CN102061168A - Method for improving luminosity of europium-doped yttrium oxide red fluorescent powder - Google Patents
Method for improving luminosity of europium-doped yttrium oxide red fluorescent powder Download PDFInfo
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- CN102061168A CN102061168A CN2011100016148A CN201110001614A CN102061168A CN 102061168 A CN102061168 A CN 102061168A CN 2011100016148 A CN2011100016148 A CN 2011100016148A CN 201110001614 A CN201110001614 A CN 201110001614A CN 102061168 A CN102061168 A CN 102061168A
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Abstract
The invention discloses a method for improving luminosity of europium-doped yttrium oxide red fluorescent powder. In the method, yttrium nitrate, europium nitrate and sodium hydroxide are used as reactants, a two-steps hydrothermal method is carries out in cooperation with subsequent thermal treatment. The method specifically comprises the steps of: firstly, synthesizing Y(OH)3:Eu<3+> at 220 DEG C hydrothermally, then, cladding the Y(OH)3 onto the surface of the Y(OH)3:Eu<3+> under the hydrothermal condition, and finally carrying out thermal treatment on the obtained product at 1000 DEG C to obtain the fluorescent powder of a Y2O3:Eu<3+>/Y2O3 nuclear-shell structure, wherein the molar ratio of the nuclear of Y2O3:Eu<3+> to the shell of Y2O3 is (3:1)-(10:1). By means of the homogeneous cladding, the surface defects of the Y2O3:Eu<3+> nano light-emitting particles can be effectively reduced, and the luminosity of the Y2O3:Eu<3+> nano light-emitting particles can be improved by 5-28% in comparison with that of like products without cladding. By means of the method, the luminosity of the homogeneous cladding product is obviously improved, the advantages of simple process, mild reaction conditions and convenience in operation are achieved, and the method is suitable for large-scale industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method who improves the brightness of europium-doped yttrium oxide red light emitting phosphor.
Background technology
Rare earth luminescent material has huge using value and potential prospect in a lot of fields, as low light level illumination, imaging demonstration, radiation detection, fields such as emergent indication, building decoration and industrial art.Present yellow-green colour and blue emitting material be widespread usage, but red illuminating material does not reach the level of above-mentioned two classes as yet on time of persistence, luminous intensity, and the research of therefore improving red illuminating material luminous intensity aspect receives much concern.
Y
2O
3: Eu
3+Be the red fluorescence material of excellent property, its luminous efficiency is high and have higher purity of color and light to keep characteristic.Its common synthetic method mainly contains high temperature solid-state method, coprecipitation method, sol-gel method, combustion method, hydrothermal method, microwave method etc.Hydrothermal method is a kind of Y that comparatively simply prepares
2O
3: Eu
3+The technology of rouge and powder, but resulting micro-nano product has more defective, reduced luminous intensity, the method for common reduction defective is to select suitable tensio-active agent, but how the optimization of option table surface-active agent and tensio-active agent add-on can bring follow-up trouble again.In recent years, be studied in a large number, as the SiO of synthetic kernel shell structure about preparing the method that nucleocapsid structure improves light-emitting phosphor intensity
2/ Y
2O
3: Eu
3+[Hyoung Sun Yoo, et al, Continuous nano-coating of Y
2O
3: Eu
3+Phosphor shell on SiO
2Core particles and its photoluminescence properties, Journal of Luminescence, 130 (2010) 153-156], and the BaSO of nucleocapsid structure
4/ Y
2O
3: Eu
3+[Ming Zhang, et al, Synthesis and characterization of monodispersed BaSO4/ Y
2O
3: Eu
3+Core – shell submicrospheres, Powder Technology, 195 (2009) 69-72] etc., but about at Y
2O
3: Eu
3+The surface homogeneity coats the research that improves its luminosity and yet there are no report.
Summary of the invention
The object of the present invention is to provide a kind of raising europium-doped yttrium oxide (Y
2O
3: Eu
3+) method of red light emitting phosphor brightness.Adopt two step hydro-thermal technologies to be aided with follow-up thermal treatment, coat by homogeneity and improved the brightness of europium-doped yttrium oxide red light emitting phosphor.
