CN1844305A - Process for preparing yttrium aluminum garnet - Google Patents
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- CN1844305A CN1844305A CN 200610076992 CN200610076992A CN1844305A CN 1844305 A CN1844305 A CN 1844305A CN 200610076992 CN200610076992 CN 200610076992 CN 200610076992 A CN200610076992 A CN 200610076992A CN 1844305 A CN1844305 A CN 1844305A
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Abstract
A method for preparation of yttrium aluminium garnet relates to a preparation technology for fluorescent powder, especially to a preparation technology for yttrium aluminium garnet activated by europium, which provides a method for preparation of yttrium aluminium garnet which adopts macromolecular network gelatinization, does not need to mill, without birdnesting or small birdnesting, can be directly used in packing and can exert its optical performance with a high limit, and is no environmental contamination and can save the cost. The method consists of adding aluminum nitrate, citric acid, yttrium nitrate and europium nitrate into a container, adding deionized water, adjusting pH value to neutral with ammonial solution,with a thermostatic bath, adding acrylamide and N,N- methylene biacrylamide, having a thermostatic bath until acrylamide and N,N- methylene biacrylamide dissolve, adding tetraethylethylene diamine and hydrogen dioxide solution to initiate the polymerization, obtaining the YAG macromolecular network gel by a thermostatic bath, then removing the moisture and the organic matter by heat treatment, by heat decomposition, decomposing concentrated nitric acid to corresponding oxidate,obtaining the powders by pre-calcination, then by high-temperature heat treatment, performing degree of crystallization to obtain YAG powders.
Description
Technical field
The present invention relates to a kind of preparation technology of fluorescent material, especially relate to the preparation technology of a kind of europkium-activated yttrium aluminum garnet (YAG:Eu).
Background technology
Yttrium aluminum garnet (Yttrium Aluminum Garnet writes a Chinese character in simplified form YAG) is the crystal that a kind of hardness is very big, fusing point is very high, has isotropy on the optics, thereby is a kind of monocrystal material of excellent property.It also has good thermal conductivity, physical strength and good chemical property in addition, has obtained widespread usage as a kind of good stupalith.A kind of especially effective luminescent material of YAG particularly is the mixed luminescent material of rare earth ion of matrix with YAG, has obtained people's common concern with its special superiority.Because the radius and the Y of trivalent rare earth ions
3+Close, be easy to mix and replace Y
3+Ion and obtain the luminous of different colours, thereby be widely used as laser and luminous substrate material and nose cone window material.The research of relevant YAG is comparative maturity, also has much about the preparation technology's of YAG patent and document, and the preparation method of bibliographical information YAG is a lot of usually, and wherein more common having is following several:
(1) high temperature solid-state method (1.IKESUE A, KAMATA K, Role of Si on Nd solid-solution of YAGceramics[J], journal of the Ceramic Society of Japan, 1995,103 (5): 489-493; 2. Xu Xu Rong, Su Mian once, luminescence is in luminescent material, Beijing: Chemical Industry Press): solid phase method is one of method that develops the earliest, also be the most general method in the present industrial production, this method adopts high temperature solid state reaction, firing temperature height (being about 1600 ℃), synthesis cycle is long, powder hardness and particle after burning till are big, and the aftertreatment difficulty needs through ball milling, destroy crystalline form (Liu Deli easily, the production technique of yttrium aluminum garnet transparent ceramic and performance [J], ceramic engineering, 1999,33 (1): 24-25), cause luminous intensity to descend.
(2) sol-gel processing (Ruan Shenkang, Zhou Jianguo dote on the people, Duan Jiefei, Yang Xianbi, Su Mianceng is with the synthetic Y of sol-gel method
3Al
5O
12: the Eu phosphorescent substance, artificial lens journal [J], 1997,26:413): with the alkoxide compound is raw material, as methyl cellosolve yttrium (europium), isobutanol aluminum solution is converted into gel through reaction process such as hydrolysis, polycondensations by colloidal sol.Gel is dried at a lower temperature, and pre-burning is ground after for some time, and calcination under differing temps respectively obtains phosphorescent substance at last again.
