CN106118640A - A kind of white light LEDs nitric oxide fluorescent powder and preparation method thereof - Google Patents
A kind of white light LEDs nitric oxide fluorescent powder and preparation method thereof Download PDFInfo
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- CN106118640A CN106118640A CN201610479655.0A CN201610479655A CN106118640A CN 106118640 A CN106118640 A CN 106118640A CN 201610479655 A CN201610479655 A CN 201610479655A CN 106118640 A CN106118640 A CN 106118640A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7729—Chalcogenides
- C09K11/7731—Chalcogenides with alkaline earth metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/58—Optical field-shaping elements
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
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Abstract
The invention discloses a kind of white light LEDs nitric oxide fluorescent powder and preparation method thereof, consist of Sr3‑xB3N3O3: xEu2+；Wherein, x span is 0.005～0.20, is made by the steps and forms: step S1, by chemical composition Sr3‑xB3N3O3Stoichiometric proportion weigh raw material, described raw material is the mixture of strontium carbonate, boron nitride and europium oxide；Step S2, adds flux and is ground, be ground and obtain mixture；Step S3, mixture step S2 obtained loads crucible, sinters 4～6 hours, cool down and i.e. obtain described nitric oxide fluorescent powder in high temperature furnace under the conditions of reducing atmosphere and 1400～1600 DEG C；Wherein, the addition of flux is the 0.7～0.9% of raw material weight, described flux be the weight ratio of the mixture of ammonium hydrogen carbonate and ammonium fluoride, ammonium hydrogen carbonate and ammonium fluoride be 6～8:1.The fluorescent material good dispersion that the present invention provides, luminous intensity is high, and stability is high, and these advantages are relevant with the weight ratio of flux ammonium hydrogen carbonate and ammonium fluoride, and when the weight ratio of ammonium hydrogen carbonate and ammonium fluoride is 6～8:1, luminous intensity is the highest.
Description
Technical field
The invention belongs to LED luminescent material field, be specifically related to a kind of white light LEDs nitric oxide fluorescent powder and preparation side
Method.
Background technology
Along with developing rapidly of green light LED, the requirement to fluorescent material is more and more higher, it is desirable to fluorescent material has higher bright
Degree and excellent serviceability.Except the conditions such as raw-material purity and calcination technique are to the brightness of fluorescent material and serviceability
Outside having an impact, the selection of flux also has the biggest shadow noon to brightness and the serviceability of fluorescent material.
White light LEDs is a kind of solid-state semiconductor device converting electrical energy into white light, also known as semiconductor lighting, has efficiency
The plurality of advantages such as high, volume is little, life-span length, safety, low-voltage, energy-saving and environmental protection, regarded as by people the electric filament lamp that continues, fluorescent lamp,
Forth generation lighting source after high-voltage gas discharging light, is the main product in following illumination market.
Summary of the invention
It is an object of the invention to provide a kind of white light LEDs nitric oxide fluorescent powder and preparation method.
The above-mentioned purpose of the present invention is achieved by techniques below scheme:
A kind of white light LEDs nitric oxide fluorescent powder, its chemical composition is Sr3-xB3N3O3: xEu2+；Wherein, x span
It is 0.005～0.20, is made by the steps and forms:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
Boron nitride and the mixture of europium oxide, wherein, x span is 0.005～0.20；
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 in high temperature furnace
Sinter 4～6 hours under the conditions of DEG C, cool down and i.e. obtain described nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.7～0.9% of raw material weight, and described flux is ammonium hydrogen carbonate and fluorination
The weight ratio of the mixture of ammonium, ammonium hydrogen carbonate and ammonium fluoride is 6～8:1.
Further, described white light LEDs nitric oxide fluorescent powder, its chemical composition is Sr3-xB3N3O3: xEu2+；Its
In, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
Boron nitride and the mixture of europium oxide, wherein, x span is 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in reducing atmosphere and 1500 DEG C of conditions in high temperature furnace
Lower sintering 5 hours, cools down and i.e. obtains described nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixed of ammonium hydrogen carbonate and ammonium fluoride
The weight ratio of compound, ammonium hydrogen carbonate and ammonium fluoride is 7:1.
Further, described white light LEDs nitric oxide fluorescent powder, its chemical composition is Sr3-xB3N3O3: xEu2+；Its
In, x value 0.005, it is made by the steps and forms:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
Boron nitride and the mixture of europium oxide, wherein, x value 0.005；
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 DEG C of conditions in high temperature furnace
Lower sintering 6 hours, cools down and i.e. obtains described nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixed of ammonium hydrogen carbonate and ammonium fluoride
The weight ratio of compound, ammonium hydrogen carbonate and ammonium fluoride is 6:1.
