CN105295915A - Method for preparing high-performance YAG yellow fluorescent powder by graphene oxide coprecipitation - Google Patents
Method for preparing high-performance YAG yellow fluorescent powder by graphene oxide coprecipitation Download PDFInfo
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- CN105295915A CN105295915A CN201510674191.4A CN201510674191A CN105295915A CN 105295915 A CN105295915 A CN 105295915A CN 201510674191 A CN201510674191 A CN 201510674191A CN 105295915 A CN105295915 A CN 105295915A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 35
- 239000000843 powder Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000000975 co-precipitation Methods 0.000 title claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 43
- 239000000463 material Substances 0.000 claims description 27
- 239000012452 mother liquor Substances 0.000 claims description 20
- 238000001556 precipitation Methods 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 10
- 229920006395 saturated elastomer Polymers 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 239000007790 solid phase Substances 0.000 claims description 7
- 239000012047 saturated solution Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 2
- 230000029087 digestion Effects 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 150000001457 metallic cations Chemical class 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000000967 suction filtration Methods 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 17
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 10
- 239000007789 gas Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 230000006641 stabilisation Effects 0.000 description 5
- 238000011105 stabilization Methods 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing high-performance YAG yellow fluorescent powder by graphene oxide coprecipitation. The structural formula of the fluorescent powder is as follows: y is3-xAl5O12:Cex(x is 0.03 to 0.07); preparing a YAG precursor solution by adopting a coprecipitation method, adding an ultrasonically stripped graphene oxide solution as a dispersing agent in the process of preparing the solution, and finally carrying out processes such as suction filtration, washing, drying, calcination and the like to obtain the product. According to the invention, due to the addition of the graphene oxide, the precipitated particles are adsorbed on the surface of the graphene oxide through the chemical physical adsorption effect, the electrostatic attraction effect among the particles is weakened, the crystallinity of a sample and the growth of the seed crystal are relatively complete, and the fluorescent powder particles formed after calcination have uniform appearance, good dispersibility and remarkably enhanced fluorescence intensity. The preparation method provided by the invention is simple, feasible and controllable, and is suitable for industrial large-scale production.
Description
Technical field
The invention belongs to YAG:Ce
3+fluorescent material technical field of modification, particularly the method for high-property YAG yellow fluorescent powder is prepared in a kind of graphene oxide co-precipitation.
Background technology
White light LEDs has efficiently, energy-saving and environmental protection, stable performance, life-span are long, shock-resistant, can the advantage such as planar package and easy exploiting, and fluorescent lamp waste frangible compared to incandescent-lamp bulb power consumption, containing shortcomings such as mercury pollution, is thought large potentiality commodity that can become alternative traditional lighting light fixture at coming 10 years by industry.
Since YAG fluorescent powder commercial applications, the cost of white light LEDs reduces greatly, and the application of white light LED lamp in productive life is generally got up gradually.Although after this various fluorescent material is successively developed, gold-tinted YAG powder body material remains the fluorescent material that suitability for industrialized production white light LED commonly uses the most, is also commercial the most successfully fluorescent material at present.
The application of current YAG fluorescent powder still also exists problems, greatly limit its application in white light LEDs field.Mainly there is following problem at present: colour rendering index low and high temperature look declines, powder dispersity is poor.Just because of the existence of these problems, we are at preparation YAG:Ce
3+graphene oxide is added when fluorescent material.Graphene oxide is a kind of laminate structure material of excellent performance, is the thinnest material found so far, has very large specific surface and good wetting ability, and this is a kind of good nucleus growth environment for solution reaction provides.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, providing a kind of size and the method for high-property YAG yellow fluorescent powder is prepared in dispersity is controlled, luminous intensity strengthens graphene oxide co-precipitation.
Technical scheme of the present invention is by doped with oxygen functionalized graphene, realizes YAG:Ce
3+the particle diameter of fluorescent material particulate and the control of dispersity, thus improve its luminous intensity; Realize simple controlled preparation method, be applicable to industrialization scale operation.GO has higher specific surface area, fluorescent material precursor surface effectively can be wrapped in as physical dispersion agent by adding GO solution, the film of one deck densification is formed at fluorescent material precursor interface, effectively intercept being adhered between particle, while high-temperature calcination, GO resolves into reducing gas, destroy the oxo bridge key between fluorescent powder grain, thus improve the shortcoming that powder easily reunites; Under high temperature, GO decomposes the reducing gas produced on the other hand, effectively can hinder Ce
3+(luminescence center) is to Ce
4+change, therefore prepared fluorescent material has the high feature of luminous intensity.
