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 PDF

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Publication number
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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solution
distilled water
yttrium
product
preparation
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CN1563269A (en
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汪浩
徐海燕
严辉
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Beijing University of Technology
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Beijing University of Technology
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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

The preparation method of nanometer vanadic acid yttrium europium fluorescent material
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.
CN 200410033902 2004-04-19 2004-04-19 Method for preparing nano luminescent powder made from yttrium europium vanadate Expired - Fee Related CN1240809C (en)

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CN1240809C true CN1240809C (en) 2006-02-08

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Families Citing this family (6)

* Cited by examiner, † Cited by third party
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 who contains the composite photocatalyst material of rare earth element
CN101864314A (en) * 2010-06-13 2010-10-20 武汉大学 Method for synthesizing fluorescent nano particles of rare earth chlorides by microwave aqueous phase
CN101984015B (en) * 2010-09-29 2013-07-17 南京工业大学 A method for preparing (Y, gd)2O3: eu luminescent material 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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