CN1740268A - Highly bulked long-afterglow luminous material - Google Patents
Highly bulked long-afterglow luminous material Download PDFInfo
- Publication number
- CN1740268A CN1740268A CN 200510036467 CN200510036467A CN1740268A CN 1740268 A CN1740268 A CN 1740268A CN 200510036467 CN200510036467 CN 200510036467 CN 200510036467 A CN200510036467 A CN 200510036467A CN 1740268 A CN1740268 A CN 1740268A
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- CN
- China
- Prior art keywords
- long
- luminous material
- afterglow luminous
- flux
- glow luminous
- Prior art date
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- Granted
Links
- 239000000463 material Substances 0.000 title claims abstract description 42
- 230000004907 flux Effects 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 9
- 239000012190 activator Substances 0.000 claims description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- ZRIUUUJAJJNDSS-UHFFFAOYSA-N ammonium phosphates Chemical compound [NH4+].[NH4+].[NH4+].[O-]P([O-])([O-])=O ZRIUUUJAJJNDSS-UHFFFAOYSA-N 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 239000013078 crystal Substances 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 4
- 238000000227 grinding Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract 2
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract 1
- 235000010216 calcium carbonate Nutrition 0.000 abstract 1
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 abstract 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 abstract 1
- 229910000018 strontium carbonate 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
- 235000019580 granularity Nutrition 0.000 description 8
- 229910052761 rare earth metal Inorganic materials 0.000 description 7
- 238000009826 distribution Methods 0.000 description 5
- 150000002910 rare earth metals Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229910052693 Europium Inorganic materials 0.000 description 3
- 150000004645 aluminates Chemical class 0.000 description 3
- 230000002688 persistence Effects 0.000 description 3
- -1 rare earth ion Chemical class 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 229920000831 ionic polymer Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- HIGRAKVNKLCVCA-UHFFFAOYSA-N alumine Chemical class C1=CC=[Al]C=C1 HIGRAKVNKLCVCA-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
The highly bulked long-afterglow luminous material has the general expression of a[(SrCO3)1-X(CaCO3) X].bAl2O3.cSiO2.kMgO:(Eu2O3)y'. (Dy2O3)z'pRO, where x, a, b, c, k, y, z and p are molar number, x is 0-1, a is 0.9-2, b is 0-4, c is 0-2, k is 0-1, y is 0.001-0.05, z is 0.001-0.05, and p is 0.01-0.1. The long-afterglow luminous material needs no grinding, and thus has greatly kept crystal grain structure. Compared with traditional long-afterglow luminous RE material of the same granularity, the present invention has 10 % raised light emitting brightness. In addition, the present invention has powder yield and lowered production cost.
Description
Technical field
The present invention relates to a kind of inorganic long after glow luminous material, particularly rare earth alkaline earth aluminate or long persistence luminescent silicate material.
Background technology
Long after glow luminous material is a kind of material of widespread use, and this luminescent material is made up of substrate material, activator and fusing assistant.Wherein host material is Al
2O
3, SiO
2, CaCO
3, MgCO
3, SrCO
3Deng, activator adopts rare earth oxide, such as Eu
2O
3, Dy
2O
3, Tb
4O
7Deng, flux is H
3BO
3Deng.
The research of long after glow luminous material has very long history, and as far back as early in the twentieth century, it is the fluorescent material of Cu, Ag, Bi, Mn sulfide that Lenard has just prepared activator, after synthesized a series of CaS:Bi again, long-persistence luminous material such as CaSrS:Bi.Because the sulfide long-afterglow material exists luminosity low, persistence is short, and under ultraviolet radiation, the easily problems such as decomposition, color blackening occur, so range of application is subjected to great restriction.