The step of technical scheme that the present invention adopts is as follows:
1) Yttrium trinitrate, europium nitrate are dissolved in the deionized water by mole per-cent, the ratio of control europium nitrate is 5% of a total rare earth cation mole number, stirs;
2) add sodium hydroxide solution in above-mentioned solution, the mole number of control sodium hydroxide is 10 times of total rare earth cation mole number, stirs;
3) above-mentioned solution is packed into autoclave adopts hydro-thermal technology, the solution centrifugal of handling well;
4) in the above-mentioned centrifugal solid product that obtains, add deionized water and form solution, stir, subsequently Yttrium trinitrate is dissolved in the described solution controlled step 1) in total rare earth cation mole number and the step 4) ratio of the mole number of Yttrium trinitrate be 3:1 ~ 10:1, stir;
5) sodium hydroxide solution is added in the step 4) solution, the mole number of sodium hydroxide is 10 times of used Yttrium trinitrate mole number in the step 4);
6) step 5) solution is packed into autoclave adopts hydro-thermal technology, the solution centrifugal of handling well, cleaning, drying;
7) dried product 1000 ℃ of thermal treatment 2h in the tubular type sintering oven, cooling obtains final product.
2, a kind of method that improves the brightness of europium-doped yttrium oxide red light emitting phosphor according to claim 1 is characterized in that: in the described twice hydro-thermal technology, temperature is 220 ℃, and the treatment time is 24 hours.
The beneficial effect that the present invention has is:
The present invention is to be reactant with Yttrium trinitrate, europium nitrate, sodium hydroxide, is aided with follow-up thermal treatment by two step hydro-thermal technologies and has synthesized the europium-doped yttrium oxide red illuminating material that yttrium oxide coats.This homogeneity coats can effectively reduce Y
2O
3: Eu
3+The surface imperfection of nano luminescent particles makes its luminous efficiency improve 5 ~ 28% than the similar product that does not coat.The luminous intensity that homogeneity coats after product be significantly improved and its technology simple, the reaction conditions gentleness, easy to operate, be fit to large-scale industrialized production.
Description of drawings
Fig. 1 is products therefrom Y (OH) among the comparative example 1
3: Eu
3+XRD figure spectrum.
Fig. 2 is products therefrom Y among the comparative example 1
2O
3: Eu
3+XRD figure spectrum.
Curve (a) and (b), (c), (d), (e), the corresponding comparative example 1 of (f) difference, embodiment 1, embodiment 2, embodiment 3, embodiment 4 and comparative example's 2 products therefrom photoluminescence emmission spectrum spectrograms among Fig. 3.
Embodiment
Embodiment 1:
Get 1.1642 gram Yttrium trinitrate (Y (NO respectively
3)
36H
2O), 0.0714 gram europium nitrate (Eu (NO
3)
36H
2O) be dissolved in 40 ml deionized water, the concentration of Yttrium trinitrate, europium nitrate is respectively 0.0760 mol, 0.0040 mol, stirs.The sodium hydroxide solution that adds 32 milliliter of 1 mol in above-mentioned solution, the mole number of control sodium hydroxide is 10 times of total rare earth cation mole number, stirs.The above-mentioned solution for preparing is put into the teflon-lined autoclave, and compactedness is 80%, and the liner volume is 100 milliliters.This solution was handled 24 hours down at 220 ℃, and cooled solution is centrifugal, obtained europium doping volumetric molar concentration and be 5% product.In the above-mentioned centrifugal solid product that obtains, add deionized water, stir, subsequently with 0.1225 gram Yttrium trinitrate (Y (NO
3)
36H
2O) be dissolved in wherein, the ratio of rare-earth cation total mole number is 1:10 before the mole number that adds Yttrium trinitrate and the above-mentioned hydro-thermal reaction, stirs, and the sodium hydroxide solution with 3.2 milliliter of 1 mol adds subsequently, stirs.The solution that stirs is put into autoclave, handles 24 hours for 220 ℃, and cooled solution is centrifugal, dry.The 1000 ℃ of thermal treatment 2 hours in the tubular type sintering oven of dried product, cooling obtains final product.
