CN102260498A - Nitric oxide orange red fluorescent powder for white LED (light-emitting diode) and preparation method thereof - Google Patents
Nitric oxide orange red fluorescent powder for white LED (light-emitting diode) and preparation method thereof Download PDFInfo
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- CN102260498A CN102260498A CN201110126493XA CN201110126493A CN102260498A CN 102260498 A CN102260498 A CN 102260498A CN 201110126493X A CN201110126493X A CN 201110126493XA CN 201110126493 A CN201110126493 A CN 201110126493A CN 102260498 A CN102260498 A CN 102260498A
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Abstract
The invention discloses a nitric oxide orange red fluorescent powder for a white LED (light-emitting diode) and a preparation method thereof. The chemical expression formula of the fluorescent powder is as follows: Sr3-xB3N3O3:xEu<2+>, wherein in the formula, x is equal to 0.001-0.10. The preparation method comprises the following steps: adding a fluxing agent into raw materials such as carbonate, nitride, oxide of elements in the chemical expression formula and the like, grinding and evenly mixing so as to obtain a mixture; and then sintering the mixture for 3-7 hours at the temperature of 1400-1600 DEG C at the reduction atmosphere so as to obtain the orange red fluorescent powder for the LED. The obtained orange red fluorescent powder emits orange red light under the excitation of an ultraviolet light, purple light or blue light chip, and the emission peak value is located near the wavelength of 610 nm. The fluorescent powder has good chemical stability and wide excitation band, the excitation band of the fluorescent powder can cover ultraviolet light, purple light and blue light regions, and the fluorescent powder can be used as a red fluorescent powder for a near ultraviolet or blue LED.
Description
Technical field
The present invention relates to rare earth luminescent material technical field, especially relate to a kind of white light LEDs oxynitride orange red fluorescent powder and manufacture method thereof.
Background technology
White light LEDs is a kind of solid-state semiconductor device that converts electrical energy into white light, claim semiconductor lighting again, have the efficient height, plurality of advantages such as volume is little, the life-span is long, safety, low voltage, energy-saving and environmental protection, by people regard as after incandescent light, luminescent lamp, high-voltage gas discharging light the 4th generation lighting source, be the main product on the following illumination market.
Occurred various white light LEDs preparation methods at present, wherein blue-light LED chip and yellow fluorescent material combination, blue-light LED chip and redness and green fluorescent material combination, purple LED chip and fluorescent material with three basic colour make up the main method that these three kinds of methods are low with price, preparation simply becomes the preparation white light LEDs.The combination of blue-light LED chip and yellow fluorescent material is that to study also be the most sophisticated method the earliest, and the white light LEDs luminous efficiency of preparation is considerably beyond incandescent light, but colour rendering index is low, and the colour temperature height can not use as interior lighting.In order to improve the color developing of white light LEDs, the various countries scientist has researched and developed the methods that blue-light LED chip and red, green fluorescent material combination and purple LED chip and red, green, blue fluorescent material with three basic colour make up other two kinds of realization white light LEDs.Adopt the white light LEDs color developing of purple LED chip and fluorescent material with three basic colour combination to be improved significantly, but the high-level efficiency fluorescent material also relatively lacks, exist color to absorb again and proportioning regulation and control problem between the fluorescent material, and purple LED chip technology of preparing is immature, domesticly also be in the laboratory study stage, these factors cause near ultraviolet conversion hysteria white light LEDs to be difficult to obtain large-scale application in a short time.The mode that blue-light LED chip excites is red, the green fluorescence material obtains white light LEDs has the advantage of preceding dual mode: employing be blue-light LED chip, this type of chip is studied maturation both at home and abroad, has obtained large-scale application; The blue light that is sent by chip mixes with ruddiness and the green glow that fluorescent material is changed out, generates white light, has good color reducibility, meets the human vision requirement.
Will seek out fast development by white light LEDs red, the preparation of green fluorescent material coupling blue-light LED chip, one of them key factor is to obtain high quality red, green fluorescent material.At present, it is ripe that green emitting phosphor has been tending towards, and still, high brightness, the red fluorescence powder that chemical stability is good still lack at present.In recent years, the researchist is primarily focused on Ce
3+Perhaps Eu
2+Activated sulfide, nitride, silicate and phosphoric acid salt.Sulfide is as (Ca
1-
x Sr
x ) S:Eu
2+Red fluorescence material, but sulfide instability at high temperature decompose easily, the toxigenicity material, and the white light LEDs life-span of preparation is short, and does not meet environmental requirement.Nitride such as Sr
2Si
5N
8: Eu
2+Deng red fluorescence material (seeing U.S. Pat 6649946), these materials have good fluorescent characteristic, but easy and air and steam reaction of alkaline-earth nitride in the raw material, complicated process of preparation, the powder purity that makes is low, at present can't scale operation.Silicate such as Sr
3SiO
5Yellow or orange fluorescent powder (seeing U.S. Pat 20070029526A1), although such fluorescent material has good chemical stability and thermostability, and the high-purity silicon dioxide raw material inexpensive, be easy to get, maturing temperature is than characteristics such as aluminates system are low, but it can not effectively be excited by blue chip, and emission wavelength peak is in the gold-tinted zone.Phosphoric acid salt such as Ca
4(PO
4)
2O:Eu
2+Red fluorescence powder (seeing Chinese patent ZL 200710055669.0), although its blue chip effectively excites, and emission wavelength peak is in the ruddiness zone, the luminous efficiency of phosphate phosphor is low, poor heat stability.
Summary of the invention
The purpose of this invention is to provide a kind of white light LEDs oxynitride orange red fluorescent powder and preparation method thereof and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is: its white light LEDs has following chemical expression formula with the oxynitride orange red fluorescent powder:
Sr
3?–xB
3N
3O
3：xEu
2+
In the formula, x is 0.001～0.10.
The preparation method of oxynitride orange red fluorescent powder of the present invention comprises the steps:
Press chemical formula Sr
3 – xB
3N
3O
3: xEu
2+Stoichiometric ratio take by weighing corresponding raw material, described raw material is respectively Strontium carbonate powder, boron nitride and europium sesquioxide, wherein x is 0.001～0.10; The back adds fusing assistant grinding mixing and obtains mixture; With this mixture crucible of packing into, in High Temperature Furnaces Heating Apparatus under reducing atmosphere and 1400～1600 ℃ of conditions sintering 3～7 hours, postcooling obtains described oxynitride orange red fluorescent powder to room temperature.
Further, fusing assistant of the present invention is any in boric acid, ammonium chloride, Neutral ammonium fluoride, Calcium Fluoride (Fluorspan), magnesium fluoride, the Sodium Fluoride, and the quality of described fusing assistant is 0.01～10:100 with the ratio of the total mass of described raw material.
Further, reducing atmosphere of the present invention is nitrogen and hydrogen mixture or CO atmosphere.
Compared with prior art, the invention has the beneficial effects as follows:
(1) oxynitrides fluorescent material of the present invention has following advantage: have splendid heat stable property, be compared to oxide fluorescent material commonly used, because the long-time heat that produces of using decays, the conversion quantum efficiency of fluorescent material of the present invention is still kept certain efficient when high temperature.Have oxidation-resistance and erosion resistance, be difficult for influencing luminosity with other material generation chemical reaction, life-time service still can be kept color saturation, and hardness is higher and have a wear-resisting property.
(2) oxynitride orange red fluorescent powder of the present invention is compared sulfide red fluorescent material, has the advantage of the good and long service life of chemical stability.Compare nitride red fluorescent powder, have raw material and be easy to get and the simple advantage of preparation technology.Compare silicate yellow fluorescent powder, have the long advantage of transmitted wave.Compare phosphate red fluorescent powder, have the high advantage of good stability and luminous efficiency.
(3) oxynitrides fluorescent material of the present invention is than other oxynitride, as Eu
2+Activated sialon fluorescent powder (seeing Chinese patent literature 200610111986.4) and silicon oxynitride (seeing american documentation literature US 20030168643), has longer emission wavelength, its emission wavelength can obviously increase the colour rendering index of white light LEDs in orange red light zone.
Description of drawings
Fig. 1 is the fluorescent powder exciting light spectrogram of embodiment 1 preparation provided by the invention;
Fig. 2 is the fluorescent powder emmission spectrum figure of embodiment 1 preparation provided by the invention;
Fig. 3 is the fluorescent powder temperature cancellation curve of embodiment 1 preparation provided by the invention;
Fig. 4 is the fluorescent powder emmission spectrum figure of embodiment 2 preparations provided by the invention.
Embodiment
Embodiment 1:
According to Sr
2.95B
3N
3O
3: 0.05Eu
2+Take by weighing raw material SrCO
38.3952g, BN 1.4352g and Eu
2O
30.1696g, add 0.001g fusing assistant boric acid (quality of fusing assistant is 0.01:100 with the ratio of the total mass of all raw materials), after abundant ground and mixed is even, place in the corundum crucible, put into again High Temperature Furnaces Heating Apparatus under CO atmosphere 1600 ℃ of roastings 3 hours, postcooling obtains the oxynitride orange red fluorescent powder to room temperature.As can be seen from Figure 1, fluorescent material excitation spectrum of the present invention is a wide range, has covered ultraviolet, purple light and blue light region, and excitation peak is positioned near the 410nm, and the spectrum peak height illustrates that fluorescent material of the present invention can effectively be excited by blue light or purple light chip.When the excitation wavelength of emmission spectrum is 410nm, as can be seen from Figure 2, the orange red light emission in the broadband that is emitted as divalent europium of fluorescent material of the present invention, emission peak is positioned near the 610nm, illustrates that fluorescent material of the present invention is fit to do blue light or purple light excited orange red fluorescent powder.As can be seen from Figure 3, fluorescent material of the present invention is when 300 ℃ of high temperature, and 85% when its luminous intensity only decays to room temperature illustrates that fluorescent material of the present invention has fabulous stability.
Embodiment 2:
According to Sr
2.999B
3N
3O
3: 0.001Eu
2+Take by weighing raw material SrCO
38.5575g, BN 1.4391g and Eu
2O
30.0034 g, add 1g fusing assistant ammonium chloride (quality of fusing assistant is 10:100 with the ratio of the total mass of all raw materials), after abundant ground and mixed is even, place in the corundum crucible, put into again High Temperature Furnaces Heating Apparatus under CO atmosphere 1400 ℃ of roastings 7 hours, postcooling obtains the oxynitride orange red fluorescent powder to room temperature.Fluorescent material excitation spectrum of the present invention is a wide range, has covered ultraviolet, purple light and blue light region, and excitation peak is positioned near the 410nm, and the spectrum peak height illustrates that fluorescent material of the present invention can effectively be excited by blue light or purple light chip.When the excitation wavelength of emmission spectrum is 410nm, as can be seen from Figure 4, the orange red light emission in the broadband that is emitted as divalent europium of fluorescent material of the present invention, emission peak is positioned near the 600nm, illustrates that fluorescent material of the present invention is fit to do blue light or purple light excited orange red fluorescent powder.Fluorescent material of the present invention in addition has fabulous stability.
Embodiment 3:
According to Sr
2.9B
3N
3O
3: 0.1Eu
2+Take by weighing raw material SrCO
38.2304 g, BN 1.4313 g and Eu
2O
30.3383 g adds 0.01g fusing assistant Neutral ammonium fluoride (quality of fusing assistant is 0.1:100 with the ratio of the total mass of all raw materials), after abundant ground and mixed is even, places in the corundum crucible, puts into High Temperature Furnaces Heating Apparatus again in 5%H
2+ 95%N
21500 ℃ of roastings 5 hours, postcooling obtained the oxynitride orange red fluorescent powder to room temperature under the nitrogen and hydrogen mixture atmosphere of (volume ratio).Fluorescent material excitation spectrum of the present invention is a wide range, has covered ultraviolet, purple light and blue light region, and excitation peak is positioned near the 410nm, and the spectrum peak height illustrates that fluorescent material of the present invention can effectively be excited by blue light or purple light chip.When the excitation wavelength of emmission spectrum is 410nm, the orange red light emission in the broadband that is emitted as divalent europium of fluorescent material of the present invention, emission peak is positioned near the 615nm, illustrates that fluorescent material of the present invention is fit to do blue light or purple light excited orange red fluorescent powder.Fluorescent material of the present invention in addition has fabulous stability.
Embodiment 4:
According to Sr
2.99B
3N
3O
3: 0.01Eu
2+Take by weighing raw material SrCO
38.5276 g, BN 1.4384 g and Eu
2O
30.0340 g adds 0.005g fusing assistant Calcium Fluoride (Fluorspan) (quality of fusing assistant is 0.05:100 with the ratio of the total mass of all raw materials), after abundant ground and mixed is even, places in the corundum crucible, puts into High Temperature Furnaces Heating Apparatus again in 5%H
2+ 95%N
21550 ℃ of roastings 5 hours, postcooling obtained the oxynitride orange red fluorescent powder to room temperature under the nitrogen and hydrogen mixture atmosphere of (volume ratio).Fluorescent material excitation spectrum of the present invention is a wide range, has covered ultraviolet, purple light and blue light region, and excitation peak is positioned near the 410nm, and the spectrum peak height illustrates that fluorescent material of the present invention can effectively be excited by blue light or purple light chip.When the excitation wavelength of emmission spectrum is 410nm, the orange red light emission in the broadband that is emitted as divalent europium of fluorescent material of the present invention, emission peak is positioned near the 610nm, illustrates that fluorescent material of the present invention is fit to do blue light or purple light excited orange red fluorescent powder.Fluorescent material of the present invention in addition has fabulous stability.
Embodiment 5:
According to Sr
2.98B
3N
3O
3: 0.02Eu
2+Take by weighing raw material SrCO
38.4945 g, BN 1.4376g and Eu
2O
30.0680 g adds 0.5g fusing assistant magnesium fluoride (quality of fusing assistant is 5:100 with the ratio of the total mass of all raw materials), after abundant ground and mixed is even, places in the corundum crucible, puts into High Temperature Furnaces Heating Apparatus again in 5%H
2+ 95%N
21450 ℃ of roastings 6 hours, postcooling obtained the oxynitride orange red fluorescent powder to room temperature under the nitrogen and hydrogen mixture atmosphere of (volume ratio).Fluorescent material excitation spectrum of the present invention is a wide range, has covered ultraviolet, purple light and blue light region, and excitation peak is positioned near the 410nm, and the spectrum peak height illustrates that fluorescent material of the present invention can effectively be excited by blue light or purple light chip.When the excitation wavelength of emmission spectrum is 410nm, the orange red light emission in the broadband that is emitted as divalent europium of fluorescent material of the present invention, emission peak is positioned near the 610nm, illustrates that fluorescent material of the present invention is fit to do blue light or purple light excited orange red fluorescent powder.Fluorescent material of the present invention in addition has fabulous stability.
Embodiment 6:
According to Sr
2.995B
3N
3O
3: 0.005Eu
2+Take by weighing raw material SrCO
38.5442 g, BN 1.4388g and Eu
2O
30.0170 g adds 0.02g fusing assistant Sodium Fluoride (quality of fusing assistant is 0.2:100 with the ratio of the total mass of all raw materials), after abundant ground and mixed is even, places in the corundum crucible, puts into High Temperature Furnaces Heating Apparatus again in 5%H
2+ 95%N
21500 ℃ of roastings 6 hours, postcooling obtained the oxynitride orange red fluorescent powder to room temperature under the nitrogen and hydrogen mixture atmosphere of (volume ratio).Fluorescent material excitation spectrum of the present invention is a wide range, has covered ultraviolet, purple light and blue light region, and excitation peak is positioned near the 410nm, and the spectrum peak height illustrates that fluorescent material of the present invention can effectively be excited by blue light or purple light chip.When the excitation wavelength of emmission spectrum is 410nm, the orange red light emission in the broadband that is emitted as divalent europium of fluorescent material of the present invention, emission peak is positioned near the 605nm, illustrates that fluorescent material of the present invention is fit to do blue light or purple light excited orange red fluorescent powder.Fluorescent material of the present invention in addition has fabulous stability.
The foregoing description is used for the present invention that explains, rather than limits the invention, and in the protection domain of spirit of the present invention and claim, any modification and change to the present invention makes all fall into protection scope of the present invention.
Claims (4)
1. a white light LEDs oxynitride orange red fluorescent powder is characterized in that, this fluorescent material has following chemical expression formula:
Sr
3 – xB
3N
3O
3: xEu
2+, wherein, x is 0.001～0.10.
2. the preparation method of the described oxynitride orange red fluorescent powder of claim 1 is characterized in that comprising the steps:
Press chemical formula Sr
3 – xB
3N
3O
3: xEu
2+Stoichiometric ratio take by weighing corresponding raw material, described raw material is respectively Strontium carbonate powder, boron nitride and europium sesquioxide, wherein x is 0.001～0.10; The back adds fusing assistant grinding mixing and obtains mixture; With this mixture crucible of packing into, in High Temperature Furnaces Heating Apparatus under reducing atmosphere and 1400～1600 ℃ of conditions sintering 3～7 hours, postcooling obtains described oxynitride orange red fluorescent powder to room temperature.
3. the preparation method of oxynitride orange red fluorescent powder as claimed in claim 2, it is characterized in that: described fusing assistant is any in boric acid, ammonium chloride, Neutral ammonium fluoride, Calcium Fluoride (Fluorspan), magnesium fluoride, the Sodium Fluoride, and the quality of described fusing assistant is 0.01～10:100 with the ratio of the total mass of described raw material.
4. as the preparation method of claim 2 or 3 described oxynitride orange red fluorescent powders, it is characterized in that: described reducing atmosphere is nitrogen and hydrogen mixture or CO atmosphere.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131946A (en) * | 2015-09-24 | 2015-12-09 | 重庆文理学院 | Blue fluorescent powder for white-light LED (Light Emitting Diode) and preparation method of blue fluorescent powder |
| CN105131944A (en) * | 2015-09-14 | 2015-12-09 | 中国计量学院 | Yellow nitric oxide fluorescent powder for white-light LED (light emitting diode) and preparation method thereof |
| WO2016055140A1 (en) * | 2014-10-09 | 2016-04-14 | Merck Patent Gmbh | Phosphors |
| CN106118640A (en) * | 2016-06-24 | 2016-11-16 | 东台市天源荧光材料有限公司 | A kind of white light LEDs nitric oxide fluorescent powder and preparation method thereof |
| CN106118639A (en) * | 2016-06-24 | 2016-11-16 | 东台市天源荧光材料有限公司 | A kind of white light LEDs nitrogen oxides orange red fluorescent powder and preparation method thereof |
| CN106190117A (en) * | 2016-06-28 | 2016-12-07 | 东台市天源荧光材料有限公司 | The nitric oxide fluorescent powder of a kind of manganese ion doping and preparation method thereof Preparation Method |
| CN112500859A (en) * | 2020-08-21 | 2021-03-16 | 徐州安达科技有限公司 | Preparation method of red fluorescent powder |
| CN112961677A (en) * | 2021-02-03 | 2021-06-15 | 杭州电子科技大学 | Broadband near-infrared emission fluorescent powder capable of being excited by blue light and preparation method thereof |
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| US20060049414A1 (en) * | 2004-08-19 | 2006-03-09 | Chandran Ramachandran G | Novel oxynitride phosphors |
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2011
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Patent Citations (1)
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| US20060049414A1 (en) * | 2004-08-19 | 2006-03-09 | Chandran Ramachandran G | Novel oxynitride phosphors |
Non-Patent Citations (1)
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016055140A1 (en) * | 2014-10-09 | 2016-04-14 | Merck Patent Gmbh | Phosphors |
| CN106795430A (en) * | 2014-10-09 | 2017-05-31 | 默克专利有限公司 | Phosphor |
| CN105131944A (en) * | 2015-09-14 | 2015-12-09 | 中国计量学院 | Yellow nitric oxide fluorescent powder for white-light LED (light emitting diode) and preparation method thereof |
| CN105131946A (en) * | 2015-09-24 | 2015-12-09 | 重庆文理学院 | Blue fluorescent powder for white-light LED (Light Emitting Diode) and preparation method of blue fluorescent powder |
| CN106118640A (en) * | 2016-06-24 | 2016-11-16 | 东台市天源荧光材料有限公司 | A kind of white light LEDs nitric oxide fluorescent powder and preparation method thereof |
| CN106118639A (en) * | 2016-06-24 | 2016-11-16 | 东台市天源荧光材料有限公司 | A kind of white light LEDs nitrogen oxides orange red fluorescent powder and preparation method thereof |
| CN106190117A (en) * | 2016-06-28 | 2016-12-07 | 东台市天源荧光材料有限公司 | The nitric oxide fluorescent powder of a kind of manganese ion doping and preparation method thereof Preparation Method |
| CN112500859A (en) * | 2020-08-21 | 2021-03-16 | 徐州安达科技有限公司 | Preparation method of red fluorescent powder |
| CN112961677A (en) * | 2021-02-03 | 2021-06-15 | 杭州电子科技大学 | Broadband near-infrared emission fluorescent powder capable of being excited by blue light and preparation method thereof |
| CN112961677B (en) * | 2021-02-03 | 2022-06-14 | 杭州电子科技大学 | Broadband near-infrared emission fluorescent powder capable of being excited by blue light and preparation method thereof |
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Application publication date: 20111130 Assignee: Zhejiang Emitting Optoelectronic Technology Co., Ltd. Assignor: China Jiliang University Contract record no.: 2016330000034 Denomination of invention: Nitric oxide orange red fluorescent powder for white LED (light-emitting diode) and preparation method thereof Granted publication date: 20130918 License type: Common License Record date: 20160317 |
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Effective date of registration: 20160523 Address after: 1, 1701, International Building, No. 998 Binhe Road, Changhe street, Binjiang District, Zhejiang, Hangzhou, 310052 Patentee after: Hangzhou norgas Photoelectric Technology Co., Ltd. Address before: Hangzhou City, Zhejiang province 310018 Xiasha Higher Education Park source Street No. 258 Patentee before: China Jiliang University |