CN 1053807 discloses a kind of europkium-activated alumine acid strontium long afterglow phosphor material and preparation method thereof.The chemical constitution formula of this material is m (Sr
1-xEu
x) O.
nAl
2O
3.yB
2O
3Its scope is 1≤m≤5,1≤n≤8,0.001≤x≤0.1,0.005≤y≤0.35.CN 1115779 discloses a kind of polyion activated alkaline earth aluminate long-afterglow photoluminescent and manufacture method, and general formula is expressed as aM
1-x-y-zO.
bAl
2O
3: Eu
x.A
y.B
z, its material is to be main luminous host with alkaline earth aluminate, the coactivated polyion of rare earth ion (Eu, Ce, Tb, Dy) and non-rare earth ion (Sb, Sn) activates luminescent material, 0.003≤x≤0.2,0.003≤y≤0.2,0.01≤z≤0.15,0.2≤a/b≤5.CN1194292 discloses a kind of chemical composition expression: aMO.bM ' O.cSiO
2.dR:Eu
x, Ln
yMaterial, wherein M is selected from Sr, Ca, one or more elements of Ba, Zn, M ' is selected from one or more elements among Mg, Cd, the Be; R is selected from B
2O
3, P
2O
5In one or both compositions, its scope is 0.6≤a≤6,0≤b≤5,1≤c≤9,0≤d≤0.7,0.00001≤x≤0.2,0≤y≤0.3.There is a common problem in above-mentioned luminescent material, adopts boric acid or boron oxide compound as the synthetic fusing assistant, makes that synthetic luminescent material hardness ratio is bigger.Secondly, the boride B in the material
2O
3Be hard solid under the normal temperature, in order to mix with various raw material, must be levigate, but finally can only obtain granularity at the B of 20～30 μ m
2O
3In order to make synthetic materials reach certain effect of fluxing, often more than 0.1 mol ratio, the result makes that product sintering hardness is bigger to actual fusing assistant addition.According to long-persistence luminous mechanism as can be known, Eu
2+Take place (
8S
7/2→ 4f5d) energy level transition, portions of electronics is captured by the trap center, and under the effect of thermal perturbation, electronics produces twilight sunset with hole-recombination again.Therefore, the crystal structure of material is more complete, and luminosity is also just more high.Actually, the size range that needs when the long afterglow material is used is between 20～200 μ m, above-mentioned materials all exists product sintering hardness big, can only be the long after glow luminous material of 20～200 μ m by grinding the acquisition granularity, by grinding the crystal formation that the material that obtains certainly will destroy luminescent material, reduce luminosity.
Summary of the invention
The present invention is directed to above-mentioned existing problems, provide a kind of highly bulked, not the rare earth long-afterglow luminescent material of the soft that need grind.
Highly bulked long after glow luminous material of the present invention can be expressed as with general formula: a[(SrCO
3)
1-x(CaCO
3)
x] .bAl
2O
3.cSiO
2.kMgO:(Eu
2O
3)
y, (Dy
2O
3)
z, pRO, wherein the ratio of x, a, b, c, k, y, z, p molal quantity is: 0≤x≤1,0.9≤a≤2,0≤b≤4,0≤c≤2,0≤k≤1,0.001≤y≤0.05,0.001≤z≤0.05,0.01≤p≤0.1, its mesostroma SrCO
3, CaCO
3, MgO, Al
2O
3Or SiO
2In have two or more compositions at least, Eu
2O
3, Dy
2O
3Be activator, RO is flux.
Fusing assistant of the present invention is two or more composition in ammonium phosphate salt, boric acid and the salt thereof.
Above-mentioned flux ammonium phosphate salt is (NH
4)
2HPO
4, NH
4H
2PO
4Or (NH
4)
3PO
4
Above-mentioned flux boric acid and salt thereof are H
3BO
3, SrB
4O
7, BaB
4O
7, Na
2B
4O
7, SrB
2O
6Or BaB
2O
6
Multiple fusing assistant Study on Efficiency is thought, in luminescent material, added a spot of fusing assistant and be very important.Because the fusing point of flux is lower, in high temperature solid-state method is synthetic, there is the synthetic material particle surface with liquid form, so that active ions Eu, Dy diffuse in the material principal phase easily, played the effect of diffusion bridge.Because the fusing assistant granularity that the present invention adopts is very little, mean particle size is at 3～5 μ m.Owing to have than bigger serface, reaching B
2O
3Or H
3BO
3In the situation of the efficient of fluxing equally, can greatly reduce the consumption of flux, general addition mol ratio is below 0.1.Secondly, also find under study for action, have significantly synergy between the different flux, can effectively reduce the use amount of flux.In addition, mixed flux can produce the gas of " explosivity " in high temperature is synthetic, and expansible gas has stoped the principal phase crystalline to be grown up effectively, has played the granularity effect of refinement steady persistence product.Improvement by to above fusing assistant granularity, flux collaborative efficient and grain refining aspect makes synthetic long afterglow product be the powder of quicksand like, and maximum particle size is below 180 μ m, and sintering hardness reduces greatly.The rare earth long-afterglow luminescent material of producing by component of the present invention need not grind, and can farthest keep the product crystal structural intergrity, compares with traditional long after glow luminous material of same granularity, and luminosity has improved more than 10%.Secondly, because of product need not grind, no powder consumption has improved the yield of powder, reduces production costs.