Concrete technical scheme of the present invention is: the method for high-property YAG yellow fluorescent powder is prepared in graphene oxide co-precipitation, and concrete steps are as follows:
(1) according to Y
3-xal
5o
12: Ce
x, wherein x=0.03 ~ 0.07, stoichiometrically takes Y (NO
3)
36H
2o, Ce (NO
3)
36H
2o and Al (NO
3)
39H
2o is dissolved in deionized water and is mixed with saturated mother liquor;
(2) by (NH
4)
2sO
4with NH
4hCO
3be 1:(40 ~ 100 in molar ratio) be dissolved in deionized water, be made into saturated solution;
(3) add graphene oxide (GrapheneOxide, GO) solution in the saturated solution prepared to step (2), mix;
(4), in the mixing solutions prepared to step (3), the pH value of ammoniacal liquor regulator solution is added;
(5) the saturated mother liquor that step (1) is prepared is dropped in the solution that step (4) prepares, obtains solid phase precipitation, after still aging, filter, washing, dry, grinding obtains the precursor powder of fluorescent material;
(6) precursor powder is put into the tube furnace being connected with mixed gas to calcine, after cooling (generally to room temperature), grinding obtains high-property YAG yellow fluorescent powder.
The concentration of the graphene oxide solution added in preferred steps (3) is 0.005 ~ 0.03g/L.The volume of the graphene oxide solution preferably added is that step (2) is made into 20 ~ 40% of saturated solution volume.
PH value described in preferred steps (4) is 8.5 ~ 11.
In preferred steps (5), the add-on of saturated mother liquor is control metallic cation in saturated mother liquor and NH
4hCO
3mol ratio be 1:(8 ~ 12).
The time for adding dropped to by the saturated mother liquor that step (1) is prepared in preferred steps (5) in the solution that step (4) prepares controlled at 1 ~ 2 hour.In preferred steps (5), digestion time is 2 ~ 5 hours; Drying temperature is 50 ~ 80 DEG C, and time of drying is 6 ~ 12 hours.
Mixed gas described in preferred steps (6) is Ar, N
2or one in He and H
2gas mixture, Ar, N wherein
2or the volume percent that He accounts for gas mixture is 90 ~ 95%.
Calcining temperature described in preferred steps (6) is 800 ~ 1200 DEG C, and calcination time is 3 ~ 5 hours.
Beneficial effect:
In the present invention, graphene oxide adds, deposit seeds is made to be adsorbed on the surface of graphene oxide by chemical physics adsorption, reduce the electrostatic attraction effect between particle, make the growth of the crystallinity of sample and crystal seed more complete, the fluorescent material powder granule-morphology formed after calcining is even, good dispersity, fluorescence intensity significantly strengthens.Preparation method provided by the present invention is simple controlled, is applicable to industrialization scale operation.
Accompanying drawing explanation
Fig. 1 is that the graphene oxide of different concns prepares YAG:Ce as initial precipitation agent
3+xRD figure; Wherein A is not for add graphene oxide, and B is embodiment 1, and C is embodiment 2, D be embodiment 3, E is embodiment 4;
Fig. 2 is YAG:Ce prepared by embodiment 2
3+fluorescent material SEM schemes; Wherein (a) does not add YAG:Ce prepared by GO
3+the SEM picture of fluorescent material; B () adds YAG:Ce prepared by GO solution
3+fluorescent material electron microscopic picture; (c) GO solution electron microscopic picture;
Fig. 3 is YAG:Ce prepared by embodiment 2
3+fluorescent phosphor utilizing emitted light spectrogram; Wherein A adds YAG:Ce prepared by GO
3+fluorescent material; B does not add YAG:Ce prepared by GO
3+fluorescent material.
Embodiment
Below in conjunction with example, the present invention is further illustrated, but invention is not limited only to these examples, and under the prerequisite not departing from present inventive concept, any improvement done is all within protection scope of the present invention.
Embodiment 1:
A kind of graphene oxide coprecipitation method prepares high-property YAG: Ce
3+yellow fluorescent powder, comprises following synthesis step:
(1) according to Y
3-xal
5o
12: Ce
x, wherein x=0.03, stoichiometrically takes 1.137gY (NO
3)
36H
2o, 0.013gCe (NO
3)
36H
2o and 1.876gAl (NO
3)
39H
2o is dissolved in 50ml deionized water and is mixed with mother liquor.
(2) 5.056gNH is taken
4hCO
3be dissolved in 50ml deionized water solution, then take 0.0126g (NH
4)
2sO
4be dissolved in as electrostatic stabilization agent in above-mentioned solution, then add the graphene oxide solution that 20ml concentration is 0.005g/L; The pH value adding ammoniacal liquor regulator solution in mixing solutions is 8.5, it can be used as precipitation agent.
(3) be slowly added drop-wise in precipitation agent by mother liquor with 2 hours, obtain solid phase precipitation, still aging 2 hours, filter, washing, drying 12 hours at 50 DEG C, grinding obtains the presoma of fluorescent material.
(4) presoma is put into be connected with argon hydrogen gas mixture (Ar:H
2=95%:5%) tube furnace in calcining 5 hours at 800 DEG C, after being cooled to room temperature, grinding obtains yellow fluorescent powder.
Embodiment 2
A kind of graphene oxide coprecipitation method prepares high-property YAG: Ce
3+yellow fluorescent powder, comprises following synthesis step:
(1) according to Y
3-xal
5o
12: Ce
x, wherein x=0.04, stoichiometrically takes 1.133gY (NO
3)
36H
2o, 0.017gCe (NO
3)
36H
2o and 1.876gAl (NO
3)
39H
2o is dissolved in 50ml deionized water and is mixed with mother liquor.
(2) 6.3275gNH is taken
4hCO
3be dissolved in 50ml deionized water solution, take 0.2g (NH
4)
2sO
4be dissolved in above-mentioned solution as electrostatic stabilization agent; Add the graphene oxide solution that 20ml concentration is 0.01g/L again; The pH value adding ammoniacal liquor regulator solution in mixing solutions is 11, it can be used as precipitation agent.
(3) be slowly added drop-wise in precipitation agent by mother liquor with 2 hours, obtain solid phase precipitation, still aging 5 hours, filter, washing, drying 6 hours at 80 DEG C, grinding obtains the presoma of fluorescent material.
(4) presoma is put into be connected with argon hydrogen gas mixture (N
2: H
2=95%:5%) tube furnace in calcining 3 hours at 1200 DEG C, after being cooled to room temperature, grinding obtains yellow fluorescent powder.Adding the phase purity of fluorescent material without impact of graphene oxide can be found out from the XRD of Fig. 1, can find out that from the SEM of Fig. 2 the fluorescent material dispersiveness made that adds of graphene oxide is improved, can find out that adding fluorescent intensity prepared by GO is enhanced from the utilizing emitted light spectrogram of Fig. 3.
Embodiment 3
A kind of graphene oxide coprecipitation method prepares high-property YAG: Ce
3+yellow fluorescent powder, comprises following synthesis step:
(1) according to Y
3-xal
5o
12: Ce
x, wherein x=0.05, stoichiometrically takes 1.130gY (NO
3)
36H
2o, 0.022gCe (NO
3)
36H
2o and 1.876gAl (NO
3)
39H
2o is dissolved in 50ml deionized water and is mixed with mother liquor.
(2) 6.3275gNH is taken
4hCO
3be dissolved in 50ml deionized water solution, take 0.2g (NH
4)
2sO
4be dissolved in above-mentioned solution as electrostatic stabilization agent; Add the graphene oxide solution that 20ml concentration is 0.02g/L again, the pH value adding ammoniacal liquor regulator solution in mixing solutions is 9.0, it can be used as precipitation agent.
(3) be slowly added drop-wise in precipitation agent by mother liquor with 1.5 hours, obtain solid phase precipitation, still aging 3 hours, filter, washing, drying 10 hours at 60 DEG C, grinding obtains the presoma of fluorescent material.
(4) presoma is put into be connected with argon hydrogen gas mixture (Ar:H
2=95%:5%) tube furnace in calcining 3 hours at 1000 DEG C, after being cooled to room temperature, grinding obtains yellow fluorescent powder.
Embodiment 4
A kind of graphene oxide coprecipitation method prepares high-property YAG: Ce
3+yellow fluorescent powder, comprises following synthesis step:
(1) according to Y
3-xal
5o
12: Ce
x, wherein x=0.06, stoichiometrically takes 1.126gY (NO
3)
36H
2o, 0.026gCe (NO
3)
36H
2o and 1.876gAl (NO
3)
39H
2o is dissolved in 50ml deionized water and is mixed with mother liquor.
(2) 6.3275gNH is taken
4hCO
3be dissolved in 50ml deionized water solution, take 0.2g (NH
4)
2sO
4be dissolved in above-mentioned solution as electrostatic stabilization agent; Add the graphene oxide solution of 20ml concentration 0.03g/L again, the pH value adding ammoniacal liquor regulator solution in mixing solutions is 10.5, it can be used as precipitation agent.
(3) be slowly added drop-wise in precipitation agent by mother liquor with 1 hour, obtain solid phase precipitation, still aging 3 hours, filter, washing, drying 12 hours at 80 DEG C, grinding obtains the presoma of fluorescent material.
(4) presoma is put into be connected with argon hydrogen gas mixture (Ar:H
2=95%:5%) tube furnace in calcining 3 hours at 1000 DEG C, after being cooled to room temperature, grinding obtains yellow fluorescent powder.
