稀土掺杂四硼酸铝钇绿色荧光粉的制备与荧光性能研究
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摘要
硼铝酸盐基质的发光材料结合了硼酸盐和铝酸盐体系两种发光材料的优点,并且在结构中含有大量的硼氧和铝氧基团,使其在真空紫外区具有很强吸收,因此有希望成为新一代的PDP用荧光粉。高温固相法是合成YAB:Tb~(3+)荧光粉的传统方法,但是这种方法所需的温度较高,且反应的时间较长,并且对样品的球磨处理在一定程度上会影响发光效率,因此改进制备工艺或寻求新的制备方法对提高荧光粉的发光性能具有一定的意义。本文通过化学共沉淀法,合成了以YAl_3(BO_3)_4为基质,Ce~(3+)为敏化剂, Tb~(3+)为激活剂的绿色荧光粉,并对所制备的粉体的结构、形貌、结晶度及荧光性能进行了分析。
为了得到发光效率较高的YAB:Ce~(3+), Tb~(3+)荧光粉,本文首先探索了Tb~(3+)的浓度对发光强度的影响,研究了Ce~(3+)离子的掺杂对Tb~(3+)离子的特征发射峰强度的影响,分析了能量传递的机理,其次以离子溶液浓度、沉淀剂浓度、硼酸含量和沉淀温度为影响参数,对YAB:Ce~(3+), Tb~(3+)荧光粉的制备条件进行了研究,最后通过热处理研究了煅烧条件对荧光粉发光强度的影响。
通过实验表明:在YAl_3(BO_3)_4基质中,稀土离子Ce~(3+)和Tb~(3+)的掺杂浓度为30%和10%时,发光强度最强,Ce→Tb之间存在着有效的能量传递;在溶液浓度为0.4mol/L,沉淀剂浓度为4mol/L、B含量为125%及水浴温度为25℃的合成条件下,荧光粉发光强度最强;在1100℃煅烧高温下,烧结2h得到的荧光粉发光强度最好。
Boron aluminate light-emitting materials combine both borate and aluminate luminescent material advantages, and in the structure contains large amounts of boron oxide and aluminum oxygen groups, so that they have strong absorption in the VUV region, therefore they are expected to become the new generation of PDP phosphors. High temperature solid state method is a traditional method to prepare YAB: Tb~(3+) phosphor, but this method requires a higher temperature and longer reaction time, and the ball milling process on the sample may influence the luminous efficiency in some extent, thereby improving preparation process or to seek new ways to improve the preparation of luminescent properties of phosphors have some significance. In this paper, the green phosphor was prepared by means of chemical co-precipitation method, which were based on YAl_3(BO_3)_4, sensitized by Ce~(3+), activated by Tb~(3+), and the structure of the prepared powders, morphology, crystallization and fluorescence performance were analyzed.
In order to obtain a higher luminous efficiency YAB: Ce~(3+), Tb~(3+) phosphor, the luminescence intensity impacted by the concentration of Tb~(3+) was explored in this paper, and the Tb~(3+) ions characteristic emission peak of strength impacte by the Ce~(3+) ion doped was also studied, and the energy transfer Mechanism was analysised, followed YAB: Ce~(3+), Tb~(3+) phosphor preparation conditions were studied by ion concentration, precipitant concentration, boric acid content and temperature as precipitation parameters, and finally the calcination conditions impact on the luminescence intensity of phosphor through the heat treatment were studied.
The experimental results indicate that: in YAl_3(BO_3)_4, rare earth ions Ce~(3+) and Tb~(3+) doping concentration is 30% and 10%, the luminous intensity strongest, Ce→Tb exists the effective energy transfer; under synthesis conditions of solution concentration is 0.4 mol/L, precipitation agent concentration is 4mol/L, B content is 125% and temperature water-bath is 25℃, phosphor luminous intensity strongest; under the 1,100℃and high temperature sintering for 2h, the fluorescence intensity of samples is best.
