CN101984015B - Preparation of (Y) by microwave radiation - Google Patents
Preparation of (Y) by microwave radiation Download PDFInfo
- Publication number
- CN101984015B CN101984015B CN201010500528.7A CN201010500528A CN101984015B CN 101984015 B CN101984015 B CN 101984015B CN 201010500528 A CN201010500528 A CN 201010500528A CN 101984015 B CN101984015 B CN 101984015B
- Authority
- CN
- China
- Prior art keywords
- reaction
- oxalic acid
- luminescent material
- microwave
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000005855 radiation Effects 0.000 title claims abstract description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 42
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 28
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 14
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 8
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 10
- -1 rare-earth salts Chemical class 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims description 2
- XEEVLJKYYUVTRC-UHFFFAOYSA-N oxomalonic acid Chemical compound OC(=O)C(=O)C(O)=O XEEVLJKYYUVTRC-UHFFFAOYSA-N 0.000 claims 1
- 230000035484 reaction time Effects 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract 2
- 150000002910 rare earth metals Chemical class 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 14
- 239000002245 particle Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000000498 ball milling Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000002073 nanorod Substances 0.000 description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- WSVPPALNMDLGQB-UHFFFAOYSA-N europium;oxalic acid Chemical compound [Eu].OC(=O)C(O)=O WSVPPALNMDLGQB-UHFFFAOYSA-N 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- QPRLZODEVQNPKY-UHFFFAOYSA-N oxalic acid;yttrium;hydrate Chemical compound O.[Y].OC(=O)C(O)=O QPRLZODEVQNPKY-UHFFFAOYSA-N 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011175 product filtration Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 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 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Images
Landscapes
- Luminescent Compositions (AREA)
Abstract
The invention relates to a microwave radiation (Y, Gd)2O3The preparation method of Eu luminescent material comprises firstly configuring 5-30 mM Re in a reaction container3+The rare earth salt solution of (1), wherein Re is Y, Gd and Eu, then adding ethylene glycol and oxalic acid, stirring and dissolving; then placing the prepared reaction raw material solution into a microwave reactor for microwave radiation reaction, filtering, washing and drying the precipitate after the reaction is finished, and then placing the precipitate into a muffle furnace for calcination to obtain (Y, Gd)2O3Eu luminescent material. Prepared by the invention (Y, Gd)2O3The Eu luminescent material has the advantages of uniform size, adjustable appearance and size, short reaction time, small-scale production and the like.
Description
Technical field
The present invention relates to a kind of microwave radiation (Y, Gd)
2O
3: the preparation method of Eu luminescent material belongs to the preparation field of inorganic materials.
Background technology
Y
2O
3Being a kind of important ceramic raw material, is to use one of more rare earth oxide in the fluorescent material.Y
2O
3Has good heat-resisting, corrosion-resistant and high-temperature stability, to the reducing medium good stability, the specific inductivity height, and can be made into the good polycrystalline ceramic of the transparency, be mainly used in window and nose cone, radome, microwave base plate, insulating support, optical fiber doping, infrared generator shell, Infrared Lens and other window pyrometers etc. of infra-red missile.Y
2O
3The super-refinement of particle can significantly improve the performance of product, and its disperse can obtain superalloy in alloy; Use ultra-fine Y
2O
3Stable zirconia powder art can sinter the stabilization zirconium oxide ceramic of high strength, high tenacity into, is used for cutter and mechanical component; Simultaneously it can also significantly improve the picture quality of colour TV, the luminous efficiency of luminescent lamp and increase the service life etc.Adding Nd
3+, Eu
3+After rare earth element, then can be used as the operation material of solid statelaser.Y
2O
3The luminescent materials, fluorescent material, superconducting material etc. of other materials preparation of mixing are widely used in numerous areas.
