CN101440284A - 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
- Publication number
- CN101440284A CN101440284A CNA2008102201419A CN200810220141A CN101440284A CN 101440284 A CN101440284 A CN 101440284A CN A2008102201419 A CNA2008102201419 A CN A2008102201419A CN 200810220141 A CN200810220141 A CN 200810220141A CN 101440284 A CN101440284 A CN 101440284A
- Authority
- CN
- China
- Prior art keywords
- phosphate
- fluorescent powder
- light transmitting
- purple light
- reducing atmosphere
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Luminescent Compositions (AREA)
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.The fluorescent material of emission purple light is mainly used in the preparation blueprint lamp, diazo copying lamp, neon light, the luminescent lamp of special purposes such as mosquito luring lamp.At present compliance with environmental protection requirements of the fluorescent material of this wave band 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 U.S. Pat 3484383, mechanically mixing often makes raw material inhomogeneous, the product performance instability.For addressing this problem, this patent provides with chemical precipitation method and prepares RE phosphate throw out presoma, directly calcination reduction, and technology is simple, the fluorescent material stable performance high conformity that obtains.
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:
A kind of europium activated phosphate purple light transmitting fluorescent powder, the moiety that it is characterized in that 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), prepare presoma: will contain strontium compound, magnesium-containing compound and contain europium compound with each atoms of elements amount ratio in this fluorescent material chemical formula and become solution and ammonium dibasic phosphate solution constantly to stir continuous prepared by co-precipitation RE phosphate throw outs down at 40～90 ℃ with nitric acid dissolve with chemical co-precipitation method, precipitation obtains the RE phosphate throw out after finishing afterwards at the ageing throw out, then to precipitation mixture filtration, washing, drying; (2), with 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, the RE phosphate throw out is crushed to desired particle size, with 70～85 ℃ of deionized water wash, dry under 120～150 ℃ of temperature, promptly obtain required product.
In the used raw material of the present invention, 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.
Also can adopt calcination-reduction two-step approach in the fluorescent material preparation process, the corundum crucible of promptly under reducing atmosphere, earlier the RE phosphate throw out being packed into before the pyroprocessing, and to place High Temperature Furnaces Heating Apparatus sintering, atmosphere be air, sintering temperature is 800-1000 ℃, and sintering time is 3～5 hours.
But in fluorescent material preparation process both H
2-N
2Reduce, the reduction mode of reducing atmosphere also can be provided with carbon dust.
The purple light fluorescent material that the mercury line that can obtain 253.7nm according to the present invention effectively excites, emission peak wavelength is 390nm ± 5nm.
Ageing of the present invention is meant under the situation of deposition condition continuity throw out is left standstill, throw out is precipitated fully.
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 characteristics of stable performance, high conformity, its preparation method technology is simple.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is the emmission spectrum figure of 390nm fluorescent material for emission wavelength of the present invention.
Embodiment
At first, take by weighing high purity reagent Strontium carbonate powder, magnesium oxide, europium sesquioxide, wherein: Eu accounts for cationic molar fraction between 0.01～0.5.Become solution and a certain amount of ammonium dibasic phosphate solution to reach continuous prepared by co-precipitation RE phosphate throw out under the constantly stirring with nitric acid dissolve at 40～90 ℃, precipitation finish the back at ageing throw out under 80 ℃ of insulations, then to precipitation mixture filtration, washing, drying after, obtain RE phosphate throw out presoma.Afterwards, with above-mentioned presoma pack into corundum crucible, compacting, and place 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%) 900～1200 ℃ were reduced 1～5 hour in.Cool to room temperature in the reduction atmosphere, with above-mentioned sinter from High Temperature Furnaces Heating Apparatus, takes out, fragmentation, with 80 ℃ of left and right sides deionized water wash three times (3L water/kg powder), 120～150 ℃ of baking ovens toast and promptly got alleged ultraviolet fluorescence powder in 6～10 hours.
