CN102181291B - Method for preparing cerium doped yttrium aluminum garnet fluorescent powder - Google Patents
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Abstract
The invention relates to a method for preparing cerium doped yttrium aluminum garnet fluorescent powder. The method comprises the steps of mixing a YAG:Ce (Yttrium Aluminum Garnet:Cerium) mother salt solution with a microbial culture solution by using a microbe-coprecipitation method; adjusting the pH value to be 9; forming a microbe-inorganic matter composite precipitate suspension through electrostatic adsorption; and synthesizing the YAG:Ce fluorescent powder with good performance through calcining after ageing, separating, washing and drying. The method provided by the invention has the advantages of simple process; and the obtained YAG:Ce powder has the advantages of uniform component, nearly spherical particles, good dispersity and good fluorescent property.
Description
(1) technical field
The present invention relates to a kind of preparation method with cerium-doped yttrium aluminum garnet (YAG:Ce) fluorescent powder of superperformance, belong to technical field of function materials.
(2) background technology
The YAG:Ce powder becomes the important luminous host material of white light emitting diode (LED) because having special fluorescence property, referring to CN1373523A (CN02100345.9).White light LEDs is regarded as new generation of green environmental protection and energy saving light source due to its non-thermal radiation, without advantages such as toxic substance pollutions, can be widely used in the fields such as illumination, cultural industry and industry, has huge market outlook and significant economic and social benefits.And the YAG:Ce fluorescent powder of processability excellence is one of gordian technique of LED application.
CN101851510A (CN201010186604.1) discloses a kind of method for preparing rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder with coprecipitation method, yttrium oxide powder is dissolved it with the excessive vitriol oil, mix with cerous nitrate and aluminum nitrate solution again and be made into metal ion solution, Y
3+: Ce
3+: Al
3+=2.94: 0.06: 5; Metal ion solution is added in precipitation agent, gets coprecipitate; Coprecipitate is cleaned, suction filtration, oven dry gets presoma; With the presoma pre-burning, get preburning powder; With the preburning powder calcining, get rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder.The coprecipitation method of using is to mix under ionic condition, and comparable mechanical mixing is more even, and reduces to mix the chance of impurity, makes accurate control stoichiometric calculation comparatively easy, and granularity can be controlled according to reaction conditions.Preferred precipitation agents etc. by coprecipitation method, just can form pure YAG phase in the time of 1100 ℃, lower approximately 500 ℃ than conventional high-temperature solid reaction process.
CN101851509A (CN201010186575.9) discloses the method for preparing rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder with network gel, and a kind of low reunion, particle size are little to obtain, well behaved fluorescent material.Yttrium oxide powder is dissolved it with the excessive vitriol oil, then mix with cerous nitrate and aluminum nitrate solution and be made into metal ion solution, wherein in molar ratio, control Y
3+: Ce
3+: Al
3+=2.94: 0.06: 5; Add NH in metal ion solution
4HCO
3, control the pH value of metal ion solution 3～5; Add acrylamide monomer, lattice reagent and initiator in the solution of gained, get wet gel after polymerization; With the wet gel oven dry, get xerogel; Xerogel pre-burning with gained gets preburning powder; Add fusing assistant in the preburning powder of gained, get rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder after calcining.
CN101602944 (CN200910100593.8) discloses a kind of production method of mixing the rare-earth yttrium-aluminium garnet nano phosphor powder, and the general formula of nano-powder is (Y
1-xLn
x)
3Al
5O
12, wherein Ln is a kind of of rare earth element ce, Eu, 0.0≤x≤0.1, with the mixing solutions of the nitrate of Al, Y and Ln or acetate as female salts solution, NH
4HCO
3With NH
3H
2The mixing solutions of O is as the composite precipitation agent solution; The pH value of regulating compound precipitants with ammoniacal liquor is 10; Then female salts solution is injected in the composite precipitation agent solution of continuous stirring after ultrasonic atomizatio, the mixing solutions that reacts completely after filtration, washing, oven dry, ball milling, the calcining rare earth ion doped YAG nano phosphor powder that can obtain evenly, disperse repeatedly, the advantage of the method be the fluorescent powder that makes evenly, dispersion, granularity little (50～70 nanometer) and to generate phase single; Its weak point is that preparation technology is more complicated, and resultant quantity is little.
