CN1306005C - Aluminate-base rare earth long afterglow luminous material synthesizing method - Google Patents
Aluminate-base rare earth long afterglow luminous material synthesizing method Download PDFInfo
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- CN1306005C CN1306005C CNB2004100812284A CN200410081228A CN1306005C CN 1306005 C CN1306005 C CN 1306005C CN B2004100812284 A CNB2004100812284 A CN B2004100812284A CN 200410081228 A CN200410081228 A CN 200410081228A CN 1306005 C CN1306005 C CN 1306005C
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- aluminate
- rare earth
- long afterglow
- reducing gas
- base rare
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Abstract
The present invention relates to an aluminate-base rare earth long afterglow luminous material synthesizing method, particularly to a luminescent material high-temperature solid-phase reaction synthesizing method adopting a microwave plasma. Material which is ground and evenly mixed is put into a high purity quartz crucible arranged in a microwave plasma resonator. Reducing gas is filled by a flow quantity of 100 ml/min. Thus, final operational pressure in the resonator achieves 4000 to 5500Pa, and microwave power achieves 1200 to 1300W, which maintains one to two hours. On one hand, the present invention has low calcining temperature and short time. A generated product can not be easily caked, and the product does not need to be pulverized and reduced. On the other hand, a reaction atmosphere is pure, texture purity is high, and product performance can be ensured. Compared with the existing producing method, the present invention has the advantages of high speed, convenience, low price and enhancement of the intermixture uniformity of the material, crystallization quality and optics performance.
Description
Affiliated technical field
The present invention is a kind of synthetic method of aluminate-base rare earth long afterglow luminous material, particularly carries out the high temperature solid state reaction synthetic method of luminescent material with the microwave plasma of weak reducing atmosphere.
Background technology
The preparation method commonly used that aluminate-base rare earth long afterglow is provided material is with highly purified luminous substrate and activator, co-activator, i.e. Eu
2O
3, Dy
2O
3, SrCO
3, Al
2O
3Even with mechanically mixing after the boric acid micronization, in high-temperature atmosphere furnace, carry out the product that high temperature solid state reaction is finally required again.The shortcoming that this method exists is: temperature of reaction height (about 1600 ℃), and the time long (being reflected at more than 3 hours), the gained material purity is low, homogeneity is relatively poor, easily lumps, and the product that burns till also need be pulverized levigate, thereby cause the crystal grain defective to increase, influenced the cost and the performance of product.To prepare material homogeneity poor in order to overcome high temperature solid-state method, the weakness that purity is low, and successively the someone has developed technical matters such as heterogeneous coprecipitation method, sol-gel method, hydrothermal method and has synthesized that purity is higher, the better steady persistence rare earth luminescent material of homogeneity.But because the final stage of these technology methods still need experience the high temperature solid state reaction process identical with high temperature solid-state method, the product that still can not avoid bringing thus easily lumps, defectives such as purity is low, the crystal grain defective is many, time consumption and energy consumption.The someone has developed the combustion reactions synthesis method again for this reason, allow starting material directly generate final product through combustion reactions by liquid phase in very low temperature (about 500 ℃), thereby need not experience the front the whole bag of tricks the high temperature solid state reaction process that must have, make that whole processing method economy is simple, degree of purity of production and better dispersed.But this method still has many difficulties that are difficult to overcome: the controllability of the bad control of the chemical dosage ratio of product, process and repeatability are very poor, and pollution is arranged, and are difficult to satisfy the requirement of production application.
Summary of the invention
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art, a kind of synthetic technology method that adopts microwave plasma to carry out the luminescent material high temperature solid state reaction as thermal source and reaction medium is provided, thereby improve the homogeneity of material greatly, crystalline quality and luminescent properties, also shorten simultaneously generated time, reduce technical process.
