CN101440284B - Europium activated phosphates purple light transmitting fluorescent powder and preparation thereof - Google Patents
Europium activated phosphates purple light transmitting fluorescent powder and preparation thereof Download PDFInfo
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- CN101440284B CN101440284B CN200810220141.9A CN200810220141A CN101440284B CN 101440284 B CN101440284 B CN 101440284B CN 200810220141 A CN200810220141 A CN 200810220141A CN 101440284 B CN101440284 B CN 101440284B
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Abstract
The invention discloses a europium-activated phosphate violetrays emission fluorescent powder. The fluorescent powder is characterized in that the compositions of the fluorescent are shown in the chemical formula: Sr2-x-yMgyP2O7:Eux, wherein x is more than or equal to 0.001 and less than or equal to 0.5, y is more than or equal to 0.1 and less than or equal to 2. The method for preparing the fluorescent powder comprises the following steps: a precursor is prepared through a chemical coprecipitation method; the precursor is treated at high temperature under reducing atmosphere; and the precursor is cooled to room temperature in the reducing atmosphere, is pulverized to the needed granularity, is washed through the deionized water at a temperature of between 70 and 85 DEG C, is dried at a temperature of between 120 and 150 DEG C and is treated through other steps. The europium-activated phosphate violetrays emission fluorescent powder has the characteristics that the product has even granularity and stable performance; the preparation method has a simple process; and the obtained fluorescent powder has stable performance and good consistency.
Description
Technical field
The invention belongs to rare earth luminescent material technical field, relate in particular to and be specially a kind of rare earth europium activated phosphates purple light transmitting fluorescent powder and manufacture method thereof.
Background technology
The hertzian wave of general wavelength 380nm～420nm is called purple light.Launch the fluorescent material of purple light mainly for the preparation of blueprint lamp, diazo copying lamp, neon light, the luminescent lamp of the special purposes such as mosquito luring lamp.What at the fluorescent material of this wave band, meet at present environmental requirement and performance requriements is strontium pyrophosphate magnesium europium.The preparation of strontium pyrophosphate magnesium europium is generally a plurality of raw material mechanically mixing and forms, and as US Patent No. 3484383, mechanically mixing often makes raw material inhomogeneous, and product performance are unstable.For addressing this problem, this patent provides by chemical precipitation method prepares RE phosphate throw out presoma, directly calcination reduction, and technique is simple, the fluorescent material stable performance high conformity obtaining.
Summary of the invention
The europium activated phosphates purple light transmitting fluorescent powder that will provide a kind of product performance stable is provided.
Another object of the present invention is the preparation method that a kind of above-mentioned fluorescent material will be provided.
The technical solution adopted for the present invention to solve the technical problems is:
An activated phosphate purple light transmitting fluorescent powder, is characterized in that the moiety of this fluorescent material is by following chemical formulation: Sr
2-x-ymg
yp
2o
7 :eu
x, wherein: 0.001≤x≤0.5,0.1≤y≤2.
The preparation method of above-mentioned europium activated phosphate purple light transmitting fluorescent powder, comprise the steps: (1), with chemical co-precipitation method, prepare presoma: the nucleidic mass ratio with each element in this fluorescent material chemical formula will and become the continuous co-precipitation of continuous stirring at 40～90 ℃ of solution and ammonium dibasic phosphate solution to prepare RE phosphate throw out containing europium compound with nitric acid dissolve containing strontium compound, magnesium-containing compound, after precipitation finishes at ageing throw out, then precipitation mixture is filtered, washing, dry after, obtain RE phosphate throw out; (2), by RE phosphate throw out pyroprocessing under reducing atmosphere, treatment temp is 900～1200 ℃, the treatment time is 1～5 hour; (3), in reducing atmosphere, drop to room temperature, RE phosphate throw out is crushed to desired particle size, with 70～85 ℃ of deionized water wash, at 120～150 ℃ of temperature, dry, obtain required product.
In the present invention's raw material used, alkaline-earth metal is metal carbonate or metal oxide or nitrate or muriate; Rare earth is oxide compound or rare earth nitrate or rare earth chloride.
In fluorescent material preparation process, also can adopt calcination-reduction two-step approach, under reducing atmosphere, before pyroprocessing, first pack RE phosphate throw out into corundum crucible, and be placed in High Temperature Furnaces Heating Apparatus sintering, atmosphere is air, sintering temperature is 800-1000 ℃, and sintering time is 3～5 hours.
Both can H in fluorescent material preparation process
2-N
2reduction, also can provide with carbon dust the reduction mode of reducing atmosphere.
According to the present invention, can obtain the purple light fluorescent material that mercury line effectively excites, emission peak wavelength is 390nm ± 5nm of 253.7nm.
Ageing of the present invention refers in the situation that deposition condition continues throw out is standing, and throw out is precipitated completely.
