CN100575452C - Orange-yellow long-lasting phosphor and preparation method thereof - Google Patents
Orange-yellow long-lasting phosphor and preparation method thereof Download PDFInfo
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- CN100575452C CN100575452C CN200710056035A CN200710056035A CN100575452C CN 100575452 C CN100575452 C CN 100575452C CN 200710056035 A CN200710056035 A CN 200710056035A CN 200710056035 A CN200710056035 A CN 200710056035A CN 100575452 C CN100575452 C CN 100575452C
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 230000005923 long-lasting effect Effects 0.000 title description 19
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 150000001875 compounds Chemical class 0.000 claims abstract 3
- 150000003839 salts Chemical class 0.000 claims abstract 3
- 230000002688 persistence Effects 0.000 claims abstract 2
- 238000005303 weighing Methods 0.000 claims abstract 2
- 239000000203 mixture Substances 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 abstract 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 14
- 229910052593 corundum Inorganic materials 0.000 description 7
- 239000010431 corundum Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 229910052697 platinum Inorganic materials 0.000 description 7
- 239000012856 weighed raw material Substances 0.000 description 6
- 238000001354 calcination Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 4
- 230000005284 excitation Effects 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 150000004645 aluminates Chemical class 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- JGIATAMCQXIDNZ-UHFFFAOYSA-N calcium sulfide Chemical compound [Ca]=S JGIATAMCQXIDNZ-UHFFFAOYSA-N 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
技术领域 technical field
本发明涉及硅酸盐基荧光粉材料及其制备方法，特别是一种在从紫外到可见光激发下能发出橙黄色长余辉的荧光粉及其制备方法。The invention relates to a silicate-based fluorescent powder material and a preparation method thereof, in particular to a fluorescent powder capable of emitting orange-yellow long afterglow under excitation from ultraviolet to visible light and a preparation method thereof.
背景技术 Background technique
常用的传统长余辉材料主要有硫化锌和硫化钙荧光体。近些年来，稀土激活的铝酸盐体系和硅酸盐体系成为长余辉材料的主体。铝酸盐体系和硅酸盐体系这两大类长余辉材料在发光亮度、余辉时间、化学稳定性方面都比传统的硫化物长余辉发光材料有所提高，但现有的商用长余辉发光材料的颜色一般为黄绿、蓝紫、蓝绿，长波发射的长余辉材料比较缺乏，难以满足需要。橙黄色长余辉材料有中国专利申请号为02188548.4，名称为《橙黄色发射稀土长余辉磷光体》和中国专利申请号为200410020722.X，名称为《橙黄色长余辉发光材料及生产方法》的专利申请技术。这两个专利申请文件所公开的橙黄色长余辉发光材料都是以Y2O3S为基质。化学组成一种是Y2O3S:Tm，Mg，Ti，其中Tm3+和Mg2+的掺杂量为0.02-0.08摩尔分数，Ti4+离子为0.01摩尔分数。另一种是aY2O3S:bTi4+，cMg2+，0.9＝a＝0.99摩尔分数，0.01＝b＝0.1摩尔分数，0.01＝c＝0.05摩尔分数，碳酸钠为助溶剂。制备过程中容易产生含硫的有害气体.Commonly used traditional long afterglow materials mainly include zinc sulfide and calcium sulfide phosphors. In recent years, rare earth activated aluminate systems and silicate systems have become the main body of long afterglow materials. The two types of long-lasting luminescent materials, aluminate system and silicate system, have improved luminous brightness, afterglow time, and chemical stability compared with traditional sulfide long-lasting luminescent materials, but the existing commercial long-lasting luminescent materials The colors of LEDs are generally yellow-green, blue-purple, and blue-green, and long-wave emission materials with long afterglow are relatively scarce, which is difficult to meet the needs. The orange-yellow long-lasting material has Chinese patent application number 02188548.4, named "orange-yellow emitting rare earth long-lasting phosphor" and Chinese patent application number 200410020722.X, named "orange-yellow long-lasting luminescent material and its production method" Apply technology. The orange-yellow long-lasting luminescent materials disclosed in these two patent application documents are both based on Y 2 O 3 S. The chemical composition is Y 2 O 3 S:Tm, Mg, Ti, wherein the doping amount of Tm 3+ and Mg 2+ is 0.02-0.08 mole fraction, and Ti 4+ ion is 0.01 mole fraction. The other is aY 2 O 3 S:bTi 4+ , cMg 2+ , 0.9=a=0.99 mole fraction, 0.01=b=0.1 mole fraction, 0.01=c=0.05 mole fraction, and sodium carbonate is a co-solvent. Harmful gases containing sulfur are easily produced during the preparation process.