Embodiment 1:
In order to guarantee accuracy, earlier used oxide reagent was handled 8 hours in 120 ℃ of baking ovens.Press chemical formula: Sr
0.9MgP
2O
7: Eu
0.01Take by weighing Strontium carbonate powder, magnesium oxide, europium sesquioxide, and Secondary ammonium phosphate, Strontium carbonate powder, magnesium oxide, europium sesquioxide are become solution a with dilute nitric acid dissolution, Secondary ammonium phosphate is dissolved into solution b with deionized water.With solution a and b 50 ℃ and constantly stir under prepared by co-precipitation RE phosphate throw out continuously, precipitation finish the back at ageing throw out under 50 ℃ of insulations, then to precipitation mixture filtration, washing, drying after, obtain RE phosphate throw out presoma.Pack into then corundum crucible and compacting.Sintering is 4 hours in 1000 ℃ of air; Cooling; Then at 1000 ℃ of H
2-N
2(H in the reducing atmosphere
2Account for 10%) reduced 3 hours.After dropping to room temperature in the reducing atmosphere, taking-up from High Temperature Furnaces Heating Apparatus, fragmentation, washing, baking promptly get required product.Test obtains exciting down at 253.7nm, and emission peak wavelength is 390nm, as shown in Figure 1.
Embodiment 2:
In order to guarantee accuracy, earlier used oxide reagent was handled 8 hours in 120 ℃ of baking ovens.Press chemical formula: Sr
0.9MgP
2O
7: Eu commands
0.01Take by weighing 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.With solution a and b 60 ℃ and constantly stir under prepared by co-precipitation RE phosphate throw out continuously, precipitation finish the back at ageing throw out under 60 ℃ of insulations, then to precipitation mixture filtration, washing, drying after, obtain RE phosphate throw out presoma.Pack into then corundum crucible and compacting.At 1000 ℃ of H
2/ N
2(H in the reducing atmosphere
2Account for 10%) directly reduced 3 hours.After dropping to room temperature in the reducing atmosphere, taking-up from High Temperature Furnaces Heating Apparatus, fragmentation, washing, baking promptly get required product.
Embodiment 3:
In order to guarantee accuracy, earlier used oxide reagent was handled 8 hours in 120 ℃ of baking ovens.Press chemical formula: Sr
0.9MgP
2O
7: Eu
0.01Take by weighing strontium chloride, magnesium chloride, Europium trichloride, and Secondary ammonium phosphate, Strontium carbonate powder, magnesium oxide, europium sesquioxide are become solution a with dilute nitric acid dissolution, Secondary ammonium phosphate is dissolved into solution b with deionized water.With solution a and b 80 ℃ and constantly stir under prepared by co-precipitation RE phosphate throw out continuously, precipitation finish the back at ageing throw out under 80 ℃ of insulations, then to precipitation mixture filtration, washing, drying after, obtain RE phosphate throw out presoma.Pack into then corundum crucible and compacting.Sintering is 4 hours in 1000 ℃ of air; Cooling; Corundum crucible overlaps big crucible outward more then, and interior dress activated carbon powder is added a cover; Under 1000 ℃, calcination.Drop to room temperature in the reducing atmosphere that carbon dust produces after, taking-up from High Temperature Furnaces Heating Apparatus, fragmentation, washing, baking promptly get required product.
Embodiment 4
In order to guarantee accuracy, earlier used oxide reagent was handled 8 hours in 120 ℃ of baking ovens.Press chemical formula: Sr
0.9MgP
2O
7: Eu
0.01Take by weighing strontium oxide, magnesium oxide, europium nitrate, and Secondary ammonium phosphate, Strontium Sulphate, sal epsom, europium sulfate are become solution a with dilute nitric acid dissolution, Secondary ammonium phosphate is dissolved into solution b with deionized water.With solution a and b 90 ℃ and constantly stir under prepared by co-precipitation RE phosphate throw out continuously, precipitation finish the back at ageing throw out under 90 ℃ of insulations, then to precipitation mixture filtration, washing, drying after, obtain RE phosphate throw out presoma.Big crucible is overlapped in pack into then corundum crucible and compacting more again outside corundum crucible, interior dress activated carbon powder is added a cover; Under 1000 ℃, calcination.Drop to room temperature in the reducing atmosphere that carbon dust produces after, taking-up from High Temperature Furnaces Heating Apparatus, fragmentation, washing, baking promptly get required product.
More than be according to essence of the present invention, specifying 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: under the situation that does not deviate from the spirit and scope of the invention, can therefrom carry out various improvement and variation, 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 that is in claims and equivalent thereof contained in the present invention.
Claims (6)
1. europium activated phosphate purple light transmitting fluorescent powder, the moiety that it is characterized in that 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.
2. described europium activated phosphate purple light transmitting fluorescent powder according to claim 1, the emission peak wavelength that it is characterized in that this fluorescent material is 390 ± 5nm.
