CN101457142A - Combustion preparation method of green infrared up-conversion material - Google Patents
Combustion preparation method of green infrared up-conversion material Download PDFInfo
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- CN101457142A CN101457142A CNA2009100764103A CN200910076410A CN101457142A CN 101457142 A CN101457142 A CN 101457142A CN A2009100764103 A CNA2009100764103 A CN A2009100764103A CN 200910076410 A CN200910076410 A CN 200910076410A CN 101457142 A CN101457142 A CN 101457142A
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Abstract
The present invention discloses a conflagate preparation method of conversion material on green infrared which belongs to the technical field of luminescent material preparation. In the invention, NaF is taken as base material and adulterated with Y<SUP>3 + < /SUP>, Yb<SUP>3+</SUP> and Ho<SUP>3+</SUP>; citric acid is taken as incendiary; the conversion material on green infrared is synthesized after burning for more than ten minutes under normal temperature and normal pressure. The present invention significantly reduces heat treating temperature, greatly shortens reaction period with low cost and simple process; the produced material has uniform granularity, good repeatability, regular sample appearance, no need seat grinding, and suitable for industrial scale production. The problem of energy consumption, time consuming, miscellaneous and little varieties of luminous colors of current conversion material on infrared are solved, the application range is expanded, the development and progress of application of conversion material on infrared on biology tag, false proof etc. is promoted.
Description
Technical field
The invention belongs to the luminescent material preparing technical field, particularly a kind of combustion preparation method of green infrared up-conversion material.
Technical background
Infrared up-conversion material is a class energy up-conversion of changing out visible light with infrared ray excited, looks into the patent information that " State Intellectual Property Office of the People's Republic of China " announces in October, 2008, relevant up-conversion and comprise Ho
3+The patent of (holmium) has 7, is respectively 200610025536.4 1 kinds of Luetcium aluminum garnet-base transparent ceramics and preparation method thereof; 200610047358.5 changing luminous material on fine oxide; 200710056669.2 infrared laser detection card and preparation method thereof; 97107133.0 preparation rare-earth ion doped LN, LT optical super lattice material and application thereof; 200710144773.7 high luminous intensity up-conversion fluorescence nano-crystal oxide and preparation method thereof; 200710144828.4 red up-conversion phosphor and preparation method thereof; 200710192649.8 multiband fluorescence infrared up-conversion material based on sensitizing agent matrix, the luminous efficiency of product diminishes with particle and lowers rapidly generally speaking, its preparation is by the retort furnace high-temperature heating treatment substantially, for up to several hrs or do not wait in tens hours, after finishing, reaction also needs under weakly reducing atmosphere, to anneal a large amount of energy of preparation process consumption and consuming time, numerous and diverse., and rear-earth-doped Ho
3+(holmium) prepares green infrared up-conversion material with combustion method and also do not see relevant report at present.
Summary of the invention
The purpose of this invention is to provide a kind of combustion preparation method of green infrared up-conversion material, it is characterized in that, this method is matrix with NaF, with Y
3+, Yb
3+, Ho
3+Codoped is made incendiary material with citric acid, and burning synthesis for preparing is equipped with green infrared up-conversion material under normal temperature, normal pressure; Concrete steps are as follows:
1. take by weighing solid xNaF by stoichiometry, x is the 70-98% of the total mole of raw material, places in the corresponding container and dissolves fully with redistilled water or deionized water, obtains solution A;
2. pipette previously prepared solution yYb by stoichiometry
3+, z Ho
3+, (1-x-y-z) Y
3+, y is the 0.8-20% of the total mole of raw material, and z is the 0.005-0.2% of the total mole of raw material, and thorough mixing gets solution B;
3. with solution A, B mixing stir about 10-30 minute, make precursor, the common adding in the crucible, the 0.5-6 times of citric acid that adds up the original ingredient quality places on the electric furnace of preheating, and mixed solution is evaporate to dryness gradually, about 10 minutes a large amount of dense smokes of emerging, residue expands suddenly and acutely burns, produce a large amount of flakes white solids, cooling promptly gets white, powdered samples, sends bright green glow under the 980nm infrared source excites.
Beneficial effect of the present invention is that employing is rear-earth-doped, just can synthesize green infrared up-conversion material in tens minutes with combustion method.Present method has significantly reduced thermal treatment temp, shortened reaction time greatly, with low cost, technology is simple, and improved the luminous efficiency of product, solved the weak problem of small grain size product luminous efficiency, the material particle size of preparing is even, sends bright green visible light under 980nm is infrared ray excited, it is good to have both reproducibility, the sample topography rule need not be ground, and is fit to commercial scale production.
Embodiment
The invention provides a kind of combustion preparation method of green infrared up-conversion material.Enumerating embodiment is below further specified.
Embodiment one
Take by weighing solid 0.2g NaF, ultrasonic to being dissolved in redistilled water or the deionized water fully, obtain settled solution A; Pipette respectively and prepare the Y that concentration is 0.2M in advance
3+20.0ml, Yb
3+3.4ml, Ho
3+0.02ml3 plant the solution thorough mixing, obtain solution B.Solution A, B are mixed, and constant temperature magnetic agitation 10 minutes adds 1.0 gram citric acid uniform mixing, inserts crucible and heats in electric furnace.About 10 minutes a large amount of dense smokes of emerging, residue expand suddenly and acutely burn, and produce a large amount of flakes white solids, and cooling promptly gets white, powdered samples, sends bright green glow under the 980nm infrared source excites.