Comparatively desirable YAG:Ce fluorescent material requires to have that component is even, powder granule is spherical in shape, the performances such as good dispersity.But at present, utilize the YAG:Ce fluorescent powder of the method preparations such as solid phase method, chemical coprecipitation, because its performance is difficult to reach above-mentioned requirements, require pH value difference easily to cause the component skewness when particularly chemical coprecipitation is because of different metal ion precipitations such as Y, Al, Ce, therefore its performance and effect are relatively poor.Therefore how the good YAG:Ce fluorescent material of processability is the important topic of this area.
(3) summary of the invention
For solve powder component skewness that prior art exists, particle agglomeration is serious and problem in irregular shape, the invention provides a kind ofly have good dispersion, particle is preparation method subsphaeroidal, the uniform cerium-doped yttrium aluminum garnet of component (YAG:Ce) fluorescent powder.
The present invention combines biotechnology with chemical synthesis process, adopt microorganism-coprecipitation method to realize purpose of the present invention.
The term explanation: YAG:Ce is (Y
1-xCe
x)
3Al
5O
12Write a Chinese character in simplified form, name is called the cerium-doped yttrium aluminum garnet.
Technical scheme of the present invention is as follows:
The preparation method of a kind of cerium-doped yttrium aluminum garnet (YAG:Ce) fluorescent powder, step is as follows:
(1) raw material is selected from: the oxide compound of cerium salt or cerium, the oxide compound of aluminium salt or aluminium, the oxide compound of yttrium salt or yttrium;
(2) prepare female salts solution
Cerium salt, yttrium salt, aluminium salt are dissolved in respectively in deionized water, and the oxide compound of cerium, yttrium, aluminium is dissolved in respectively in nitric acid,
Press Y
3-xCe
xAl
5O
12(x=0.02～0.10) stoichiometric ratio mixes, and gets female salts solution, is designated as solution A.
(3) preparation microbial culture medium
Yeast and glucose are pressed 1: the mixing solutions of (0.5～1.5) mass ratio, cultivated 0.5～2.0 hour under 20～40 ℃ of conditions, with the nutrient solution purifying, obtain microbial culture medium, be designated as solution B.
(4) under agitation condition, solution A is added drop-wise in solution B, and stirred 2～5 hours, obtain solution C.In solution C, metal ion is combined with yeast cell.
(5) add basic solution to regulate pH value to 9 in solution C, make it produce throw out, form suspension, and stir ageing 24～72 hours.
(6) with after throw out separation, washing in above-mentioned suspension, drying is 12～72 hours under 80 ℃, obtains cerium-doped yttrium aluminum garnet (YAG:Ce) presoma.This presoma good dispersity, TEM sees Fig. 2.
(7) with above-mentioned cerium-doped yttrium aluminum garnet (YAG:Ce) presoma, calcined 1～3 hour under 900～1200 ℃ of conditions, get cerium-doped yttrium aluminum garnet (YAG:Ce) fluorescent powder.Gained YAG:Ce fluorescent powder properties is good, as Fig. 3, Fig. 4 and shown in Figure 5.
According to the present invention, preferred, in the raw material of step (1), described cerium salt is cerous nitrate, and described yttrium salt is Yttrium trinitrate, and described aluminium salt is aluminum nitrate.
Further preferred, the raw material of step (1) adopts yttrium oxide, aluminum nitrate and cerous nitrate.
Further preferred, the raw material of step (1) adopts cerous nitrate, aluminum nitrate and Yttrium trinitrate.
