CN106010534A - Phosphate white fluorescent powder for white LEDs and preparation method of phosphate white fluorescent powder - Google Patents
Phosphate white fluorescent powder for white LEDs and preparation method of phosphate white fluorescent powder Download PDFInfo
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- CN106010534A CN106010534A CN201610477704.7A CN201610477704A CN106010534A CN 106010534 A CN106010534 A CN 106010534A CN 201610477704 A CN201610477704 A CN 201610477704A CN 106010534 A CN106010534 A CN 106010534A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7795—Phosphates
- C09K11/7796—Phosphates with alkaline earth metals
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Abstract
The invention discloses a phosphate white fluorescent powder for white LEDs and a preparation method of the phosphate white fluorescent powder. The phosphate white fluorescent powder is Ba3Gd1-x(PO4)3:xEu3+, wherein x ranges from 0.015 to 0.20. The preparation method of the phosphate white fluorescent powder includes the following steps that firstly, a mixture of raw materials including barium carbonate, gadolinium oxide, ammonium dihydrogen phosphate and europium oxide is weighed according to the stoichiometric ratio of Ba3Gd1-x(PO4)3:xEu3+, wherein x ranges from 0.015 to 0.20; secondly, a fluxing agent is added for grinding, and the mixture is obtained after the raw materials are ground and mixed evenly; thirdly, the mixture obtained in the second step is put into a crucible, sintered for 4-6 h in a high-temperature furnace under the conditions of a reducing atmosphere and the temperature of 1400-1600 DEG C and cooled, and the phosphate white fluorescent powder is obtained, wherein the fluxing agent accounts for 0.7-0.9% of the weight of the raw materials according to the addition amount, the fluxing agent is a mixture of ammonium chloride and sodium sulfide, and the weight ratio of ammonium chloride to sodium sulfide is (6-8):1. The phosphate white fluorescent powder is good in dispersity and high in luminous intensity and stability, wherein the advantages are related to the weight ratio of ammonium chloride to sodium sulfide in the fluxing agent, and the highest luminous intensity can be obtained when the weight ratio of ammonium chloride to sodium sulfide is (6-8):1.
Description
Technical field
The invention belongs to field of light emitting materials, be specifically related to a kind of white light LEDs phosphate white emitting fluorescent powder and preparation method thereof.
Background technology
White light LEDs has life-span length, energy-conservation height, the advantage of environmental protection to receive much concern, and is continue fluorescent lamp, electric filament lamp and high pressure gas
The forth generation novel illumination light source that body discharging lamp grows up.
The realization of white light is generally obtained by two ways: (1) is glimmering with blue-ray LED+red green fluorescence powder or blue-ray LED+gold-tinted
Light powder constitutes white light.(2) LED is synthesized with ultraviolet or purple LED+RGB (RGB) three primary colors fluorescent powder.But
Color re-absorption and proportioning regulation and control problem, by contrast, single-matrix fluorescent material colour stable, color is there is between mixed fluorescent powder
Color Well-recovered.At present, the excitation source used in the world typically wavelength is the InGaN based light-emitting diode of 350～470nm,
InGaN base chip is provided that higher excitation energy, improves the light intensity of white light LEDs further.Therefore, exploitation effective UV swashs
The single-substrate white fluorescent powder sent out becomes the focus of this field research and development, and tool is of great significance.
Summary of the invention
It is an object of the invention to provide a kind of white light LEDs phosphate white emitting fluorescent powder and preparation method thereof.
The above-mentioned purpose of the present invention is achieved by techniques below scheme:
A kind of white light LEDs phosphate white emitting fluorescent powder, its chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein, x value
0.015～0.20, it is made by the steps and forms:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.015～0.20；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in reducing atmosphere and 1400～1600 DEG C of conditions in high temperature furnace
Lower sintering 4～6 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.7～0.9% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide,
The weight ratio of ammonium chloride and sodium sulfide is 6～8:1.
Further, described phosphate white emitting fluorescent powder, its chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein, x takes
Value 0.10, is made by the steps and forms:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide, chlorine
The weight ratio changing ammonium and sodium sulfide is 7:1.
Further, described phosphate white emitting fluorescent powder, its chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein, x takes
Value 0.015, is made by the steps and forms:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.015；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1400 DEG C
Tie 6 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide, chlorine
The weight ratio changing ammonium and sodium sulfide is 6:1.
Further, described phosphate white emitting fluorescent powder, its chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein, x takes
Value 0.20, is made by the steps and forms:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.20；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1600 DEG C
Tie 4 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.9% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide, chlorine
The weight ratio changing ammonium and sodium sulfide is 8:1.
Further, described reducing atmosphere is Carbon monoxide reduction atmosphere.
Advantages of the present invention:
The phosphate white emitting fluorescent powder good dispersion that the present invention provides, luminous intensity is high, and stability is high, these advantages and flux
Middle ammonium chloride is relevant with the weight ratio of sodium sulfide, and when the weight ratio of ammonium chloride and sodium sulfide is 6～8:1, luminous intensity is the highest.
Detailed description of the invention
Further illustrate the essentiality content of the present invention below in conjunction with embodiment, but do not limit scope with this.To the greatest extent
The present invention is explained in detail by pipe with reference to preferred embodiment, it will be understood by those within the art that, can be to the present invention
Technical scheme modify or equivalent, without deviating from the spirit and scope of technical solution of the present invention.
Embodiment 1: the preparation of phosphate white emitting fluorescent powder
Chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide, chlorine
The weight ratio changing ammonium and sodium sulfide is 7:1.
Embodiment 2: the preparation of phosphate white emitting fluorescent powder
Chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein, x value 0.015, it is made by the steps and forms:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.015；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1400 DEG C
Tie 6 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide, chlorine
The weight ratio changing ammonium and sodium sulfide is 6:1.
Embodiment 3: the preparation of phosphate white emitting fluorescent powder
Chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein, x value 0.20, it is made by the steps and forms:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.20；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1600 DEG C
Tie 4 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.9% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide, chlorine
The weight ratio changing ammonium and sodium sulfide is 8:1.
Embodiment 4: the preparation of phosphate white emitting fluorescent powder
Chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide, chlorine
The weight ratio changing ammonium and sodium sulfide is 6:1.
Embodiment 5: the preparation of phosphate white emitting fluorescent powder
Chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide, chlorine
The weight ratio changing ammonium and sodium sulfide is 8:1.
Embodiment 6: the preparation of phosphate white emitting fluorescent powder
Chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide, chlorine
The weight ratio changing ammonium and sodium sulfide is 5:1.
Embodiment 7: the preparation of phosphate white emitting fluorescent powder
Chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide, chlorine
The weight ratio changing ammonium and sodium sulfide is 9:1.
Embodiment 8: effect example
The luminescent properties of the fluorescent material of testing example 1～7 preparation respectively, the excitation and emission spectra of different embodiment fluorescent material
Position is basically identical, but luminous intensity, stability of photoluminescence and dispersibility have relatively big difference, result such as table 1.Wherein, luminous strong
Degree, on the basis of embodiment 1, is set to 100, and remaining embodiment is the relative luminous intensity relative to embodiment 1.
The luminescent properties of the different embodiment fluorescent material of table 1 and dispersibility
| Luminous intensity | Stability of photoluminescence | Dispersibility | |
| Embodiment 1 | 100 | Highly stable | Dispersibility is the best |
| Embodiment 4 | 99 | More stable | Dispersibility is preferable |
| Embodiment 5 | 99 | More stable | Dispersibility is preferable |
| Embodiment 6 | 74 | Unstable | Poor dispersion |
| Embodiment 7 | 72 | Unstable | Poor dispersion |
The test result of embodiment 2,3 is basically identical with embodiment 4,5.
Above-mentioned test result indicate that, the phosphate white emitting fluorescent powder good dispersion that the present invention provides, luminous intensity is high, and stability is high,
These advantages are relevant with the weight ratio of ammonium chloride in flux and sodium sulfide, when the weight ratio of ammonium chloride and sodium sulfide is 6～8:1,
Luminous intensity is the highest.
The effect of above-described embodiment indicates that the essentiality content of the present invention, but does not limit protection scope of the present invention with this.
It will be understood by those within the art that, technical scheme can be modified or equivalent, and not take off
Essence and protection domain from technical solution of the present invention.
Claims (5)
1. a white light LEDs phosphate white emitting fluorescent powder, its chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein, x takes
Value 0.015～0.20, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.015～0.20；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in reducing atmosphere and 1400～1600 DEG C of conditions in high temperature furnace
Lower sintering 4～6 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.7～0.9% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide,
The weight ratio of ammonium chloride and sodium sulfide is 6～8:1.
Phosphate white emitting fluorescent powder the most according to claim 1, its chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein,
X value 0.10, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide, chlorine
The weight ratio changing ammonium and sodium sulfide is 7:1.
Phosphate white emitting fluorescent powder the most according to claim 1, its chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein,
X value 0.015, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.015；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1400 DEG C
Tie 6 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide, chlorine
The weight ratio changing ammonium and sodium sulfide is 6:1.
Phosphate white emitting fluorescent powder the most according to claim 1, its chemical composition is Ba3Gd1-x(PO4)3:xEu3+；Wherein,
X value 0.20, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Ba3Gd1-x(PO4)3:xEu3+Stoichiometric proportion weigh raw material, described raw material be brium carbonate,
The mixture of Gadolinia., ammonium dihydrogen phosphate and europium oxide, wherein, x value 0.20；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1600 DEG C
Tie 4 hours, cool down and i.e. obtain described phosphate white emitting fluorescent powder；
Wherein, the addition of flux is the 0.9% of raw material weight, and described flux is the mixture of ammonium chloride and sodium sulfide, chlorine
The weight ratio changing ammonium and sodium sulfide is 8:1.
5. according to the arbitrary described phosphate white emitting fluorescent powder of Claims 1 to 4, it is characterised in that: described reducing atmosphere is an oxygen
Change carbon reducing atmosphere.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108732694A (en) * | 2018-08-06 | 2018-11-02 | 南京邮电大学 | A kind of fiber coupling output system |
-
2016
- 2016-06-27 CN CN201610477704.7A patent/CN106010534A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| QIUMEI DI ET AL.: "Synthesis and luminescence properties of Eu3+-doped Ba3Gd(PO4)3 phosphors for light-emitting diodes", 《OPTICAL ENGINEERING》 * |
| 李雪莹等: "Ba3Gd(PO4)3:Eu3+荧光粉的合成及发光性质", 《无机材料学报》 * |
| 洪广言: "《稀土发光材料——基础与应用》", 30 April 2011, 科学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108732694A (en) * | 2018-08-06 | 2018-11-02 | 南京邮电大学 | A kind of fiber coupling output system |
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