CN103555323B - Optical-excitation fluorescent powder and preparation method thereof - Google Patents
Optical-excitation fluorescent powder and preparation method thereof Download PDFInfo
- Publication number
- CN103555323B CN103555323B CN201310518875.6A CN201310518875A CN103555323B CN 103555323 B CN103555323 B CN 103555323B CN 201310518875 A CN201310518875 A CN 201310518875A CN 103555323 B CN103555323 B CN 103555323B
- Authority
- CN
- China
- Prior art keywords
- optical
- fluorescent powder
- excitation fluorescent
- reducing atmosphere
- sio
- 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.)
- Expired - Fee Related
Links
- 239000000843 powder Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 20
- 238000000227 grinding Methods 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 8
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 claims description 7
- 230000003287 optical effect Effects 0.000 abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 3
- 238000004891 communication Methods 0.000 abstract description 2
- 229910052909 inorganic silicate Inorganic materials 0.000 abstract 2
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 abstract 1
- 238000003331 infrared imaging Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000013307 optical fiber Substances 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 238000005245 sintering Methods 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 abstract 1
- 229910000018 strontium carbonate Inorganic materials 0.000 abstract 1
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium (III) oxide Inorganic materials [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 12
- 230000008859 change Effects 0.000 description 7
- 238000004020 luminiscence type Methods 0.000 description 7
- 229910052593 corundum Inorganic materials 0.000 description 5
- 239000010431 corundum Substances 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 3
- 230000004044 response Effects 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 239000005084 Strontium aluminate Substances 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 229910052950 sphalerite Inorganic materials 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
Landscapes
- Luminescent Compositions (AREA)
Abstract
The invention relates to optical-excitation fluorescent powder and a preparation method thereof, belonging to the technical field of rear-earth luminescent materials. Optical-excitation fluorescent powder is sosoloid with a general formula of alpha-Sr[2-x-y]SiO4:xEu<2+>, yTm<3+> (x is not less than 0.01 and not greater than 0.03, and y is not less than 0.01 and not greater than 0.03). The preparation method comprises the following steps of mixing and batching SrCO3, SiO2, Eu2O3 and Tm2O3 according to a general formula proportion of the finally prepared fluorescent powder, and adding alcohol to grind, so that the materials are uniformly mixed; sintering the uniformly mixed materials for 3 hours-5 hours under a reducing atmosphere at a temperature of 1100 DEG C-1300 DEG C, cooling to the room temperature under a reducing atmosphere, and grinding to obtain the optical-excitation fluorescent powder alpha-Sr[2-x-y]SiO4:xEu<2+>, yTm<3+>. The luminescent material disclosed by the invention can be extensively applied to multiple subject fields of near-infrared laser detection, laser spot display, optical fiber communication indication, optical information storage, infrared imaging and the like.
Description
Technical field
The present invention relates to a kind of Optical-excitation fluorescent powder and preparation method thereof, belong to rare earth luminescent material technical field.
Background technology
Photostimulated phosphor is owing to having write, reading and erasing speed fast (nanosecond), the infrared response time is short, the advantages such as unlimited writing and reading cycle life and wide infrared response scope (0.8-1.6 micron), a new path has been opened up in the research for optical storage medium.Photostimulated phosphor has much potential application, and as laser tag, optical communication, stores, display and imaging technique.
In photostimulated phosphor, current carrier (electronics and hole) Trapping Centers has a very important role.Under photostimulated phosphor being exposed to ultraviolet or visible ray, optical information is stored in the material, makes electronics and hole-recombination produce visible ray excitation luminescence subsequently by infrared stimulation or hot activation.
Up to the present, the photostimulated phosphor mainly alkaline sulfides that commercial optical stimulated luminescence intensity used is the highest and storage capacity is maximum, as SrS:Eu, Sm, ZnS:Cu, Co.But its chemical stability and thermostability are all poor, people are devoted to find oxide compound photostimulated phosphor to replace sulfide.As everyone knows, optical stimulated luminescence phenomenon is also observed in the compound of some oxide compounds, as Sr3SiO5:Eu2+, Dy3+, SrAl2O4:Eu, Dy, Sr4 (Si3O8) 2:Eu2+, Dy3+.But its optical stimulated luminescence intensity and storage capacity are difficult to meet practical application.
Summary of the invention
The object of this invention is to provide a kind of Optical-excitation fluorescent powder and preparation method thereof, its chemical stability and thermostability high, optical stimulated luminescence intensity is high and storage capacity is large.
Technical scheme of the present invention is: Optical-excitation fluorescent powder is sosoloid, and general formula is α-Sr
2-x-ysiO
4: xEu
2+, yTm
3+(0.01≤x≤0.03,0.01≤y≤0.03), the average grain of product is 15 ~ 20 microns, and its principal phase structure belongs to rhombic system.
Optical-excitation fluorescent powder of the present invention adopts high temperature solid-state method synthesis, and concrete steps comprise as follows:
(1) by SrCO
3, SiO
2, Eu
2o
3and Tm
2o
3according to final obtained fluorescent material general formula proportioning mix, add alcohol grinding and make it mix;
(2) be 1100 by the above-mentioned compound mixed in temperature
oc ~ 1300
osinter 3 ~ 5h under the reducing atmosphere of C, and be cooled to room temperature under this reducing atmosphere, after grinding, namely obtain Optical-excitation fluorescent powder α-Sr
2siO
4: Eu
2+, Tm
3+.
Described SrCO
3, SiO
2, Eu
2o
3and Tm
2o
3purity be more than 99.99wt%.
The purity of described alcohol is more than 98wt%, and add-on is 80% ~ 120% of mixture volume.
Described reducing atmosphere is the H of 5vol%
2with the N of 95vol%
2mixed gas.
The invention has the beneficial effects as follows: photostimulated phosphor prepared by the present invention is placed in atmosphere for a long time can not deliquescence, and phase structure can not change, chemical stability and thermostability high.The advantages such as this fluorescent material is after uv light irradiation 10min, and can be excited by near infrared (980nm) and realize yellow green light and launch, emission band is wide, and the high and storage capacity of optical stimulated luminescence intensity is large; Can be applicable to medical diagnosis image, industrial non-destructive flaw detection and the detection etc. to infrared source.
Accompanying drawing explanation
Fig. 1 is the optical stimulated luminescence attenuate light spectrogram of embodiment of the present invention four.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment one: the photostimulated phosphor of present embodiment is α-Sr
1.98siO
4: 0.01Eu
2+, 0.01Tm
3+.This fluorescent material average grain is 15 ~ 20 microns, and its principal phase structure belongs to rhombic system.Concrete preparation method is:
(1) by the mol ratio=1:1:0.01:0.01 of Sr:Si:Eu:Tm, precise SrCO
3(99.99%), SiO
2(99.99%), Eu
2o
3(99.99%), Tm
2o
3(99.99%) be mixed in agate mortar, add alcohol grinding 0.5h and make it mix.
(2) compound of step (1) gained is placed in corundum crucible, at reducing atmosphere (5%H
2+ 95%N
2) in 1200
osinter 4h under C, in reducing atmosphere, be cooled to room temperature, after grinding, namely obtain Optical-excitation fluorescent powder α-Sr
1.98siO
4: 0.01Eu
2+, 0.01Tm
3+.The luminescent material prepared is received after UV-light at aspiration, and can place at ambient temperature can not deliquescence, and phase structure can not change, and can temperature stored energy.Yellow-green fluorescence can be discharged for a long time under near infrared 980nm light source irradiation.
Embodiment two: the photostimulated phosphor of present embodiment is α-Sr
1.97siO
4: 0.02Eu
2+, 0.01Tm
3+.This fluorescent material average grain is 15 ~ 20 microns, and its principal phase structure belongs to rhombic system.Concrete preparation method is:
(1) by the mol ratio=1:1:0.02:0.01 of Sr:Si:Eu:Tm, precise SrCO
3(99.99%), SiO
2(99.99%), Eu
2o
3(99.99%), Tm
2o
3(99.99%) be mixed in agate mortar, add alcohol grinding 0.5h and make it mix.
(2) compound of step (1) gained is placed in corundum crucible, at reducing atmosphere (5%H
2+ 95%N
2) in 1200
osinter 4h under C, in reducing atmosphere, be cooled to room temperature, after grinding, namely obtain Optical-excitation fluorescent powder α-Sr
1.97siO
4: 0.02Eu
2+, 0.01Tm
3+.The luminescent material prepared is received after UV-light at aspiration, and can place at ambient temperature can not deliquescence, and phase structure can not change, and can temperature stored energy.Yellow-green fluorescence can be discharged for a long time under near infrared 980nm light source irradiation.
Embodiment three: the photostimulated phosphor of present embodiment is α-Sr
1.965siO
4: 0.02Eu
2+, 0.015Tm
3+, this fluorescent material average grain is 15 ~ 20 microns, and its principal phase structure belongs to rhombic system.Concrete preparation method is:
(1) by the mol ratio=1:1:0.02:0.015 of Sr:Si:Eu:Tm, precise SrCO
3(99.99%), SiO
2(99.99%), Eu
2o
3(99.99%), Tm
2o
3(99.99%) be mixed in agate mortar, add alcohol grinding 0.5h and make it mix.
(2) compound of step (1) gained is placed in corundum crucible, at reducing atmosphere (5%H
2+ 95%N
2) in 1200
osinter 4h under C, after grinding, namely obtain Optical-excitation fluorescent powder α-Sr
1.965siO
4: 0.02Eu
2+, 0.015Tm
3+.The luminescent material prepared is received after UV-light at aspiration, and can place at ambient temperature can not deliquescence, and phase structure can not change, and can temperature stored energy.Yellow-green fluorescence can be discharged for a long time under near infrared 980nm light source irradiation.
Embodiment four: as shown in Figure 1, the photostimulated phosphor of present embodiment is α-Sr
1.96siO
4: 0.02Eu
2+, 0.02Tm
3+.This fluorescent material average grain is 15 ~ 20 microns, and its principal phase structure belongs to rhombic system.Concrete preparation method is:
(1) by the mol ratio=1:1:0.02:0.02 of Sr:Si:Eu:Tm, precise SrCO
3, SiO
2, Eu
2o
3, Tm
2o
3be mixed in agate mortar, add alcohol grinding 0.5h and make it mix.
(2) compound of step (1) gained is placed in corundum crucible, at reducing atmosphere (5%H
2+ 95%N
2) in 1200
osinter 4h under C, after grinding, namely obtain Optical-excitation fluorescent powder α-Sr
1.96siO
4: 0.02Eu
2+, 0.02Tm
3+.The luminescent material prepared is received after UV-light at aspiration, and can place at ambient temperature can not deliquescence, and phase structure can not change, and can temperature stored energy.Yellow-green fluorescence can be discharged for a long time under near infrared 980nm light source irradiation.
Embodiment five: the photostimulated phosphor of present embodiment is α-Sr
1.955siO
4: 0.02Eu
2+, 0.025Tm
3+.This fluorescent material average grain is 15 ~ 20 microns, and its principal phase structure belongs to rhombic system.Concrete preparation method is:
(1) by the mol ratio=1:1:0.02:0.025 of Sr:Si:Eu:Tm, precise SrCO
3, SiO
2, Eu
2o
3, Tm
2o
3be mixed in agate mortar, add alcohol grinding 0.5h and make it mix.
(2) compound of step (1) gained is placed in corundum crucible, at reducing atmosphere (5%H
2+ 95%N
2) in 1200
osinter 4h under C, after grinding, namely obtain Optical-excitation fluorescent powder α-Sr
1.955siO
4: 0.02Eu
2+, 0.025Tm
3+.The luminescent material prepared is received after UV-light at aspiration, and can place at ambient temperature can not deliquescence, and phase structure can not change, and can temperature stored energy.Yellow-green fluorescence can be discharged for a long time under near infrared 980nm light source irradiation.
Below by reference to the accompanying drawings the specific embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.
Claims (2)
1. an Optical-excitation fluorescent powder, is characterized in that: Optical-excitation fluorescent powder is sosoloid, and general formula is α-Sr
2-x-ysiO
4: xEu
2+, yTm
3+, wherein 0.01≤x≤0.03,0.01≤y≤0.03;
Described fluorescent material average grain is 15 ~ 20 microns, and its principal phase structure belongs to rhombic system.
2. a preparation method for Optical-excitation fluorescent powder as claimed in claim 1, is characterized in that:
(1) by SrCO
3, SiO
2, Eu
2o
3and Tm
2o
3according to final obtained fluorescent material general formula proportioning mix, add alcohol grinding and make it mix;
(2) be 1100 by the above-mentioned compound mixed in temperature
oc ~ 1300
osinter 3 ~ 5h under the reducing atmosphere of C, and be cooled to room temperature under this reducing atmosphere, after grinding, namely obtain Optical-excitation fluorescent powder α-Sr
2siO
4: Eu
2+, Tm
3+;
The purity of described alcohol is more than 98wt%, and add-on is 80% ~ 120% of mixture volume;
Described reducing atmosphere is the H of 5vol%
2with the N of 95vol%
2mixed gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310518875.6A CN103555323B (en) | 2013-10-29 | 2013-10-29 | Optical-excitation fluorescent powder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310518875.6A CN103555323B (en) | 2013-10-29 | 2013-10-29 | Optical-excitation fluorescent powder and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103555323A CN103555323A (en) | 2014-02-05 |
| CN103555323B true CN103555323B (en) | 2015-06-03 |
Family
ID=50009695
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310518875.6A Expired - Fee Related CN103555323B (en) | 2013-10-29 | 2013-10-29 | Optical-excitation fluorescent powder and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103555323B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104212441B (en) * | 2014-07-24 | 2016-09-07 | 昆明理工大学 | A kind of green Optical-excitation fluorescent powder and preparation method thereof |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5227254A (en) * | 1991-06-19 | 1993-07-13 | E. I. Du Pont De Nemours And Company | Photostimulable europium-doped barium fluorobromide phosphors |
| JP2001011439A (en) * | 1999-07-02 | 2001-01-16 | Fuji Photo Film Co Ltd | Tetradecahedral rare earth-activated alkaline earth metal fluoride halide-based stimulable phosphor and radiographic image-converting panel |
| JP4836429B2 (en) * | 2004-10-18 | 2011-12-14 | 株式会社東芝 | Phosphor and light emitting device using the same |
| CN101124296B (en) * | 2004-12-17 | 2013-04-17 | 新南部创新有限公司 | Radiation storage phosphor and applications |
| CN102925154B (en) * | 2012-11-23 | 2014-04-16 | 中国科学院长春光学精密机械与物理研究所 | Sulfide-based triple-doped electron trapping material and preparation method thereof |
| CN103194230B (en) * | 2013-04-23 | 2014-09-10 | 中国科学院新疆理化技术研究所 | Europium and samarium-doped lithium magnesium phosphate photostimulated luminescent material and preparation method thereof |
-
2013
- 2013-10-29 CN CN201310518875.6A patent/CN103555323B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN103555323A (en) | 2014-02-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wang et al. | Mn2+ activated green, yellow, and red long persistent phosphors | |
| Liu et al. | Crystal structure and photoluminescence properties of red‐emitting Ca9La1− x (VO4) 7: xEu3+ phosphors for white light‐emitting diodes | |
| Marin et al. | Photoluminescence properties of YAG: Ce3+, Pr3+ phosphors synthesized via the Pechini method for white LEDs | |
| CN101962542B (en) | Niobate-based red fluorescent powder for white LED as well as preparation method and application thereof | |
| CN113717722B (en) | Bismuth ion doped borate narrow-band blue fluorescent powder, preparation method thereof and luminescent device | |
| CN105131950A (en) | Tungstate upconversion luminescence temperature sensitive material doped with rare-earth elements Er and Yb and preparation method thereof | |
| CN102585828B (en) | Yb3+-doped vanadate up-conversion fluorescent material and preparation method thereof | |
| Ju et al. | The influence of auxiliary codopants on persistent phosphor Sr2P2O7: Eu2+, R3+ (R= Y, La, Ce, Gd, Tb and Lu) | |
| US8591768B2 (en) | Germanate luminescence material and its preparation | |
| US8703020B2 (en) | Bismuth ion sensitized rare earth germanate luminescence materials and preparation methods thereof | |
| CN110467915A (en) | A kind of SrAl2O4: Dy3+/Eu2+The synthesis of green long afterglow fluorescent material | |
| Wang et al. | Synthesis and luminescence properties of SrGd2O4: Eu3+ red phosphors | |
| CN102942928B (en) | Zirconate-base red phosphor, method for preparing same and application | |
| CN103555323B (en) | Optical-excitation fluorescent powder and preparation method thereof | |
| CN102268258A (en) | Strontium aluminate based up-conversion luminescent material and preparation method thereof | |
| CN104031644B (en) | Molybdate up-conversion luminescent material, preparation method and application thereof | |
| CN102660286B (en) | Vanadate up-conversion light-emitting material activated by erbium ions Er<3+> and preparation method thereof | |
| CN101671561A (en) | Method for preparing blue long afterglow luminescence C12A7 powder | |
| WO2010130075A1 (en) | Full-color light-emitting material and preparation method thereof | |
| CN105860971B (en) | Rare earth ion doped zirconium niobate fluorescent powder and preparation method thereof | |
| CN104212441B (en) | A kind of green Optical-excitation fluorescent powder and preparation method thereof | |
| Gupta et al. | White light emitting nanocrystalline Y1− xGdxPO4: Dy3+ and improved PLQY on Gd3+ co-doping | |
| CN103113893B (en) | A kind of Yb 3+boron tungstate up-conversion luminescent material activated and preparation method thereof | |
| CN101987957B (en) | Red phosphor powder for white LED as well as preparation method and application thereof | |
| CN105524615A (en) | Niobate red phosphor for white-light LEDs and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for 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 | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150603 Termination date: 20201029 |