为了得到发光效率较高的YAB:Ce~(3+), Tb~(3+)荧光粉,本文首先探索了Tb~(3+)的浓度对发光强度的影响,研究了Ce~(3+)离子的掺杂对Tb~(3+)离子的特征发射峰强度的影响,分析了能量传递的机理,其次以离子溶液浓度、沉淀剂浓度、硼酸含量和沉淀温度为影响参数,对YAB:Ce~(3+), Tb~(3+)荧光粉的制备条件进行了研究,最后通过热处理研究了煅烧条件对荧光粉发光强度的影响。
通过实验表明:在YAl_3(BO_3)_4基质中,稀土离子Ce~(3+)和Tb~(3+)的掺杂浓度为30%和10%时,发光强度最强,Ce→Tb之间存在着有效的能量传递;在溶液浓度为0.4mol/L,沉淀剂浓度为4mol/L、B含量为125%及水浴温度为25℃的合成条件下,荧光粉发光强度最强;在1100℃煅烧高温下,烧结2h得到的荧光粉发光强度最好。
Boron aluminate light-emitting materials combine both borate and aluminate luminescent material advantages, and in the structure contains large amounts of boron oxide and aluminum oxygen groups, so that they have strong absorption in the VUV region, therefore they are expected to become the new generation of PDP phosphors. High temperature solid state method is a traditional method to prepare YAB: Tb~(3+) phosphor, but this method requires a higher temperature and longer reaction time, and the ball milling process on the sample may influence the luminous efficiency in some extent, thereby improving preparation process or to seek new ways to improve the preparation of luminescent properties of phosphors have some significance. In this paper, the green phosphor was prepared by means of chemical co-precipitation method, which were based on YAl_3(BO_3)_4, sensitized by Ce~(3+), activated by Tb~(3+), and the structure of the prepared powders, morphology, crystallization and fluorescence performance were analyzed.
In order to obtain a higher luminous efficiency YAB: Ce~(3+), Tb~(3+) phosphor, the luminescence intensity impacted by the concentration of Tb~(3+) was explored in this paper, and the Tb~(3+) ions characteristic emission peak of strength impacte by the Ce~(3+) ion doped was also studied, and the energy transfer Mechanism was analysised, followed YAB: Ce~(3+), Tb~(3+) phosphor preparation conditions were studied by ion concentration, precipitant concentration, boric acid content and temperature as precipitation parameters, and finally the calcination conditions impact on the luminescence intensity of phosphor through the heat treatment were studied.
The experimental results indicate that: in YAl_3(BO_3)_4, rare earth ions Ce~(3+) and Tb~(3+) doping concentration is 30% and 10%, the luminous intensity strongest, Ce→Tb exists the effective energy transfer; under synthesis conditions of solution concentration is 0.4 mol/L, precipitation agent concentration is 4mol/L, B content is 125% and temperature water-bath is 25℃, phosphor luminous intensity strongest; under the 1,100℃and high temperature sintering for 2h, the fluorescence intensity of samples is best.
引文
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[24]武祥,邵义,康煜平.溶胶凝胶法制备PDP用荧光粉BaAl_(12)O_(19):Mn[J].沈阳工业大学学报, 2005, 27(5): 502-505.
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[31] XU G, ZHANG X, HE W, et al. The Study of Surfactant Application on Synthesis of YAG Nano-Sized Powders[J]. Powder Technology, 2006, 163(3): 202-205.
[32] CAI W, LI H, ZHANG Y. Influences of Processing Techniques of the H_2O_2-Precipitated Pseudoboehmite on the Structural and Textural Properties ofγ-Al_2O_3[J]. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 2007, 295(1-3): 185-192.
[33] LV Y F, WU X J, WU D X, et al. Synthesis of Barium Fluoride Nano-Particles by Precipitation in Ethanol-Aqueous Mixed Solvents[J]. Powder Technology, 2007, 173(3): 174-178.
[34]董岩,蒋建清,吴直森,等.化学共沉淀法合成小粒径BaAl_(12)O_(19):Mn~(2+)绿色荧光粉[J].功能材料, 2005, 36(12): 1931-1933.
[35]景晓燕,郑传伟,王君,等.化学共沉淀法制备PDP荧光粉BaAl_(12)O_(19):Mn研究[J].哈尔滨工程大学学报, 2003, 24(2): 229-232.