Technical scheme of the present invention is: a kind of synthetic method of aluminate-base rare earth long afterglow luminous material is characterized in that being undertaken by following processing step
A, raw material ground and mixed that proportioning is good are even;
B, the material that mixes is inserted in the synthetic chamber of microwave plasma, charge into reducing gas after vacuumizing, open microwave generator;
C, charge into reducing gas, regulate microwave power to 250～750W with 100～300ml/min flow control;
D, increase reducing gas flow to 500～800ml/min, after the adjusting operating pressure was 4000～5500Pa, the re-adjustment microwave power was to 1200-1300W;
Kept 1～2 hour under e, the above-mentioned d condition.
Microwave plasma synthesis method of the present invention, with reducing gas as plasma medium, reducing gas is the thermal source of material at high temperature solid state reaction during high-temperature calcination like this, it is again the gaseous component of reduction reaction, add chemistry and thermal property that microwave plasma is exclusive, calcining temperature is reduced, the time shortens, product prevented from caking after calcining need not
Pulverize levigate; Reaction atmosphere is pure on the other hand, material purity height, and product performance can be guaranteed.The controllability of microwave plasma device, repeatability and the security when using hazardous gas are more superior than traditional heating device in addition, so the present invention has better technical qualification guarantee and industrialization prospect.
Reducing gas of the present invention can be H
2, N
2Or the gas mixture of the two and Ar and H
2Or N
2Mixed gas.
In the solution of the present invention, when flow rises to 500～800ml/min, the adjusting operating pressure is 5000～5500Pa, and the re-adjustment microwave power is to 1300W.
The present invention compared with prior art has the following advantages:
(1) the solid state reaction temperature is low, speed is fast.Temperature of reaction generally can be finished reaction than low 200～300 ℃ of reaction in the retort furnace about 1 hour.
(2) the powder product of Sheng Chenging is loose, fine size.The manual size of making grinding back gained powder slightly is about 2000nm, and centralized particle diameter.
(3) because the high chemically reactive of plasma body and the rate of heating that microwave plasma is exceedingly fast have greatly strengthened the elemental diffusion transfer ability, the good uniformity that product middle-weight rare earths element mixes up.
(4) overcome thermal runaway and the incubation cavity problem of microwave when synthetic.
(5) reaction atmosphere is pure, material purity height, crystalline quality and good luminous performance.
Embodiment
Embodiment 1:
The uniform material of ground and mixed is put into high-purity silica pot places microwave plasma to synthesize the chamber; Vacuumize the back and open microwave generator, charge into N with the 100ml/min flow
2Gas is regulated microwave power to 500W; And then adjusting N
2Flow is to 700ml/min, and pressure reaches 5500Pa, and microwave power transfers to 1300W, keeps 1.5 hours.
Embodiment 2:
The uniform material of ground and mixed is put into high-purity silica pot place microwave plasma resonant cavity; Vacuumize the back and open microwave generator, charge into Ar gas with the 100ml/min flow respectively, regulate microwave power to 500W; And then regulate the Ar flow to 750ml/min, charge into H with the 15ml/min flow
2, pressure reaches 5500Pa, and microwave power transfers to 1300W, keeps 1.5 hours.
Embodiment 3:
The uniform material of ground and mixed is put into high-purity silica pot place microwave plasma resonant cavity; Vacuumize the back and open microwave generator, charge into H with the molten amount of 100ml/min
2Gas is regulated microwave power to 500W; And then adjusting H
2Flow is to 780ml/min, and pressure reaches 5500Pa, and microwave power transfers to 1300W, keeps 1.5 hours.
Claims (4)
1, a kind of synthetic method of aluminate-base rare earth long afterglow luminous material is characterized in that being undertaken by following processing step
A, raw material ground and mixed that proportioning is good are even;
B, the material that mixes is inserted in the synthetic chamber of microwave plasma, charge into reducing gas after vacuumizing, open microwave generator;
C, the reducing gas that charges into 100～300ml/min flow control are regulated microwave power to 250～750W;
D, increase reducing gas flow to 500～800ml/min, after the adjusting operating pressure is 4000～5500Pa, re-adjustment microwave power to 1200～1300W;
Kept 1～2 hour under e, the above-mentioned d condition.
