CN101074372A - Silicate long-afterglow luminescent material and its production - Google Patents
Silicate long-afterglow luminescent material and its production Download PDFInfo
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- CN101074372A CN101074372A CN 200710014820 CN200710014820A CN101074372A CN 101074372 A CN101074372 A CN 101074372A CN 200710014820 CN200710014820 CN 200710014820 CN 200710014820 A CN200710014820 A CN 200710014820A CN 101074372 A CN101074372 A CN 101074372A
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- powder
- long
- long persistence
- persistence luminescent
- silicate material
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Abstract
A yellow-green silicate long persistence luminescent material and its production are disclosed. The chemical formula is aSrO. bCaO. cMgO. dSio2. eB203.Eux.Lny; Ln is lanthanide element except Eu, it reinforces persistent effect; a, b, c, d, e, x and y are mol coefficients, proportion of a: b: c: d: e: x: y is 1: 0.2-5: 0.3-15: 0.4-20: 0.01-1: 0.001-0.1: 0.001-1 mol. It has high brightness, fast reactive speed under weak-light excitation condition, stable chemical property and various applied environments.
Description
Technical field
The invention belongs to the long after glow luminous material field, relate to a kind of long persistence luminescent silicate material and preparation method thereof.
Background technology
Rare earth aluminate luminescent material and rare earth silicate luminescent material, owing to the brightness height, characteristics such as the time is long, chemical stability good, no radiologic hazard receive much concern, and more enter into daily life, wherein the aluminate luminescent material of Zhu Dao yellow-green colour luminous (520nm) occupies 90% the market share.But aluminate luminescent material exist hold long between the light time, energy level difference big, unstable in the water, defective such as material hardness is big.
The patent CN1132777A of the basic KCC of Japan discloses a kind of aluminate yellow-green colour luminescent material, and structural formula is MAL
2O
4The compound of (M is elements such as calcium, strontium, barium) is classical yellow-green colour luminescent material.Relevant patent is also just like CN1115779A, and CN1152018A etc. have introduced the preparation method of blue green emitting (490nm) aluminate and sky blue luminous (460nm) silicate, violet light (440nm) aluminate substantially.
Chinese patent application 01138883.8 discloses a kind of aluminate high brightness long afterglow luminous material and preparation method thereof, relates to a kind of aluminate high brightness long afterglow luminous material and preparation method thereof, belongs to fluorescent material and preparation method thereof in the luminous physics.This material is with following general expression: M, N, Al
2-XB
XO
4Represent, with raw material SrCO
3, Al
2O
3, Eu
2O
3, Dy
2O
3NH
4Cl
2Carry out mixing and ball milling and with carbon reducing agent, sintering carries out ball mill pulverizing again, gradation sieves.
Chinese patent application 200510012222.6 discloses a kind of method for preparing ultrafine long afterglow luminous material, belongs to ultra-fine strontium aluminate phase long after glow luminous material preparing technical field.The employing citric acid is a sequestrant, the oxide compound europium sesquioxide of inorganic aluminate, strontium or calcium, barium salt, rare earth and dysprosium oxide and solubility boron-containing compound boric acid or boron oxide etc. are raw material, adopt earlier sol-gel method to prepare presoma, again synthesizing aluminate system long after glow luminous material under 1200～1250 ℃ and weakly reducing atmosphere; Boron-containing compound boric acid adds in the process of preparation presoma synchronously.
But above-mentioned aluminate luminescent material all exist hold that long between the light time, energy level difference is big, unstable in the water, defective such as material hardness is big.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, silicate luminescent material of a kind of yellow-green colour luminous (520nm) and preparation method thereof is provided.
Long persistence luminescent silicate material of the present invention, its chemical constitution is:
aSrO·bCaO·cMgO·dSiO
2·eB
2O
3·Eu
x·Ln
y
Wherein Ln is the lanthanon except that Eu, and auxiliary Eu strengthens the twilight sunset effect; A wherein, b, c, d, e, x, y is mole coefficient; A: b: c: d: e: x: y=1: 0.2～5: 0.3～15: 0.4～20: 0.01～1: 0.001～0.1: 0.001～1, mol ratio.