发明内容 Contents of the invention
本发明的目的是提供一种制备方法简单、无污染、成本低、在200nm-550nm波长光激发后能发出明亮的橙黄色长余辉的橙黄色长余辉荧光粉及其制备方法。The purpose of the present invention is to provide an orange-yellow long-lasting phosphor with a simple preparation method, no pollution, low cost, and can emit bright orange-yellow long-lasting afterglow after being excited by light at a wavelength of 200nm-550nm, and a preparation method thereof.
本发明提出的橙黄色长余辉荧光粉是一种由稀土元素铕掺杂的硅酸盐，其化学结构式为Sr3-x-ySiO5:Eux，Dyy，其中x、y为摩尔分数，x、y的取值范围：0＜x＝0.1，0＝y＝0.1，在200nm-550nm波长光(即从紫外到可见光)激发后发出橙黄色长余辉。The orange-yellow long-lasting phosphor powder proposed by the present invention is a silicate doped with rare earth element europium, and its chemical structural formula is Sr 3-xy SiO 5 : Eu x , Dy y , where x and y are mole fractions, and x , The value range of y: 0<x=0.1, 0=y=0.1, after being excited by light with a wavelength of 200nm-550nm (ie from ultraviolet to visible light), it emits a long orange-yellow afterglow.
本发明橙黄色长余辉荧光粉的制备方法如下：The preparation method of orange-yellow long afterglow fluorescent powder of the present invention is as follows:
1)按化学计量比称取通式中元素的氧化物或相应的碳酸盐类，研磨混匀。1) Weigh the oxides or corresponding carbonates of the elements in the general formula according to the stoichiometric ratio, grind and mix them evenly.
2)将前面步骤得到的混合体，置入高纯刚玉坩埚或铂坩埚中，放入高温炉中。在1250℃-1400℃温度内，在还原性气氛下条件下，加热2-4小时即得到该橙黄色长余辉荧光粉。2) Put the mixture obtained in the previous step into a high-purity corundum crucible or a platinum crucible, and put it into a high-temperature furnace. The orange-yellow long-lasting phosphor is obtained by heating for 2-4 hours at a temperature of 1250° C.-1400° C. under a reducing atmosphere.
3)将前面步骤得到的烧结产物经研磨后即得橙黄色长余辉荧光粉成品。3) Grinding the sintered product obtained in the previous step to obtain the finished orange-yellow long-lasting phosphor.
采用本发明方法合成的荧光粉可在200nm-550nm波长光激发下发出500nm-700nm波长橙黄色光，橙黄色宽带发射的峰值位于570nm。经太阳光或紫外光照射几分钟，去掉激发源之后，暗室里人眼可以观察到5小时以上的橙色长余辉。其制备方法简单，无污染，原料成本低。The fluorescent powder synthesized by the method of the invention can emit orange-yellow light with a wavelength of 500nm-700nm under the excitation of light with a wavelength of 200nm-550nm, and the peak value of the orange-yellow broadband emission is located at 570nm. After being irradiated by sunlight or ultraviolet light for a few minutes, and after the excitation source is removed, the long orange afterglow can be observed by human eyes for more than 5 hours in a dark room. The preparation method is simple, pollution-free and low in raw material cost.
附图说明 Description of drawings
图1为实施例2 Sr2.99SiO5:Eu0.01荧光粉的发射光谱(460nm激发，监测570nm)。Fig. 1 is the emission spectrum (excitation at 460nm, monitoring at 570nm) of the Sr 2.99 SiO 5 :Eu 0.01 phosphor in Example 2.
图2为实施例2 Sr2.99SiO5:Eu0.01荧光粉的余辉衰减曲线(监测570nm)。Fig. 2 is the afterglow decay curve (monitored at 570nm) of the Sr 2.99 SiO 5 :Eu 0.01 phosphor in Example 2.