(3) (Zhao Zengqin etc. are with the synthetic Y of 3 kinds of methods for Zhou Yonghui, Lin Jun for citric acid-gel method
3Al
5O
12: Re
3+(Re=Eu, Dy) comparative study of luminescent powder [J], China's rare-earth journal, 2001,19 (6): 575-578): each self-corresponding metal-nitrate solutions is mixed by stoichiometric ratio, again above mixing liquid is joined in the citric acid, and satisfy the total amount of substance of metal ion and the citric acid amount of substance reaches certain proportion.Above-mentioned mixed solution is heated for some time at a certain temperature, become colloidal sol, more this colloidal sol insulation for some time is become Gelatin powder, after high-temperature heat treatment obtains the YAG powder, the powder particle that obtains is little, but luminous intensity is not high.
(4) (Zhao Zengqin etc. are with the synthetic Y of 3 kinds of methods for Zhou Yonghui, Lin Jun for coprecipitation method
3Al
5O
12: Re
3+(Re=Eu, Dy) comparative study of luminescent powder [J], China's rare-earth journal, 2001,19 (6): 575-578): with Yttrium trinitrate or Yttrium trichloride is raw material, be dissolved in the deionized water, add the coprecipitate of precipitation agents such as ammoniacal liquor (or anti-adding) formation aluminium hydroxide and yttrium hydroxide again, through multiple times of filtration, cleaning, dry back is in high-temperature calcination, finish the powder crystallization process, obtain the high pure and ultra-fine powder after further pulverizing.This method can reach the metal ion ratio of final product by the control that GOLD FROM PLATING SOLUTION is belonged to ionic concn, thereby makes various compositions even, and post precipitation carries out thermolysis again and obtains the compound metal oxide powder.Compare with solid state reaction, this method can make purity height, chemical uniformity is good, composition is controlled powder; But multiple times of filtration, cleaning make technological process numerous and diverse, and manufacturing cost height, particularly water loss are very big, and cause environmental pollution serious.
(5) polymer-network gel method (1.Qiang Li, Lian Gao, Dongsheng Yan, The crystal structure andspectra of nano-scale YAG:Ce
3+[J], Materials Chemistry and Physics, 2000 (64): 41-44; 2. Li Qiang, high Lian, Yan Dongsheng, YAG:Ce
3+The preparation of micro mist and spectrum property, Journal of Inorganic Materials, 1997,12 (4): 575-578; 3.Hongwu Zhang, Xiaoyan Fu, Shuyun Niu, Gongquan Sun, Qin Xin, Low temperature synthesisof nanocrystalline YVO4:Eu via polyacrylamide gel method[J], Journal of Solid State Chemistry, 2004,177:2649-2654): at Y
3+, Al
3+, Ce
3+Add acrylamide monomer in the corresponding nitrate aqueous solution, N,N methylene bis acrylamide lattice reagent and ammonium persulfate initiator, polymerization obtains gel under constant temperature.Then, the gained gel is obtained product with high-temperature heat treatment.
Raw material segregation and speed of response were slow when above-mentioned technology had overcome general solid reaction process synthetic powder, and it is serious to reunite, the crystalline phase havoc causes degradation problem under the luminous efficiency after pulverizing, common sol-gel method is except productive rate is very low, this method can also avoid solving the problem of secondary agglomeration, the technology of having avoided the cleaning of chemical coprecipitation multiple times of filtration to bring again is numerous and diverse, a large amount of water consumptions, easily cause problems such as environmental pollution, it is few to have the facility investment expense, production technique is simplified, production cost is low, basic non-environmental-pollution, advantages such as good product quality, especially be fit to carry out industrialized production, this kind method can successful industrialization, has successfully used this kind method scale operation aluminum oxide as the mining industry that gets the better of in Fujian.
Publication number provides a kind of three primary colors fluorescent powder and synthetic method of stimulated by purple-light LED for 1397625 application for a patent for invention, and what adopted is that high temperature solid state reaction prepares YAG:Eu.
Publication number adopts above-mentioned citric acid-gel method of mentioning to prepare YAG:Eu for 1398948 application for a patent for invention provides a kind of preparation method of high-luminance pink LED.