According to the present invention, preferred, in step (2), cerium salt, yttrium salt, aluminium salt are dissolved in respectively deionized water, and solution ion concentration is respectively 0.2～1.5mol/L.
According to the present invention, preferred, in step (2), the oxide compound of cerium, yttrium, aluminium is dissolved in respectively in nitric acid, and solution ion concentration is respectively 0.2～1.5mol/L.
According to the present invention, preferred, the yeast in step (3) is bread yeast, candiyeast or cereuisiae fermentum.
According to the present invention, preferred, the basic solution of step (5) is bicarbonate of ammonia or ammonia soln, and concentration is 0.1～1.5mol/L.
adopt the inventive method, gordian technique is that microbial technique is combined with the chemical coprecipitation technique method, the female salts solution of YAG:Ce is mixed with yeast culture liquid, make the Al of positively charged, Y, the Ce metal ion is adsorbed onto on electronegative yeast cell very easily simultaneously in proportion, form the stable cell granule that contains three metal ion species with coating layer, when pH reaches certain value, certain metal ion species just forms carbonate or oxyhydroxide hydrate and cell granule and other metal ion is precipitated simultaneously, not only make YAG:Ce precursor uniform component distribution, and good dispersity, the reunion of YAG:Ce particle in the time of can effectively alleviating calcining.The concentration of female salts solution and yeast culture liquid and both ratios and pH value have material impact to the performance of synthetic YAG:Ce powder.
The present invention compared with prior art, successfully solved powder component skewness that prior art exists, particle agglomeration is serious and problem in irregular shape, it is advantageous that and utilize cheap microorganism, adopt simple microorganism-coprecipitation technique, synthesized well behaved YAG:Ce fluorescent powder; Its component is even, and it is subsphaeroidal that particle is, good dispersity; Its fluorescence property is better than the synthetic YAG:Ce powder of coprecipitation method, sees Fig. 5.YAG:Ce fluorescent powder with the present invention's preparation can be used for preparing the luminescent device that use in the fields such as industry, illumination, cultural industry.
(4) description of drawings
Fig. 1 is the Photomicrograph that in embodiment 1, metal ion is combined with yeast cell,
Fig. 2 is the TEM picture of synthetic YAG:Ce precursor in embodiment 1,
Fig. 3 is the XRD figure spectrum of synthetic YAG:Ce fluorescent powder in embodiment 1,
Fig. 4 is the SEM picture of synthetic YAG:Ce fluorescent powder in embodiment 1,
Fig. 5 is the fluorescence spectrum comparison diagram of the YAG:Ce fluorescent powder that in fluorescence spectrum and the Comparative Examples of synthetic YAG:Ce fluorescent powder in embodiment 1, coprecipitation method is synthesized, and wherein curve a, c are respectively fluorescence excitation spectrum and the emmission spectrum of microorganism of the present invention-coprecipitation method synthetic powder; Curve b, d are respectively fluorescence excitation spectrum and the emmission spectrum of Comparative Examples coprecipitation method synthetic powder.
(5) embodiment
Below in conjunction with the present invention will be further described with embodiment and accompanying drawing, but be not limited to this.
Embodiment 1.
With analytical pure Y
2O
3Be dissolved in salpeter solution, with analytical pure Al (NO
3)
39H
2O and Ce (NO
3)
36H
2O is dissolved in respectively in distilled water, and solution ion concentration is all 0.2mol/L respectively, presses Y
2.94Ce
0.06Al
5O
12Stoichiometric ratio is mixed above-mentioned three kinds of solution, and stirs 1 hour, obtains solution A.
Press 1: 0.5 quality of bread yeast and glucose than obtain solution, purifying after cultivating 2 hours under 20 ℃ obtains solution B.
The 100ml solution A is dropwise joined in 100ml B solution, stir and mixed in 2 hours, obtain solution C.In solution C, metal ion is combined with yeast cell, and Photomicrograph is seen Fig. 1.Then while stirring to solution C drip concentration be the ammonium bicarbonate aqueous solution of 0.1mol/L to pH=9, make it form precipitation suspension, after still aging 24 hours, centrifugation throw out (seeing Fig. 2); After washing three times in 80 ℃ of dry 12h.Calcining insulation 3h under 900 ℃, obtain well behaved YAG:Ce fluorescent powder at last.
