CN107365070A - A kind of white light LEDs red green composite fluorescence glass and preparation method thereof - Google Patents
A kind of white light LEDs red green composite fluorescence glass and preparation method thereof Download PDFInfo
- Publication number
- CN107365070A CN107365070A CN201710823250.9A CN201710823250A CN107365070A CN 107365070 A CN107365070 A CN 107365070A CN 201710823250 A CN201710823250 A CN 201710823250A CN 107365070 A CN107365070 A CN 107365070A
- Authority
- CN
- China
- Prior art keywords
- glass
- white light
- red
- light leds
- red green
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000011521 glass Substances 0.000 title claims abstract description 129
- 239000011174 green composite Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 77
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000000146 host glass Substances 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000002131 composite material Substances 0.000 claims abstract description 17
- 239000000428 dust Substances 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 35
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims description 34
- 229910052681 coesite Inorganic materials 0.000 claims description 28
- 229910052906 cristobalite Inorganic materials 0.000 claims description 28
- 239000000377 silicon dioxide Substances 0.000 claims description 28
- 229910052682 stishovite Inorganic materials 0.000 claims description 28
- 229910052905 tridymite Inorganic materials 0.000 claims description 28
- 239000002994 raw material Substances 0.000 claims description 23
- 238000005245 sintering Methods 0.000 claims description 19
- 239000002184 metal Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 14
- 108010043121 Green Fluorescent Proteins Proteins 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 8
- 230000004927 fusion Effects 0.000 claims description 8
- 238000010791 quenching Methods 0.000 claims description 8
- 230000000171 quenching effect Effects 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 230000009466 transformation Effects 0.000 claims description 6
- 238000002795 fluorescence method Methods 0.000 claims description 5
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 claims description 4
- 230000005284 excitation Effects 0.000 claims description 4
- 238000005538 encapsulation Methods 0.000 abstract description 6
- 238000000137 annealing Methods 0.000 abstract 1
- 238000007500 overflow downdraw method Methods 0.000 abstract 1
- 239000004615 ingredient Substances 0.000 description 13
- 238000011835 investigation Methods 0.000 description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 238000009766 low-temperature sintering Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004643 material aging Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
- C03C3/068—Glass compositions containing silica with less than 40% silica by weight containing boron containing rare earths
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a kind of white light LEDs red green composite fluorescence glass, include host glass, red fluorescence powder and green emitting phosphor, its preparation method is to prepare glass basis with fusion method first, is ground into glass dust, and glass dust is mixed with fluorescent material, red green composite fluorescence glass is obtained after sintered annealing, the LED specular removals that described composite fluorescence glass is prepared with blue chip encapsulation, height colour developing, low light attenuation, color drift is small, and color tolerance is small.
Description
Technical field
The present invention relates to a kind of fluorescent glass and preparation method thereof, more particularly to a kind of white light LEDs red green is compound glimmering
Light glass and preparation method thereof.
Background technology
For large power white light LED encapsulation, the effect of fluorescent material is photochromic compound, forms white light, conventional is glimmering
Light powder application pattern is to mix fluorescent material with packaging plastic (epoxy resin or silica gel), and then point is coated in LED chip, due to applying
Coating process is difficult to accurately control the thickness and shape of fluorescent powder coated layer, and the colour temperature and colour rendering for causing LED component refer to
Number fluctuation is very big, influences product quality.Further, since fluorescent material glue-line be by epoxy resin or silica gel and fluorescent material allotment and
Into heat resistance, ageing resistance and anti-moisture poor-performing.Chinese patent literature (publication number 102442778A) discloses a kind of glimmering
100-150 DEG C of light glass and preparation method and application, glass micro mist and fluorescent material mixing are dried to obtain fluorescent glass, but prepare
Obtained fluorescent glass light efficiency is low.LED is encapsulated using fluorescent glass, not only eliminates fluorescent material and packaging plastic in encapsulation process
Preparation and coating processes, improve white-light LED encapsulation efficiency, and improve the uniformity and heat endurance of fluorescence, so as to change
It has been apt to the luminous mass and reliability of LED component.
But there is the difficulty (red fluorescence powder being difficult to red fluorescence powder and host glass powder co-sintering for the studies above
The lattice environment malleable of light emitting ionic), it more difficult to prepare composite fluorescence vitreum.
The content of the invention
The present invention provides a kind of white light LEDs red green composite fluorescence glass and preparation method thereof, by host glass
The design of component, obtain low-temperature sintering and to the unresponsive glass ingredient of nitride rouge and powder, can successfully mix nitride rouge and powder,
Can solve to be difficult to the difficulty by red fluorescence powder and host glass powder co-sintering.