Publication number provides a kind of preparation method of trivalent europium ion activated spherical luminescent material for 1468935 application for a patent for invention, employing be that spray drying unit prepares YAG:Eu.
Publication number prepares the method for white-light emitting diode for 1558453 application for a patent for invention provides a kind of diode wafer that adopts blue light-emitting or purple light, what adopt is that sol-gel processing prepares YAG:Eu, use yttium acetate, the acetate europium aqueous solution, add the isobutanol aluminum aqueous hydrolysis and form gel, all be different from our polymer-network gel method from the former preparation technology of expecting.
Publication number provides a kind of multi-crest fluorescence inorganic matter of semiconductor light source for 1605613 application for a patent for invention, though mention YAG:Eu, basic no preparation technology.
Wait " the YAG:Ce that was published in " Journal of Inorganic Materials " in 1997 Li Qiang
3+The preparation of micro mist and spectrum property " in set forth the method that the high-molecular gel grid method prepares YAG:Ce, its adulterated ion is Ce, but the optimum value of not mentioned doping does not have clear conclusions to variation of temperature.
Summary of the invention
The objective of the invention is to bring into play the optical property of YAG:Eu and the problem of industrialization difficulty fully at existing product, a kind of employing polymer-network gel method is provided, the YAG:Eu that produces need not be through the process of ball milling, being that the process high-temperature heat treatment is come out do not have the powder of reuniting or seldom reuniting, can be directly used in encapsulation, can bring into play the optical property of YAG:Eu to greatest extent, and the problem of environmental pollution that can avoid other liquid phase methods to bring, save the process for preparing yttrium aluminum garnet of cost simultaneously.
Its general formula of yttrium aluminum garnet of the present invention is (Y[1-x] Eu[x]) [3] Al[5] O[12], 0＜x＜0.1 wherein.
Step of the present invention is:
1) take by weighing raw material:
Content by each raw material of mass ratio is: aluminum nitrate 100, citric acid 188.77～404.42, Yttrium trinitrate 55.06～61.31, europium nitrate 0～7.14, acrylamide 103.63～414.51, N, N-methylene-bisacrylamide 8.63～41.45, tetraethylethylenediamine 0.80～5.00 and massfraction are 3% aqueous hydrogen peroxide solution 26.60～170.00, deionized water 500.00～3000.00;
2) polyacrylamide-gel of preparation YAG:
Raw material aluminum nitrate, citric acid, Yttrium trinitrate and europium nitrate are added in the container, add deionized water and stirring to dissolving fully, regulate the pH value to neutrality with ammoniacal liquor, 70～90 ℃ of following waters bath with thermostatic control, add acrylamide and N,N methylene bis acrylamide again, continue water bath with thermostatic control to acrylamide and N, N-methylene-bis acryloyl dissolves fully, adds the aqueous solution initiated polymerization of tetraethylethylenediamine and hydrogen peroxide, continues water bath with thermostatic control to the polyacrylamide-gel that obtains YAG;
3) high-temperature heat treatment:
Will be by step 2) polyacrylamide-gel of the YAG that obtains removes wherein moisture and organism through 600～700 ℃ thermal treatment earlier, and the nitrate thermolysis of inciting somebody to action wherein is corresponding oxide compound, obtain the powder that pre-burning is handled, carry out crystallization through 850～1550 ℃ of high-temperature heat treatment again, get the YAG powder.
The present invention adopts polymer-network gel method to prepare YAG:Eu, to replace traditional high temperature solid-state method and liquid phase method.The present invention comprises the preparation from gel, to the high-temperature heat treatment of fluorescent material, forms not have and reunites or low fluorescent powder of reuniting.This fluorescent powder is to be matrix with YAG, mixes, and forms the energy-conservation fluorescent powder with good luminous usefulness.Wait the human similar approach to be Li Qiang simultaneously, preparation technology's refinement of the YAG:Ce of single doped Ce is extended to other ion dopings, as: YAG:Eu, dopant ion are Eu, and the system that the present invention sets forth is different from the systems that the people reported such as Li Qiang.
