[J]. Optical Materials, 2007, 29: 1591 - 1594.
[7]王涛,井艳军,朱月华等.白光LED用钨、钼酸盐红色荧光粉的研究进展[J].中国照明电器, 2008, 2: 16 - 20.
[8]张凯,刘河洲,胡文彬.白光LED用荧光粉的研究进展[J].材料导报, 2005, 19(9): 50 - 53.
[9] Haque M M, Lee H I, Kim D K. Luminescent properties of Eu3+-activated molybdate-based novel-emitting phosphors for LEDs[J]. Journal of Alloys and Compounds, 2009, 481: 792 - 796.
[10]肖志国.白光电致发光二极管用发光材料研究进展[J].化学通报, 2008, 2: 19 - 23.
[11]刘行仁,薛胜薛,黄德森等.白光LED现状和问题[J].光源与照明, 2003, 3: 4 - 8.
[12]刘行仁,王晓君,何大伟.加入WTO后我国稀土发光材料面临的机遇和挑战[J].中国稀土学报, 2002, 20(6): 491 - 494.
[13] Tyminski J K, Powell R C. Luminescence of calcium tungstate crystals[J]. Journal of Chemical Physics, 1974, 61 (10): 4003 - 4011.
[14] Tyminski J K, Lawson C M, Powell R C. Energy transfer between Eu3+ ions in LiNOO3, CaWO4 and EuxY1-xP5O14 crystals[J]. Journal of Chemical Physics, 1982, 77 (9): 4318 - 4322.
[15] Pode R B, Dhoble S J. Photoluminescence in CaWO4:Bi3+,Eu3+ Material[J].Material,1997, 203: 571 - 577.
[16] Wang Z L, Liang H B, Wang Q, et al. Novel red phosphor of Eu3+, Bi3+ coactivated double tungstates[J]. Physical Status Solidi A, 2009, 206: 1589 - 1593.
[17] Wang F, Fan X P, Pi D B, et al. Hydrothermal synthesis and luminescence behavior of rare-earth-doped NaLa(WO4)2 powders[J]. Journal of Solid State chemistry, 2005, 178: 825 - 830.
[18] Hwang K S, Hwangbo S, Kim J T. Sol-gel synethesis of red-emitting LiEuW2O8 powder as a near-ultraviolet convertible phosphor[J]. Ceramics International, 2009, 35: 2517 - 2519.
[19] Yan S X, Zhang J H, Zhang Xia, et al. Enhanced Red Emission in CaMoO4: Bi3+,Eu3+[J]. Journal of Physical chemistry, 2007, 111: 13256 - 13260.
[20] Jin Y, Zhang J H, LüS Z, et al. Fabrication of Eu3+ and Sm3+ Codoped Micro/Nanosized MMoO4 (M = Ca, Ba and Sr ) via Facile Hydrothermal Method and Their Photoluminescence Properties through Energy[J]. Journal of Physical chemistry, 2008, 112: 5860 - 5864.
[21] Wang Z L, Liang H B, Gong M L, et al. Luminescence investigation of Eu3+ activated double molybdate red phosphors with scheelite structure[J]. Journal of Alloys and Compounds, 2007, 432: 308 - 312.
[22] Wang Z L, Liang H B, Zhou L Y, et al. Luminescence of (Li0.333Na0.334K0.333)Eu(MoO4)2 and its application in near UV InGaN-based light - emitting diode[J]. chemical Physics Letters, 2005, 412: 313 - 316.
[23] Wang Z L, Liang H B, Wang J, et al. A novel red phosphor for near UV InGaN light - emitting diode and its luminescent properties[J]. Material Research Bulletin, 2008, 43: 907 - 911.
[24] Wang Z L, Liang H B, Gong M L, et al. Novel red phosphor of Bi3+, Sm3+ co-actived NaEu(MoO4)2[J]. Optical Materials, 2007, 29: 896 - 900.
[25] Wang Z L, Liang H B, Zhou L Y, et al. NaEu0.96Sm0.04(MoO4)2 as a promising red - emitting phosphor for LED solid - state lighting prepared by the Pechini process[J]. Journal of Luminescence, 2008, 128: 147 - 154.
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