CN106978176B - A kind of yellow fluorescent powder and preparation method and its application in luminescent device - Google Patents
A kind of yellow fluorescent powder and preparation method and its application in luminescent device Download PDFInfo
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- CN106978176B CN106978176B CN201710352345.7A CN201710352345A CN106978176B CN 106978176 B CN106978176 B CN 106978176B CN 201710352345 A CN201710352345 A CN 201710352345A CN 106978176 B CN106978176 B CN 106978176B
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7767—Chalcogenides
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- 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
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
Abstract
The present invention discloses a kind of yellow fluorescent powder and preparation method thereof and the application in field of LED illumination, belongs to luminescent material preparation and application field.It is Ba (Ce that the fluorescent powder, which forms expression formula,xSc1‑x)2O4, wherein 0 x≤0.5 <.By by the source Ba, the source Ce and Sc source compound according to molar ratio Ba:Ce:Sc=1:2x:2-2x ingredient, and successively mixed, briquetting, just burnings, grinding, briquetting, two burnings and grind, the yellow fluorescent powder can be obtained.The diode chip for backlight unit and above-mentioned yellow fluorescent powder for being 430-460 nm in conjunction with launch wavelength, can be realized the preparation of white light LED luminescent device.The preparation manufacture craft of above-mentioned yellow fluorescent powder and its associated light emitting device proposed by the invention is simple, easily operated, is conducive to realize material devices integration and Integration Design, the potentiality with industrialization and batch production.
Description
Technical field
The invention belongs to luminescent material and its preparation field, it is related to a kind of yellow fluorescent powder and preparation method and it is shining
Application in device.
Background technique
Compared to traditional incandescent lamp and fluorescent lighting, White-light LED illumination has power consumption as lighting source of new generation
The advantages that measuring that small, the service life is long, reaction speed is fast and be small in size, it has also become current lighting area prior development direction.Currently,
White light LEDs implementation method generally has following two: 1, combining realization by three kinds of LED of red, green and blue.Although this method can be with
Realize that the white light of different-colour exports, but higher cost.2, using single blue light or ultraviolet leds, in conjunction with corresponding fluorescent powder,
Realize shining for different color temperature area.Design cost not only can be effectively reduced in such method, but also by adjusting fluorescent powder spy
Different white applications demands may be implemented in property, is the mainstay scheme of Current commercial white light LEDs.Wherein, based on single
The design of fluorescent powder can more effectively avoid colo(u)r bias brought by a variety of fluorescent powder difference thermal quenching characteristics, and cost is lower
It is honest and clean, it is conducive to realize industrialization and mass production.(day is sub- chemical (Nichia) for blue-ray LED combination Ce:YAG fluorescent powder
US599892 patent) realized white light LEDs output be the white light LEDs for being widely recognized, and being widely used at present
Implementation.However, the white light LEDs realized export colour temperature since Ce:YAG lacks the covering of visible light wave range red light region
It is higher, it is unfavorable for realizing warm white LED output (colour temperature < 4000 K), needs bound fraction red fluorescence powder to improve its colour temperature
With the corresponding red spectral band colour rendering index (R9) of raising.Therefore, the yellow fluorescent powder of development covering visible light red spectral band is still
The urgent need of white light LEDs (especially warm white LED) illumination development.
Summary of the invention
In view of the above shortcomings of the prior art, the present invention provide a kind of yellow fluorescent powder and preparation method thereof and its
Application in luminescent device.
Technical scheme is as follows:
A kind of yellow fluorescent powder, chemical general formula are Ba (CexSc1-x)2O4, wherein 0 x≤0.5 <, preferably 0 x≤0.05 <.
Further, the yellow fluorescent powder average grain diameter is 0.5~15 μm.
Further, the yellow fluorescent powder, excitation wavelength are 375~500 nm, and launch wavelength is 500~750 nm；
Excitation wavelength is preferably 430~450 nm.
