CN105838371A - Nitric oxide fluorescent powder for LED and preparation method - Google Patents
Nitric oxide fluorescent powder for LED and preparation method Download PDFInfo
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- 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
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Abstract
The invention relates to nitric oxide fluorescent powder for an LED and a preparation method .According to the technical scheme, the nitric oxide fluorescent powder is prepared from M3N2, SiO2, Si3N4 and EuN, wherein M represents at least one of Ca, Sr and Ba .The chemical reaction equation for preparing the nitric oxide fluorescent powder for the LED can be seen in the description, and the chemical structural formula of the nitric oxide fluorescent powder for the LED is M1-xEuxSi2O2N2, wherein x is larger than or equal to 0.005 and smaller than or equal to 0.1 .The nitric oxide fluorescent powder has the advantages that the synthesized target fluorescent powder is high in product purity, low in impurity phase purity and more regular in crystal type, and the light-emitting strength is remarkably improved; the effective excitation wavelength of the fluorescent powder is 300-460 nm, the emission spectrum is 480-600 nm, and the application requirements of the high-quality white LED or the colorful LED can be better met .
Description
Technical field
The present invention relates to one and be mainly used in White-light LED illumination, color LED is decorated, and LED backlight of LCD
The preparation method of the nitric oxide fluorescent powder of illumination etc., particularly to a kind of LED nitric oxide fluorescent powder and preparation method.
Background technology
Comparing conventional illumination sources, LED has energy-saving and environmental protection, life-span length, the little many advantages such as encapsulation that are prone to of volume, quilt
It is described as 21 century most promising new light sources, is expected to become after incandescent lamp, fluorescent lamp and high-intensity gas discharge lamp etc.
Forth generation light source.At present, obtain illumination, the main way of ornamental LED is fluorescent material transformation approach, wherein fluorescent material performance
Quality has been largely fixed the height of LED quality.Present stage, the study hotspot of domestic and international LED fluorescent powder is nearly all concentrated
On pure nitride or pure-oxide, such as pure nitride Sr2Si5N8: Eu red fluorescence powder, and pure-oxide (Y, Lu,
Gd)3(Al,Ga)5O12: Ce yellowish green fluorescent powder etc., but these fluorescent material the most more or less existence and stability is poor, and hot-quenching is gone out
The shortcomings such as temperature is relatively low, limit the further lifting of LED quality.Nitric oxide fluorescent powder just can solve this problem,
Therefore, in order to obtain the LED illumination product of high-quality, need to develop physical and chemical performance stable, luminescent properties preferably nitrogen oxides
Fluorescent material.
CaSi2O2N2And SrSi2O2N2It is at CaO-Si at first Deng alkaline-earth metal nitrogen oxides3N4-AlN system and Sr-Si-
O-N system is in the news.2005, H. T. Hintzen et al. was with MCO3(M=Ca, Sr, Ba), SiO2、Si3N4And Eu2O3For
Raw material, has synthesized MSi2O2-δN2+2/3δ:Eu2+(M=Ca, Sr, Ba) fluorescent material, and successfully it is applied to white light LEDs
Making.MSi in early days2O2N2(M=Ca, Sr, Ba) is about two kinds of the preparation path of the phosphor material powder of matrix, a kind of
It is one-step method, i.e. uses MCO3(M=Ca, Sr, Ba), SiO2、Si3N4And Eu2O3For raw material, once sintered shaping.Another kind is then two
Footwork, i.e. first step MCO3(M=Ca, Sr, Ba), SiO2And Eu2O3Reaction first synthesizes mesophase Sr2SiO4: Eu, then
Two steps add Si3N4Sintering obtains M again1-xEuxSi2O2N2(M= Ca, Sr, Ba).What both preparation methods all existed asks
Topic is to be difficult to synthesize pure M1-xEuxSi2O2N2(M=Ca, Sr, Ba) thing phase, Comparatively speaking, the method for two-step sintering obtains
The thing of fluorescent material is the most single, therefore tradition M1-xEuxSi2O2N2The preparation of (M=Ca, Sr, Ba) nitric oxide fluorescent powder
Use two-step method more.Even so, the M of two-step method synthesis1-xEuxSi2O2N2(M=Ca, Sr, Ba) nitric oxide fluorescent powder is also
Owing to there is more dephasign, and causing the luminous intensity of fluorescent material the highest, two-step process is loaded down with trivial details in addition, fluorescence easily occurs
Powder batch is inconsistent, it is difficult to meet the demand of high performance lED encapsulation.