The used initiator of the present invention is a hydrogen peroxide, is different from the used ammonium persulphates of people such as Li Qiang, has avoided possibility because the residual YAG matrix that causes of sulphur is damaged, and causes the decline of luminous efficiency; The gelation time 2h that the people adopted such as Li Qiang can be shortened to about 10min simultaneously, more help industrialization.In addition existing YAG:Eu preparation technology's post-processed is improved, can directly be obtained the suitable particles degree or even nano level YAG:Eu powder, overcome the agglomeration traits of YAG:Eu powder, avoided the trouble of post-processed.
This shows that the present invention has greatly saved the energy, bring into play the optical property of YAG to greatest extent, produce higher-quality YAG:Eu powder.
Description of drawings
Fig. 1 is the standard x RD collection of illustrative plates of YAG.
Fig. 2 is the XRD figure spectrum of 850 ℃ YAG:Eu for calcining temperature.
Fig. 3 is the XRD figure spectrum of 1550 ℃ YAG:Eu for calcining temperature.
Fig. 4 is the laser spectrum of YAG:Eu.
Fig. 5 is the emmission spectrum of YAG:Eu.
Fig. 6 is laser and the emmission spectrum of YAG:Eu.
In Fig. 1～3, X-coordinate diffraction angle 2 θ (°).
In Fig. 4～6, X-coordinate is wavelength X (nm).
Embodiment
Following examples will the present invention is further illustrated in conjunction with the accompanying drawings.
1, pure YAG
61.31g Yttrium trinitrate, 100g aluminum nitrate and 269.60g citric acid are joined in the 860g deionized water, stirring and dissolving, and regulate the pH value to pH=7 with ammoniacal liquor.Behind 70 ℃ of water-bath 10min, add 207.25g acrylamide and 17.27gN, the N-methylene-bisacrylamide, adding 0.80g tetraethylethylenediamine and 26.60g massfraction are 3% aqueous hydrogen peroxide solution behind 75 ℃ of water bath heat preservation 20min, and 75 ℃ of water bath heat preservations are to the gel that is converted into white.The prepared gel in front is incubated 3h down at 700 ℃, moisture and organism all can have been burnt, obtain the powder of white.With the white powder of gained 850 ℃ down insulation 1h get final product the YAG powder of pure phase, 1550 ℃ down insulation 3h can obtain YAG nanometer powder fine crystalline phase and good luminous performance.
Identify through Jade software, can determine that its principal crystalline phase is YAG, spectroscopic identification and document (Wei-Tse Hsu, Wei-HongWu, Chung-Hsin Lu, Synthesis and luminescent properties ofnano-sized Y
3Al
5O
12: Eu
3+Phosphors, Materials Science and Engineering, 2003 (B 104): 40-44) coupling.
2, the YAG:Eu of 3%Eu doping
58.79g Yttrium trinitrate, 100g aluminum nitrate, 179.73g citric acid and 2.85g europium nitrate are joined in the 3000g deionized water, stirring and dissolving, and regulate the pH value to pH=7 with ammoniacal liquor.Behind 90 ℃ of water-bath 10min, add 414.51g acrylamide and 41.45g N, the N-methylene-bisacrylamide, behind 90 ℃ of water bath heat preservation 20min, add 4.14g tetraethylethylenediamine and 138g massfraction and be 3% hydrogen peroxide solution, at 90 ℃ of water bath heat preservations as for the gel that is converted into white.The prepared gel in front is incubated 3h down at 600 ℃, moisture and organism all can have been burnt, obtain the powder of white.With the white powder of gained 850 ℃ down insulation 1h get final product the YAG:Eu nanometer powder of pure phase, 1550 ℃ down insulation 3h can obtain YAG:Eu powder fine crystalline phase and good luminous performance.
Identify through Jade software, can determine that its principal crystalline phase is YAG, its spectroscopic identification and document (Wei-Tse Hsu, Wei-Hong Wu, Chung-Hsin Lu, Synthesis and luminescent properties of nano-sizedY
3Al
5O
12: Eu
3+Phosphors, Materials Science and Engineering, 2003 (B104): 40-44) coupling.