A kind of preparation method of the yellow fluorescent powder, step include:
It 1) is that 1:2x:2-2x takes Ba source compound, Ce source compound and Sc source compound according to molar ratio Ba:Ce:Sc,
It by the dry-mixed method mixing of alcohol wet mixing or ball milling, and is ground, obtains the powder that average grain diameter is 0.5~20 μm；
2) then the powder briquetting for mixing step 1) just burns 0.5~20 h in 1000~1500 DEG C of air,
It is cooled to room temperature, is ground, obtain just burning block shape powder；
3) the first burning block shape powder of step 2 is subjected to briquetting again, then in a reducing atmosphere, in 1300~1900 DEG C
It carries out two and burns 1~20 h, be down to room temperature, the blocky powder of sintering is ground, Ba (Ce is madexSc1-x)2O4, i.e. yellow is glimmering
Light powder.
Further, in step 1), the Ba source compound, Ce source compound and Sc source compound purity are greater than 99.9%,
Average grain diameter is at 0.5~5 μm.
Further, in step 1), the source Ba be BaO(barium monoxide), Ba (NO3)2(barium nitrate), BaCl2(chlorination
Barium), Ba (OH)2(barium hydroxide), BaCO3(barium carbonate), BaC2O4(barium oxalate) and Ba (CH2COOH)2In (barium acetate) extremely
Few one kind, preferably BaCO3。
Further, in step 1), the source Ce is CeO2(cerium oxide), Ce (NO3)3(cerous nitrate), CeCl3(chlorination
Cerium), Ce2(C2O4)3(cerium oxalate) and Ce (CH2COOH)3At least one of (cerous acetate), preferably CeO2。
Further, in step 1), the source Sc is Sc2O3(scandium oxide), Sc (NO3)3(scandium nitrate), ScCl3(chlorination
Scandium), Sc2(C2O4)3(oxalic acid scandium) and Sc (CH2COOH)3At least one of (acetic acid scandium), preferably Sc2O3。
Further, in step 1), preferably ethanol wet mixing, incorporation time is 0.5~3 h.
Further, described just to burn in step 2, preferably 1200~1400 DEG C of temperature, time preferably 4~7 h.
Further, in step 3), the reducing atmosphere is the covering of hot carbon, H2、CO、H2/N2、H2/Ar、CO/N2And CO/Ar
At least one of.
Further, in step 3), described two burn, and preferably 1400~1700 DEG C of temperature, time preferably 4~6 h.
Further, in step 2 and step 3), the pressure of briquetting process is 30~60 MPa, and compacting shape is preferably round
Column or square block；Briquetting size is adjusted according to the space of sintering furnace, and briquetting purpose is to increase powder consistency, is suppressed close
Degree reaches 90 % or more of theoretical density.
Further, just burnt described in step 2 and step 3) described in two burn, heating rate and rate of temperature fall be 2~
It 5 DEG C/min, is preferably carried out in corundum crucible or platinum crucible.
Further, in step 2 and step 3), preferably 0.5~15 μm of powder average grain diameter after grinding.
The present invention also provides application of the above-mentioned yellow fluorescent powder in luminescent device, it is particularly suitable for shining in white light LEDs
Application in bright.
A kind of luminescent device comprising yellow fluorescent powder of the present invention, preparation method are to mix resin with yellow fluorescent powder
It is even, it is uniformly spin-coated in LED chip, dry solidification is to get luminescent device.
Further, in the above method, the resin is epoxy resin or silicone resin, the silicon tree of preferred index > 1.4
Rouge；
Further, in the above method, the yellow fluorescent powder accounts for resin and contains with the percentage in yellow fluorescence powder mixture
Amount is 5~80 wt.%.
Further, in the above method, preferred emission wavelength is the LED chip of 430~460 nm.