Technical scheme is as follows：
A kind of white light LEDs red green composite fluorescence glass, includes host glass, red fluorescence powder and green emitting phosphor；
The host glass is mainly by R2O、ZnO、B2O3、SiO2Be prepared with the raw material of R'O components, wherein each component by mole point
Number is calculated as：R2O 5-20% molar fractions, ZnO 10-30% molar fractions, B2O320-50% molar fractions, SiO20-20%
Molar fraction, R'O 0-20% molar fractions.
Preferably, the R2O is selected from Li2O、Na2O or K2More than one in O.
Preferably, the R'O in MgO, CaO, SrO or BaO more than one.
Preferably, the SiO2Molar fraction be 1-18%.
Preferably, the molar fraction of the R'O is 1-18%.
Preferably, the red fluorescence powder is Ca1-xSrxAlSiN3:Eu2+(Ca1-x Srx)2Si5N8:Eu2+, wherein 0≤
X≤1, its excitation wavelength are 450-470nm, and its launch wavelength is 600-670nm.
Preferably, the green emitting phosphor is Lu3-xYxAl5O12:Ce3+, wherein 0≤x≤1, its excitation wavelength is 450-
470nm, its launch wavelength are 500-570nm.
The present invention also provides a kind of white light LEDs red green composite fluorescence method for glass preparation, and methods described includes following
Step：
(1) weighed by following molar fraction：R2O 5-20% molar fractions, ZnO 10-30% molar fractions, B2O3 20-
50% molar fraction, SiO20-20% molar fractions, R'O 0-20% molar fractions, wherein, R2O、ZnO、B2O3、SiO2And R'O
It is respectively derived from raw material R2CO3、ZnO、H3BO3、SiO2And R'CO3；
(2) by the raw material R2CO3、ZnO、H3BO3、SiO2And R'CO3Melted after well mixed, fusion temperature is
900 DEG C -1200 DEG C, 1-3 hours are incubated, obtain glass metal；
(3) glass metal is poured into cold water, carries out water quenching cooling, obtain residuite glass；
(4) by glass grinds, the composite phosphor formed with red fluorescence powder and the green emitting phosphor is according to quality
Than uniformly mixing, sintered in Muffle furnace, sintering temperature is 400 DEG C -700 DEG C, sintering time 10-50min, then in glass
Transition temperature starts to anneal, and cools to 20 DEG C, 5-10 DEG C/h of rate of temperature fall, produces white light LEDs red fluorescence glass.
Preferably, the mass ratio of glass dust described in step (4) and the composite phosphor is 1:0.001-1:0.1, institute
The mass ratio for stating red fluorescence powder and the green emitting phosphor is 1:1-1:30.
Preferably, the R2O is selected from Li2O、Na2O or K2More than one in O, the R'O are selected from MgO, CaO, SrO or BaO
In more than one.
Compared with prior art, beneficial effects of the present invention are as follows：
By the design to host glass component, low-temperature sintering is obtained and to the unresponsive glass ingredient of nitride rouge and powder,
Nitride rouge and powder can be successfully mixed, can solve to be difficult to the difficulty by red fluorescence powder and host glass powder co-sintering.
First, by the design to glass ingredient, using cheap oxide component, process costs are reduced, and carry
The high performance of fluorescent glass piece, i.e. low stress, high conversion efficiency；
2nd, realized by different packaging technologies, the fluorescent glass piece encapsulates available for assorted LED chip, both can be real
Now single LEDs chip package, it can also be used to multiple chips array LED module and LED lamp encapsulation；
3rd, low-temperature sintering method prepares fluorescent glass, can prepare the fluorescent glass piece of different shape, size, meet LED
Encapsulation requires.
Certainly, any product for implementing the present invention it is not absolutely required to reach all the above advantage simultaneously.
Brief description of the drawings
Fig. 1 is the pictorial diagram of the red green composite fluorescence glass of embodiment 1；
Fig. 2 is the launching light spectrogram of the red green composite fluorescence glass of embodiment 1；
Fig. 3 is the launching light spectrogram of the red green composite fluorescence glass of embodiment 2；
Fig. 4 is the launching light spectrogram of the red green composite fluorescence glass of embodiment 3.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate this hair
It is bright, rather than limit protection scope of the present invention.Those skilled in the art change according to what the present invention made in actual applications
Enter and adjust, still fall within protection scope of the present invention.
In order to better illustrate the present invention, the present invention is described in detail below with accompanying drawing.