Embodiment
With analytically pure SrCO
3, CaCO
3, MgO, 99～99.99%Al
2O
3, 99～99.99%SiO
2And 99.5～99.99%Eu
2O
3, Dy
2O
3, mix in table 1 ratio, batch mixing is 8 hours in closed container, then with mixture at N
2+ H
2Under the atmosphere, insulation is 5 hours in 1300～1500 ℃ of high temperature furnaces, can obtain a kind of rare earth long-afterglow luminescent material of quicksand like, need not grind, and can obtain respectively the rare earth long-afterglow luminescent material that 30～200 μ m granularities do not wait.Fig. 1,2,3,4 is respectively the particle size distribution figure of embodiment 1,2,6,7.
Table 1
| Sequence number | Composition of raw materials is formed (mol ratio) | RO solubility promoter kind and ratio | Peak value nm | Granularity μ m | Relative |
| Embodiment | |||||
| 1 | 1SrCO 3.1Al 2O 3.0.001MgO∶ 0.005Eu 2O 3，0.005Dy 2O 3， 0.02RO | H 3BO 3∶Na 2B 4O 7∶(NH 4) 3PO4 ＝1∶1∶1 | 520 | Size-grade distribution is seen Fig. 1 | 10869 |
| Embodiment 2 | 0.995SrCO 3.1Al 2O 3.0.05CaCO 3. ∶0.003Eu 2O 30.003Dy 2O 3， 0.04RO | H 3BO 3∶Na 2B 4O 7∶(NH 4) 3PO4 ＝1∶2∶2 | 524 | Size-grade distribution is seen Fig. 2 | 7739 |
| Embodiment 3 | 0.995SrCO 3.1Al 2O 3.0.005 CaCO 3.∶0.0035Eu 2O 3 0.0035Dy 2O 30.06RO | BaCl 2∶BaB 2O 6∶NH 4H 2PO 4 ＝2∶2∶1 | 522 | / | 8673 |
| Embodiment 4 | 1.98SrCO 3.2SiO 2.0.02CaCO 3. 1MgO∶0.004Eu 2O 30.004Dy 2O 3， 0.035RO | BaB 2O 6∶NH 4H 2PO 4 ＝2∶1 | 473 | / | 3100 |
| Embodiment 5 | 2SrCO 3.2SiO 2.1MgO∶0.006 Eu 2O 30.006Dy 2O 3，0.05RO | BaB 4O 7∶NH 4H 2PO 4 ＝2∶1 | 470 | / | 4050 |
| Embodiment 6 | 1SrCO 3.1CaCO 3.2SiO 2.1MgO∶ 0.005Eu 2O 30.005Dy 2O 3， 0.06RO | H 3BO 3∶SrB 4O 7∶(NH 4) 2HPO 4 ＝1∶2∶2 | 498 | Size-grade distribution is seen Fig. 3 | 2690 |
| Embodiment 7 | 2SrCO 3.3.5Al 2O 3∶0.015Eu 2O 3， 0.03Dy 2O 3，0.01RO | BaCl 2∶BaB 2O 6∶NH 4H 2PO 4 ＝2∶2∶1 | 490 | Size-grade distribution is seen Fig. 4 | 6586 |
| Embodiment 8 | 2SrCO 3.3.5Al 2O 3∶0.007Eu 2O 3， 0.014Dy 2O 3，0.02RO | H 3BO 3∶BaB 2O 6∶NH 4H 2PO 4 ＝2∶2∶1 | 490 | / | 6991 |
| Embodiment 9 | 1.98SrCO 30.02CaCO 3.3.5Al 2O 3 ∶0.004Eu 2O 30.04Dy 2O 30.03RO | H 3BO 3∶(NH 4) 3PO 4 ＝2∶1 | 495 | / | 4078 |
| CN 1194292 | 1SrO.1CaO.2SiO 2.MgO∶ 0.005Eu0.08Dy，0.05B 2O 3 | 0.1H 3BO 3 | 500 | Broken mistake-100 order | 3591 |
| Commercially available | ZnS∶Cu | / | 520 | 26.8 | 100 |
Annotate: 1. test condition: 1000lux excites 20min, room temperature.