2, the synthetic method of aluminate-base rare earth long afterglow luminous material according to claim 1 is characterized in that reducing gas is H
2, N
2Or the gas mixture of the two and Ar and H
2Or N
2Mixed gas.
3, the synthetic method of aluminate-base rare earth long afterglow luminous material according to claim 1 and 2 is characterized in that initially charging into the reducing gas flow control at 100ml/min, regulates microwave power to 500W.
4, the synthetic method of aluminate-base rare earth long afterglow luminous material according to claim 1 and 2 is characterized in that rising to 500～800ml/min when flow, and the adjusting operating pressure is 5000～5500Pa, and the re-adjustment microwave power is to 1300W.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100812284A CN1306005C (en) | 2004-11-15 | 2004-11-15 | Aluminate-base rare earth long afterglow luminous material synthesizing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100812284A CN1306005C (en) | 2004-11-15 | 2004-11-15 | Aluminate-base rare earth long afterglow luminous material synthesizing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1775903A CN1775903A (en) | 2006-05-24 |
| CN1306005C true CN1306005C (en) | 2007-03-21 |
Family
ID=36765625
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100812284A Expired - Fee Related CN1306005C (en) | 2004-11-15 | 2004-11-15 | Aluminate-base rare earth long afterglow luminous material synthesizing method |
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|---|---|
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5507976A (en) * | 1993-11-24 | 1996-04-16 | Eastman Kodak Company | Stabilized phosphor intermediates, storage phosphors, radiation image storage panels, and preparation methods |
| CN1141946A (en) * | 1995-05-19 | 1997-02-05 | 中山大学 | Micro-wave thermosynthesizing of fluorescent powder |
| CN1157311A (en) * | 1996-12-14 | 1997-08-20 | 中山大学 | Diffusing, doping and synthetizing phosphor powder by microwave heating method |
| KR20020015504A (en) * | 2000-08-22 | 2002-02-28 | 김충섭 | Process for preparing of blue emitting phosphor particles by optimizing the precursor materials using spray pyrolysis |
| CN1363643A (en) * | 2001-11-26 | 2002-08-14 | 袁曦明 | Process for preparing nano yttrium aluminate as fluorescent powder |
| CN1366017A (en) * | 2002-03-15 | 2002-08-28 | 中国科学院长春应用化学研究所 | Vacuum ultraviolet ray excited green barium magnesium aluminate as fluorescent substance and its preparing process |
| CN1396234A (en) * | 2002-06-14 | 2003-02-12 | 中国地质大学（武汉） | Process for preparing long-afterglow luminous alaminate powder |
-
2004
- 2004-11-15 CN CNB2004100812284A patent/CN1306005C/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5507976A (en) * | 1993-11-24 | 1996-04-16 | Eastman Kodak Company | Stabilized phosphor intermediates, storage phosphors, radiation image storage panels, and preparation methods |
| CN1141946A (en) * | 1995-05-19 | 1997-02-05 | 中山大学 | Micro-wave thermosynthesizing of fluorescent powder |
| CN1157311A (en) * | 1996-12-14 | 1997-08-20 | 中山大学 | Diffusing, doping and synthetizing phosphor powder by microwave heating method |
| KR20020015504A (en) * | 2000-08-22 | 2002-02-28 | 김충섭 | Process for preparing of blue emitting phosphor particles by optimizing the precursor materials using spray pyrolysis |
| CN1363643A (en) * | 2001-11-26 | 2002-08-14 | 袁曦明 | Process for preparing nano yttrium aluminate as fluorescent powder |
| CN1366017A (en) * | 2002-03-15 | 2002-08-28 | 中国科学院长春应用化学研究所 | Vacuum ultraviolet ray excited green barium magnesium aluminate as fluorescent substance and its preparing process |
| CN1396234A (en) * | 2002-06-14 | 2003-02-12 | 中国地质大学（武汉） | Process for preparing long-afterglow luminous alaminate powder |
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| Publication number | Publication date |
|---|---|
| CN1775903A (en) | 2006-05-24 |
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