[36]狄卫华,王晓君,陈宝玖,等. YPO_4:Tb荧光粉的制备及其VUV激发下的发光性能[J].发光学报, 2005, 26(5): 592-595.
[37] ZHANG P, XU M X, ZHENG ZH T, et al. Rapid Formation of Red Long Afterglow Phosphor Sr3Al2O6:Eu~(2+), Dy~(3+) by Microwave Irradiation[J]. Materials Science and Engineering: B, 2007, 136(2-3): 159-164.
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[2] OVERSLUIZEN G, KLEIN M, S, et al. Improvement of the Discharge Efficiency in Plasma Displays[J]. Journal of Applied Physics, 2002, 91(4): 85-60.
[3]陶怡,李岚,王达健,等. PDP荧光粉的优化研究[J].天津理工大学学报, 2005, 21(4): 74-77.
[4]李岚,梁翠果,谢宝森,等.绿色荧光粉YAGG: Tb, Gd用于FED的尝试[J].发光学报, 2002, 23(3): 253-254.
[5] BALLMAN A A. A New Series of Synthetic Borates Isostructural with the Carbonate Mineral Huntite [J]. Amer Mineral, 1962, 47(3): 1380-1383.
[6] MILLS A D. Crystallographic Data for New Rare Earth Borate Compounds, RX_3(BO_3)_4[J]. Inorganic Chemistry, 1962, 1(4): 960-961.
[7] GRAF D L, Bradley W F. The Crystal Structure of Huntite, Mg_3Ca(CO_3)_4[J]. Acta Crystallographica, 1962, 15(3): 238-242.
[8] PAN SH K, WANG G F. Structure of Low Temperature Phaseβ-Ba_3Y(BO_3)_3 Crystal[J]. Structure Chemistry, 2003, 22(2): 187-189.
[9] PAN SH K, WANG G F. Structure of High Temperature Phaseα-Ba_3Y(BO_3)_3 Crystal[J]. Structure Chemistry, 2003, 22(5): 550-552.
[10] LIN ZH B, HU Z SH, ZHANG L ZH, et al. Growth an Characterization of Crystal Nd_(0.06)Y_(0.94)Sr_6Sc(BO_3)_6[J]. Structure Chemistry, 2002, 21(6): 637-639.
[11] VERSTEGEN J M P J. A Survey of a Group of Phosphors, Based on Hexagonal Aluminate and Gallate Host Lattices[J]. Journal of Electrochemical Society, 1974, 121(12): 1623-1627.
[12] BUDDHUDU S, KAM C H, NG S L, et al. Green Color Luminescence in Tb~(3+) : (La, Ln)PO_4 (Ln = Gd or Y) Photonic Materials[J]. Materials Science and Engineering B, 2000, 72(1): 27-30.
[13] KAO F S, CHEN T M. A Study on the Luminescent Properties of New Green-Emitting Terbium-Activated Caln_2O_4: xTb Phosphors[J]. Journal of Luminescence, 2002, 96(2-4): 261-267.
[14] KAM C H, Buddhudu S. Emission Properties of GdOBr: Ce~(3+) and Tb~(3+) Phosphors [J]. Materials Letters, 2002, 54(5-6): 337-342.
[15] HE D W, YANG SH, GUAN Y F, et al. Research on Performance of ZnS: TbF_3 Thin Film Electroluminescence Device[J]. Rare Earths, 2003, 21(l): 19-22.
[16]陈宝玖,王海宁,秦伟平,等. Yb~(3+)和Er~(3+)共掺杂氟硼酸盐玻璃材料光学跃迁及红外到可见上转换[J].发光学报, 2000, 21(1): 38-42.
[17] VETRONE F, BOYER J C, CAPOBIANCO J A, et al. Significance of Yb~(3+) Concentration on the Up Conversion Mechanisms in Co-doped Y_2O_3: Er~(3+), Yb~(3+) Nano-Crystals [J]. Applied Physics, 2004, 96(1): 661-667.