具体实施方式 Detailed ways
实施例1Example 1
制备Sr3-xSiO5:Eux，其中x＝0.0075摩尔分数，具体表达式为：Sr2.9925SiO5:Eu0.075。按化学计量比称取4.4178gSrCO3，0.6008gSiO2，0.0132gEu2O3，将称取的原料研磨混匀后，置入高纯刚玉坩埚或铂坩埚，放入高温炉中。在1250℃-1400℃温度内，在CO或氮氢混合气体还原气氛条件下，培烧2-4小时后研磨，即得到橙黄色长余辉荧光粉Sr2.9925SiO5:Eu0.075。Prepare Sr 3-x SiO 5 :Eu x , where x=0.0075 mole fraction, the specific expression is: Sr 2.9925 SiO 5 :Eu 0.075 . Weigh 4.4178gSrCO 3 , 0.6008gSiO 2 , and 0.0132gEu 2 O 3 according to the stoichiometric ratio, grind and mix the weighed raw materials, put them into a high-purity corundum crucible or a platinum crucible, and put them into a high-temperature furnace. In the temperature range of 1250°C-1400°C, under CO or nitrogen-hydrogen mixed gas reducing atmosphere, after calcination for 2-4 hours, grind to obtain orange-yellow long-lasting phosphor Sr 2.9925 SiO 5 :Eu 0.075 .
实施例2Example 2
制备Sr3-xSiO5:Eux，其中x＝0.01摩尔分数，具体表达式为：Sr2.99SiO5:Eu0.01。按化学计量比称取4.4142gSrCO3，0.6008gSiO2，0.0176g Eu2O3，将称取的原料充分研细混匀后，置入高纯刚玉坩埚或铂坩埚，放入高温炉中。在1250℃-1400℃温度内，在CO或氮氢混合气体还原气氛条件下，培烧2-4小时后研磨，即得到橙黄色长余辉荧光粉Sr2.99SiO5:Eu0.01。Prepare Sr 3-x SiO 5 :Eu x , where x=0.01 mole fraction, the specific expression is: Sr 2.99 SiO 5 :Eu 0.01 . Weigh 4.4142g SrCO 3 , 0.6008g SiO 2 , and 0.0176g Eu 2 O 3 according to the stoichiometric ratio, thoroughly grind and mix the weighed raw materials, put them into high-purity corundum crucibles or platinum crucibles, and put them into high-temperature furnaces. At a temperature of 1250°C-1400°C, under CO or nitrogen-hydrogen mixed gas reducing atmosphere, after calcination for 2-4 hours, grind to obtain orange-yellow long-lasting phosphor Sr 2.99 SiO 5 :Eu 0.01 .
图1所示为Sr2.99SiO5:Eu0.01荧光粉的发射光谱。图2所示为Sr2.99SiO5:Eu0.01荧光粉的余辉衰减曲线。Figure 1 shows the emission spectrum of Sr 2.99 SiO 5 :Eu 0.01 phosphor. Figure 2 shows the afterglow decay curve of Sr 2.99 SiO 5 :Eu 0.01 phosphor.
实施例3Example 3
制备Sr3-xSiO5:Eux，其中x＝0.03摩尔分数，具体表达式为：Sr2.99SiO5:Eu0.03。按化学计量比称取4.3846gSrCO3，0.6008gSiO2，0.0527g Eu2O3，将称取的原料充分研细混匀后，置入高纯刚玉坩埚或铂坩埚，放入高温炉中。在1250℃-1400℃温度内，在CO或氮氢混合气体还原气氛条件下，培烧2-4小时后研磨，即得到橙黄色长余辉荧光粉Sr2.99SiO5:Eu0.03。Prepare Sr 3-x SiO 5 :Eu x , where x=0.03 mole fraction, the specific expression is: Sr 2.99 SiO 5 :Eu 0.03 . Weigh 4.3846g SrCO 3 , 0.6008g SiO 2 , and 0.0527g Eu 2 O 3 according to the stoichiometric ratio, thoroughly grind and mix the weighed raw materials, put them into high-purity corundum crucibles or platinum crucibles, and put them into high-temperature furnaces. At a temperature of 1250°C-1400°C, under CO or nitrogen-hydrogen mixed gas reducing atmosphere, after calcination for 2-4 hours, grind to obtain orange-yellow long-lasting phosphor Sr 2.99 SiO 5 :Eu 0.03 .
