CN1240809C - Method for preparing nano luminescent powder made from yttrium europium vanadate - Google Patents
Method for preparing nano luminescent powder made from yttrium europium vanadate Download PDFInfo
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- CN1240809C CN1240809C CN 200410033902 CN200410033902A CN1240809C CN 1240809 C CN1240809 C CN 1240809C CN 200410033902 CN200410033902 CN 200410033902 CN 200410033902 A CN200410033902 A CN 200410033902A CN 1240809 C CN1240809 C CN 1240809C
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- PXMLGXWGOVHNQX-UHFFFAOYSA-N [Y].[Eu] Chemical compound [Y].[Eu] PXMLGXWGOVHNQX-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 title abstract description 11
- 239000000843 powder Substances 0.000 title abstract description 7
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title abstract 3
- 239000012153 distilled water Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 16
- 230000005855 radiation Effects 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical compound [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 claims abstract description 9
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims abstract description 9
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 claims description 14
- 238000005119 centrifugation Methods 0.000 claims description 8
- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical compound [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 claims description 8
- 239000000047 product Substances 0.000 abstract description 24
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 238000003756 stirring Methods 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 4
- 230000035484 reaction time Effects 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000000593 microemulsion method Methods 0.000 abstract description 3
- 239000012467 final product Substances 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000011858 nanopowder Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000003746 solid phase reaction Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 229910052727 yttrium Inorganic materials 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- -1 rare earth ion Chemical class 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- QWVYNEUUYROOSZ-UHFFFAOYSA-N trioxido(oxo)vanadium;yttrium(3+) Chemical compound [Y+3].[O-][V]([O-])([O-])=O QWVYNEUUYROOSZ-UHFFFAOYSA-N 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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Abstract
The present invention relates to a preparation method of nano yttrium europium vanadate luminescent powder, which belongs to the technical field of luminescent materials. The existing method normally needs longer reaction time and relatively more complicated steps, and the particle size of a final product is difficult to control to be lower than 10 nm, so the fluorescent luminous efficiency can be reduced greatly. The preparation method of nano yttrium europium vanadate luminescent powder provided by the present invention is characterized in that the method comprises the following steps: mixing solid of 100 mol% of sodium metavanadate, 95 mol% of yttrium nitrate and 5 mol% of europium nitrate in distilled water and uniformly stirring the raw materials into solution; regulating the pH value to 4 to 11; causing the solution to react for 5 to 10 minutes under 260 to 560 W of microwave radiation; centrifugally separating the solution after being radiated by microwave and washing the separated solution with distilled water. In this way, the required product is obtained by drying the washed solution. The method adopts a microwave radiation method which is relatively simpler than other preparation methods, such as a solid phase reaction method, a hydrothermal method, a microemulsion method, etc., so the production technology is simple. Because the reaction rate is high, the reaction time is considerably shortened, and the obtained product is nano powder with uniform size.
Description
Technical field
A kind of preparation method of nanometer vanadic acid yttrium europium fluorescent material belongs to field of light emitting materials.
Background technology
The vanadic acid yttrium belongs to cubic zircon crystalloid structure, is a kind of good substrate material, can carry out the doping of trivalent transition metal ion and rare earth ion.Because of its in the application of aspects such as polarizer, fluorescence and laserable material and the demand of fundamental research, be subjected to paying close attention to widely in solid state chemistry and material science always.Because the vanadic acid yttrium is a kind of single shaft crystalline substance birefringece crystal, can be used as polarizer; Rear-earth-doped yttrium vanadate single crystal can be used as good solid laser material, the adulterated vanadic acid yttrium of trivalent europium ion powder then is a kind of material of red emission efficiently, with body phase vanadic acid yttrium europium, under electron-beam excitation, its fluorescent yield can be up to 70%, thereby in aspect extensive application such as Field Emission Display, cathode tube and colour television sets.
In view of the important application of vanadic acid yttrium at photoelectric field, it is very extensive and go deep into that the preparation of relevant monocrystalline, polycrystalline vanadic acid yttrium and performance study have carried out ground.A lot of single crystal technology all have been used to prepare the big yttrium vanadate single crystal of high optical quality, but because vanadic acid yttrium high-melting-point (1810 ℃) and temperature instability, and the carburation by evaporation of Vanadium Pentoxide in FLAKES (690 ℃), at high temperature form oxygen vacancy easily, thereby require relatively harsh preparation condition.In addition, hydrothermal reaction at low temperature (＜200 ℃), precipitation at room temperature reaction method and microemulsion method etc. are also successfully prepared the various rare earth ion doped vanadic acid yttrium powder of nano-scale.Yet these methods generally need the long reaction times, and the particle size of relatively Fu Za program, and final product is difficult to be controlled at below 10 nanometers, and this can have a strong impact on the luminous efficiency of its fluorescence.In addition, the amount of products therefrom is less, is not suitable for producing in batches.
Summary of the invention
Problem to be solved by this invention provide a kind of fast synthetic, the energy is low and production technique is simple, yardstick is evenly distributed, the red emission material nano vanadic acid yttrium europium (Eu:YVO that suitable batch is produced
4) preparation method of fluorescent material.
The preparation method of nanometer vanadic acid yttrium europium fluorescent material provided by the invention is characterized in that it may further comprise the steps:
1. sodium metavanadate and Yttrium trinitrate, europium nitrate solid mixed in distilled water in 1: 0.95: 0.05 in molar ratio, be stirred into solution;
2. the pH value of regulating above-mentioned solution is to 4-11;
3. the solution of above-mentioned adjusting pH value to the 4-11 reacted 5-10 minute under the microwave radiation of 260W-560W;
4. after centrifugation after the above-mentioned microwave radiation, distilled water wash, drying, promptly get product of the present invention.