Embodiment 5
A kind of graphene oxide coprecipitation method prepares high-property YAG: Ce
3+yellow fluorescent powder, comprises following synthesis step:
(1) according to Y
3-xal
5o
12: Ce
x, wherein x=0.07, stoichiometrically takes 1.122gY (NO
3)
36H
2o, 0.03gCe (NO
3)
36H
2o and 1.876gAl (NO
3)
39H
2o is dissolved in 50ml deionized water and is mixed with mother liquor.
(2) 6.3275gNH is taken
4hCO
3be dissolved in 50ml deionized water solution, take 0.2g (NH
4)
2sO
4be dissolved in above-mentioned solution as electrostatic stabilization agent; Add the graphene oxide solution that 16ml concentration is 0.01g/L again, the pH value adding ammoniacal liquor regulator solution in mixing solutions is 11, it can be used as precipitation agent.
(3) be slowly added drop-wise in precipitation agent by mother liquor with 2 hours, obtain solid phase precipitation, still aging 5 hours, filter, washing, drying 6 hours at 80 DEG C, grinding obtains the presoma of fluorescent material.
(4) presoma is put into be connected with argon hydrogen gas mixture (He:H
2=90%:10%) tube furnace in calcining 3 hours at 1200 DEG C, after being cooled to room temperature, grinding obtains yellow fluorescent powder.
Claims (9)
1. the method for high-property YAG yellow fluorescent powder is prepared in graphene oxide co-precipitation, and concrete steps are as follows:
(1) according to Y
3-xal
5o
12: Ce
x, wherein x=0.03 ~ 0.07, stoichiometrically takes Y (NO
3)
36H
2o, Ce (NO
3)
36H
2o and Al (NO
3)
39H
2o is dissolved in deionized water and is mixed with saturated mother liquor;
(2) by (NH
4)
2sO
4with NH
4hCO
3be 1:(40 ~ 100 in molar ratio) be dissolved in deionized water, be made into saturated solution;
(3) add graphene oxide solution in the saturated solution prepared to step (2), mix;
(4), in the mixing solutions prepared to step (3), the pH value of ammoniacal liquor regulator solution is added;
(5) the saturated mother liquor that step (1) is prepared is dropped in the solution that step (4) prepares, obtains solid phase precipitation, after still aging, filter, washing, dry, grinding obtains the precursor powder of fluorescent material;
(6) precursor powder is put into the tube furnace being connected with mixed gas to calcine, after cooling, grinding obtains high-property YAG yellow fluorescent powder.
2. method according to claim 1, is characterized in that the concentration of the graphene oxide solution described in step (3) is 0.005 ~ 0.03g/L.
3. method according to claim 1, is characterized in that the volume of the graphene oxide solution added in step (3) is that step (2) is made into 20 ~ 40% of saturated solution volume.
4. method according to claim 1, is characterized in that the pH value described in step (4) is 8.5 ~ 11.
5. method according to claim 1, is characterized in that the add-on of saturated mother liquor in step (5) is control metallic cation in saturated mother liquor and NH
4hCO
3mol ratio be 1:(8 ~ 12).
6. method according to claim 1, the time for adding that it is characterized in that being dropped to by the saturated mother liquor that step (1) is prepared in step (5) in the solution that step (4) prepares is 1 ~ 2 hour.
7. method according to claim 1, is characterized in that in step (5), digestion time is 2 ~ 5 hours; Drying temperature is 50 ~ 80 DEG C, and time of drying is 6 ~ 12 hours.
8. method according to claim 1, is characterized in that in step (6), mixed gas is Ar, N
2or He and H
2mixing, Ar, N wherein
2or the volume percent that He accounts for gas mixture is 90 ~ 95%.
9. method according to claim 1, it is characterized in that the calcining temperature described in step (6) is 800 ~ 1200 DEG C, calcination time is 3 ~ 5 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114477989A (en) * | 2020-11-11 | 2022-05-13 | 中国科学院福建物质结构研究所 | Graphene-modified green-light transparent ceramic material and preparation method and application thereof |
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| CN102031112A (en) * | 2010-11-10 | 2011-04-27 | 西北师范大学 | Graphene/europium oxide photoelectric composite material and preparation method thereof |
| CN103333687A (en) * | 2013-07-22 | 2013-10-02 | 中国人民解放军国防科学技术大学 | Inorganic photoluminescent material and preparation method thereof |
| KR101548539B1 (en) * | 2014-11-07 | 2015-09-01 | 성균관대학교산학협력단 | Graphene-containing remote phosphor composite and preparing method of the same |
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2015
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| CN102031112A (en) * | 2010-11-10 | 2011-04-27 | 西北师范大学 | Graphene/europium oxide photoelectric composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114477989A (en) * | 2020-11-11 | 2022-05-13 | 中国科学院福建物质结构研究所 | Graphene-modified green-light transparent ceramic material and preparation method and application thereof |
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| CN105295915B (en) | 2017-06-06 |
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