3, the YAG:Eu of 5%Eu doping
58.20g Yttrium trinitrate, 100g aluminum nitrate, 188.77g citric acid and 3.58g europium nitrate are joined in the 1000g deionized water, stirring and dissolving, and regulate the pH value to pH=7 with ammoniacal liquor, behind 75 ℃ of water-bath 10min, add 259.07 acrylamides and 17.27g N, the N-methylene-bisacrylamide, behind 75 ℃ of water bath heat preservation 20min, add 2.59 tetraethylethylenediamines and 86.30g massfraction and be 3% hydrogen peroxide solution, at 75 ℃ of water bath heat preservations to the gel that is converted into white.The prepared gel in front is incubated 3h down at 700 ℃, moisture and organism all can have been burnt, obtain the powder of white.With the white powder of gained 850 ℃ down insulation 1h get final product the YAG:Eu nanometer powder of pure phase, 1550 ℃ down insulation 2h can obtain YAG:Eu powder fine crystalline phase and good luminous performance.
Identify through Jade software, can determine that its principal crystalline phase is YAG, its spectroscopic identification and document (Wei-Tse Hsu, Wei-Hong Wu, Chung-Hsin Lu, Synthesis and luminescent properties of nano-sizedY
3Al
5O
12: Eu
3+Phosphors, Materials Science and Engineering, 2003 (B104): 40-44) coupling.
4, the YAG:Eu of 6%Eu doping
57.58g Yttrium trinitrate, 100g aluminum nitrate, 269.60g citric acid and 4.28g europium nitrate are joined in the 500g deionized water, stirring and dissolving, and regulate the pH value to pH=7 with ammoniacal liquor, behind 90 ℃ of water-bath 10min, add 103.63g acrylamide and 8.63gN, the N-methylene-bisacrylamide, behind 90 ℃ of water bath heat preservation 20min, add 0.80g tetraethylethylenediamine and 26.60g massfraction and be 3% hydrogen peroxide solution, at 90 ℃ of water bath heat preservations to the gel that is converted into white.The prepared gel in front is incubated 3h down at 600 ℃, moisture and organism all can have been burnt, obtain the powder of white.With the white powder of gained 850 ℃ down insulation 1h get final product the YAG:Eu nanometer powder of pure phase, 1550 ℃ down insulation 3h can obtain YAG:Eu powder fine crystalline phase and good luminous performance.
Identify through Jade software, can determine that its principal crystalline phase is YAG, its spectroscopic identification and document (Wei-Tse Hsu, Wei-Hong Wu, Chung-Hsin Lu, Synthesis and luminescent properties of nano-sizedY
3Al
5O
12: Eu
3+Phosphors, Materials Science and Engineering, 2003 (B104): 40-44) coupling.
5, the YAG:Eu of 8%Eu doping
56.48g Yttrium trinitrate, 100g aluminum nitrate, 269.60g citric acid and 5.70g europium nitrate are joined in the 2000g deionized water, stirring and dissolving, and regulate the pH value to pH=7 with ammoniacal liquor, behind 90 ℃ of water-bath 10min, add 207.25g acrylamide and 17.27g N, the N-methylene-bisacrylamide, behind 90 ℃ of water bath heat preservation 20min, add 2.20g tetraethylethylenediamine and 75.90g massfraction and be 3% hydrogen peroxide solution, at 90 ℃ of water bath heat preservations to the gel that is converted into white.The prepared gel in front is incubated 3h down at 600 ℃, moisture and organism all can have been burnt, obtain the powder of white.With the white powder of gained 850 ℃ down insulation 1h get final product the YAG:Eu nanometer powder of pure phase, 1550 ℃ down insulation 3h can obtain YAG:Eu powder fine crystalline phase and good luminous performance.Identify through Jade software, can determine that its principal crystalline phase is YAG, spectroscopic identification and document (Wei-Tse Hsu, Wei-Hong Wu, Chung-Hsin Lu, Synthesis and luminescentproperties of nano-sized Y
3Al
5O
12: Eu
3+Phosphors, Materials Science and Engineering, 2003 (B104): 40-44) coupling.
6, the YAG:Eu of 10%Eu doping
55.06g Yttrium trinitrate, 100g aluminum nitrate, 404.42g citric acid and 7.14g europium nitrate are joined in the 2500g deionized water, stirring and dissolving, and regulate the pH value to pH=7 with ammoniacal liquor, behind 90 ℃ of water-bath 10min, add 207.25 acrylamides and 17.27g N, the N-methylene-bisacrylamide, behind 90 ℃ of water bath heat preservation 20min, add 2.00g tetraethylethylenediamine and 66.70g massfraction and be 3% hydrogen peroxide solution, 90 ℃ of water-baths to the gel that is converted into white.The prepared gel in front is incubated 3h down at 700 ℃, moisture and organism all can have been burnt, obtain the powder of white.With the white powder of gained 850 ℃ down insulation 1h get final product the YAG:Eu nanometer powder of pure phase, 1550 ℃ down insulation 4h can obtain YAG:Eu powder fine crystalline phase and good luminous performance.
Identify through Jade software, can determine that its principal crystalline phase is YAG, spectroscopic identification and document (Wei-Tse Hsu, Wei-HongWu, Chung-Hsin Lu, Synthesis and luminescent properties of nano-sized Y
3Al
5O
12: Eu
3+Phosphors, Materials Science and Engineering, 2003 (B 104): 40-44) coupling.
Through XRD analysis, identify that with Jade software can determine that its principal crystalline phase is YAG, for details, see the appendix 1 and Fig. 1～3 for its analytical data; Spectroscopic identification and document (Wei-Tse Hsu, Wei-Hong Wu, Chung-Hsin Lu, Synthesis andluminescent properties of nano-sized Y
3Al
5O
12: Eu
3+Phosphors, Materials Science andEngineering, 2003 (B104): 40-44) coupling, see Fig. 3～6 for details.
The comparison of appendix 1 YAG:Eu and pure YAG standard x RD collection of illustrative plates
Card numbering: 33-0040
Diffraction angle spacing peak by force than diffraction angle spacing peak by force than diffraction angular difference
2 θ (°) the routine I of d (nm) (%) crystalline phase 2 θ (°) the routine I of d (nm) (%) value 2 θ (°)
18.087 49.006 48.6A15Y3O12 18.071 49.050 27 -0.016
20.926 42.416 19.6Al5Y3O12 20.899 42.470 7 -0.027
27.809 32.055 30Al5Y3O12 27.769 32.100 19 -0.040
29.749 30.008 35.6Al5Y3O12 29.736 30.020 27 -0.013
33.318 26.869 100Al5Y3O12 33.317 26.870 100 -0.001
36.549 24.565 28.2Al5Y3O12 36.618 24.520 20 0.069
38.148 23.572 15Al5Y3O12 38.184 23.550 6 0.036
41.121 21.933 27.4Al5Y3O12 41.147 21.920 23 0.026
42.583 21.213 13.2Al5Y3O12 42.569 21.220 5 -0.014
46.511 19.509 27.3Al5Y3O12 46.600 19.474 26 0.089
52.715 17.350 20.2Al5Y3O12 52.780 17.330 17 0.065
55.062 16.665 29.8Al5Y3O12 55.107 16.652 31 0.045
56.166 16.363 14Al5Y3O12 56.259 16.338 9 0.093
57.289 16.069 27.7Al5Y3O12 57.377 16.046 28 0.088
60.580 15.272 10.2Al5Y3O12 60.689 15.247 4 0.109
61.692 15.023 14.8Al5Y3O12 61.770 15.006 10 0.078
69.970 13.434 10.7Al5Y3O12 70.038 13.423 7 0.068
71.843 13.130 16.2Al5Y3O12 72.018 13.102 17 0.175
73.085 12.937 8.5Al5Y3O12 73.005 12.949 2 -0.080
73.953 12.806 9.7Al5Y3O12 73.995 12.800 6 0.042
76.890 12.389 7.8Al5Y3O12 76.895 12.388 2 0.005
81.616 11.786 7.3Al5Y3O12 81.704 11.776 2 0.088
84.556 11.450 8Al5Y3O12 84.548 11.451 3 -0.008
87.294 11.160 13Al5Y3O12 87.383 11.151 14 0.089
89.095 10.981 8.9Al5Y3O12 89.265 10.964 6 0.171
Claims (1)
1. process for preparing yttrium aluminum garnet is characterized in that its general formula of described yttrium aluminum garnet is:
(Y[1-x] Eu[x]) [3] Al[5] O[12], 0＜x＜0.1 wherein;