Preferably, the ratio of above-mentioned a and x is more than or equal to 0.001 and less than 0.1; The ratio of above-mentioned a and y is greater than 0.001 and less than 1.
The present invention also provides the synthetic method of described long persistence luminescent silicate material, and step is as follows:
1) powder with Strontium carbonate powder, lime carbonate, magnesium oxide, silicon-dioxide, boric acid and rare earth oxide, Eu oxide compound is combined by the mole coefficient, and ball milling 6～10 hours is combined evenly, and the mixture that obtains is called powder;
2) powder is packed into alumina crucible, with carbon dust or hydrogen reducing, at 1200-1400 ℃ of following sintering 2-5 hour, powder sintering was a powder agglomates;
3) after being cooled to room temperature, take out powder agglomates, be crushed to powder, obtain yellow-green colour (520nm) long after glow luminous material.
Preferably, the ball milling time in the step 1) is 8 hours.
The method that the present invention adopts is called and is the high temperature solid state reaction synthesis method.
The yellow-green colour luminescent material is as main long-afterglow material, develops into the aluminate type from the sulfuration zinc-copper, and brightness is significantly improved (approximately having improved 10 times), and weathering resistance has also had very big improvement.And develop into silicate-type from the aluminate type, and brightness not only is significantly improved once more, and (approximately having improved 2 times) also solved the stability problem in the water, reduced the hardness of material, thus the type luminescent material has application prospects more.
The silicate luminescent material of yellow-green colour of the present invention luminous (520nm), the brightness height, particularly under low light level shooting conditions, reflection is fast, and chemical property is stable (being included in the water) more, and applied environment is more extensive.
Embodiment
Following examples are to further specify of the present invention, but the present invention is not limited thereto.
Embodiment 1:
Proportioning raw materials:
Material mol ratio weight
SrCO
3 1 147
CaCO
3 2 200
MgO 1 40
SiO
2 2 120
H
3BO
3 0.1 6.2
Eu
2O
3 0.01 3.52
Dy
2O
3 0.01 3.73
The powder of Strontium carbonate powder, lime carbonate, magnesium oxide, silicon-dioxide, boric acid and Dy oxide compound, Eu oxide compound is combined by the mole coefficient, and ball milling 8 hours is combined evenly, and the mixture that obtains is called powder; With the powder alumina crucible of packing into, use carbon reducing agent, 1200 ℃ of following sintering 5 hours, powder sintering was a powder agglomates; After being cooled to room temperature, take out powder agglomates, be crushed to powder, obtain yellow-green colour (520nm) long after glow luminous material.After exciting, yellow-green fluorescence (520nm) is sent in the dark place, and excites soon, brightness height, particularly initial stage better effects if, and through the X-diffraction analysis, material is yellow long structure.
Embodiment 2:
Proportioning raw materials:
Material mol ratio weight
SrCO
3 2 294
CaCO
3 2 200
MgO 1 40
SiO
2 2 120
H
3BO
3 0.1 6.2
Eu
2O
3 0.01 3.52
Dy
2O
3 0.01 3.73
The powder of Strontium carbonate powder, lime carbonate, magnesium oxide, silicon-dioxide, boric acid and rare earth oxide, Eu oxide compound is combined by the mole coefficient, and ball milling 7 hours is combined evenly, and the mixture that obtains is called powder; With the powder alumina crucible of packing into, use hydrogen reducing, 1330 ℃ of following sintering 3 hours, powder sintering was a powder agglomates; After being cooled to room temperature, take out powder agglomates, be crushed to powder, obtain yellow-green colour (520nm) long after glow luminous material.After exciting, yellow-green fluorescence (520nm) is sent in the dark place, and excites soon, brightness height, particularly initial stage better effects if, and through the X-diffraction analysis, material is yellow long structure.
Embodiment 3
Material mol ratio weight
SrCO
3 1 147
CaCO
3 4 400
MgO 0.5 20
SiO
2 10 600
H
3BO
3 0.05 3.1
Eu
2O
3 0.04 14.08
Nd
2O
3 0.03 10.08。
Claims (5)
1. long persistence luminescent silicate material, its chemical constitution is:
aSrO·bCaO·cMgO·dSiO
2·eB
2O
3·Eu
x·Ln
y
Wherein Ln is the lanthanon except that Eu, and auxiliary Eu strengthens the twilight sunset effect; A wherein, b, c, d, e, x, y is mole coefficient; A: b: c: d: e: x: y=1: 0.2～5: 0.3～15: 0.4～20: 0.01～1: 0.001～0.1: 0.001～1, mol ratio.