This method adopts the easy more microwave irradiation with respect to preparation methods such as solid reaction process, hydrothermal method and microemulsion methods, production technique is simple, because speed of response is fast, not only shortened the reaction times greatly, and products therefrom is the uniform nanometer powder of yardstick.
Adopt Japanese Bruker Advance D-8X ray powder diffraction instrument (Cu K
αRadiation, λ=1.5406 ) measures the structure of prepared material.Adopt the particle size and the pattern of the prepared material of JEM-2000FX determination of transmission electron microscopy.The fluorescent emission performance that adopts Spex Fluoromax 2 fluorescence spectrophotometer to test prepared material.
As shown in Figure 1, products therefrom is the vanadic acid yttrium europium with pure tetragonal phase structure, and wide diffraction peak halfwidth shows that the products therefrom grain-size is less; As shown in Figure 2, products therefrom is the uniform nanometer powder of particle scale, and mean sizes is about 4 nanometers; As shown in Figure 3, products therefrom has a superior red emission performance.
Description of drawings
Fig. 1: the X-ray powder diffraction figure of product a～f;
Fig. 2: the transmission electron microscope picture of product c;
Fig. 3: the luminescent spectrum figure of product c.
Embodiment
1. with the solid of 1: 0.95: 0.05 sodium metavanadate of mol ratio, Yttrium trinitrate and europium nitrate, add in the distilled water, mix, stir, regulate pH value to 4 with rare nitric acid, reaction is 10 minutes under the 260W microwave radiation, and product is through centrifugation, distilled water wash after the drying, promptly gets product a.
2. with the solid of 1: 0.95: 0.05 sodium metavanadate of mol ratio, Yttrium trinitrate and europium nitrate, add in the distilled water, mix, stir, regulate pH value to 6 with rare nitric acid, reaction is 10 minutes under the 260W microwave radiation, and product is through centrifugation, distilled water wash after the drying, promptly gets product b.
3. with the solid of 1: 0.95: 0.05 sodium metavanadate of mol ratio, Yttrium trinitrate and europium nitrate, add in the distilled water, mix, stir, this moment, pH value was 7, and reaction is 10 minutes under the 260W microwave radiation, and product is through centrifugation, distilled water wash after the drying, promptly gets product c.
4. with the solid of 1: 0.95: 0.05 sodium metavanadate of mol ratio, Yttrium trinitrate and europium nitrate, add in the distilled water, mix, stir, regulate pH value to 8 with sodium hydroxide solution, reaction is 10 minutes under the 260W microwave radiation, and product is through centrifugation, distilled water wash, after the drying, promptly get product d.
5. with the solid of 1: 0.95: 0.05 sodium metavanadate of mol ratio, Yttrium trinitrate and europium nitrate, add in the distilled water, mix, stir, regulate pH value to 11 with sodium hydroxide solution, reaction is 10 minutes under the 260W microwave radiation, and product is through centrifugation, distilled water wash, after the drying, promptly get product e.
6. with the solid of 1: 0.95: 0.05 sodium metavanadate of mol ratio, Yttrium trinitrate and europium nitrate, add in the distilled water, mix, stir, regulate pH value to 11 with sodium hydroxide solution, reaction is 5 minutes under the 560W microwave radiation, and product is through centrifugation, distilled water wash, after the drying, promptly get product f.
Claims (1)
1. the preparation method of nanometer vanadic acid yttrium europium fluorescent material is characterized in that it may further comprise the steps:
(1) sodium metavanadate and Yttrium trinitrate, europium nitrate solid mixed in distilled water in 1: 0.95: 0.05 in molar ratio, be stirred into solution;
(2) regulate the pH value of above-mentioned solution to 4-11;
(3) solution of above-mentioned adjusting pH value to the 4-11 reacted 5-10 minute under the microwave radiation of 260W-560W;
(4) after centrifugation after the above-mentioned microwave radiation, distilled water wash, drying, promptly get product of the present invention.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410033902 CN1240809C (en) | 2004-04-19 | 2004-04-19 | Method for preparing nano luminescent powder made from yttrium europium vanadate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410033902 CN1240809C (en) | 2004-04-19 | 2004-04-19 | Method for preparing nano luminescent powder made from yttrium europium vanadate |
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| Publication Number | Publication Date |
|---|---|
| CN1563269A CN1563269A (en) | 2005-01-12 |
| CN1240809C true CN1240809C (en) | 2006-02-08 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100566821C (en) * | 2008-01-17 | 2009-12-09 | 同济大学 | A kind of preparation method of composite photocatalytic material containing rare earth element |
| CN101864314A (en) * | 2010-06-13 | 2010-10-20 | 武汉大学 | Method for Synthesizing Rare Earth Fluoride Fluorescent Nanoparticles in Microwave Liquid Phase |
| CN101984015B (en) * | 2010-09-29 | 2013-07-17 | 南京工业大学 | Preparation of (Y) by microwave radiation |
| CN101979460B (en) * | 2010-09-30 | 2013-10-02 | 广东炜林纳功能材料有限公司 | Method for preparing microwave-assisted non ball milling rare-earth superfine powder |
| CN105733584B (en) * | 2016-04-18 | 2018-12-25 | 吉林大学 | Yttrium Orthovanadate nanoparticle and rare earth ion doped Yttrium Orthovanadate nanoparticle and preparation method thereof |
| CN106006731B (en) * | 2016-06-21 | 2018-06-29 | 安徽铭源新型建材科技有限公司 | A kind of rare earth Yttrium Orthovanadate, preparation method and application |
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