The invention has the beneficial effects as follows: europium activated phosphates purple light transmitting fluorescent powder of the present invention have product granularity evenly, the feature of stable performance, high conformity, its preparation method technique is simple.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is that emission wavelength of the present invention is the utilizing emitted light spectrogram of 390nm fluorescent material.
Embodiment
First, take high purity reagent Strontium carbonate powder, magnesium oxide, europium sesquioxide, wherein: Eu accounts for cationic molar fraction between 0.01～0.5.With nitric acid dissolve become solution and a certain amount of ammonium dibasic phosphate solution 40～90 ℃ and constantly stir under continuously co-precipitation prepare RE phosphate throw out, after precipitation finishes under 80 ℃ of insulations ageing throw out, then to precipitation mixture filter, washing, dry after, obtain RE phosphate throw out presoma.Afterwards, pack above-mentioned presoma into corundum crucible, compacting, and be placed in High Temperature Furnaces Heating Apparatus, be warmed up to 800-1000 ℃, sintering time is 3～5 hours.Then at H
2/ N
2reduction (H
2volume content 5～20%) in, 900～1200 ℃ are reduced 1～5 hour.Cool to room temperature in reduction atmosphere, by above-mentioned sinter from High Temperature Furnaces Heating Apparatus, takes out, fragmentation, with 80 ℃ of left and right deionized water wash three times (3L water/kg powder), 120～150 ℃ of baking ovens toast and within 6～10 hours, obtain alleged ultraviolet fluorescence powder.
embodiment 1:
In order to guarantee accuracy, first oxide reagent used is processed 8 hours in 120 ℃ of baking ovens.Press chemical formula: Sr
0.99mgP
2o
7: Eu
0.01take Strontium carbonate powder, magnesium oxide, europium sesquioxide, and Secondary ammonium phosphate, Strontium carbonate powder, magnesium oxide, europium sesquioxide are become to solution a with dilute nitric acid dissolution, Secondary ammonium phosphate is dissolved into solution b with deionized water.By solution a and b 50 ℃ and constantly stir under continuously co-precipitation prepare RE phosphate throw out, after precipitation finishes under 50 ℃ of insulations ageing throw out, then to precipitation mixture filter, washing, dry after, obtain RE phosphate throw out presoma.Then pack corundum crucible compacting into.In 1000 ℃ of air, sintering is 4 hours; Cooling; Then at 1000 ℃ of H
2-N
2(H in reducing atmosphere
2account for 10%) reduce 3 hours.In reducing atmosphere, drop to after room temperature, taking-up from High Temperature Furnaces Heating Apparatus, fragmentation, washing, baking, obtain required product.Test obtains under 253.7nm excites, and emission peak wavelength is 390nm, as shown in Figure 1.
embodiment 2:
In order to guarantee accuracy, first oxide reagent used is processed 8 hours in 120 ℃ of baking ovens.Press chemical formula: Sr
0.9mgP
2o
7: Eu
0.01take strontium nitrate, magnesium nitrate, europium nitrate, and Secondary ammonium phosphate, strontium nitrate, magnesium nitrate, europium nitrate are dissolved into solution a with deionized water, Secondary ammonium phosphate is dissolved into solution b with deionized water.By solution a and b 60 ℃ and constantly stir under continuously co-precipitation prepare RE phosphate throw out, after precipitation finishes under 60 ℃ of insulations ageing throw out, then to precipitation mixture filter, washing, dry after, obtain RE phosphate throw out presoma.Then pack corundum crucible compacting into.At 1000 ℃ of H
2/ N
2(H in reducing atmosphere
2account for 10%) direct-reduction 3 hours.In reducing atmosphere, drop to after room temperature, taking-up from High Temperature Furnaces Heating Apparatus, fragmentation, washing, baking, obtain required product.
embodiment 3:
In order to guarantee accuracy, first oxide reagent used is processed 8 hours in 120 ℃ of baking ovens.Press chemical formula: Sr
0.9mgP
2o
7: Eu
0.01take strontium chloride, magnesium chloride, Europium trichloride, and Secondary ammonium phosphate, Strontium carbonate powder, magnesium oxide, europium sesquioxide are become to solution a with dilute nitric acid dissolution, Secondary ammonium phosphate is dissolved into solution b with deionized water.By solution a and b 80 ℃ and constantly stir under continuously co-precipitation prepare RE phosphate throw out, after precipitation finishes under 80 ℃ of insulations ageing throw out, then to precipitation mixture filter, washing, dry after, obtain RE phosphate throw out presoma.Then pack corundum crucible compacting into.In 1000 ℃ of air, sintering is 4 hours; Cooling; Then corundum crucible overlaps large crucible outward again, and in-built activated carbon powder, adds a cover; At 1000 ℃, calcination.In the reducing atmosphere producing at carbon dust, drop to after room temperature, taking-up from High Temperature Furnaces Heating Apparatus, fragmentation, washing, baking, obtain required product.