3. the preparation method of an europium activated phosphate purple light transmitting fluorescent powder as claimed in claim 1, it is characterized in that comprising the steps: (1), prepare presoma with chemical co-precipitation method: will contain strontium compound with each atoms of elements amount ratio in this fluorescent material chemical formula, magnesium-containing compound and contain europium compound and become solution and ammonium dibasic phosphate solution constantly to stir continuous prepared by co-precipitation RE phosphate throw outs down at 40～90 ℃ with nitric acid dissolve, precipitation finishes the back at the ageing throw out, then precipitation mixture is filtered, washing, after the drying, obtain the RE phosphate throw out; (2), with 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, the RE phosphate throw out is crushed to desired particle size, with 70～85 ℃ of deionized water wash, dry under 120～150 ℃ of temperature, promptly obtain required product.
4. described europium activated phosphate purple light transmitting fluorescent powder preparation method according to claim 3 is characterized in that alkaline-earth metal is metal carbonate or metal oxide or nitrate or muriate in the used raw material; Rare earth is oxide compound or rare earth nitrate or rare earth chloride.
5. described europium activated phosphate purple light transmitting fluorescent powder preparation method according to claim 3, it is characterized in that the corundum crucible of under reducing atmosphere, earlier the RE phosphate throw out being packed into before the pyroprocessing, and place the High Temperature Furnaces Heating Apparatus sintering, atmosphere is air, sintering temperature is 800-1000 ℃, and sintering time is 3～5 hours.
6. described europium activated phosphate purple light transmitting fluorescent powder preparation method according to claim 3 is characterized in that described reducing atmosphere is H
2-N
2Reducing atmosphere or the reducing atmosphere that provides with carbon dust.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810220141.9A CN101440284B (en) | 2008-12-18 | 2008-12-18 | Europium activated phosphates purple light transmitting fluorescent powder and preparation thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810220141.9A CN101440284B (en) | 2008-12-18 | 2008-12-18 | Europium activated phosphates purple light transmitting fluorescent powder and preparation thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101440284A true CN101440284A (en) | 2009-05-27 |
| CN101440284B CN101440284B (en) | 2014-02-19 |
Family
ID=40724897
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200810220141.9A Expired - Fee Related CN101440284B (en) | 2008-12-18 | 2008-12-18 | Europium activated phosphates purple light transmitting fluorescent powder and preparation thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101440284B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115671A (en) * | 2010-01-04 | 2011-07-06 | 海洋王照明科技股份有限公司 | Phosphate-base red luminescent material and preparation method thereof |
| CN102775987A (en) * | 2012-07-08 | 2012-11-14 | 河北联合大学 | Synthetic method of manganese-ion-doped zinc phosphate luminescent nanorods |
| CN102796984A (en) * | 2011-05-23 | 2012-11-28 | 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 |
| CN104818018A (en) * | 2015-03-18 | 2015-08-05 | 江门市科恒实业股份有限公司 | Coprecipitation preparation method for pyrophosphate phosphor containing alkali earth metal, and phosphor and application thereof |
| CN104910907A (en) * | 2015-05-28 | 2015-09-16 | 彩虹集团电子股份有限公司 | Near ultraviolet fluorescent powder pyrophosphate strontium europium preparation method |
| CN105441075A (en) * | 2015-12-14 | 2016-03-30 | 江门市科恒实业股份有限公司 | Titanium barium pyrophosphate phosphor and preparation method thereof |
| CN110903828A (en) * | 2019-11-11 | 2020-03-24 | 江苏师范大学 | Eu (Eu)3+Ion activated red fluorescent powder and preparation method and application thereof |
| CN110964523A (en) * | 2019-11-11 | 2020-04-07 | 江苏师范大学 | Cr (chromium)3+Ion-activated near-infrared fluorescent powder and preparation method and application thereof |
-
2008
- 2008-12-18 CN CN200810220141.9A patent/CN101440284B/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115671A (en) * | 2010-01-04 | 2011-07-06 | 海洋王照明科技股份有限公司 | Phosphate-base red luminescent material and preparation method thereof |