Preparation Y
2O
3The preparation method of matrix luminescent material mainly is divided into solid phase method, liquid phase method.Wherein the implementing method of solid phase method is, be with oxalic acid hydrate yttrium and oxalic acid europium, the ammoniacal liquor of sneaking into certain volume mixes by a certain percentage, add an amount of agate ball then and put into the agate jar, place on the planetary mills, ball milling method and required time of speed ball milling with setting obtain the ball-milling reaction product, vacuum-drying then, and the presoma that obtains is at last calcined at a certain temperature and is obtained oxide powder.The required calcination temperature of this method is more than 1000 ℃, calcination after product particle diameter is bigger, needs ball mill pulverizing again to satisfy the modern crafts needs to reduce particle diameter, and ball milling can make the crystal habit of fluorescent material destroy, cause luminous intensity to descend significantly, have a strong impact on the use properties of fluorescent material.
Liquid phase method is to select one or more soluble metal salts, is mixed with solution by the composition metering of prepared material, makes each element become ionic state, selects a kind of suitable precipitation agent again, adopts method synthetic powders such as heating, evaporation, distillation, hydrolysis.
During microwave hydrothermal is synthetic, the essence of microwave action is that hertzian wave is to the effect of charged particle, be that material adds polarizability vector that the polarization of interior media under the electromagnetic field effect produces outside and lags behind electric field change and cause producing with the electric current of electric field homophase, caused the in-fighting of material, therefore microwave action and its frequency and power density are closely related, also closely related with the dielectric properties of medium.Why microwave can be used in the field of chemical synthesis, is because of having various polar molecules such as water, alcohols, carboxylic-acid in the related reactant of chemical reaction.Under normal conditions, these molecules are rambling kinestate, when microwave oven magnetic gives off the microwave of very high frequency, the micro-wave energy field is with negative polarity under the speed conversion constantly of per second twenty or thirty hundred million times, great change has taken place in molecular motion, molecular arrangement is got up and high-speed motion, produces to collide mutually, rub, push, thereby makes kinetic energy-micro-wave energy be converted into heat energy.From reactant solvents inside, itself does not need the medium that conduct heat in this kind energy on the mountain, and by convection current, sample temperature just can very fast rising, thus can be comprehensively, fast, reacting by heating thing solvent equably, reach the purpose that improves chemical reaction rate.Microwave also has non-thermal effect except heat effect is arranged.Can heat selectively, thereby make chemical reaction have certain selectivity.Conclusion is got up, and under the hydrothermal condition there is the effect of water: (1) is sometimes as the chemical composition react with; (2) promotor of reaction and rearrangement; (3) play pressure and transmit media; (4) play solvent action; (5) play low melting point; (6) improve solubility of substances.
People such as Liu Guixia (Chinese Journal of Inorganic Chemistry, 2006,22 (8): 1535～1539) synthesized the yttrium oxide spheroidal particle that europium mixes with three step hydro-thermals: at first form the hydrogen-carbonate colloidal oxide solution, hydro-thermal carbonate synthesis salt precursor body is calcined at last and is obtained oxide compound then.The concrete implementation step of this method is: the first, yttrium oxide (99.99%) and europium sesquioxide (99.99%) are dissolved in a small amount of nitric acid, and evaporation drying adds a certain amount of water preparation Yttrium trinitrate and europium nitrate solution then, forms the Y (NO of 0.05mol/L
3)
3Eu (NO with 0.01mol/L
3)
3Again with the (NH of 2mol/L
3)
2CO mixes, and the mixing solutions of gained is incubated 2 hours 80 ℃ cover tightly in the beaker, forms the colloid thing; Second autoclave that jelly is put into 50ml is put into baking oven 120 ℃ of insulations 18 hours; The 3rd with resulting product filtration, 80 ℃ of oven dry down, the presoma of gained is calcined 2 hours down at 850 ℃ again, makes required oxide compound.This method more complicated, required time is long, and the size of the yttrium oxide that makes (europium) nano particle is bigger, and is dispersed poor, and big or small inhomogeneous agglomeration is serious.Therefore more difficult control pattern during a large amount of synthesizing is not suitable for industrialization.