By the XRD figure of Fig. 3 as can be known, institute's synthetic powder is the pure phase yttrium aluminum garnet; By Fig. 4 SEM picture as can be known, synthetic powder is better dispersed, and it is subsphaeroidal that particle is, and average particle size particle size is 420nm; Curve c fluorescence emission spectrum by Fig. 5 knows, its fluorescent emission intensity of synthetic powder of the present invention is higher than the emissive porwer (seeing the curve d of Fig. 5) of coprecipitation method synthetic powder.
Embodiment 2.
With analytical pure Y (NO
3)
39H
2O, Al (NO
3)
39H
2O, Ce (NO
3)
36H
2O is dissolved in respectively in distilled water, and ionic concn is 0.8mol/L, presses Y
2.94Ce
0.06Al
5O
12Stoichiometric ratio is mixed above-mentioned three kinds of salts solutions and was stirred 1 hour, obtains solution A.Press candiyeast and the glucose mass ratio of 1: 0.8 preparation mixed aqueous solution, purifying after cultivating 1 hour under 28 ℃ obtains solution B.The 100ml solution A is dropwise joined in the 100ml solution B, stir and it was mixed in 3 hours, be solution C.Then while stirring to solution C drip concentration be the ammonia soln of 1mol/L to pH=9, make it form precipitation suspension, after still aging 50 hours, the centrifugation throw out; After washing three times in 80 ℃ of dry 24h.Calcining insulation 1.5h under 1100 ℃, obtain well behaved YAG:Ce fluorescent powder at last.
Embodiment 3.
With analytical pure Y
2O
3Be dissolved in salpeter solution, with analytical pure Al (NO
3)
39H
2O and Ce (NO
3)
36H
2O is dissolved in respectively in distilled water, and ionic concn is 1.5mol/L, presses Y
2.94Ce
0.06Al
5O
12Stoichiometric ratio is mixed in proportion three kinds of solution, and stirs 1 hour, obtains solution A.Be mixed into the aqueous solution by cereuisiae fermentum and the glucose mass ratio of 1: 1.5, purifying after cultivating 0.5 hour under 40 ℃ obtains solution B.The 100ml solution A is dropwise joined in the 100ml solution B, stir and mixed in 5 hours, obtain solution C.Then while stirring to C solution drip concentration be the ammonium bicarbonate aqueous solution of 1.5mol/L to pH=9, make it form precipitation suspension, after still aging 72 hours, the centrifugation throw out; After washing three times in 80 ℃ of dry 72h.Calcining insulation 1h under 1200 ℃, obtain well behaved YAG:Ce fluorescent powder at last.
Embodiment 4.
As described in Example 1, difference is that the stoichiometric ratio of synthetic YAG:Ce is Y
2.98Ce
0.02Al
5O
12
Embodiment 5.
As described in Example 2, difference is that the stoichiometric ratio of synthetic YAG:Ce is Y
2.90Ce
0.10Al
5O
12Comparative Examples: coprecipitation method is synthesized the YAG:Ce fluorescent powder
In order to contrast with embodiment 1, adopt the synthetic YAG:Ce powder of coprecipitation method.With analytical pure Y
2O
3Be dissolved in salpeter solution, with analytical pure Al (NO
3)
39H
2O and Ce (NO
3)
36H
2O is dissolved in respectively in distilled water, and ionic concn is 0.2mol/L, presses Y
2.94Ce
0.06Al
5O
12Stoichiometric ratio is mixed above-mentioned three kinds of solution, and stirs 1 hour, obtains solution A.With solution A dropwise join concentration be the ammonium bicarbonate aqueous solution of 0.1mol/L to pH=9, make it form precipitation suspension, after still aging 24 hours, the centrifugation throw out; 80 ℃ of dry 12h after washing three times.Calcining insulation 3h under 900 ℃, obtain the synthetic YAG:Ce fluorescent powder of coprecipitation method at last, and its fluorescence spectrum is seen curve b, d in Fig. 5.