| 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 |
| CN102796984A (en) * | 2011-05-23 | 2012-11-28 | 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 |
| CN102775987A (en) * | 2012-07-08 | 2012-11-14 | 河北联合大学 | Synthetic method of manganese-ion-doped zinc phosphate luminescent nanorods |
| CN102775987B (en) * | 2012-07-08 | 2014-12-17 | 河北联合大学 | Synthetic method of manganese-ion-doped zinc phosphate luminescent nanorods |
| CN104818018A (en) * | 2015-03-18 | 2015-08-05 | 江门市科恒实业股份有限公司 | Coprecipitation preparation method for pyrophosphate phosphor containing alkali earth metal, and phosphor and application thereof |
| 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 |
| CN104910907A (en) * | 2015-05-28 | 2015-09-16 | 彩虹集团电子股份有限公司 | Near ultraviolet fluorescent powder pyrophosphate strontium europium preparation method |
| CN105441075A (en) * | 2015-12-14 | 2016-03-30 | 江门市科恒实业股份有限公司 | Titanium barium pyrophosphate phosphor and preparation method thereof |
| 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 |
| CN110903828A (en) * | 2019-11-11 | 2020-03-24 | 江苏师范大学 | Eu (Eu)3+Ion activated red fluorescent powder and preparation method and application thereof |
| CN110964523A (en) * | 2019-11-11 | 2020-04-07 | 江苏师范大学 | Cr (chromium)3+Ion-activated near-infrared fluorescent powder and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101440284B (en) | 2014-02-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101440284B (en) | Europium activated phosphates purple light transmitting fluorescent powder and preparation thereof | |
| Li et al. | NaBaLa2 (PO4) 3: a novel host lattice for Sm3+-doped phosphor materials emitting reddish-orange light | |
| Ekambaram et al. | Synthesis of lamp phosphors: facile combustion approach | |
| KR100700952B1 (en) | A process for producing aluminate-based phosphor | |
| Wang et al. | Luminescence properties of nanocrystalline YVO4: Eu3+ under UV and VUV excitation | |
| EP1053560B1 (en) | Method of preparing high brightness, small particle red-emitting phosphor and the phosohor | |
| WO2011094937A1 (en) | Terbium doped phosphate-based green luminescent material and preparation method thereof | |
| Guo et al. | Pechini sol-gel synthesis of La2CaB8O16: Eu3+ red phosphor and its photoluminescence spectral properties | |
| CN101439869B (en) | Preparation of cerium activated rare earth aluminate ultraviolet transmitting fluorescent powder | |
| US5989454A (en) | Method for making small particle blue emitting lanthanum phosphate based phosphors | |
| CN1974718A (en) | Cerium activated ultraviolet emitting RE phosphate phosphor and its prepn process | |
| Zou et al. | Structure and luminescent properties of Ca 3 Bi (PO 4) 3: Sm 3+ orange phosphor | |
| Singh et al. | Pl and ESR study on UVB-emitting Gadolinium-doped BaMgAl 10 O 17 hexagonal phase obtained by combustion synthesis | |
| Singh et al. | Effect of annealing on photoluminescence properties of combustion synthesized ultraviolet-emitting cerium-ion-doped LiAl5O8 phosphor | |
| CN103351865B (en) | Vanadate red phosphor material and preparation method thereof | |
| CN101586029B (en) | Yttrium-gadolinium-europium borate red phosphors and preparation method thereof | |
| CN104388081A (en) | Synthetic method for aluminate doped with valence-state-controllable rare earth element and product thereof | |
| CN102352249A (en) | (Y1-x-yGdy,Eux)(P1-a,Va)O4 red phosphor and preparation method thereof | |
| Du et al. | Sol-gel processing, spectral features and thermal stability of Li-stuffed Li6CaLa2Nb2O12: RE garnet phosphors (RE= Pr, Sm, Tb, Dy) | |
| Cao et al. | Synthesis and Luminescent Properties of Eu3+-Doped NaCaPO4 Nano-Particles Under VUV–UV Excitation | |
| CN101696356B (en) | Method for manufacturing borate green phosphor | |
| Tian et al. | Facile combustion synthesis and luminescent properties of Eu3+ doped alkali-alkaline earth metal phosphate red phosphor | |
| Park et al. | Enhanced photoluminescence of Gd0. 94 (P1− xVx) O4: Eu0. 06 red-emitting (0≤ x≤ 1.0) phosphors | |
| CN113150782B (en) | Preparation method of rare earth ion doped orthorhombic indium acid gadolinium-calcium-titanium ore fluorescent powder | |
| JPH09255950A (en) | Preparation of light-storing luminescent pigment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140219 Termination date: 20211218 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |