CN102719245B - Secondary excitation type orange-red fluorescent powder and preparation method thereof - Google Patents
Secondary excitation type orange-red fluorescent powder and preparation method thereof Download PDFInfo
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- CN102719245B CN102719245B CN201210209234.8A CN201210209234A CN102719245B CN 102719245 B CN102719245 B CN 102719245B CN 201210209234 A CN201210209234 A CN 201210209234A CN 102719245 B CN102719245 B CN 102719245B
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- fluorescent powder
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- 239000000843 powder Substances 0.000 title claims abstract description 15
- 230000005284 excitation Effects 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 27
- 238000001354 calcination Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 6
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 3
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 3
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 3
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract 2
- 239000003814 drug Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 230000002688 persistence Effects 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000003836 solid-state method Methods 0.000 claims description 4
- 238000009841 combustion method Methods 0.000 claims description 3
- 229910016036 BaF 2 Inorganic materials 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 claims 1
- 238000000498 ball milling Methods 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000012216 screening Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 238000004020 luminiscence type Methods 0.000 description 5
- 229910005793 GeO 2 Inorganic materials 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000904 thermoluminescence Methods 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910003668 SrAl Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- JNVCSEDACVAATK-UHFFFAOYSA-L [Ca+2].[S-]SSS[S-] Chemical compound [Ca+2].[S-]SSS[S-] JNVCSEDACVAATK-UHFFFAOYSA-L 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005474 detonation Methods 0.000 description 1
- 230000005264 electron capture Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229940051851 sulfurated lime Drugs 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 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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- Luminescent Compositions (AREA)
Abstract
The invention relates to secondary excitation type orange-red fluorescent powder and a preparation method thereof, belonging to the technical field of luminescent materials. The fluorescent powder is Sr1-a-bCa1-x-cAl2-yMexREyO4S:aEu<2+>,bDy<3+> and cTm<3+>, where Me is at least one of Zn, Cd, Mg, RE is at least one of Ga, Zn, Ge, and Si, 0<x<0.1,0<y<0.2, 0<a<0.12, 0<b<0.1, and 0<c<0.1. The design idea is that: Eu<2+> and Tm<3+> are taken as a luminescent center and Dy<3+> and the like are added to be taken as an auxiliary excitant; the light of the Eu<2+> and Tm<3+> interacts; incident light from outside excitates Eu<2+> to emit light which excitates Tm<3+> to emit light again to form a secondary excitation type light emission; the relative ratio of Eu<2+> to Tm<3+> determines the color of the emitted light; and the concentration of Dy<3+> determines the afterglow time of the secondary excitation long-afterglow fluorescent powder. The preparation method comprises the following steps: weighing each oxide raw material according to the ratio of each element in the structural formula, adding a fluxing agent into the raw materials and uniformly mixing the mixture by ball milling, placing the obtained product in a reducing atmosphere for calcinations, and crushing and screening the obtained product to obtain the required fluorescent powder. The secondary excitation type orange-red fluorescent powder can emit orange-red fluorescent light, and the afterglow time can reach 8 to 12 h.
Description
Technical field
The invention belongs to luminescent material technical field, be specifically related to a kind of secondary excitation type orange red fluorescent powder and preparation method thereof.
Technical background
Long after glow luminous material is the important photo-induced energy storage functional materials of a class, has feature that is energy-conservation, that can be recycled.This kind of material industrial and agricultural production, military affairs, fire-fighting and people life many in be used widely.Long after glow luminous material is a kind of special thermoluminescence material, is also thermoluminescence material at room temperature.For this type of electron capture material, its luminescence phenomenon is caused by the trap level structure in material.According to long-persistence luminous general mechanism, if cause in matrix certain density at room temperature can by thermal perturbation store fault offset trap level out, just can produce long-persistence luminous.Traditional long after glow luminous material mainly contains zinc sulphide and sulfurated lime fluor.Nowadays the non-traditional long after glow luminous material of practical application is obtained, mainly SrAl
2o
4: Eu
2+, Dy
3+green glow long-afterglow material, Sr
4al
14o
25: Eu
2+, Dy
3+blue green light long-afterglow material, Sr
2mgSi
2o
7: Eu
2+, Dy
3+blue light long-afterglow material, Y
2o
2s:Eu
3+, Ln
3+ruddiness long-afterglow material.The preparation of a lot of patent fluorescent material in the past exists pollutes the shortcomings such as large, manufacturing cost is high, and Eu now
2+lack longwave transmissions long-afterglow material in aluminates system and silicate systems long after glow luminous material, be difficult to meet market demand, therefore, be necessary development of new high-performance and the long wave long after glow luminous material that more enriches of color.
At present, the synthetic method of long after glow luminous material mainly contains high temperature solid-state method, chemical coprecipitation, sol-gel method, microwave process for synthesizing, combustion method, hydro-thermal (solvent) synthesis method, microemulsion method, spray pyrolysis, Detonation Process etc.Wherein high temperature solid-state method is traditional in luminescent material industry is also current topmost preparation method, production technique comparative maturity.Because high temperature solid-state method is easy and simple to handle, technique and Preparation equipment is simple, cost is low, producing many is at present main in this way.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, long persistence luminescent powder of a kind of secondary excitation type and preparation method thereof is provided.The present invention adopts solid state reaction legal system for long-afterglow fluorescent Sr
1-a-bca
1-x-cal
2-yme
xrE
yo4S:aEu
2+, bDy
3+, cTm
3+, the method is easy and simple to handle, and fluorescent powder grain is large, good luminous performance.
The present invention is achieved by the following technical solutions, and secondary excitation type fluorescent material of the present invention, consists of Sr
1-a-bca
1-x-cal
2-yme
xrE
yo4S:aEu
2+, bDy
3+, cTm
3+.In formula, Me is at least one in Zn, Cd, Mg, and RE is at least one in Ga, Zn, Ge, Si; Wherein 0<x<0.1; 0<y<0.2; 0<a<0.12; 0<b<0.1; 0<c<0.1.Mentality of designing is: with Eu
2+, Tm
3+for luminescence center, add Dy
3+deng being auxiliary activator; There is interaction in its luminescence; Extraneous incident light excites Eu
2+luminescence, Eu
2+utilizing emitted light excite Tm again
3+luminescence, forms combined luminescence; Eu
2+and Ce
3+relative proportion determine radiative color; Dy
3+concentration determine time of persistence of secondary excitation type fluorescent material.Concrete steps are as follows:
(1) according to structural formula Sr
1-a-bca
1-x-cal
2-yme
xrE
yo4S:aEu
2+, bDy
3+, cTm
3+, take SrCO respectively in molar ratio
3, CaCO
3, Al
2o
3, MeCO
3, REO
2or RE
2o
3, S, Eu
2o
3, Dy
2o
3and Tm
2o
3;
(2) take the fusing assistant of above medicine total mass 0.001wt% ~ 10.0wt% more respectively, fusing assistant is H
3bO
3, BaF
2, at least one in NaF;
(3) raw material and fusing assistant is even by ground and mixed, under reducing atmosphere 950 DEG C ~ 1600 DEG C, calcination time is 2 ~ 8h, obtains target product.
In the present invention, described reducing atmosphere is provided by activated carbon powder, carbon black combustion method, or uses nitrogen/hydrogen mixed gas.
Compared with prior art, tool of the present invention has the following advantages:
1, the present invention prepares fluorescent material and adopts new mentality of designing, and compared with traditional long persistence luminescent powder, color is abundanter, can launch orange to red fluorescence.
2, the fluorescent powder grain prepared of the present invention is large, and brightness is high, crystallinity and coating property good, and there is good circulation ratio.
3, preparation method of the present invention is simple, easy handling, cost are low.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the preparation method of the long persistence luminescent powder of secondary excitation type provided by the present invention;
Fig. 2 is Sr of the present invention
0.86ca
0.92al
1.96zn
0.02si
0.04o
4s:0.08Eu
2+, 0.06Dy
3+, 0.06Tm
3+x-ray diffraction spectrogram;
Fig. 3 is Sr of the present invention
0.86ca
0.92al
1.96zn
0.02si
0.04o4S:0.08Eu
2+, 0.06Dy
3+, 0.06Tm
3+excite and utilizing emitted light spectrogram.