Yellow fluorescent powder of the present invention and based on luminescent device thereon, has the advantage that
1, Ba (Ce in the present inventionxSc1-x)2O4BaSc used in yellow fluorescent powder2O4Matrix is congruent melting compound, is melted
, belong to monoclinic system C2/c space group (Agafonov V, Kahn A, Michel D, et al. at up to 2100 DEG C of point
Crystal structure of BaSc2O4; its relation with perovskite[J]. Materials
Research bulletin, 1983,18 (8): 975-981), physicochemical properties are stablized.
2、Ba(CexSc1-x)2O4Fluorescence emission wavelengths cover 475~750 nm, have high luminous efficiency, and center is sent out
Ejected wave is grown in 580 nm or so；It is about 550 nm compared to Ce:YAG(center emission wavelength), Ba (CexSc1-x)2O4Fluorescent powder can
More effectively to improve corresponding red spectral band colour rendering index (R9), colour temperature is reduced, is conducive to realize warm white LED illumination.
3, Ba (Ce is prepared using solid-phase sinteringxSc1-x)2O4Yellow fluorescent powder, simple process are easily operated；Adjust fluorescence
The white-light illuminating of different-colour requirement may be implemented in conjunction with the LED chip of 430~460 nm in the concentration that powder is mixed with resin；It is whole
A preparation process is with short production cycle, high production efficiency, is conducive to realize material devices integration and Integration Design, has industrialization
With the potentiality of batch production.
Detailed description of the invention
Fig. 1 is the X-ray powder diffraction data of 2 yellow fluorescent powder of embodiment, and (a) is Ba (CexSc1-x)2O4X-ray
Powder diffraction data (b) is standard BaSc2O4(ICSD:35592) theoretical X-ray powder diffraction data；
Fig. 2 is the excitation spectrum (when launch wavelength is 585 nm) and emission spectrum (excitation wave of 2 yellow fluorescent powder of embodiment
A length of 445 nm)；
Fig. 3 is the excitation spectrum (when launch wavelength is 575 nm) and emission spectrum (excitation wave of 3 yellow fluorescent powder of embodiment
A length of 435 nm)；
Fig. 4 is the excitation spectrum (when launch wavelength is 575 nm) and emission spectrum (excitation wave of 5 yellow fluorescent powder of embodiment
A length of 435 nm)；
Fig. 5 is 6 white light LED part of embodiment, in figure: 1, resin, 2, closing line, 3, contain Ba (CexSc1-x)2O4Fluorescence
The resin of powder, 4, blue-light LED chip, 5, anode connection, 6, cathode connection, 7, Ba (CexSc1-x)2O4Fluorescent powder absorbs blue-ray LED
The light of transmitting and the sodium yellow generated, 8, the blue light of blue-ray LED transmitting.
Specific embodiment
With reference to the accompanying drawings and examples technical solution of the present invention in detail, completely illustrate and describe.
Embodiment 1:
One kind (Ce0.003Sc0.997)2O4Yellow fluorescent powder, steps are as follows for preparation method:
1) with BaO, Sc2O3With Ce (NO3)3As initial feed, the molar ratio according to Ba:Ce:Sc is 1:0.04:1.96
Ingredient is carried out, using dry-mixed 5 h of planetary ball mill and is ground, the powder of uniform particle sizes' distribution is obtained；
2) powder that step 1) mixes is pressed into cylindric at 40 MPa, be put into platinum crucible, with 2~5
DEG C/min is warming up to 1300 DEG C, 5 h are burnt at the beginning of 1300 DEG C in air, room temperature is then down to 2~5 DEG C/min, is ground,
Obtain 0.5~15 μm of average grain diameter of first burning block shape powder；
3) it by the first burning block shape powder of the step 2 briquet at 40 MPa again, is put into platinum crucible, in CO/
In reducing atmosphere of the Ar(volume ratio for 5:90), 1500 DEG C of two 5 h of burning is warming up to 2~5 DEG C/min, obtains corresponding blocky powder
Body is ground to 0.5~15 μm of average grain diameter of powder, and final Ba (Ce can be obtained0.003Sc0.997)2O4Yellow fluorescent powder.