Summary of the invention
The objective of the invention is in order to improve the deficiency of existing synthetic method, and provide a kind of microwave irradiation preparation (Y, Gd)
2O
3: the method for Eu luminescent material, the material purity height of this method preparation, even particle size distribution and control the granularity pattern easily satisfies modern industry and scientific technological advance to the performance demands of material.
Technical scheme of the present invention is: and the microwave irradiation preparation (Y, Gd)
2O
3: the method for Eu luminescent material, concrete steps are as follows:
A. in reaction vessel, dispose the Re of 5～30mM
3+Rare earths salt, wherein Re is Y, Gd and Eu, Y: Gd: the mol ratio of Eu element is 8～19: 3～12: 1, the volume ratio in ethylene glycol (EG) and rare earths salt is that 1～10: 1 ratio adds ethylene glycol (EG) then; Add oxalic acid again, and stirring makes the oxalic acid dissolving;
B. the above-mentioned reaction raw materials solution for preparing is put in the microwave reactor microwave radiation and reacts, and with sedimentation and filtration, washing, oven dry, is put into then and is warmed up to 600～1000 ℃ of calcining 1～3h in the retort furnace after reaction finishes, obtain (Y, Gd)
2O
3: the Eu luminescent material.
The add-on of preferred oxalic acid is that the mol ratio of oxalic acid and rare earth element Re 3+ is 3～20: 1.Preferred described rare-earth salts is rare nitrate of going up.
The power of preferred above-mentioned microwave reactor is 15～50W, and the reaction times is 5～60min.
The present invention prepared (Y, Gd)
2O
3: the Eu luminescent material is micron film, micron bar or nano rod, and pattern depends on the volume of EG and rare earths salt.
Beneficial effect:
By this invention prepared (Y, Gd)
2O
3: the Eu luminescent material is little or nanometer sheet, is nano rod perhaps, has big or small homogeneous, pattern and adjustable size, and the present invention also to have the reaction times short, but advantages such as small-scale production.
Description of drawings
Fig. 1 example 1 gained (Y, Gd)
2O
3: the X-ray diffractogram of Eu powder;
Fig. 2 example 1 gained (Y, Gd)
2O
3: the scanning electron microscope secondary electron image of Eu powder;
Fig. 3 example 1 gained (Y, Gd)
2O
3: the emission of Eu powder and excite (illustration) spectrogram;
Fig. 4 example 2 gained (Y, Gd)
2O
3: the scanning electron microscope secondary electron image of Eu powder;
Fig. 5 example 3 gained (Y, Gd)
2O
3: the scanning electron microscope secondary electron image of Eu powder.
Embodiment
Embodiment 1:
Re (the NO of configuration 10mM
3)
3(Re=Y, Gd, Eu; Element mol ratio Y: rare earths salt 30ml Gd: Eu=14.25: 4.75: 1), add 30ml ethylene glycol, and then the oxalic acid stirring and dissolving that adds, the concentration of last oxalic acid is 60mM.It is 15W reaction 30min that the above-mentioned reaction raw materials for preparing is put into the inside, microwave reaction chamber control microwave power.The precipitation that obtains distilled water wash 5 times are put into baking oven and are dried by the fire 6h down at 80 ℃, and then calcine 2h with retort furnace at 700 ℃, obtain (Y, Gd)
2O
3: the powder of Eu.
The powder art of gained is a cube phase structure (see figure 1) through X-ray diffraction analysis, and as can be seen from the figure, the product of gained is and a cube phase Y
2O
3(JCPDS No.83-0927) is corresponding.
Get a little (Y, Gd)
2O
3: the Eu powder places 10ml ethanol, ultra-sonic dispersion 2min in Ultrasonic Cleaners.Drip on copper sample table, with scanning electron microscopic observation granule-morphology and granular size (see figure 2) thereof, pattern is that the length of side is 5～10 μ m micron side's sheets uniformly.