Embodiment
Embodiment 1
According to structural formula Sr
0.86ca
0.92al
1.96zn
0.02si
0.04o
4s:0.08Eu
2+, 0.06Dy
3+, 0.06Tm
3+take SrCO respectively
3(A.R.) 0.086mol, CaCO
3(A.R.) 0.092mol, Al
2o
3(A.R.) 0.098mol, ZnCO
3(A.R.) 0.002mol, SiO
2(A.R.) 0.004mol, Eu
2o
3(A.R.) 0.004mol, Dy
2o
3(A.R.) 0.003mol and Tm
2o
3(A.R.) 0.003mol, then the fusing assistant H taking above medicine total mass 5wt% respectively
3bO
3; Mixed by the above-mentioned raw material taken, then calcine under activated carbon powder burning provides reducing atmosphere, calcining temperature is 1200 DEG C, and calcination time is 6h, obtains target product.
Embodiment 2
According to structural formula Sr
0.97ca
0.97al
1.96mg
0.02ga
0.04o
4s:0.02Eu
2+, 0.01Dy
3+, 0.01Tm
3+take SrCO respectively
3(A.R.) 0.097mol, CaCO
3(A.R.) 0.097mol, Al
2o
3(A.R.) 0.098mol, MgCO
3(A.R.) 0.002mol, Ga
2o
3(A.R.) 0.002mol, Eu
2o
3(A.R.) 0.001mol, Dy
2o
3(A.R.) 0.0005mol and Tm
2o
3(A.R.) 0.0005mol, then the fusing assistant BaF taking above medicine total mass 3wt% respectively
2; The above-mentioned raw material taken is mixed, then at H
2-N
2calcine under (volume ratio 5:95) reducing atmosphere, calcining temperature is 1380 DEG C, and calcination time is 4h, obtains target product.
Embodiment 3
According to structural formula Sr
0.90ca
0.88al
1.92cd
0.06ge
0.08o
4s:0.04Eu
2+, 0.06Dy
3+, 0.06Tm
3+take SrCO respectively
3(A.R.) 0.09mol, CaCO
3(A.R.) 0.088mol, Al
2o
3(A.R.) 0.096mol, CdCO
3(A.R.) 0.006mol, GeO
2(A.R.) 0.004mol, Eu
2o
3(A.R.) 0.002mol, Dy
2o
3(A.R.) 0.003mol and Tm
2o
3(A.R.) 0.003mol, then the fusing assistant NaF taking above medicine total mass 0.5wt% respectively; The above-mentioned raw material taken is mixed, then at H
2-N
2calcine under (volume ratio 10:90) reducing atmosphere, calcining temperature is 1500 DEG C, and calcination time is 2h, obtains target product.
Embodiment 4
According to structural formula Sr
0.88ca
0.88al
1.84zn
0.06ga
0.08si
0.08o
4s:0.06Eu
2+, 0.06Dy
3+, 0.06Tm
3+take SrCO respectively
3(A.R.) 0.088mol, CaCO
3(A.R.) 0.088mol, Al
2o
3(A.R.) 0.092mol, ZnCO
3(A.R.) 0.006mol, Ga
2o
3(A.R.) 0.004mol, SiO
2(A.R.) 0.008mol, Eu
2o
3(A.R.) 0.003mol, Dy
2o
3(A.R.) 0.003mol and Tm
2o
3(A.R.) 0.003mol, then the fusing assistant H taking above medicine total mass 1wt% respectively
3bO
3with the fusing assistant BaF of 1wt%
2; Mixed by the above-mentioned raw material taken, then calcine under activated carbon powder burning provides reducing atmosphere, calcining temperature is 1100 DEG C, and calcination time is 8h, obtains target product.
Embodiment 5
According to structural formula Sr
0.86ca
0.88al
1.82mg
0.06ge
0.08si
0.1o
4s:0.08Eu
2+, 0.06Dy
3+, 0.06Tm
3+take SrCO respectively
3(A.R.) 0.086mol, CaCO
3(A.R.) 0.088mol, Al
2o
3(A.R.) 0.091mol, MgCO
3(A.R.) 0.006mol, GeO
2(A.R.) 0.008mol, SiO
2(A.R.) 0.01mol, Eu
2o
3(A.R.) 0.004mol, Dy
2o
3(A.R.) 0.003mol and Tm
2o
3(A.R.) 0.003mol, then the fusing assistant H taking above medicine total mass 5wt% respectively
3bO
3with the fusing assistant NaF of 0.1wt%; Mixed by the above-mentioned raw material taken, then calcine under activated carbon powder burning provides reducing atmosphere, calcining temperature is 1500 DEG C, and calcination time is 3h, obtains target product.
Embodiment 6
According to structural formula Sr
0.86ca
0.92al
1.92zn
0.02ga
0.04ge
0.04o
4s:0.08Eu
2+, 0.06Dy
3+, 0.06Tm
3+take SrCO respectively
3(A.R.) 0.086mol, CaCO
3(A.R.) 0.092mol, Al
2o
3(A.R.) 0.096mol, ZnCO
3(A.R.) 0.002mol, Ga
2o
3(A.R.) 0.002mol, GeO
2(A.R.) 0.004mol, Eu
2o
3(A.R.) 0.004mol, Dy
2o
3(A.R.) 0.003mol and Tm
2o
3(A.R.) 0.003mol, then the fusing assistant H taking above medicine total mass 0.5wt% respectively
3bO
3with the fusing assistant BaF of 8wt%
2; The above-mentioned raw material taken is mixed, then at H
2-N
2calcine under (volume ratio 5:95) reducing atmosphere, calcining temperature is 1400 DEG C, and calcination time is 5h, obtains target product.
Claims (3)
1. a secondary excitation type orange red fluorescent powder, is characterized in that the composition Sr of fluorescent material
1-a-b ca
1-x-c al
2-y me
x rE
y o
4s:
aeu
2+,
bdy
3+,
ctm
3+, in formula, Me is at least one in Zn, Cd, Mg, and RE is at least one in Ga, Zn, Ge, Si; Wherein 0<x<0.1; 0<y<0.2; 0<a<0.12; 0<b<0.1; 0<c<0.1.
2. the preparation method of fluorescent material described in claim 1, it is characterized in that the method uses high temperature solid-state method synthesis secondary excitation type long persistence luminescent powder, concrete steps are as follows:
(1) according to structural formula Sr
1-a-b ca
1-x-c al
2-y me
x rE
y o
4s:
aeu
2+,
bdy
3+,
ctm
3+, take SrCO respectively in molar ratio
3, CaCO
3, Al
2o
3, MeCO
3, REO
2or RE
2o
3, S, Eu
2o
3, Dy
2o
3and Tm
2o
3;
(2) take the fusing assistant of above medicine total mass 0.001 wt% ~ 10.0 wt% more respectively, fusing assistant is H
3bO
3, BaF
2, at least one in NaF;
(3) raw material and fusing assistant is even by ground and mixed, under reducing atmosphere 950 DEG C ~ 1600 DEG C, calcination time is 2 ~ 8 h, obtains target product.
3. the preparation method of fluorescent material described in claim 2, is characterized in that described in step (3), reducing atmosphere is provided by activated carbon powder, carbon black combustion method, or uses nitrogen/hydrogen mixed gas.
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|---|---|---|---|
| CN201210209234.8A CN102719245B (en) | 2012-06-25 | 2012-06-25 | Secondary excitation type orange-red fluorescent powder and preparation method thereof |
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| Publication Number | Publication Date |
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| CN102719245B true CN102719245B (en) | 2015-04-08 |
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| CN103160278A (en) * | 2013-03-20 | 2013-06-19 | 广东工业大学 | Red long-lasting phosphor material and preparation method thereof |
| CN104073256B (en) * | 2014-03-20 | 2016-11-09 | 王海容 | A kind of thioborate fluorophor and application thereof |
| CN104073257B (en) * | 2014-03-20 | 2016-11-09 | 王海容 | A kind of thiosilicic acid salt fluorophor and application thereof |
| CN115321579B (en) * | 2022-08-18 | 2023-08-08 | 北京科技大学 | Preparation method of high-performance oxysulfide fluorescent powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1194292A (en) * | 1997-03-26 | 1998-09-30 | 肖志国 | Long persistence luminescent silicate material and its producing method |
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2012
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1194292A (en) * | 1997-03-26 | 1998-09-30 | 肖志国 | Long persistence luminescent silicate material and its producing method |
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Address after: 402160 Honghe A Campus, 319 Honghe Avenue, Yongchuan District, Chongqing Co-patentee after: SICHUAN University Patentee after: CHONGQING University OF ARTS AND SCIENCES Address before: No. 319, Honghe Avenue, Yongchuan District, Chongqing City, Chongqing Co-patentee before: Sichuan University Patentee before: Chongqing University of Arts and Sciences |
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Granted publication date: 20150408 |