Embodiment 2:
A kind of Ba (Ce0.003Sc0.997)2O4Yellow fluorescent powder, steps are as follows for preparation method:
1) with BaCO3、Sc2O3And CeO2As initial feed, the molar ratio according to Ba:Ce:Sc is 1:0.006:1.994
Ingredient is carried out, it is then dry in draught cupboard at room temperature and ground using 1 h of alcoholic solution wet mixing, obtain uniform particle sizes point
The powder of cloth；
2) powder that step 1) mixes is pressed into cylindric at 40 MPa, be put into corundum crucible, with 2~5
DEG C/min is warming up to 1300 DEG C, 5 h are burnt at the beginning of 1300 DEG C in air, room temperature is then down to 2~5 DEG C/min, is ground,
Obtain 0.5~15 μm of average grain diameter of first burning block shape powder；
3) it by the first burning block shape powder of the step 2 briquet at 40 MPa again, is put into corundum crucible, in H2/N2
In (volume ratio 5:95) reducing atmosphere, 1500 DEG C of two 5 h of burning is warming up to 2~5 DEG C/min, obtains corresponding blocky powder,
It is ground, final Ba (Ce can be obtained0.003Sc0.997)2O4Yellow fluorescent powder.
As shown in Figure 1, the X-ray powder diffraction data of this fluorescent powder and standard diffraction card have good consistency,
Illustrate that the fluorescent powder of sintering has and BaSc2O4Consistent crystal structure.
As shown in Fig. 2, 2 yellow fluorescent powder of embodiment, a length of 445 nm of optimum excitation wave, highest launch wavelength are 585
nm。
Embodiment 3:
A kind of Ba (Ce0.003Sc0.997)2O4Yellow fluorescent powder, steps are as follows for preparation method:
1) with BaCO3、Sc2O3And CeO2As initial feed, the molar ratio according to Ba:Ce:Sc is 1:0.006:1.994
Ingredient is carried out, it is then dry in draught cupboard at room temperature and ground using 1 h of alcoholic solution wet mixing, obtain uniform particle sizes point
The powder of cloth；
2) powder for mixing step 1) briquet at 40 MPa, is put into corundum crucible, with 2~5 DEG C/min
1300 DEG C are warming up to, burns 5 h at the beginning of 1300 DEG C in air, room temperature is then down to 2~5 DEG C/min, is ground, is put down
The first burning block shape powder of equal 0.5~15 μm of partial size；
3) the first burning block shape powder of step 2 is pressed at 40 MPa cylindric again, be put into corundum crucible,
H2/N2In (volume ratio 5:95) reducing atmosphere, 1600 DEG C of two 5 h of burning is warming up to 2~5 DEG C/min, obtains corresponding blocky powder
Body is ground, and final Ba (Ce can be obtained0.003Sc0.997)2O4Yellow fluorescent powder.
Compared to 2(1500 DEG C two of embodiment burn), 3(1600 DEG C two of embodiment burning) yellow fluorescent powder (as shown in Figure 3)
Maximum excitation wavelength becomes 435 nm；Highest launch wavelength becomes 575 nm, and emissive porwer doubles.This says
The bright performance for improving sintering temperature and being conducive to improve yellow fluorescent powder.
Embodiment 4:
A kind of Ba (Ce0.02Sc0.98)2O4Yellow fluorescent powder, steps are as follows for preparation method:
1) with BaO, Sc2(C2O4)3With Ce (NO3)3It is 1:0.04 according to the molar ratio of Ba:Ce:Sc as initial feed:
1.96 carry out ingredient, using dry-mixed 5 h of planetary ball mill and are ground, and the powder of uniform particle sizes' distribution is obtained；
2) powder that step 1) mixes is pressed at 40 MPa square block, be put into platinum crucible, with 2~5
DEG C/min is warming up to 1300 DEG C, 5 h are burnt at the beginning of 1300 DEG C in air, room temperature is then down to 2~5 DEG C/min, is ground,
Obtain 0.5~15 μm of average grain diameter of first burning block shape powder；
3) it by the first burning block shape powder of the step 2 briquet at 40 MPa again, is put into platinum crucible, in CO/Ar
In the reducing atmosphere of (volume ratio 10:90), 1600 DEG C of two 5 h of burning is warming up to 2~5 DEG C/min, obtains corresponding blocky powder
Body is ground to 0.5~15 μm of average grain diameter of powder, and final Ba (Ce can be obtained0.02Sc0.98)2O4Yellow fluorescent powder.
Embodiment 5:
A kind of Ba (Ce0.02Sc0.98)2O4Yellow fluorescent powder, steps are as follows for preparation method:
1) with BaCO3、Sc2O3And CeO2As initial feed, the molar ratio according to Ba:Ce:Sc be 1:0.04:1.96 into
Row ingredient, it is then dry in draught cupboard at room temperature and ground using 1 h of wet mixing in alcoholic solution, obtain uniform particle sizes point
The powder of cloth；
2) powder for mixing step 1) briquet at 40 MPa, is put into corundum crucible, with 2~5 DEG C/min
1300 DEG C are warming up to, 5 h of sintering is burnt at the beginning of 1300 DEG C in air, room temperature is then down to 2~5 DEG C/min, is ground, is obtained
To 0.5~15 μm of average grain diameter of first burning block shape powder；
3) by the first burning block shape powder of step 2 at 40 MPa briquet, be put into corundum crucible, in H2/N2(volume
Than for 1500 DEG C of 4 h of sintering in 5:95) reducing atmosphere, obtaining corresponding blocky powder, is ground, can be obtained final
Ba(Ce0.02Sc0.98)2O4Yellow fluorescent powder.
5 yellow fluorescent powder of embodiment, maximum excitation wavelength (435 nm) and highest launch wavelength (575 nm).
As shown in Figure 3 and Figure 4, Ba (Ce0.003Sc0.997)2O4With Ba (Ce0.02Sc0.98)2O4The excitation and transmitting of fluorescent powder
Characteristic peak is very consistent, further illustrates the repeatability of technical solution of the present invention.In addition, along with the increase of concentration, hair
Reduced trend is presented in light efficiency, further specifies effective Ce3+Ion doping concentration range.
Embodiment 6:
A kind of luminescent device comprising yellow fluorescent powder of the present invention, main working parts are Ba (Ce0.003Sc0.997)2O4It is yellow
The blue-light LED chip that color fluorescent powder and launch wavelength are 450 nm；
It is specific as follows: silicone resin is uniformly mixed with yellow fluorescent powder 1:1 in mass ratio, is uniformly spin-coated in LED chip,
Dry solidification, i.e. white light LED part, structure are as shown in Figure 5.Without adding other fluorescent powders in the present embodiment 6, using as
Solidify Ba (Ce0.003Sc0.997)2O4The material of fluorescent powder and outer enclosure protection.After this device powers on, blue light is utilized
The blue light (8 in Fig. 5) and fluorescent powder that LED is issued, which absorb the yellow (7 in Fig. 5) that blue light is issued, can be realized white light output.
Certainly, the present invention can also have other various embodiments, without deviating from the spirit and substance of the present invention, ripe
It knows those skilled in the art and makes various corresponding changes and modification, but these corresponding changes and change in accordance with the present invention
Shape all should fall within the scope of protection of the appended claims of the present invention.
Claims (10)
1. a kind of yellow fluorescent powder, it is characterised in that: chemical general formula is Ba (CexSc1-x)2O4, wherein 0 x≤0.5 <；It is described
BaSc2O4For monocline C2/c space group.