The steps include:
1) take by weighing raw material:
Content by each raw material of mass ratio is: aluminum nitrate 100, citric acid 188.77～404.42, Yttrium trinitrate 55.06～61.31, europium nitrate 0～7.14, acrylamide 103.63～414.51, N, N-methylene-bisacrylamide 8.63～41.45, tetraethylethylenediamine 0.80～5.00 and massfraction are 3% aqueous hydrogen peroxide solution 26.60～170.00, deionized water 500.00～3000.00;
2) polyacrylamide-gel of preparation YAG:
Raw material aluminum nitrate, citric acid, Yttrium trinitrate and europium nitrate are added in the container, add deionized water and stirring to dissolving fully, regulate the pH value to neutrality with ammoniacal liquor, 70～90 ℃ of following waters bath with thermostatic control, add acrylamide and N,N methylene bis acrylamide again, continue water bath with thermostatic control to acrylamide and N, N-methylene-bis acryloyl dissolves fully, adds the aqueous solution initiated polymerization of tetraethylethylenediamine and hydrogen peroxide, continues water bath with thermostatic control to the polyacrylamide-gel that obtains YAG;
3) high-temperature heat treatment:
Will be by step 2) polyacrylamide-gel of the YAG that obtains removes wherein moisture and organism through 600～700 ℃ thermal treatment earlier, and the nitrate thermolysis of inciting somebody to action wherein is corresponding oxide compound, obtain the powder that pre-burning is handled, carry out crystallization through 850～1550 ℃ of high-temperature heat treatment again, get the YAG powder.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100441658C (en) * | 2007-02-06 | 2008-12-10 | 江苏苏博特新材料股份有限公司 | Method of preparing yttrium aluminium garnet fluorescent powder |
| CN105154081A (en) * | 2015-10-10 | 2015-12-16 | 惠州学院 | YAG phosphor powder doped with Ce<3+>, Pr<3+> and Cr<3+> and preparation method thereof |
| WO2022134040A1 (en) * | 2020-12-25 | 2022-06-30 | 苏州君诺新材科技有限公司 | Preparation method for eu2+ ion doped yttrium aluminum garnet structure fluorescent powder |
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| FR3103191A1 (en) * | 2019-11-15 | 2021-05-21 | Centre National De La Recherche Scientifique | SOL-GEL PROCESS FOR MANUFACTURING A PRECURSOR GEL, A XEROGEL AND A YTTRIUM AND ALUMINUM GARNET POWDER AND THEIR USE TO FORM ARTICLES |
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| DE19961673A1 (en) * | 1999-12-21 | 2001-06-28 | Philips Corp Intellectual Pty | Flat x-ray detector with alkali halide scintillator |
| CN1236012C (en) * | 2001-07-20 | 2006-01-11 | 南帝化学工业股份有限公司 | Making process of high-luminance pink LED |
| JP2004152993A (en) * | 2002-10-30 | 2004-05-27 | Okaya Electric Ind Co Ltd | Light emitting diode |
| TW200525779A (en) * | 2004-01-27 | 2005-08-01 | Super Nova Optoelectronics Corp | White-like light emitting device and its manufacturing method |
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| CN100441658C (en) * | 2007-02-06 | 2008-12-10 | 江苏苏博特新材料股份有限公司 | Method of preparing yttrium aluminium garnet fluorescent powder |
| CN105154081A (en) * | 2015-10-10 | 2015-12-16 | 惠州学院 | YAG phosphor powder doped with Ce<3+>, Pr<3+> and Cr<3+> and preparation method thereof |
| WO2022134040A1 (en) * | 2020-12-25 | 2022-06-30 | 苏州君诺新材科技有限公司 | Preparation method for eu2+ ion doped yttrium aluminum garnet structure fluorescent powder |
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