Embodiment 2:
Get 1.1642 gram Yttrium trinitrate (Y (NO respectively
3)
36H
2O), 0.0714 gram europium nitrate (Eu (NO
3)
36H
2O) be dissolved in 40 ml deionized water, the volumetric molar concentration of Yttrium trinitrate, europium nitrate is respectively 0.0760 mol, 0.0040 mol, stir, the sodium hydroxide solution that in above-mentioned solution, adds 32 milliliter of 1 mol, the mole number of control sodium hydroxide is 10 times of total rare earth cation mole number, stirs.The solution that stirs is put into the teflon-lined autoclave, and compactedness is 80%, and the liner volume is 100 milliliters.This solution was handled 24 hours down at 220 ℃, and cooled solution is centrifugal, dry, and wherein the doping content of europium accounts for 5% of rare earth element total mole number.In the above-mentioned centrifugal solid product that obtains, add deionized water, stir, subsequently with 0.1532 gram Yttrium trinitrate (Y (NO
3)
36H
2O) be dissolved in wherein, the ratio of rare-earth cation mole number is 1:8 before the mole number that newly adds Yttrium trinitrate and the above-mentioned hydro-thermal reaction, stirs.Sodium hydroxide solution with 4 milliliter of 1 mol adds above-mentioned solution subsequently, and the mole number of sodium hydroxide is new 10 times of adding the Yttrium trinitrate mole number.The solution that stirs is put into autoclave, handles 24 hours down at 220 ℃, and cooled solution is centrifugal, dry, the 1000 ℃ of thermal treatment 2 hours in the tubular type sintering oven of dried product, and cooling obtains final product.
Embodiment 3:
Get 1.1642 gram Yttrium trinitrate (Y (NO respectively
3)
36H
2O), 0.0714 gram europium nitrate (Eu (NO
3)
36H
2O) be dissolved in 40 ml deionized water, the volumetric molar concentration of Yttrium trinitrate, europium nitrate is respectively 0.0760 mol, 0.0040 mol, stirs.The sodium hydroxide solution that adds 32 milliliter of 1 mol in above-mentioned solution, the mole number of control sodium hydroxide is 10 times of total rare earth cation mole number, stirs.The above-mentioned solution for preparing is put into the teflon-lined autoclave, and compactedness is 80%, and the liner volume is 100 milliliters.This solution was handled 24 hours down at 220 ℃, and cooled solution is centrifugal, and wherein the doping content of europium accounts for 5% of total rare earth total mole number.In the above-mentioned centrifugal solid product that obtains, add deionized water, stir, subsequently with 0.2450 gram Yttrium trinitrate (Y (NO
3)
36H
2O) be dissolved in wherein, the ratio of total rare earth cation mole number is 1:5 before the mole number that wherein newly adds Yttrium trinitrate and the above-mentioned hydro-thermal reaction, stir, and be that the sodium hydroxide solution of 1 mol adds above-mentioned solution subsequently with 6.4 ml concns, stir.The solution that stirs is put into autoclave, and this solution was handled 24 hours down at 220 ℃, and cooled solution is centrifugal, dry, the 1000 ℃ of thermal treatment 2 hours in the tubular type sintering oven of dried product, and cooling obtains final product.
Embodiment 4:
Get 1.1642 gram Yttrium trinitrate (Y (NO respectively
3)
36H
2O), 0.0714 gram europium nitrate (Eu (NO
3)
36H
2O) be dissolved in 40 ml deionized water, the volumetric molar concentration of Yttrium trinitrate, europium nitrate is respectively 0.0760 mol, 0.0040 mol, stirs.The sodium hydroxide solution that adds 32 milliliter of 1 mol in above-mentioned solution, the mole number of control sodium hydroxide is 10 times of total rare earth cation mole number, stirs.Subsequently the solution that stirs is put into the teflon-lined autoclave, compactedness is 80%, and the liner volume is 100 milliliters.This solution was handled 24 hours down at 220 ℃, and the solution centrifugal of handling well, wherein the doping content of europium accounts for 5% of rare earth element total mole number.In the above-mentioned centrifugal solid product that obtains, add deionized water, stir, subsequently with 0.4085 Yttrium trinitrate (Y (NO
3)
36H
2O) be dissolved in wherein, the ratio of total rare earth cation mole number is 1:3 before the mole number that newly adds Yttrium trinitrate and the above-mentioned hydro-thermal reaction, stirs.Sodium hydroxide solution with 10.7 milliliter of 1 mol adds above-mentioned solution subsequently, and the mole number of sodium hydroxide is new 10 times of adding the Yttrium trinitrate mole number.The above-mentioned solution for preparing is put into autoclave, and this solution was handled 24 hours down at 220 ℃, and cooled solution is centrifugal, dry, dried product 1000 ℃ of thermal treatment 2h in the tubular type sintering oven, and cooling obtains final product.