2. a long persistence luminescent silicate material as claimed in claim 1 is characterized in that, the ratio of above-mentioned a and x is more than or equal to 0.001 and less than 0.1; The ratio of above-mentioned a and y is greater than 0.001 and less than 1.
3. the synthetic method of a long persistence luminescent silicate material as claimed in claim 1, step is as follows:
1) powder with Strontium carbonate powder, lime carbonate, magnesium oxide, silicon-dioxide, boric acid and rare earth oxide, Eu oxide compound is combined by the mole coefficient, and ball milling 6～10 hours is combined evenly, and the mixture that obtains is called powder;
2) powder is packed into alumina crucible, with carbon dust or hydrogen reducing, at 1200-1400 ℃ of following sintering 2-5 hour, powder sintering was a powder agglomates;
3) after being cooled to room temperature, take out powder agglomates, be crushed to powder, obtain yellow-green colour (520nm) long after glow luminous material.
4. a long persistence luminescent silicate material as claimed in claim 1 is characterized in that, the ball milling time in the step 1) is 8 hours.
5. a long persistence luminescent silicate material as claimed in claim 1 is characterized in that, the method that the present invention adopts is called and is the high temperature solid state reaction synthesis method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710014820 CN101074372A (en) | 2007-06-22 | 2007-06-22 | Silicate long-afterglow luminescent material and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710014820 CN101074372A (en) | 2007-06-22 | 2007-06-22 | Silicate long-afterglow luminescent material and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101074372A true CN101074372A (en) | 2007-11-21 |
Family
ID=38975645
Family Applications (1)
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|---|---|---|---|
| CN 200710014820 Pending CN101074372A (en) | 2007-06-22 | 2007-06-22 | Silicate long-afterglow luminescent material and its production |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104099092A (en) * | 2013-04-09 | 2014-10-15 | 海洋王照明科技股份有限公司 | Dysprosium-doped alkali fluoborosilicate glass up-conversion luminescent material, and preparation method and application thereof |
| CN104974757A (en) * | 2015-07-20 | 2015-10-14 | 浙江工贸职业技术学院 | Fluorescent material capable of preparing oxygen and preparation method thereof |
| CN108531071A (en) * | 2017-11-02 | 2018-09-14 | 王小琴 | A kind of coating |
| CN112280554A (en) * | 2020-11-20 | 2021-01-29 | 广东电网有限责任公司电力科学研究院 | Energy storage type environment-friendly luminescent material and preparation method thereof |
-
2007
- 2007-06-22 CN CN 200710014820 patent/CN101074372A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104099092A (en) * | 2013-04-09 | 2014-10-15 | 海洋王照明科技股份有限公司 | Dysprosium-doped alkali fluoborosilicate glass up-conversion luminescent material, and preparation method and application thereof |
| CN104974757A (en) * | 2015-07-20 | 2015-10-14 | 浙江工贸职业技术学院 | Fluorescent material capable of preparing oxygen and preparation method thereof |
| CN104974757B (en) * | 2015-07-20 | 2016-11-16 | 浙江工贸职业技术学院 | A kind of fluorescent material of oxygen processed and preparation method thereof |
| CN108531071A (en) * | 2017-11-02 | 2018-09-14 | 王小琴 | A kind of coating |
| CN108949164A (en) * | 2017-11-02 | 2018-12-07 | 王小琴 | A kind of yellow longpersistent light-emitting component |
| CN112280554A (en) * | 2020-11-20 | 2021-01-29 | 广东电网有限责任公司电力科学研究院 | Energy storage type environment-friendly luminescent material and preparation method thereof |
| CN112280554B (en) * | 2020-11-20 | 2022-04-29 | 广东电网有限责任公司电力科学研究院 | Energy storage type environment-friendly luminescent material and preparation method thereof |
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Open date: 20071121 |