实施例4Example 4
制备Sr3-xSiO5:Eux，其中x＝0.07摩尔分数，具体表达式为：Sr2.99SiO5:Eu0.07。按化学计量比称取4.3256gSrCO3，0.6008gSiO2，0.1232g Eu2O3，将称取的原料充分研磨混匀后，置入高纯刚玉坩埚或铂坩埚，放入高温炉中。在1250℃-1400℃温度内，在CO或氮氢混合气体还原气氛条件下，培烧2-4小时后研磨，即得到橙黄色长余辉荧光粉Sr2.99SiO5:Eu0.07。Prepare Sr 3-x SiO 5 :Eu x , where x=0.07 mole fraction, the specific expression is: Sr 2.99 SiO 5 :Eu 0.07 . Weigh 4.3256g SrCO 3 , 0.6008g SiO 2 , and 0.1232g Eu 2 O 3 according to the stoichiometric ratio. After fully grinding and mixing the weighed raw materials, put them into a high-purity corundum crucible or a platinum crucible, and put them into a high-temperature furnace. At a temperature of 1250°C-1400°C, under CO or nitrogen-hydrogen mixed gas reducing atmosphere, after calcination for 2-4 hours, grind to obtain orange-yellow long-lasting phosphor Sr 2.99 SiO 5 :Eu 0.07 .
实施例5Example 5
制备Sr3-x-ySiO5:Eux，Dyy，，其中x＝0.01摩尔分数，y＝0.03摩尔分数。具体表达式为：Sr2.96SiO5:Eu0.01，Dy0.03。按化学计量比称取4.3697gSrCO3，0.6008gSiO2，0.0176g Eu2O3，0.0560g Dy2O3，将称取的原料充分研磨混匀后，置入高纯刚玉坩埚或铂坩埚，放入高温炉中。在1250℃-1400℃温度内，在CO或氮氢混合气体还原气氛条件下，培烧2-4小时后研磨，即得到橙黄色长余辉荧光粉Sr2.96SiO5:Eu0.01，Dy0.03。Preparation of Sr 3-xy SiO 5 : Eu x , Dy y , where x=0.01 mole fraction, y=0.03 mole fraction. The specific expression is: Sr 2.96 SiO 5 :Eu 0.01 , Dy 0.03 . Weigh 4.3697gSrCO 3 , 0.6008gSiO 2 , 0.0176g Eu 2 O 3 , 0.0560g Dy 2 O 3 according to the stoichiometric ratio, grind and mix the weighed raw materials thoroughly, put them into high-purity corundum crucible or platinum crucible, put into the high temperature furnace. At a temperature of 1250°C-1400°C, under the reducing atmosphere of CO or nitrogen-hydrogen mixed gas, burn for 2-4 hours and then grind to obtain orange-yellow long-lasting phosphor Sr 2.96 SiO 5 :Eu 0.01 , Dy 0.03 .
实施例6Example 6
制备Sr3-x-ySiO5：Eux，Dyy，，其中x＝0.1摩尔分数，y＝0.1摩尔分数。具体表达式为：Sr2.8SiO5:Eu01，Dy0.1。按化学计量比称取4.1337gSrCO3，0.6008gSiO2，0.1760g Eu2O3，0.1865g Dy 2O3，将称取的原料充分研磨混匀后，置入高纯刚玉坩埚或铂坩埚，放入高温炉中。在1250℃-1400℃温度内，在CO或氮氢混合气体还原气氛条件下，培烧2-4小时后研磨，即得到橙黄色长余辉荧光粉Sr2.8SiO5:Eu0.1，Dy0.1。Preparation of Sr 3-xy SiO 5 : Eu x , Dy y , where x=0.1 mole fraction, y=0.1 mole fraction. The specific expression is: Sr 2.8 SiO 5 :Eu 01 , Dy 0.1 . Weigh 4.1337g SrCO 3 , 0.6008g SiO 2 , 0.1760g Eu 2 O 3 , 0.1865g Dy 2 O 3 according to the stoichiometric ratio, grind and mix the weighed raw materials thoroughly, put them into high-purity corundum crucible or platinum crucible, put into the high temperature furnace. At a temperature of 1250°C-1400°C, under CO or nitrogen-hydrogen mixed gas reducing atmosphere, after calcination for 2-4 hours, grind to obtain orange-yellow long-lasting phosphor Sr 2.8 SiO 5 :Eu 0.1 , Dy 0.1 .
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| CN104232081B (en) * | 2014-08-11 | 2016-11-09 | 北京大学包头创新研究院 | A kind of light converting function material and its preparation method and application |
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| CN1410508A (en) * | 2002-11-22 | 2003-04-16 | 中国科学院长春应用化学研究所 | Orange yellow coloured emission rare earth long afterglow phosphorescent body |
| CN1583950A (en) * | 2004-06-09 | 2005-02-23 | 大连中邦化学工业股份有限公司 | Orange long persistence fluorescent material and its production |
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| CN1583950A (en) * | 2004-06-09 | 2005-02-23 | 大连中邦化学工业股份有限公司 | Orange long persistence fluorescent material and its production |
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