Claims (5)
1. the preparation method of a cerium doped yttrium aluminum garnet fluorescent powder, step is as follows:
(1) raw material is selected from: the oxide compound of cerium salt or cerium, the oxide compound of aluminium salt or aluminium, the oxide compound of yttrium salt or yttrium;
(2) prepare female salts solution
Cerium salt, yttrium salt, aluminium salt are dissolved in respectively in deionized water, and solution ion concentration is respectively 0.2 ~ 1.5mol/L;
The oxide compound of cerium, yttrium, aluminium is dissolved in respectively in nitric acid, and solution ion concentration is respectively 0.2 ~ 1.5mol/L;
Press Y
3-xCe
xAl
5O
12(x=0.02 ~ 0.10) stoichiometric ratio mixes, and gets female salts solution, is designated as solution A;
(3) preparation microbial culture medium
Yeast and glucose are pressed 1:(0.5～1.5) mixing solutions of mass ratio, cultivated 0.5～2.0 hour under 20～40 ℃ of conditions, with the nutrient solution purifying, obtain microbial culture medium, be designated as solution B;
(4) under agitation condition, solution A is added drop-wise in solution B, and stirred 2～5 hours, obtain solution C; In solution C, metal ion is combined with yeast cell;
(5) add basic solution to regulate pH value to 9 in solution C, make it produce throw out, form suspension, and stir ageing 24～72 hours; Described basic solution is bicarbonate of ammonia or ammonia soln, and strength of solution is 0.1 ~ 1.5mol/L;
(6) with after throw out separation, washing in above-mentioned suspension, drying is 12～72 hours under 80 ℃, obtains cerium-doped yttrium aluminum garnet presoma;
(7) with above-mentioned cerium-doped yttrium aluminum garnet presoma, calcined 1 ~ 3 hour under 900 ~ 1200 ℃ of conditions, get cerium doped yttrium aluminum garnet fluorescent powder.
2. preparation method according to claim 1, is characterized in that in the raw material of step (1), and described cerium salt is cerous nitrate, and described yttrium salt is Yttrium trinitrate, and described aluminium salt is aluminum nitrate.
3. preparation method according to claim 1, is characterized in that the raw material of step (1) adopts yttrium oxide, aluminum nitrate and cerous nitrate.
4. preparation method according to claim 1, is characterized in that the raw material of step (1) adopts cerous nitrate, aluminum nitrate and Yttrium trinitrate.
5. preparation method according to claim 1, is characterized in that the yeast in step (3) is bread yeast, candiyeast or cereuisiae fermentum.
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| CN103013185A (en) * | 2011-09-23 | 2013-04-03 | 北京大学 | Inorganic yellow pigment and preparation method thereof |
| RU2533709C2 (en) * | 2012-10-05 | 2014-11-20 | Общество с ограниченной ответственностью "Минерал" | Monocrystalline fluorescent material for white light-emitting diodes |
| CN104119907B (en) * | 2013-04-26 | 2016-08-10 | 海洋王照明科技股份有限公司 | The YAG luminescent material of hollow-core construction and preparation method |
| CN104830338A (en) * | 2015-05-18 | 2015-08-12 | 广东工业大学 | Preparation method of spherical YAG (yttrium aluminum garnet):Ce |
| CN116103760A (en) * | 2023-02-16 | 2023-05-12 | 合肥中科瑞恒新材料科技有限责任公司 | Processing method of cerium-doped yttrium iron garnet wafer |
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| US20030111644A1 (en) * | 2001-12-14 | 2003-06-19 | National Cheng Kung University | Process for producing nanoscale yttrium aluminum garnet (YAG) fluorescent powders |
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