Further, described white light LEDs nitric oxide fluorescent powder, its chemical composition is Sr3-xB3N3O3: xEu2+；Its
In, x value 0.20, it is made by the steps and forms:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
Boron nitride and the mixture of 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, in reducing atmosphere and 1600 DEG C of conditions in high temperature furnace
Lower sintering 4 hours, cools down and i.e. obtains described nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.9% of raw material weight, and described flux is the mixed of ammonium hydrogen carbonate and ammonium fluoride
The weight ratio of compound, ammonium hydrogen carbonate and ammonium fluoride is 8:1.
Further, described reducing atmosphere is Carbon monoxide reduction atmosphere.
Advantages of the present invention:
The nitric oxide fluorescent powder transmitting wavelength that the present invention provides, in orange red light region, can substantially increase the aobvious of white light LEDs
Colour index.This fluorescent material good dispersion, grain size is little, and luminous intensity is high, and stability is high, these advantages and carbonic acid in flux
Hydrogen ammonium is relevant with the weight ratio of ammonium fluoride, and when the weight ratio of ammonium hydrogen carbonate and ammonium fluoride 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 the present invention with this and protect model
Enclose.Although the present invention being explained in detail with reference to preferred embodiment, it will be understood by those within the art that, can be right
Technical scheme is modified or equivalent, without deviating from the spirit and scope of technical solution of the present invention.
Embodiment 1: the preparation of nitric oxide fluorescent powder
Chemical composition is Sr3-xB3N3O3: xEu2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
Boron nitride and the mixture of europium oxide, wherein, x span is 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in high temperature furnace in Carbon monoxide reduction atmosphere and
Sinter 5 hours under the conditions of 1500 DEG C, cool down and i.e. obtain described nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixed of ammonium hydrogen carbonate and ammonium fluoride
The weight ratio of compound, ammonium hydrogen carbonate and ammonium fluoride is 7:1.
Embodiment 2: the preparation of nitric oxide fluorescent powder
Chemical composition is Sr3-xB3N3O3: xEu2+；Wherein, x value 0.005, it is made by the steps and forms:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
Boron nitride and the mixture of europium oxide, wherein, x value 0.005；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in high temperature furnace in Carbon monoxide reduction atmosphere and
Sinter 6 hours under the conditions of 1400 DEG C, cool down and i.e. obtain described nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixed of ammonium hydrogen carbonate and ammonium fluoride
The weight ratio of compound, ammonium hydrogen carbonate and ammonium fluoride is 6:1.
Embodiment 3: the preparation of nitric oxide fluorescent powder
Chemical composition is Sr3-xB3N3O3: xEu2+；Wherein, x value 0.20, it is made by the steps and forms:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
Boron nitride and the mixture of 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, in high temperature furnace in Carbon monoxide reduction atmosphere and
Sinter 4 hours under the conditions of 1600 DEG C, cool down and i.e. obtain described nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.9% of raw material weight, and described flux is the mixed of ammonium hydrogen carbonate and ammonium fluoride
The weight ratio of compound, ammonium hydrogen carbonate and ammonium fluoride is 8:1.
Embodiment 4: the preparation of nitric oxide fluorescent powder
Chemical composition is Sr3-xB3N3O3: xEu2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
Boron nitride and the mixture of europium oxide, wherein, x span is 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in high temperature furnace in Carbon monoxide reduction atmosphere and
Sinter 5 hours under the conditions of 1500 DEG C, cool down and i.e. obtain described nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixed of ammonium hydrogen carbonate and ammonium fluoride
The weight ratio of compound, ammonium hydrogen carbonate and ammonium fluoride is 6:1.
Embodiment 5: the preparation of nitric oxide fluorescent powder
Chemical composition is Sr3-xB3N3O3: xEu2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
Boron nitride and the mixture of europium oxide, wherein, x span is 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in high temperature furnace in Carbon monoxide reduction atmosphere and
Sinter 5 hours under the conditions of 1500 DEG C, cool down and i.e. obtain described nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixed of ammonium hydrogen carbonate and ammonium fluoride
The weight ratio of compound, ammonium hydrogen carbonate and ammonium fluoride is 8:1.
The weight ratio of embodiment 6: comparative example, ammonium hydrogen carbonate and ammonium fluoride is 5:1
Chemical composition is Sr3-xB3N3O3: xEu2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
Boron nitride and the mixture of europium oxide, wherein, x span is 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in high temperature furnace in Carbon monoxide reduction atmosphere and
Sinter 5 hours under the conditions of 1500 DEG C, cool down and i.e. obtain described nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixed of ammonium hydrogen carbonate and ammonium fluoride
The weight ratio of compound, ammonium hydrogen carbonate and ammonium fluoride is 5:1.
The weight ratio of embodiment 7: comparative example, ammonium hydrogen carbonate and ammonium fluoride is 9:1
Chemical composition is Sr3-xB3N3O3: xEu2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
Boron nitride and the mixture of europium oxide, wherein, x span is 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in high temperature furnace in Carbon monoxide reduction atmosphere and
Sinter 5 hours under the conditions of 1500 DEG C, cool down and i.e. obtain described nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixed of ammonium hydrogen carbonate and ammonium fluoride
The weight ratio of compound, ammonium hydrogen carbonate and ammonium fluoride is 9:1.
Embodiment 8: effect example
The respectively luminescent properties of the fluorescent material of testing example 1～7 preparation, the exciting and launch of different embodiment fluorescent material
The position of spectrum is basically identical, but luminous intensity, stability of photoluminescence and dispersibility have relatively big difference, result such as table 1.Wherein, send out
Light intensity, 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 | 71 | Unstable | Poor dispersion |
| Embodiment 7 | 73 | Unstable | Poor dispersion |
The test result of embodiment 2,3 is basically identical with embodiment 4,5.
Above-mentioned test result indicate that, the nitric oxide fluorescent powder that the present invention provides launches wavelength in orange red light region, can be bright
The aobvious color rendering index increasing white light LEDs.This fluorescent material good dispersion, luminous intensity is high, and stability is high, these advantages and flux
Middle ammonium hydrogen carbonate is relevant with the weight ratio of ammonium fluoride, and when the weight ratio of ammonium hydrogen carbonate and ammonium fluoride is 6～8:1, luminous intensity is
High.
The effect of above-described embodiment indicates that the essentiality content of the present invention, but does not limit the protection of the present invention with this
Scope.It will be understood by those within the art that, technical scheme can be modified or equivalent,
Essence and protection domain without deviating from technical solution of the present invention.
Claims (5)
1. a white light LEDs nitric oxide fluorescent powder, its chemical composition is Sr3-xB3N3O3:xEu2+；Wherein, x span is
0.005～0.20, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material is strontium carbonate, nitridation
Boron and the mixture of europium oxide, wherein, x span is 0.005～0.20；
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 bars in high temperature furnace
Sinter 4～6 hours under part, cool down and i.e. obtain described nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.7～0.9% of raw material weight, and described flux is ammonium hydrogen carbonate and ammonium fluoride
The weight ratio of mixture, ammonium hydrogen carbonate and ammonium fluoride is 6～8:1.
White light LEDs nitric oxide fluorescent powder the most according to claim 1, its chemical composition is Sr3-xB3N3O3: xEu2+；
Wherein, x value 0.10, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material is strontium carbonate, nitridation
Boron and the mixture of europium oxide, wherein, x span is 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 nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixing of ammonium hydrogen carbonate and ammonium fluoride
The weight ratio of thing, ammonium hydrogen carbonate and ammonium fluoride is 7:1.
White light LEDs nitric oxide fluorescent powder the most according to claim 1, its chemical composition is Sr3-xB3N3O3: xEu2+；
Wherein, x value 0.005, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material is strontium carbonate, nitridation
Boron and the mixture of europium oxide, wherein, x value 0.005；
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 nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixing of ammonium hydrogen carbonate and ammonium fluoride
The weight ratio of thing, ammonium hydrogen carbonate and ammonium fluoride is 6:1.
White light LEDs nitric oxide fluorescent powder the most according to claim 1, its chemical composition is Sr3-xB3N3O3: xEu2+；
Wherein, x value 0.20, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Sr3-xB3N3O3:xEu2+Stoichiometric proportion weigh raw material, described raw material is strontium carbonate, nitridation
Boron and the mixture of 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 nitric oxide fluorescent powder；
Wherein, the addition of flux is the 0.9% of raw material weight, and described flux is the mixing of ammonium hydrogen carbonate and ammonium fluoride
The weight ratio of thing, ammonium hydrogen carbonate and ammonium fluoride is 8:1.
5. according to the arbitrary described white light LEDs nitric oxide fluorescent powder of Claims 1 to 4, it is characterised in that: described reducing gases
Atmosphere is Carbon monoxide reduction atmosphere.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260498A (en) * | 2011-05-17 | 2011-11-30 | 中国计量学院 | Nitric oxide orange red fluorescent powder for white LED (light-emitting diode) and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260498A (en) * | 2011-05-17 | 2011-11-30 | 中国计量学院 | Nitric oxide orange red fluorescent powder for white LED (light-emitting diode) and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 洪广言: "《稀土发光材料——基础与应用》", 30 April 2011, 科学出版社 * |
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Application publication date: 20161116 |