The comparative example 1:
Get 1.1642 gram Yttrium trinitrate (Y (NO respectively
3)
36H
2O), 0.0714 gram europium nitrate (Eu (NO
3)
36H
2O) be dissolved in 40 ml deionized water, the concentration of Yttrium trinitrate, europium nitrate is respectively 0.0760 mol, 0.0040 mol, stirs.The sodium hydroxide solution that adds 32 milliliter of 1 mol in above-mentioned solution, the mole number of control sodium hydroxide is 10 times of total rare earth cation mole number, stirs.The solution that stirs is put into the teflon-lined autoclave, and compactedness is 80%, and the liner volume is 100 milliliters.This solution was handled 24 hours at 220 ℃, the solution centrifugal of handling well, drying, obtained Y (OH)
3: Eu
3+, wherein the doping content of europium accounts for 5% of rare earth element total mole number.Figure 1 shows that its XRD figure spectrum, as can be seen from the figure its characteristic peak and Y (OH)
3Standard card (JCPDS no.24-1422) fit like a glove a small amount of Eu
3+Ionic mixes the variation that does not cause structure.Dried product is 1000 ℃ of thermal treatment 2h in the tubular type sintering oven, and cooling obtains Y
2O
3: Eu
3+Powder.Figure 2 shows that the XRD figure spectrum of thermal treatment after product, as can be seen from the figure its characteristic peak and Y
2O
3Standard card (JCPDS no.25-1200) fit like a glove.
The comparative example 2:
Get 1.1642 gram Yttrium trinitrate (Y (NO respectively
3)
36H
2O), 0.0714 gram europium nitrate (Eu (NO
3)
36H
2O) be dissolved in 40 ml deionized water, the volumetric molar concentration of Yttrium trinitrate, europium nitrate is respectively 0.0760 mol, 0.0040 mol, stirs.The sodium hydroxide solution that adds 32 milliliter of 1 mol in above-mentioned solution, the mole number of control sodium hydroxide is 10 times of total rare earth cation mole number, stirs.The solution that stirs is put into the teflon-lined autoclave, and compactedness is 80%, and the liner volume is 100 milliliters.This solution was handled 24 hours down at 220 ℃, and cooled solution is centrifugal, obtained europium doping volumetric molar concentration and be 5% product.In the above-mentioned centrifugal solid product that obtains, add deionized water, stir, subsequently with 1.2255 gram Yttrium trinitrate (Y (NO
3)
36H
2O) be dissolved in it, the ratio of rare-earth cation total mole number is 1:1 before the mole number that adds Yttrium trinitrate and the above-mentioned hydro-thermal reaction, stir, and be that the sodium hydroxide solution of 1 mol adds above-mentioned solution with 32 ml concns, stir.The solution that stirs is put into autoclave, handles 24 hours for 220 ℃, and cooled solution is centrifugal, dry.Dried product is 1000 ℃ of thermal treatment 2h in the tubular type sintering oven, and cooling obtains final product.Fig. 3 is a synthetic product photoluminescence emmission spectrum, and wherein Fig. 3 (a) is product Y among the comparative example 1
2O
3: Eu
3+The emmission spectrum of powder, spectrogram presents Eu
3+The feature emission spectrum, color is based on redness.Fig. 3 (b), 3 (c), 3 (d), 3 (e), 3 (f) are followed successively by embodiment 1, embodiment 2, embodiment 3, embodiment 4 and comparative example's 2 emmission spectrum spectrogram.More as can be seen, among the embodiment in the luminous strength ratio Comparative Examples of product the luminous intensity of product raising has in various degree been arranged.
Claims (2)
1. method that improves the brightness of europium-doped yttrium oxide red light emitting phosphor is characterized in that the step of this method is as follows:
1) Yttrium trinitrate, europium nitrate are dissolved in the deionized water by mole per-cent, the ratio of control europium nitrate is 5% of a total rare earth cation mole number, stirs;
2) add sodium hydroxide solution in above-mentioned solution, the mole number of control sodium hydroxide is 10 times of total rare earth cation mole number, stirs;
3) above-mentioned solution is packed into autoclave adopts hydro-thermal technology, the solution centrifugal of handling well;
4) in the above-mentioned centrifugal solid product that obtains, add deionized water and form solution, stir, subsequently Yttrium trinitrate is dissolved in the described solution controlled step 1) in total rare earth cation mole number and the step 4) ratio of the mole number of Yttrium trinitrate be 3:1 ~ 10:1, stir;
5) sodium hydroxide solution is added in the step 4) solution, the mole number of sodium hydroxide is 10 times of used Yttrium trinitrate mole number in the step 4);
6) step 5) solution is packed into autoclave adopts hydro-thermal technology, the solution centrifugal of handling well, cleaning, drying;
7) dried product 1000 ℃ of thermal treatment 2h in the tubular type sintering oven, cooling obtains final product.
2. a kind of method that improves the brightness of europium-doped yttrium oxide red light emitting phosphor according to claim 1 is characterized in that: in the described twice hydro-thermal technology, temperature is 220 ℃, and the treatment time is 24 hours.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103450899A (en) * | 2013-01-24 | 2013-12-18 | 深圳信息职业技术学院 | Preparation method of yttrium oxide doped nanometer fluorescent powder |
| WO2014067114A1 (en) * | 2012-10-31 | 2014-05-08 | 海洋王照明科技股份有限公司 | Sulfur oxide luminescent material and preparation method therefor |
| CN107056057A (en) * | 2017-04-21 | 2017-08-18 | 梅庆波 | A kind of preparation method of the long-persistence luminous glaze of low-temperature sintering isotypy |
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| JP2782962B2 (en) * | 1991-01-14 | 1998-08-06 | 日亜化学工業株式会社 | Phosphor surface treatment method |
| CN101368098A (en) * | 2008-07-29 | 2009-02-18 | 浙江理工大学 | YVO4:Eu3/YPO4 core-shell structure nano-fluorescent powder and preparation method thereof |
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2011
- 2011-01-06 CN CN2011100016148A patent/CN102061168A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2782962B2 (en) * | 1991-01-14 | 1998-08-06 | 日亜化学工業株式会社 | Phosphor surface treatment method |
| CN101368098A (en) * | 2008-07-29 | 2009-02-18 | 浙江理工大学 | YVO4:Eu3/YPO4 core-shell structure nano-fluorescent powder and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| DORENDRAJIT SINGH, ET AL.: "Preparation of Eu3+ doped Y2O3 and core-shell Y2O3:Eu-Y2O3 nanoparticles: Photoluminescence study", 《INDIAN JOURNAL OF ENGINEERING & MATERIALS SCIENCES》 * |
| SHENGLIANG ZHONG, ET AL.: "Spindlelike Y2O3:Eu3+ nanorod bundles: hydrothermal synthesis and photoluminescence properties", 《J MATER SCI》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014067114A1 (en) * | 2012-10-31 | 2014-05-08 | 海洋王照明科技股份有限公司 | Sulfur oxide luminescent material and preparation method therefor |
| CN104736668A (en) * | 2012-10-31 | 2015-06-24 | 海洋王照明科技股份有限公司 | Sulfur oxide luminescent material and preparation method therefor |
| US9650562B2 (en) | 2012-10-31 | 2017-05-16 | Ocean's King Lighting Science & Technology Co., Ltd. | Rare earth oxysulfide luminescent material and preparation method therefor |
| CN103450899A (en) * | 2013-01-24 | 2013-12-18 | 深圳信息职业技术学院 | Preparation method of yttrium oxide doped nanometer fluorescent powder |
| CN103450899B (en) * | 2013-01-24 | 2014-12-17 | 深圳信息职业技术学院 | Preparation method of yttrium oxide doped nanometer fluorescent powder |
| CN107056057A (en) * | 2017-04-21 | 2017-08-18 | 梅庆波 | A kind of preparation method of the long-persistence luminous glaze of low-temperature sintering isotypy |
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Application publication date: 20110518 |