Summary of the invention
The purpose of the present invention is aiming at the drawbacks described above that prior art exists, it is provided that a kind of LED nitrogen oxides fluorescence
Powder and preparation method, it is possible to prepare a kind of physical and chemical performance stable, luminescent properties excellence, and the M without dephasign1-xEuxSi2O2N2
(M=Ca, Sr, Ba) nitrogen oxides LED fluorescent powder, its effective excitation wavelength is positioned at 300 ~ 460nm, and emission spectrum is positioned at 480 ~
600nm, can preferably meet high-quality white light LEDs or the nitric oxide fluorescent powder of color LED application requirement.
Its technical scheme is: include following raw material components: M3N2、SiO2、Si3N4、EuN；Wherein M represents Ca, Sr, Ba tri-kinds
At least one in element, N is nitrogen element, and Eu represents europium element, and Si represents that element silicon, O represent oxygen element；
Described M3N2For Ba3N2、Ca3N2Or Sr3N2；
Described LED nitric oxide fluorescent powder of preparing includes the component of following weight portion: Ba3N257.23 part, SiO223.68
Part, Si3N418.43 parts, EuN0.65 part；
Described LED nitric oxide fluorescent powder of preparing includes the component of following weight portion: Ca3N230.54 part, SiO237.89
Part, Si3N429.48 parts, EuN2.09 part；
Described LED nitric oxide fluorescent powder of preparing includes the component of following weight portion: Sr3N244.44 part, SiO228.99
Part, Si3N422.56 parts, EuN4.00 part；
The chemical equation preparing described LED nitric oxide fluorescent powder is:
The chemical structural formula of described LED nitric oxide fluorescent powder is as follows: M1-xEuxSi2O2N2, wherein 0.005≤x≤0.1.
The preparation method of a kind of LED nitric oxide fluorescent powder, comprises the steps:
A) with Ca3N2、Sr3N2Or Ba3N2, Si3N4, SiO2It is raw material with EuN；
B) in the glove box being filled with argon gas or nitrogen protection, according to the component of described raw material, corresponding raw material is weighed；
C) adding flux in above-mentioned sample, the addition of flux accounts for the 0.5% ~ 7% of raw material gross mass；
D) with raw material, flux being carried out ball milling to mix, the ball mill mixing time is 3 ~ 8 hours, crosses 150 ~ 400 mesh silk screens after mixing
Sieve；
E) above-mentioned sieve after mixture load in corundum crucible, in 1350 ~ 1500 under the nitrogen and hydrogen mixture atmosphere protection of flowing
DEG C calcining 6 ~ 12h, crushes after having sintered, grinds, sieves, pickling, washes and dry, i.e. can get described nitrogen oxides fluorescence
Powder.
Preferably, M3N2Purity ＞ 99.5%；Described EuN purity is more than 99.5%；Described SiO2Purity is more than 99.5%；Described
Si3N4Purity ＞ 99.5%.
Preferably, Si3N4α phase Si that diameter of particle is 50 nanometers to 10 microns3N4, wherein α phase Si3N4Purity ＞ 90%；
Preferably, the atmosphere of sintering furnace is nitrogen and hydrogen mixture, wherein H2Purity be 5% ~ 15%, stream pressure is 0.1MPa, stream
Speed about 30 ~ 80mL/min.
Preferably, maximum sintering temperature is 1350 ~ 1500 DEG C, and temperature retention time is 6 ~ 12h.
Preferably, pickling refers to soak 30 ~ 120min in the acid solution that pH value is 3 ~ 5, miscellaneous with remove in fluorescent material
Matter, then cleans to pH value to neutrality by deionized water, and described acid solution is NH4Cl、BaF2Or KCl.
Preferably, it is 70 ~ 100 DEG C that fluorescent material washes drying temperature, and drying time is 1-3h.
Preferably, flux is the alkali halide of monovalence or the alkaline-earth halide of divalence or ammonia salt, its
The addition of middle flux accounts for the 0.5% ~ 7% of raw material gross mass.
Preferably, wire mesh screens material is non-metallic material.
The invention has the beneficial effects as follows:
(1) the target fluorescent powder product purity synthesized is high, and dephasign purity is low, and crystal formation is more regular, and luminous intensity has obtained significantly carrying
High；
(2) once sintered complete, it is to avoid the sintering process that two-step method is complicated, it is possible to be precisely controlled fluorescent material proportioning, produce
Efficiency is significantly enhanced；
(3) the effective excitation wavelength of fluorescent material is positioned at 300 ~ 460nm, and emission spectrum is positioned at 480 ~ 600nm, can preferably meet height
Quality white light LEDs or color LED application requirement.
Accompanying drawing explanation
Fig. 1 is the Ba of preparation method of the present invention and the acquisition of existing preparation method0.99Eu0.01Si2O2N2The XRD of fluorescent material
Thing compares figure；
Fig. 2 is the Ba of preparation method of the present invention and the acquisition of existing preparation method0.99Eu0.01Si2O2N2The transmitting light of fluorescent material
Spectral intensity comparison diagram；
Fig. 3 is embodiment 1 Ba0.99Eu0.01Si2O2N2Fluorescent material excitation and emission spectra figure；
Fig. 4 is embodiment 3 Sr0.99Eu0.01Si2O2N2The XRD of fluorescent material；
Fig. 5 is embodiment 3 Sr0.99Eu0.01Si2O2N2The excitation and emission spectra figure of fluorescent material.
Detailed description of the invention
In conjunction with accompanying drawing 1-5, the invention will be further described:
The present invention includes following raw material components: M3N2、SiO2、Si3N4、EuN；During wherein M represents tri-kinds of elements of Ca, Sr, Ba extremely
Few one, N is nitrogen element, and Eu represents europium element, and Si represents that element silicon, O represent oxygen element；
Described M3N2For Ba3N2、Ca3N2Or Sr3N2；
Described acid solution is NH4Cl、BaF2Or KCl；
The chemical equation preparing described nitric oxide fluorescent powder is:
The chemical structural formula of described nitric oxide fluorescent powder is as follows: M1-xEuxSi2O2N2, wherein 0.005≤x≤0.1.
The preparation method of LED Nitride phosphor in the present invention is described in detail below with specific embodiment；
Embodiment 1:
In being filled with the glove box of nitrogen or argon shield, weigh Ba respectively3N2(purity is more than 99.5%) 57.23g, SiO2
(purity is more than 99.5%) 23.68g, Si3N4(purity be more than 99.5%) 18.43g, EuN(purity is more than 99.5%) 0.65g and
NH4Cl(purity is more than 99.5%) 1.00g, wherein, Si3N4α phase Si that diameter of particle is 50 nanometers3N4, add in above-mentioned sample
The alkali halide adding monovalence accounts for the 0.5% of raw material gross mass as flux, the addition of flux, in vacuum sphere grinding jar
Middle ball mill mixing 3h；Then crossing 150 mesh wire mesh screens, the material of this wire mesh screens is non-metallic material；By sieving, later raw material mixes
Compound tinning, is placed in H2Purity is 5%, and stream pressure is 0.1MPa, flow velocity about 30mL/min, nitrogen and hydrogen mixture under the conditions of, burn
Junction temperature is 1350 DEG C, and temperature retention time is 6h；Sintered product is after crushing, grind, sieving, in the acid solution that pH value is 3
Soak 120min, to remove the impurity in fluorescent material, then clean to pH value to neutrality by deionized water；Finally, 70
DEG C oven for drying 3h, stoichiometric proportion is Ba0.99Eu0.01Si2O2N2Nitric oxide fluorescent powder.
Embodiment 2:
In being filled with the glove box of nitrogen or argon shield, weigh Ca respectively3N2(purity is more than 99.5%) 30.54g, SiO2
(purity is more than 99.5%) 37.89g, Si3N4(purity is more than 99.5%), 29.48g, EuN(purity was more than 99.5%) 2.09g and KCl
(purity is more than 99.5%) 1.00g, wherein, Si3N4α phase Si that diameter of particle is 1000 nanometers3N4, add in above-mentioned sample
The alkaline-earth halide of divalence accounts for the 4% of raw material gross mass as flux, the addition of flux, in vacuum sphere grinding jar
Ball mill mixing 5h；Then crossing 300 mesh wire mesh screens, the material of this wire mesh screens is non-metallic material；The raw material mixing that will sieve later
Thing tinning, is placed in H2Purity is 10%, and stream pressure is 0.1MPa, under the conditions of the nitrogen and hydrogen mixture of flow velocity about 50mL/min, and sintering
Temperature is 1400 DEG C, and temperature retention time is 9h；Sintered product, after crushing, grind, sieving, soaks in the acid solution that pH value is 4
Bubble 75min, to remove the impurity in fluorescent material, then cleans to pH value to neutrality by deionized water；Finally, 90 DEG C of bakings
Case dry 2h, stoichiometric proportion is Ca0.98Eu0.02Si2O2N2Nitric oxide fluorescent powder.
Embodiment 3:
In being filled with the glove box of nitrogen or argon shield, weigh Sr respectively3N2(purity is more than 99.5%) 44.44g, SiO2
(purity is more than 99.5%) 28.99g, Si3N4(purity is more than 99.5%), 22.56g, EuN(purity was more than 99.5%) 4.00g and BaF2
(purity is more than 99.5%) 1.00g, wherein, Si3N4α phase Si that diameter of particle is 10 microns3N4, above-mentioned sample adds ammonia
Salt accounts for the 7% of raw material gross mass as flux, the addition of flux, ball mill mixing 8h in vacuum sphere grinding jar；Then cross
400 mesh wire mesh screens, the material of this wire mesh screens is non-metallic material；The raw mixture tinning that will sieve later, is placed in H2Purity
Being the nitrogen hydrogen of 15%, stream pressure is 0.1MPa, and under the conditions of flow velocity about 80mL/min gaseous mixture, sintering temperature is 1500 DEG C, insulation
Time is 12h；Sintered product, after crushing, grind, sieving, soaks 30min in the acid solution that pH value is 5, glimmering to remove
Impurity in light powder, then cleans to pH value to neutrality by deionized water；Finally, 100 DEG C of oven for drying 1h,
Stoichiometric proportion is Sr0.95Eu0.05Si2O2N2Nitric oxide fluorescent powder.
The above, be only presently preferred embodiments of the present invention, and any those of ordinary skill in the art are all possibly also with upper
The present invention is revised or is revised as the technical scheme of equivalent by the technical scheme stating elaboration.Therefore, according to the present invention's
Any simple modification that technical scheme is carried out or substitute equivalents, belong to the greatest extent the scope of protection of present invention.
Claims (10)
1. a LED nitric oxide fluorescent powder, is characterized in that: include following raw material components: M3N2、SiO2、Si3N4、EuN；Its
Middle M represents at least one in tri-kinds of elements of Ca, Sr, Ba, and N is nitrogen element, and Eu represents europium element, and Si represents that element silicon, O represent
Oxygen element；
Described M3N2For Ba3N2、Ca3N2Or Sr3N2；
Described LED nitric oxide fluorescent powder of preparing includes the component of following weight portion: Ba3N257.23 part, SiO223.68
Part, Si3N418.43 parts, EuN0.65 part；
Described LED nitric oxide fluorescent powder of preparing includes the component of following weight portion: Ca3N230.54 part, SiO237.89
Part, Si3N429.48 parts, EuN2.09 part；
Described LED nitric oxide fluorescent powder of preparing includes the component of following weight portion: Sr3N244.44 part, SiO228.99
Part, Si3N422.56 parts, EuN4.00 part；
The chemical equation preparing described LED nitric oxide fluorescent powder is:
The chemical structural formula of described LED nitric oxide fluorescent powder is as follows: M1-xEuxSi2O2N2, wherein 0.005≤x≤0.1.
The preparation method of a kind of LED nitric oxide fluorescent powder the most according to claim 1, it is characterised in that: include as
Lower step:
A) with Ca3N2、Sr3N2Or Ba3N2, Si3N4, SiO2It is raw material with EuN；
B) in the glove box being filled with argon gas or nitrogen protection, according to the ingredients weight parts of described raw material, corresponding raw material is weighed；
C) adding flux in above-mentioned sample, the addition of flux accounts for the 0.5% ~ 7% of raw material gross mass；
D) with raw material, flux being carried out ball milling to mix, the ball mill mixing time is 3 ~ 8 hours, crosses 150 ~ 400 mesh silk screens after mixing
Sieve；
E) above-mentioned sieve after mixture load in corundum crucible, in 1350 ~ 1500 under the nitrogen and hydrogen mixture atmosphere protection of flowing
DEG C calcining 6 ~ 12h, crushes after having sintered, grinds, sieves, pickling, washes and dry, i.e. can get described nitrogen oxides fluorescence
Powder.
3., according to the preparation method of a kind of LED nitric oxide fluorescent powder described in claim 2, it is characterized by: described M3N2Pure
Degree ＞ 99.5%；Described EuN purity is more than 99.5%；Described SiO2Purity is more than 99.5%；Described Si3N4Purity ＞ 99.5%.
4., according to the preparation method of a kind of LED nitric oxide fluorescent powder described in claim 1, it is characterized by: described Si3N4
α phase Si that diameter of particle is 50 nanometers to 10 microns3N4, wherein α phase Si3N4Purity ＞ 90%.
5. according to the preparation method of a kind of nitric oxide fluorescent powder described in claim 2, it is characterized by: the gas of described sintering furnace
Atmosphere is nitrogen and hydrogen mixture, wherein H2Purity be 5% ~ 15%, stream pressure is 0.1MPa, flow velocity about 30 ~ 80mL/min.
6., according to the preparation method of a kind of LED nitric oxide fluorescent powder described in claim 2, it is characterized by: described
High sintering temperature is 1350 ~ 1500 DEG C, and temperature retention time is 6 ~ 12h.
7., according to the preparation method of a kind of LED nitric oxide fluorescent powder described in claim 2, it is characterized by: described pickling
Refer to soak 30 ~ 120min in the acid solution that pH value is 3 ~ 5, to remove the impurity in fluorescent material, then clear by deionized water
Being washed till pH value to neutrality, described acid solution is NH4Cl、BaF2Or KCl.
8., according to the preparation method of a kind of LED nitric oxide fluorescent powder described in claim 2, it is characterized by: described is glimmering
It is 70 ~ 100 DEG C that light powder washes drying temperature, and drying time is 1-3h.
9., according to the preparation method of a kind of LED nitric oxide fluorescent powder described in claim 2, it is characterized by: described helps
Flux is the alkali halide of monovalence or the alkaline-earth halide of divalence or ammonia salt, and wherein the addition of flux accounts for
The 0.5% ~ 7% of raw material gross mass.
10., according to the preparation method of a kind of LED nitric oxide fluorescent powder described in claim 2, it is characterized by, described silk screen
Sieve material is non-metallic material.
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| CN109111924A (en) * | 2018-09-18 | 2019-01-01 | 江苏锐阳照明电器设备有限公司 | A kind of LED light fluorescent powder and preparation method thereof that can improve yields |
| CN109233835A (en) * | 2018-09-18 | 2019-01-18 | 江苏锐阳照明电器设备有限公司 | A kind of LED light fluorescent powder and preparation method thereof can be reduced the reaction time |
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