Embodiment two
Take by weighing solid 0.2g NaF, ultrasonic to being dissolved in redistilled water or the deionized water fully, obtain settled solution A; Pipette respectively and prepare the Y that concentration is 0.2M in advance
3+10.0ml, Yb
3+3.4ml, Ho
3+0.05ml3 plant the solution thorough mixing, obtain solution B.A, B mixing constant temperature magnetic agitation 10 minutes add 0.3 gram citric acid uniform mixing, insert crucible and heat in electric furnace.About 10 minutes a large amount of dense smokes of emerging, residue expand suddenly and acutely burn, and produce a large amount of flakes white solids, and cooling promptly gets white, powdered samples, sends bright green glow under the 980nm infrared source excites.
Embodiment three
Take by weighing solid 0.2g NaF, ultrasonic to being dissolved in the secondary deionized water fully, obtain settled solution A; Pipette respectively and prepare the Y that concentration is 0.2M in advance
3+26.0ml, Yb
3+3.4ml, Ho
3+1.5ml 3 kinds of solution thorough mixing obtain solution B.A, B mixing constant temperature magnetic agitation 10 minutes add 0.8 gram citric acid uniform mixing, insert crucible and heat in electric furnace.About 10 minutes a large amount of dense smokes of emerging, residue expand suddenly and acutely burn, and produce a large amount of flakes white solids, and cooling promptly gets white, powdered samples, sends bright green glow under the 980nm infrared source excites.
Embodiment four
Take by weighing solid 0.2g NaF, ultrasonic to being dissolved in the redistilled water fully, obtain settled solution A; Pipette respectively and prepare the Y that concentration is 0.2M in advance
3+16.0ml, Yb
3+3.4ml, Ho
3+2.0ml 3 kinds of solution thorough mixing obtain solution B.A, B mixing constant temperature magnetic agitation 10 minutes add 0.5 gram citric acid uniform mixing, insert crucible and heat in electric furnace.About 10 minutes a large amount of dense smokes of emerging, residue expand suddenly and acutely burn, and produce a large amount of flakes white solids, and cooling promptly gets white, powdered samples, sends bright green glow under the 980nm infrared source excites.
Claims (1)
1. the combustion preparation method of a green infrared up-conversion material is characterized in that, this method is a matrix with NaF, with Y
3+, Yb
3+, Ho
3+Codoped is made incendiary material with citric acid, and burning synthesis for preparing is equipped with green infrared up-conversion material under normal temperature, normal pressure; Concrete steps are as follows:
(1) take by weighing solid xNaF by stoichiometry, x is the 70-98% of the total mole of raw material, places in the corresponding container and dissolves fully with redistilled water or deionized water, obtains solution A;
(2) pipette previously prepared solution yYb by stoichiometry
3+, z Ho
3+, (1-x-y-z) Y
3+, y is the 0.8-20% of the total mole of raw material, and z is the 0.005-0.2% of the total mole of raw material, and thorough mixing gets solution B;
(3) solution A, B are mixed stirring 10-30 minute, make precursor, the common adding in the crucible, the 0.5-6 times of citric acid that adds up the original ingredient quality places on the electric furnace of preheating, and mixed solution is evaporate to dryness gradually, 10 minutes a large amount of dense smokes of emerging, residue expands suddenly and acutely burns, produce a large amount of flakes white solids, cooling promptly gets white, Powdered green infrared up-conversion material sample, sends bright green glow under the 980nm infrared source excites.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100764103A CN101457142B (en) | 2009-01-07 | 2009-01-07 | Combustion preparation method of green infrared up-conversion material |
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| CN2009100764103A CN101457142B (en) | 2009-01-07 | 2009-01-07 | Combustion preparation method of green infrared up-conversion material |
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| CN101457142A true CN101457142A (en) | 2009-06-17 |
| CN101457142B CN101457142B (en) | 2012-05-23 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965112A (en) * | 2012-12-07 | 2013-03-13 | 东北林业大学 | Intense ultraviolet up-converting micron fluoride material and preparation method thereof |
| US20170040385A1 (en) * | 2015-08-03 | 2017-02-09 | Boe Technology Group Co., Ltd. | Oled display apparatus and method for producing the same and color filter substrate and method for producing the same |
| CN112607775A (en) * | 2020-12-28 | 2021-04-06 | 中山大学 | Ho3+Activated green down-conversion phosphor and method of making |
-
2009
- 2009-01-07 CN CN2009100764103A patent/CN101457142B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965112A (en) * | 2012-12-07 | 2013-03-13 | 东北林业大学 | Intense ultraviolet up-converting micron fluoride material and preparation method thereof |
| US20170040385A1 (en) * | 2015-08-03 | 2017-02-09 | Boe Technology Group Co., Ltd. | Oled display apparatus and method for producing the same and color filter substrate and method for producing the same |
| US10608053B2 (en) * | 2015-08-03 | 2020-03-31 | Boe Technology Group Co., Ltd. | OLED with upconversion layer |
| CN112607775A (en) * | 2020-12-28 | 2021-04-06 | 中山大学 | Ho3+Activated green down-conversion phosphor and method of making |
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| Publication number | Publication date |
|---|---|
| CN101457142B (en) | 2012-05-23 |
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