The powder art excites and the emmission spectrum (see figure 3) through testing it with fluorescence spectrophotometer behind the briquetting, and as we can see from the figure, under the 611nm emission, the excitation spectrum main peak is 238nm; Excite down at 238nm, emission peak is 611nm.
Embodiment 2:
Re (the NO of configuration 20mM
3)
3(Re=Y, Gd, Eu; Element mol ratio Y: rare earths salt 20ml Gd: Eu=9: 10: 1), add 60ml ethylene glycol, and then the oxalic acid stirring and dissolving that adds, the concentration of last oxalic acid is 75mM.The microwave power that uses is 30W, and is identical in other step and the example 1, obtain (Y, Gd)
2O
3: the powder of Eu is 15 μ m with scanning electron microscopic observation (Fig. 4) for length, and width is about the micron bar of 100nm.
Embodiment 3:
Re (the NO of configuration 30mM
3)
3(Re=Y, Gd, Eu; Element mol ratio Y: rare earths salt 10ml Gd: Eu=16: 3: 1), add 50ml ethylene glycol, and then the oxalic acid stirring and dissolving that adds, the concentration of oxalic acid is 20mM.Be 1000 ℃ of down calcining 1h in temperature, identical in other step and the example 1, obtain (Y, Gd)
2O
3: the powder of Eu is 2 μ m with scanning electron microscopic observation (Fig. 5), pattern for length, and width is about the nano rod of 20nm.
Claims (2)
1. microwave irradiation preparation (Y, Gd)
2O
3: the method for Eu luminescent material, concrete steps are as follows:
A. in reaction vessel, dispose the Re of 5 ~ 30 mM
3+Rare earths salt, wherein Re is Y, Gd and Eu, the mol ratio of Y:Gd:Eu element is 8 ~ 19:3 ~ 12:1, and then is that 1 ~ 10:1 ratio adds ethylene glycol in the volume ratio of ethylene glycol and rare earths salt, adds oxalic acid again, and stirs and make the oxalic acid dissolving; The add-on of its mesoxalic acid is oxalic acid and rare earth element Re
3+Mol ratio be 3 ~ 20:1;
B. the above-mentioned reaction raw materials solution for preparing is put into microwave radiation reaction 5 ~ 60 min in the microwave reactor that power is 15 ~ 50 W, after reaction finishes with sedimentation and filtration, washing, oven dry, be put into then and be warmed up to 600 ~ 1000 ℃ of calcining 1 ~ 3 h in the retort furnace, obtain (Y, Gd)
2O
3: the Eu luminescent material.
2. method according to claim 1 is characterized in that described rare-earth salts is rare earth nitrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010500528.7A CN101984015B (en) | 2010-09-29 | 2010-09-29 | Preparation of (Y) by microwave radiation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010500528.7A CN101984015B (en) | 2010-09-29 | 2010-09-29 | Preparation of (Y) by microwave radiation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101984015A CN101984015A (en) | 2011-03-09 |
| CN101984015B true CN101984015B (en) | 2013-07-17 |
Family
ID=43641184
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010500528.7A Expired - Fee Related CN101984015B (en) | 2010-09-29 | 2010-09-29 | Preparation of (Y) by microwave radiation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101984015B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106635005A (en) * | 2016-06-13 | 2017-05-10 | 郑甘裕 | Europium-doped gadolinium oxide luminescent material as well as preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803973A (en) * | 2006-01-20 | 2006-07-19 | 哈尔滨工业大学 | Method for preparing red nano fluoresent powder of rare earth |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1230490C (en) * | 2003-09-05 | 2005-12-07 | 中国科学院上海硅酸盐研究所 | Method for preparing rare earth oxide group nanometer luminescent powder |
| CN1240809C (en) * | 2004-04-19 | 2006-02-08 | 北京工业大学 | Method for preparing nano luminescent powder made from yttrium europium vanadate |