[18] WANG Y H. Synthesis of Gd_(1-x)Eu_xA_(13)(BO_3)_4(0
[20] LI X X, WANG Y H. Synthesis of Gd_(1-x)Tb_xA_(13)(BO_3)_4(0.05≤x≤1) and Its Luminescence Properties Under VUV Excitation[J]. Journal of Luminescence, 2007, 122-123(1-4): 1000-1002.
[21] LIN K M, LIN C C, LI Y Y, et al. Synthesis of Gd2Ti2O7:Eu~(3+),V~(4+) Phosphors by Sol-Gel Process and Its Luminescent Properties[J]. Journal of Luminescence, 2007, 127(2): 561-567.
[22] JI H, XIE G, LU Y, et al. A New Phosphor with Flower-Like Structure and Luminescent Properties of Sr_2MgSi_2O_7:Eu~(2+), Dy~(3+) Long After Glow Materials by Sol-Gel Method[J]. Journal of Sol-Gel Science and Technology, 2007, 44(2): 133-137.
[23] MANAVBASI A, LACOMBE J C. A New Blue-Emitting Phosphor, SrZnO_2:Pb~(2+), Synthesized by the Adipic Acid Templated Sol-Gel Route[J]. Journal of Luminescence, 2008, 128(1): 129-134.
[24]武祥,邵义,康煜平.溶胶凝胶法制备PDP用荧光粉BaAl_(12)O_(19):Mn[J].沈阳工业大学学报, 2005, 27(5): 502-505.
[25] YANG H, REN ZH Y, CUI Y M, et al. Luminescent Properties of YAl_3(BO_3)_4:Eu~(3+) Phosphors[J]. Material Science, 2006, 41(2): 4133-4136.
[26] WANG Y H, WANG L L, LI H D. Electronic Structure and Linear OpticalProperties of YAl_3(BO_3)_4[J]. Journal of Applied Physics, 2007, 102(1): 1-5.
[27] HISASHI YOSHIDA, RYO YOSSHIMATSU, KAZUYOSHI OGASAWARA. Luminescence Properties of YAl_3(BO_3)_4 : Gd~(3+) Phosphors Substituted with Sc~(3+) Ions[J]. Journal of Luminescence, 2007, 122-123(1-4): 488-491.
[28] BEREGI E, WATTERICH A, KOVACS L, MADARASZ J. Solid-State Reactions in Y2_O_3:3Al_2O_3:4B_2O_3 System Studied by FTIR Spectroscopy and X-ray Diffraction[J]. Vibrational Spectroscopy, 2000, 22(1-2): 169-173.
[29]尤洪鹏,吴雪艳,洪广言,等. BaMgAl_(10)O_(17): R~(2+) (R= Eu, Mn)的真空紫外光谱特性[J].发光学报, 2002, 20(6): 572-574.
[30]刘端阳,何大伟,康凯,等. (Y, Gd)Al_3(BO_3)_4: Tb~(3+)的真空紫外光谱特性[J].光谱学与光谱分析, 2005, 25(7): 1034-1036.
[31] XU G, ZHANG X, HE W, et al. The Study of Surfactant Application on Synthesis of YAG Nano-Sized Powders[J]. Powder Technology, 2006, 163(3): 202-205.
[32] CAI W, LI H, ZHANG Y. Influences of Processing Techniques of the H_2O_2-Precipitated Pseudoboehmite on the Structural and Textural Properties ofγ-Al_2O_3[J]. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 2007, 295(1-3): 185-192.
[33] LV Y F, WU X J, WU D X, et al. Synthesis of Barium Fluoride Nano-Particles by Precipitation in Ethanol-Aqueous Mixed Solvents[J]. Powder Technology, 2007, 173(3): 174-178.
[34]董岩,蒋建清,吴直森,等.化学共沉淀法合成小粒径BaAl_(12)O_(19):Mn~(2+)绿色荧光粉[J].功能材料, 2005, 36(12): 1931-1933.
[35]景晓燕,郑传伟,王君,等.化学共沉淀法制备PDP荧光粉BaAl_(12)O_(19):Mn研究[J].哈尔滨工程大学学报, 2003, 24(2): 229-232.
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