2. yellow fluorescent powder according to claim 1, it is characterised in that: 0 x≤0.05 <；The yellow fluorescent powder is average
Partial size is 0.5~15 μm, and excitation wavelength is 375~500 nm, and launch wavelength is 500~750 nm.
3. yellow fluorescent powder according to claim 2, it is characterised in that: excitation wavelength is 430~450 nm.
4. a kind of preparation method of any one of claims 1 to 3 yellow fluorescent powder, which is characterized in that step includes:
1) it is that 1:2x:2-2x takes Ba source compound, Ce source compound and Sc source compound according to molar ratio Ba:Ce:Sc, passes through
Alcohol wet mixing or the dry-mixed method mixing of ball milling, and are ground, obtain the powder that average grain diameter is 0.5~20 μm；
2) then the powder briquetting for mixing step 1) just burns 0.5~20 h in 1000~1500 DEG C of air, is down to
It after room temperature, is ground, obtains just burning block shape powder；
3) the first burning block shape powder of step 2 is subjected to briquetting again, then in a reducing atmosphere, is carried out in 1300~1900 DEG C
Two burn 1~20 h, are down to room temperature, grind to the blocky powder of sintering, and Ba (Ce is madexSc1-x)2O4, i.e. yellow fluorescent powder.
5. the preparation method according to claim 4, it is characterised in that: in step 1), the Ba source compound, the source Ce chemical combination
Object and Sc source compound purity are greater than 99.9%, and average grain diameter is at 0.5~5 μm；The source Ba is BaO, Ba (NO3)2、BaCl2、
Ba(OH)2、BaCO3And BaC2O4At least one of；The source Ce is CeO2、Ce(NO3)3、CeCl3And Ce2(C2O4)3In extremely
Few one kind；The source Sc is Sc2O3、Sc(NO3)3、ScCl3And Sc2(C2O4)3At least one of；Mixed method is that alcohol is wet
Mixed, incorporation time is 0.5~3 h；
It is described just to burn in step 2,1200~1400 DEG C of temperature, 4~7 h of time；
In step 3), the reducing atmosphere is the covering of hot carbon, H2、CO、H2/N2、H2/Ar、CO/N2At least one of with CO/Ar；
Described two burn, and 1400~1700 DEG C of temperature, 4~6 h of time.
6. preparation method according to claim 5, it is characterised in that: in step 1), the source Ba is BaCO3；The source Ce
For CeO2；The source Sc is Sc2O3。
7. the preparation method according to claim 4, it is characterised in that: in step 2 and step 3), the pressure of briquetting process
It is 30~60 MPa, compacting shape is cylindric or square block；Powder average grain diameter is 0.5~15 μm after grinding；Step 2
Described in just burn and step 3) described in two burn, heating rate and rate of temperature fall are 2~5 DEG C/min, preferably in corundum crucible
Or it is carried out in platinum crucible.
8. a kind of luminescent device comprising any one of claims 1 to 3 yellow fluorescent powder, it is characterised in that: preparation method
It for resin to be uniformly mixed with yellow fluorescent powder, is uniformly spin-coated in LED chip, dry solidification is to get luminescent device.
9. luminescent device according to claim 8, it is characterised in that: the resin is epoxy resin or silicone resin；The Huang
The percentage composition that color fluorescent powder accounts in resin and yellow fluorescence powder mixture is 5~80 wt.%；LED chip is that launch wavelength is
The LED chip of 430~460 nm.
10. luminescent device according to claim 9, it is characterised in that: the resin is the silicone resin of refractive index > 1.4.
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| CN110118312A (en) * | 2018-02-07 | 2019-08-13 | 深圳光峰科技股份有限公司 | Wavelength converter |
| CN109135745B (en) * | 2018-09-13 | 2021-12-14 | 济南大学 | Preparation method and application of yellow fluorescent powder for white light LED |
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