embodiment 4
In order to guarantee accuracy, first oxide reagent used is processed 8 hours in 120 ℃ of baking ovens.By chemical formula: Sr0.9MgP2O7:Eu0.01, take strontium oxide, magnesium oxide, europium nitrate, and Secondary ammonium phosphate, Strontium Sulphate, sal epsom, europium sulfate are become to solution a with dilute nitric acid dissolution, Secondary ammonium phosphate is dissolved into solution b with deionized water.By solution a and b 90 ℃ and constantly stir under continuously co-precipitation prepare RE phosphate throw out, after precipitation finishes under 90 ℃ of insulations ageing throw out, then to precipitation mixture filter, washing, dry after, obtain RE phosphate throw out presoma.Then pack corundum crucible compacting into, then overlap large crucible outward at corundum crucible again, in-built activated carbon powder, adds a cover; At 1000 ℃, calcination.In the reducing atmosphere producing at carbon dust, drop to after room temperature, taking-up from High Temperature Furnaces Heating Apparatus, fragmentation, washing, baking, obtain required product.
More than according to essence of the present invention, illustrating rare earth europium activated phosphates purple light transmitting fluorescent powder and preparation method thereof in conjunction with the embodiments, but it is evident that for the person of ordinary skill of the art: in the situation that not deviating from the spirit and scope of the invention, can therefrom carry out various modifications and variations, as alkaline-earth metal i.e. metal carbonate, metal oxide, other metal-salts also, example hydrochloric acid salt, nitrate etc., rare earth is oxide compound both, also other rare-earth saltss, example hydrochloric acid salt, carbonate, nitrate etc.Improvement of the present invention and the variation within the scope in claims and equivalent thereof contained in the present invention.
Claims (1)
1. an europium activated phosphate purple light transmitting fluorescent powder, its preparation method is:
1) press composition formula: Sr
0.99mgP
2o
7: Eu
0.01take Strontium carbonate powder, magnesium oxide, europium sesquioxide and Secondary ammonium phosphate, Strontium carbonate powder, magnesium oxide, europium sesquioxide are become to solution a with dilute nitric acid dissolution, Secondary ammonium phosphate is dissolved into solution b with deionized water;
2) by solution a and b 50 ℃ and constantly stir under continuously co-precipitation prepare RE phosphate throw out, after precipitation finishes under 50 ℃ of insulations ageing throw out, then to precipitation mixture filter, washing, dry after, obtain RE phosphate throw out presoma, then pack corundum crucible compacting into;
3) sintering 4 hours in 1000 ℃ of air, cooling;
4) then at 1000 ℃ of H
2account for 10% H
2-N
2in reducing atmosphere, reduce 3 hours;
5) in reducing atmosphere, drop to after room temperature, taking-up from High Temperature Furnaces Heating Apparatus, fragmentation, washing, baking, obtain required product.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102115671B (en) * | 2010-01-04 | 2013-08-07 | 海洋王照明科技股份有限公司 | Phosphate-base red luminescent material and preparation method thereof |
| CN102796984B (en) * | 2011-05-23 | 2014-07-09 | 海洋王照明科技股份有限公司 | Multielement-doped strontium phosphate luminescent film, and preparation method and applications thereof |
| CN102775987B (en) * | 2012-07-08 | 2014-12-17 | 河北联合大学 | Synthetic method of manganese-ion-doped zinc phosphate luminescent nanorods |
| CN104818018B (en) * | 2015-03-18 | 2016-09-14 | 江门市科恒实业股份有限公司 | The co-precipitation preparation method of the pyrophosphate phosphor of alkaline including earth metal element, fluorescent material and application |
| CN104910907B (en) * | 2015-05-28 | 2017-01-04 | 彩虹集团电子股份有限公司 | A kind of preparation method of near ultraviolet fluorescent powder strontium pyrophosphate europium |
| CN105441075B (en) * | 2015-12-14 | 2018-01-09 | 江门市科恒实业股份有限公司 | A kind of barium pyrophosphate titanium fluorescent material and preparation method thereof |
| CN110964523B (en) * | 2019-11-11 | 2022-06-17 | 江苏师范大学 | Cr (chromium)3+Ion-activated near-infrared fluorescent powder and preparation method and application thereof |
| CN110903828B (en) * | 2019-11-11 | 2022-06-17 | 江苏师范大学 | Eu (Eu)3+Ion activated red fluorescent powder and preparation method and application thereof |
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Non-Patent Citations (4)
| Title |
|---|
| D. S. Thakare, et al..UV-emitting phosphors: synthesis, photoluminescence and applications.《Physica Status Solidi(a)》.2004,第201卷(第3期),第574-581页. * |
| D.S.Thakare et al..UV-emitting phosphors: synthesis |
| 孙家跃等.9.9.4 Sr2P2O7:Eu荧光粉的制备.《固体发光材料》.2003,第395页. * |
| 王惠琴等.不同反应条件对焦磷酸锶:铕(Ⅱ)磷光体发光性能的影响及其机制.《稀土》.1985,(第4期),第38-41页. * |
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