| KR101458026B1 (en) * | 2007-11-29 | 2014-11-06 | 삼성디스플레이 주식회사 | A rare earth nano phosphor and synthetic method thereof |
| KR20100058299A (en) * | 2008-11-24 | 2010-06-03 | 삼성에스디아이 주식회사 | Method for preparing oxide based nanophosphors |
-
2010
- 2010-09-29 CN CN201010500528.7A patent/CN101984015B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803973A (en) * | 2006-01-20 | 2006-07-19 | 哈尔滨工业大学 | Method for preparing red nano fluoresent powder of rare earth |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101984015A (en) | 2011-03-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Som et al. | Synthesis of strong red emitting Y 2 O 3: Eu 3+ phosphor by potential chemical routes: comparative investigations on the structural evolutions, photometric properties and Judd–Ofelt analysis | |
| CA2942322C (en) | Method for the production of multiphase composite materials using microwave plasma process | |
| Quan et al. | Synthesis and characterization of spherical ZrO2: Eu3+ phosphors by spray pyrolysis process | |
| Boyer et al. | Structural and optical characterizations of YAG: Eu3+ elaborated by the sol–gel process | |
| Aytimur et al. | Magnesia stabilized zirconia doped with boron, ceria and gadolinia | |
| Elsagh et al. | Characterization of SrAl 2 O 4: Eu 2+, Dy 3+ phosphor nano-powders produced by microwave synthesis route | |
| Wang et al. | Multiple irradiation triggered the formation of luminescent LaVO4: Ln 3+ nanorods and in cellulose gels | |
| Paulraj et al. | Photoluminescence efficiencies of nanocrystalline versus bulk Y2O3: Eu phosphor—revisited | |
| Zalga et al. | On the sol–gel preparation of different tungstates and molybdates | |
| Cheng et al. | Sol-gel synthesis and photoluminescence characterization of La 2 Ti 2 O 7: Eu 3+ nanocrystals | |
| Lian et al. | Synthesis and optical properties of (Gd1− x, Eux) 2O2SO4 nano-phosphors by a novel co-precipitation method | |
| Yan et al. | Preparation of YAG: Ce3+ phosphor by sol-gel low temperature combustion method and its luminescent properties | |
| Wang et al. | Photoluminescence of (La, Eu) 2 O 2 SO 4 red-emitting phosphors derived from layered hydroxide | |
| Chung et al. | Preparation and Mechanism of Nest‐Like YBO3: Tb3+ Phosphors Synthesized Via the Microemulsion‐Mediated Hydrothermal Process | |
| CN101984015B (en) | Preparation of (Y) by microwave radiation | |
| Wu et al. | Photoluminescence intensity of YxGd1− xVO4: Eu3+ dependence on hydrothermal synthesis time and variable ratio of Y/Gd | |
| Zhai et al. | Hydrothermal synthesis, characterization and luminescence properties of orange–red-emitting phosphors SnO 2: Eu | |
| CN100497518C (en) | Process for preparing aluminate luminescent materials | |
| Jiu et al. | Preparation and luminescent properties of hollow Y2O3: Tb3+ microspheres | |
| Wu et al. | Influence of praseodymium doping concentration on the structural and optical properties of strontium molybdate crystals | |
| Yang et al. | Synthesis and luminescence properties of a novel Eu3+-doped γ-LiAlO2 phosphor | |
| Min et al. | Preparation and upconversion luminescence of YAG (Y3Al5O12): Yb3+, Ho3+ nanocrystals | |
| Lee et al. | Thermal-shock-assisted solid-state process for the production of BaMgAl10O17: Eu phosphor | |
| Qi et al. | Facile hydrothermal synthesis for size-controlled YVO 4: Eu 3+ micro/nanosheets and its luminescence properties | |
| CN101429431B (en) | Microwave excitation low-temperature liquid-phase combustion synthesis process for producing rare earth activated nano-self-luminescence powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130717 Termination date: 20200929 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |