CN106147759A - A kind of white light LEDs borate substrate fluorescent powder and preparation method thereof - Google Patents
A kind of white light LEDs borate substrate fluorescent powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of white light LEDs borate substrate fluorescent powder and preparation method thereof.This technique uses high temperature solid-state method to prepare NaSr1‑x‑y‑zCexSmyTbzBO3Single-matrix fluorescent material, wherein the span of x, y and z is 0≤x≤0.10,0≤y≤0.40,0≤z≤0.40, raw materials used for highly purified Na2CO3、SrCO3、H3BO3、CeO2、Tb4O7、Sm2O3.Gained fluorescent material emits white light under ultraviolet excitation, and can be by regulation doping Ce3+、Sm3+、Tb3+The purity of ion concentration regulation white light.Preparation method technique of the present invention is simple, and synthesis reaction temperature is low, gained NaSrBO3: the chromaticity coordinates of Ce, Sm, Tb fluorescent material can be by regulation Ce3+、Tb3+、Sm3+Doping content adjust, luminous efficiency is high, and Heat stability is good has the white light LEDs application prospect being applied to burst of ultraviolel.
Description
Technical field
The invention belongs to field of light emitting materials, particularly to a kind of white light LEDs single-matrix fluorescent material of preparation
And preparation method thereof.
Background technology
Light emitting diode (Light Emitting Diodes, LED) is that the New Solid that developed recently gets up shines
Funerary objects part, because having efficiency height, life-span length, the advantage such as energy-conservation, pollution-free, has broad application prospects
And potential market, by the extensive concern of countries in the world, it is considered 21 century green illumination light source.
At present, changed the mechanism by fluorescent material and realize white light LEDs and mainly have two kinds of methods.One is to use blue light
LED coordinates the fluorescent material of Yellow light-emitting low temperature, is compounded to form white light.At present, this scheme is in technology and technique the most
Through the most ripe, it it is the main product of industrialization.But there is energy loss, no in the white light that this method obtains
Easily realizing low colour temperature, cause its color rendering index the highest owing to lacking HONGGUANG in spectral component, color reproducibility is poor.
It addition, except YAG:Ce3+With some organic fluorescent powders, the yellow fluorescent powder that alternative luminous efficiency is high
Relatively fewer.Another kind is the LED chip deexcitation red, green, blue three primary colors fluorescent powder using black light
Obtain white light.The advantage of the method is the abundant species that high-efficiency fluorescence powder selects, and can obtain specular removal, high
Color rendering index and various correlated color temperature are alternative strong.But, due to emission spectrum between different fluorescent material
Overlap and there is weight absorbing phenomenon, thus cause luminous efficiency to decline；And the proportioning regulation and control problem of fluorescent material is also
It is difficult to solve.
But, the single-matrix white fluorescent powder of near ultraviolet excitation can directly send white light, and these are many with other
The fluorescent material of matrix system is compared, and has significant advantage.First, the vision of the mankind is to black light region
And insensitive, the color of fluorescent material depends entirely on the luminescence of white light LEDs, thus colour stable, Ke Yishi
Existing high color reducibility；Secondly, single-matrix compound can avoid spectrum heavily to absorb the energy loss caused,
Improve luminous efficiency；Again, single-matrix system can be effectively prevented from making because multiple substrate interacts
The color detuning phenomena become, thus improve color rendering index；Finally, cheap cost is also single-matrix white
One considerable advantage of fluorescent material.
The present invention i.e. provide a kind of can be by the single-matrix white emitting phosphor of ultraviolet excitation.
Summary of the invention
It is an object of the invention to provide a kind of can be by the single borate matrix white light emission of ultraviolet excitation
Fluorescent material and its production and use.
The object of the invention is achieved through the following technical solutions:
The borate single-matrix white light emitting phosphor that a kind of cerium, samarium and three kinds of rare earth ions of terbium are co-doped with,
Its ingredient formula is NaSr1-x-y-zCexSmyTbzBO3, wherein 0 < x≤0.10,0 < y≤0.40,0 < z
≤0.40。
According to the present invention, in the fluorescent material of described doping, cerium, samarium and three kinds of rare earth ions of terbium be trivalent from
Son, it may be assumed that NaSr1-x-y-zBO:xCe3+,ySm3+,zTb3+。
According to the present invention, wherein, it is preferred that 0.005≤x≤0.08, the most preferably 0.01≤x≤0.04；Excellent
Choosing, 0.005≤y≤0.20, the most preferably 0.05≤y≤0.10；Preferably, 0.005≤z≤0.30, the most excellent
Choosing, 0.05≤z≤0.20, more there are choosing, 0.05≤z≤0.08.
According to the present invention, the molecular formula of described fluorescent material is NaSr1-x-y-zCexSmyTbzBO3, wherein x is
0.01, y is 0.05, and z is 0.05-0.08.
Present invention also offers the preparation method of above-mentioned white light emitting phosphor, it comprises the following steps:
(1) by Na2CO3、SrCO3、H3BO3、CeO2、Sm2O3、Tb4O7Mix, each former
The mol ratio of material controls at 0.5:1-x-y-z:(1-1.2): x:y:z, wherein 0 < x≤0.10,0 < y≤0.40,0 <
z≤0.40；
(2) the above-mentioned raw material mixed is mixed with organic solvent, then grind, be dried, by dried former
Material is calcined in 300-650 DEG C；
(3) by the material obtained in above-mentioned steps (2) again 800-950 DEG C, burn under reducing atmosphere
Knot.
According to the present invention, in described step (1), described raw material Na2CO3、SrCO3、H3BO3、CeO2、
Sm2O3、Tb4O7For highly purified, its purity is higher than 99%, preferably above 99.9%, more preferably higher than
99.99%.The mixing of each material is preferably carried out in agate mortar.
According to the present invention, wherein, it is preferred that 0.005≤x≤0.08, the most preferably 0.01≤x≤0.04；Excellent
Choosing, 0.005≤y≤0.20, the most preferably 0.05≤y≤0.10；Preferably, 0.005≤z≤0.30, the most excellent
Choosing, 0.05≤z≤0.20, more there are choosing, 0.05≤z≤0.08.
According to the present invention, in described step (1), preferably add H3BO3As flux, further preferably
, the molar contents that add are the H of 5% more3BO3As flux, it may be assumed that Na2CO3、SrCO3、
H3BO3、CeO2、Sm2O3、Tb4O7Mol ratio be 0.5:1-x-y-z:1.05:x:y:z.
According to the present invention, in described step (2), described organic solvent can be acetone, ethanol etc., described in grind
Mill is to be fully ground in ball grinder.
According to the present invention, in described step (2), wherein said calcining is preferably carried out in high temperature Muffle furnace.
The temperature of described calcining is preferably 400-500 DEG C；The time of calcining is preferably 1-20 hour, more preferably 5-10
Hour.
According to the present invention, in described step (3), before sintering, the material that first will obtain in step (2)
It is ground, is sintered the most again；Described grinding is preferably carried out in Achates crucible；
According to the present invention, in described step (3), described in be sintered in high-temperature atmosphere tube furnace carrying out, described
The temperature of sintering is preferably 850-900 DEG C.Described reducing atmosphere is N2And H2Gaseous mixture；
According to the present invention, in described step (3), by the product cooling after sintering, grind, wash (preferably
Repeatedly), it is vacuum dried, after being ground the most again, crosses 200 mesh sieves, obtain described white light and launch fluorescence
Powder.
According to the present invention, the borate single-matrix white light that described cerium, terbium and three kinds of rare earth ions of samarium are co-doped with
The preparation method of emitting phosphor, comprises the following steps:
(1) Na is taken2CO3、SrCO3、H3BO3、CeO2、Sm2O3、Tb4O7Put into agate mortar,
The mol ratio of each raw material controls at 0.5:1-x-y-z:1.05:x:y:z, and wherein x is 0.01, and y is 0.05, and z is
0.05-0.08；
(2) the above-mentioned raw material mixed is added acetone, grind in ball grinder, be placed on drying baker afterwards
In to be dried, remove acetone, transfer to, in corundum crucible, put in high temperature Muffle furnace by dried raw material
Calcining；
(3) semi-finished product of gained after above-mentioned first sintering are put in Achates crucible grind further；Grind
Gained semi-finished product transfer to corundum crucible, and under reducing atmosphere, in high temperature process furnances, under the conditions of 850 DEG C, secondary burns
Knot, reducing atmosphere is N2And H2Gaseous mixture；
(4) after reaction terminates, it is cooled to room temperature, takes out sample process and grind, repeatedly wash, be vacuum dried,
Gained sample obtains target product after crossing 200 mesh sieves after grinding.
White light LEDs borate single-matrix fluorescent material prepared by the present invention can be by the black light of 360nm
Excite, send white light.X-ray diffraction (XRD) spectrogram of this fluorescent material and NaSrBO3Standard card
ICSD-170420 is consistent, shows that the sample of synthesis is pure phase.There are three positions in the emission spectrum of this fluorescent material
In the emission peak of 424nm, 543nm, 646nm, they are respectively belonging to Ce3+、Tb3+、Sm3+Special
Levy emission spectrum；The bands of a spectrum superposition of three wave bands blue, green, red thus in single-matrix, achieve white light send out
Penetrate.By regulation Ce3+、Sm3+、Tb3+The doping content of ion, thus it is possible to vary the chromaticity coordinates of fluorescent material,
The purity of regulation white light.The light-emitting phosphor efficiency of the present invention is high, and Heat stability is good can apply to ultraviolet
In the white light LEDs excited.
Present invention also offers above-mentioned white light emitting phosphor purposes in LED.
Relative to prior art, present invention have an advantage that
(1) the white light emission fluorescent material of the present invention is single-matrix, and it can emit white light under ultraviolet excitation,
And can be by regulation doping Ce3+、Sm3+、Tb3+The purity of ion concentration regulation white light.The present invention's
Light-emitting phosphor efficiency is high, Heat stability is good.
(2) the preparation method technique of fluorescent material of the present invention is simple, and synthesis reaction temperature is low.
Accompanying drawing explanation
The XRD spectra of Fig. 1 embodiment 3 gained sample；
The excitation spectrum of Fig. 2 embodiment 3 gained sample；
The white emitting fluorescent powder emission spectrum figure of different levels of doping prepared by Fig. 3 embodiment 1-4.
Detailed description of the invention
Below by embodiment, the present invention is described in further details.But skilled in the art realises that, under
Stating embodiment is not limiting the scope of the invention, any improvement made on the basis of the present invention and change
Change all within protection scope of the present invention.
Embodiment 1
It is NaSr according to chemical composition0.89BO3:0.01Ce3+,0.05Sm3+,0.05Tb3+Weigh 0.5304g respectively
Natrium carbonicum calcinatum Na2CO3, 1.3144g strontium carbonate SrCO3, 0.6474g boric acid H3BO3, 0.0181g oxygen
Change cerium CeO2, 0.0872g Disamarium trioxide Sm2O3, 0.0935g terbia. Diterbium trioxide Tb4O7, put into agate mortar preliminary
Mixing.It is subsequently adding the acetone of 2 times of volumes, is fully ground in ball grinder 30 minutes, afterwards at drying baker
In be dried 1-5 hour, remove acetone, dried raw material is transferred in corundum crucible, puts into high temperature Muffle
Stove is calcined 10 hours under the conditions of 400-500 DEG C；The semi-finished product of gained after above-mentioned first sintering are put into
Achates crucible grinds further；Grind gained semi-finished product and transfer to corundum crucible, at high temperature under reducing atmosphere
Double sintering under the conditions of 850 DEG C in tube furnace, reducing atmosphere is N2And H2Gaseous mixture, calcination time is 8
Hour；After reaction terminates, naturally cool to room temperature, take out sample and do through grinding, repeatedly washing, vacuum
Dry, gained sample obtains target product NaSr after crossing 200 mesh sieves after grinding0.89BO3:0.01Ce3+,
0.05Sm3+,0.05Tb3+Fluorescent material.
Refering to described in Fig. 3, curve a is the emission spectrum of the white emitting fluorescent powder obtained by the method for embodiment 1,
Therefrom learn, be positioned at tri-emission band superpositions of 424nm, 543nm, 646nm thus at single-matrix
NaSrBO3Achieving white light emission in fluorescent material, chromaticity coordinates is (0.282,0.180).
Embodiment 2
It is NaSr according to chemical composition0.88BO3:0.01Ce3+,0.05Sm3+,0.06Tb3+Weigh 0.5307g respectively
Natrium carbonicum calcinatum Na2CO3, 1.2995g strontium carbonate SrCO3, 0.6478g boric acid H3BO3, 0.0172g oxygen
Change cerium CeO2, 0.0879g Disamarium trioxide Sm2O3, 0.1131g terbia. Diterbium trioxide Tb4O7, put into agate mortar preliminary
Mixing.It is subsequently adding the acetone of 2 times of volumes, is fully ground in ball grinder 30 minutes, afterwards at drying baker
In be dried 1-5 hour, remove acetone, dried raw material is transferred in corundum crucible, puts into high temperature Muffle
Stove is calcined 10 hours under the conditions of 400-500 DEG C；The semi-finished product of gained after above-mentioned first sintering are put into
Achates crucible grinds further；Grind gained semi-finished product and transfer to corundum crucible, at high temperature under reducing atmosphere
Double sintering under the conditions of 850 DEG C in tube furnace, reducing atmosphere is N2And H2Gaseous mixture, calcination time is 8
Hour；After reaction terminates, naturally cool to room temperature, take out sample and do through grinding, repeatedly washing, vacuum
Dry, gained sample obtains target product NaSr after crossing 200 mesh sieves after grinding0.88BO3:0.01Ce3+,
0.05Sm3+,0.06Tb3+Fluorescent material.
Refering to described in Fig. 3, curve b is the emission spectrum of the white emitting fluorescent powder obtained by the method for embodiment 2,
Therefrom learn, be positioned at tri-emission band superpositions of 424nm, 543nm, 646nm thus at single-matrix
NaSrBO3Achieving white light emission in fluorescent material, chromaticity coordinates is (0.303,0.217).
Embodiment 3
It is NaSr according to chemical composition0.87BO3:0.01Ce3+,0.05Sm3+,0.07Tb3+Weigh 0.5306g respectively
Natrium carbonicum calcinatum Na2CO3, 1.2849g strontium carbonate SrCO3, 0.6466g boric acid H3BO3, 0.0175g oxygen
Change cerium CeO2, 0.0879g Disamarium trioxide Sm2O3, 0.1314g terbia. Diterbium trioxide Tb4O7, put into agate mortar preliminary
Mixing.It is subsequently adding the acetone of 2 times of volumes, is fully ground in ball grinder 30 minutes, afterwards at drying baker
In be dried 1-5 hour, remove acetone, dried raw material is transferred in corundum crucible, puts into high temperature Muffle
Stove is calcined 10 hours under the conditions of 400-650 DEG C；The semi-finished product of gained after above-mentioned first sintering are put into
Achates crucible grinds further；Grind gained semi-finished product and transfer to corundum crucible, at high temperature under reducing atmosphere
Double sintering under the conditions of 850 DEG C in tube furnace, reducing atmosphere is N2And H2Gaseous mixture, calcination time is 8
Hour；After reaction terminates, naturally cool to room temperature, take out sample and do through grinding, repeatedly washing, vacuum
Dry, gained sample obtains target product NaSr after crossing 200 mesh sieves after grinding0.87BO3:0.01Ce3+,
0.05Sm3+,0.07Tb3+Fluorescent material.
Refering to described in Fig. 3, curve c is the emission spectrum of the white emitting fluorescent powder obtained by the method for embodiment 3,
Therefrom learn, be positioned at tri-emission band superpositions of 424nm, 543nm, 646nm thus at single-matrix
NaSrBO3Achieving white light emission in fluorescent material, chromaticity coordinates is (0.310,0.243).
Embodiment 4
It is NaSr according to chemical composition0.86BO3:0.01Ce3+,0.05Sm3+,0.08Tb3+Weigh 0.5303g respectively
Natrium carbonicum calcinatum Na2CO3, 1.2698g strontium carbonate SrCO3, 0.6470g boric acid H3BO3, 0.0174g oxygen
Change cerium CeO2, 0.0880g Disamarium trioxide Sm2O3, 0.1495g terbia. Diterbium trioxide Tb4O7, put into agate mortar preliminary
Mixing.It is subsequently adding the acetone of 2 times of volumes, is fully ground in ball grinder 30 minutes, afterwards at drying baker
In be dried 1-5 hour, remove acetone, dried raw material is transferred in corundum crucible, puts into high temperature Muffle
Stove is calcined 10 hours under the conditions of 400-500 DEG C；The semi-finished product of gained after above-mentioned first sintering are put into
Achates crucible grinds further；Grind gained semi-finished product and transfer to corundum crucible, at high temperature under reducing atmosphere
Double sintering under the conditions of 850 DEG C in tube furnace, reducing atmosphere is N2And H2Gaseous mixture, calcination time is 8
Hour；After reaction terminates, naturally cool to room temperature, take out sample and do through grinding, repeatedly washing, vacuum
Dry, gained sample obtains target product NaSr after crossing 200 mesh sieves after grinding0.86BO3:0.01Ce3+,
0.05Sm3+,0.08Tb3+Fluorescent material.
Refering to described in Fig. 3, curve d is the emission spectrum of the white emitting fluorescent powder obtained by the method for embodiment 4,
Therefrom learn, be positioned at tri-emission band superpositions of 424nm, 543nm, 646nm thus at single-matrix
NaSrBO3Achieving white light emission in fluorescent material, chromaticity coordinates is (0.311,0.314).
Fig. 1, Fig. 2 are XRD figure spectrum and the excitation spectrum of embodiment 3 gained sample.Further, embodiment 1,
2, the XRD figure spectrum of 4 gained samples is identical with embodiment 3 with excitation spectrum.The XRD of this fluorescent material
Spectrogram and NaSrBO3Standard card ICSD-170420 is consistent, shows that the sample of synthesis is pure phase.
Claims (10)
1. a white light LEDs borate substrate fluorescent powder, it is characterised in that its chemical formula is
NaSr1-x-y-zCexSmyTbzBO3, wherein x, y and z are molar fraction, and the value of x, y and z is respectively
0 < x≤0.10,0 < y≤0.40,0 < z≤0.40.
Fluorescent material the most according to claim 1, wherein, cerium, samarium and terbium are trivalent ion, it may be assumed that
NaSr1-x-y-zBO:xCe3+,ySm3+,zTb3+；
Preferably, 0.005≤x≤0.08, the most preferably 0.01≤x≤0.04；Preferably, 0.005≤y≤0.20,
The most preferably 0.05≤y≤0.10；Preferably, 0.005≤z≤0.30, the most preferably, 0.05≤z≤0.20, more
There is choosing, 0.05≤z≤0.08.
Preferably, the molecular formula of described fluorescent material is NaSr1-x-y-zCexSmyTbzBO3, wherein x is 0.01,
Y is 0.05, and z is 0.05-0.08.
3. the preparation method of the fluorescent material described in claim 1 or 2, comprises the following steps:
(1) by Na2CO3、SrCO3、H3BO3、CeO2、Sm2O3、Tb4O7Mix, each former
The mol ratio of material controls at 0.5:1-x-y-z:(1-1.2): x:y:z, wherein 0 < x≤0.10,0 < y≤0.40,0 <
z≤0.40；
(2) the above-mentioned raw material mixed is mixed with organic solvent, then grind, be dried, by dried former
Material is calcined in 300-650 DEG C；
(3) by the material obtained in above-mentioned steps (2) again 800-950 DEG C, burn under reducing atmosphere
Knot.
Preparation method the most according to claim 3, wherein, in described step (1), described raw material
Na2CO3、SrCO3、H3BO3、CeO2、Sm2O3、Tb4O7For highly purified, its purity is higher than 99%,
Preferably above 99.9%, more preferably higher than 99.99%；The mixing of each material is preferably carried out in agate mortar.
Preferably, Na2CO3、SrCO3、H3BO3、CeO2、Sm2O3、Tb4O7Mol ratio be
0.5:1-x-y-z:1.05:x:y:z。
Preferably, 0.005≤x≤0.08, the most preferably 0.01≤x≤0.04；Preferably, 0.005≤y≤0.20,
The most preferably 0.05≤y≤0.10；Preferably, 0.005≤z≤0.30, the most preferably, 0.05≤z≤0.20, more
There is choosing, 0.05≤z≤0.08.
Preparation method the most according to claim 3, wherein, in described step (2), described organic molten
Agent can be acetone, ethanol etc., and described grinding is to be fully ground in ball grinder.
Preparation method the most according to claim 3, wherein, in described step (2), wherein said forges
Burn and carry out in high temperature Muffle furnace.The temperature of described calcining is preferably 400-500 DEG C；The time of calcining is preferred
For 1-20 hour, more preferably 5-10 hour.
Preparation method the most according to claim 3, wherein, according to the present invention, in described step (3),
Before sintering, first the material obtained in step (2) is ground, is sintered the most again；Described grinding
Preferably carry out in Achates crucible；
Preparation method the most according to claim 3, wherein, in described step (3), described in be sintered in
Carrying out in high-temperature atmosphere tube furnace, the temperature of described sintering is preferably 850-900 DEG C.Described reducing atmosphere
For N2And H2Gaseous mixture；
Preferably, in described step (3), will sintering after product cooling, grind, wash (the most repeatedly),
Vacuum drying, crosses 200 mesh sieves, obtains described white light emitting phosphor after being ground the most again.
Preparation method the most according to claim 3, wherein, described method comprises the steps:
(1) by Na2CO3、SrCO3、H3BO3、CeO2、Sm2O3、Tb4O7Put into agate mortar,
The mol ratio of each raw material controls at 0.5:1-x-y-z:1.05:x:y:z, and wherein x is 0.01, and y is 0.05, and z is
0.05-0.08；
(2) the above-mentioned raw material mixed is added acetone, grind in ball grinder, be placed on drying baker afterwards
In to be dried, remove acetone, transfer to, in corundum crucible, put in high temperature Muffle furnace by dried raw material
Calcining；
(3) semi-finished product of gained after above-mentioned first sintering are put in Achates crucible grind further；Grind
Gained semi-finished product transfer to corundum crucible, and under reducing atmosphere, in high temperature process furnances, under the conditions of 850 DEG C, secondary burns
Knot, reducing atmosphere is N2And H2Gaseous mixture；
(4) after reaction terminates, it is cooled to room temperature, takes out sample process and grind, repeatedly wash, be vacuum dried,
Gained sample obtains target product after crossing 200 mesh sieves after grinding.
10. the fluorescent material of claim 1 or 2 purposes in LED.
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| CN115820255A (en) * | 2022-12-21 | 2023-03-21 | 云南大学 | Single-matrix warm white fluorescent powder and preparation method thereof |
| CN116574505A (en) * | 2023-04-27 | 2023-08-11 | 桂林电子科技大学 | Preparation method of gallate stress luminescent material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111944527A (en) * | 2020-07-10 | 2020-11-17 | 贺州学院 | Synthesis method of ultraviolet light excited multicolor emission fluorescent powder |
| CN112094646A (en) * | 2020-10-30 | 2020-12-18 | 淮北师范大学 | White light fluorescent powder and preparation method thereof |
| CN112094646B (en) * | 2020-10-30 | 2022-08-26 | 淮北师范大学 | White light fluorescent powder and preparation method thereof |
| CN112500853A (en) * | 2020-12-14 | 2021-03-16 | 新沂市锡沂高新材料产业技术研究院有限公司 | Ce3+Doped zero-thermal quenching fluorescent powder and preparation method thereof |
| CN115820255A (en) * | 2022-12-21 | 2023-03-21 | 云南大学 | Single-matrix warm white fluorescent powder and preparation method thereof |
| CN115820255B (en) * | 2022-12-21 | 2023-09-26 | 云南大学 | Single-matrix warm white fluorescent powder and preparation method thereof |
| CN116574505A (en) * | 2023-04-27 | 2023-08-11 | 桂林电子科技大学 | Preparation method of gallate stress luminescent material |
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