2. the after-glow brightness when brightness is 1min.
Claims (4)
1. a highly bulked long after glow luminous material is characterized in that available general formula is expressed as: a[(SrCO
3)
1-x(CaCO
3)
x] .bAl
2O
3.cSiO
2.kMgO:(Eu
2O
3)
y, (Dy
2O
3)
z, pRO, wherein the ratio of x, a, b, c, k, y, z, p molal quantity is: 0≤x≤1,0.9≤a≤2,0≤b≤4,0≤c≤2,0≤k≤1,0.001≤y≤0.05,0.001≤z≤0.05,0.01≤p≤0.1, its mesostroma SrCO
3, CaCO
3, MgO, Al
2O
3Or SiO
2In have two or more compositions at least, Eu
2O
3, Dy
2O
3Be activator, RO is flux.
2. long after glow luminous material according to claim 1 is characterized in that fusing assistant is two or more composition in ammonium phosphate salt, boric acid and the salt thereof.
3. long after glow luminous material according to claim 1 and 2 is characterized in that described flux ammonium phosphate salt is (NH
4)
2HPO
4, NH
4H
2PO
4Or (NH
4)
3PO
4
4. long after glow luminous material according to claim 1 and 2 is characterized in that described flux boric acid and salt thereof are H
3BO
3, SrB
4O
7, BaB
4O
7, Na
2B
4O
7, SrB
2O
6Or BaB
2O
6
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100364672A CN100368507C (en) | 2005-08-10 | 2005-08-10 | Highly bulked long-afterglow luminous material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100364672A CN100368507C (en) | 2005-08-10 | 2005-08-10 | Highly bulked long-afterglow luminous material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1740268A true CN1740268A (en) | 2006-03-01 |
| CN100368507C CN100368507C (en) | 2008-02-13 |
Family
ID=36092802
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100364672A Expired - Fee Related CN100368507C (en) | 2005-08-10 | 2005-08-10 | Highly bulked long-afterglow luminous material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100368507C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105315995A (en) * | 2015-12-03 | 2016-02-10 | 河北利福光电技术有限公司 | Fluxing agent and method for preparing YAG fluorescent powder |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1053807A (en) * | 1991-03-09 | 1991-08-14 | 复旦大学 | Long-decay phosphor material and preparation thereof |
| CN1115779A (en) * | 1994-10-17 | 1996-01-31 | 肖志国 | Multiple-ion activated long-decay photoluminescent alkaline-earth aluminate material and its prepn |
| CN1062581C (en) * | 1997-03-26 | 2001-02-28 | 肖志国 | Long persistence luminescent silicate material and its producing method |
| CN1206313C (en) * | 2000-12-30 | 2005-06-15 | 大连路明发光科技股份有限公司 | New type long-persistence material |
-
2005
- 2005-08-10 CN CNB2005100364672A patent/CN100368507C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105315995A (en) * | 2015-12-03 | 2016-02-10 | 河北利福光电技术有限公司 | Fluxing agent and method for preparing YAG fluorescent powder |
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| Publication number | Publication date |
|---|---|
| CN100368507C (en) | 2008-02-13 |
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