A kind of white light LEDs red green composite fluorescence method for glass preparation, the described method comprises the following steps：
(1) weighed by following molar fraction：R2O 5-20% molar fractions, ZnO 10-30% molar fractions, B2O3 20-
50% molar fraction, SiO20-20% molar fractions, R'O 0-20% molar fractions, wherein, R2O、ZnO、B2O3、SiO2And R'O
It is respectively derived from raw material R2CO3, ZnO, H3BO3, SiO2, R'CO3；
(2) by the raw material R2CO3, ZnO, H3BO3, SiO2, R'CO3Melted after well mixed, fusion temperature 900
DEG C -1200 DEG C, 1-3 hours are incubated, obtain glass metal；
(3) glass metal is poured into cold water, carries out water quenching cooling, obtain residuite glass；
(4) by glass grinds, the composite phosphor formed with red fluorescence powder and the green emitting phosphor is according to quality
Than uniformly mixing, sintered in Muffle furnace, sintering temperature is 400 DEG C -700 DEG C, sintering time 10-50min, then in glass
Transition temperature starts to anneal, and cools to 20 DEG C, 5-10 DEG C/h of rate of temperature fall, produces white light LEDs red fluorescence glass.
Specific component composition and proportioning are referring to the following examples in the above method.
Embodiment 1
A kind of white light LEDs red green composite fluorescence glass, it includes host glass, red fluorescence powder and green fluorescence
Powder；Described host glass is mainly by R2O、ZnO、B2O3、SiO2It is prepared with the raw material of R'O components, wherein R2O is Na2O,
R'O is BaO；Specific glass ingredient (molar fraction)：
The red fluorescence powder is Ca1-xSrxAlSiN3:Eu2+(Ca1-x Srx)2Si5N8:Eu2+, 0≤x≤1 is described
Green emitting phosphor is Lu3-xYxAl5O12:Ce3+, 0≤x≤1；
Wherein, the mass ratio of host glass, red fluorescence powder and green emitting phosphor is glass dust：Red fluorescence powder：Green
Fluorescent material=1:0.05:0.003.
The red green of above-mentioned gained is answered using XRF (FLS8900, Edinburgh, Britain Instruments company)
Close fluorescent glass to be measured, the transmitting spectrogram of gained is as shown in Figure 2；The pictorial diagram of the red green composite fluorescence glass of gained is such as
Shown in Fig. 1.The fluorometric investigation result of embodiment 1 illustrates that the transmitting spectrogram of composite fluorescence glass is a broadband, and emission peak is
600nm。
Embodiment 2
A kind of white light LEDs red green composite fluorescence glass, it includes host glass, red fluorescence powder and green fluorescence
Powder；Described host glass is mainly by R2O、ZnO、B2O3、SiO2It is prepared with the raw material of R'O components, wherein R2O is Na2O,
R'O is BaO；Specific glass ingredient (molar fraction)：
The red fluorescence powder is Ca1-xSrxAlSiN3:Eu2+(Ca1-x Srx)2Si5N8:Eu2+, 0≤x≤1 is described
Green emitting phosphor is Lu3-xYxAl5O12:Ce3+, 0≤x≤1；
Wherein, the mass ratio of host glass, red fluorescence powder and green emitting phosphor is glass dust：Red fluorescence powder：Green
Fluorescent material=1:0.05:0.001.
The red green of above-mentioned gained is answered using XRF (FLS8900, Edinburgh, Britain Instruments company)
Close fluorescent glass to be measured, the transmitting spectrogram of gained is as shown in Figure 3.The fluorometric investigation result of embodiment 2 illustrates composite fluorescence
The transmitting spectrogram of glass is a broadband, emission peak 600nm, and the transmitting spectrogram intensity of embodiment 2 is less than the transmitting of embodiment 1
Intensity.
Embodiment 3
A kind of white light LEDs red green composite fluorescence glass, it includes host glass, red fluorescence powder and green fluorescence
Powder；Described host glass is mainly by R2O、ZnO、B2O3、SiO2It is prepared with the raw material of R'O components, wherein R2O is Na2O,
R'O is BaO；Specific glass ingredient (molar fraction)：
The red fluorescence powder is Ca1-xSrxAlSiN3:Eu2+(Ca1-x Srx)2Si5N8:Eu2+, 0≤x≤1 is described
Green emitting phosphor is Lu3-xYxAl5O12:Ce3+, 0≤x≤1；
Wherein, the mass ratio of host glass, red fluorescence powder and green emitting phosphor is glass dust：Red fluorescence powder：Green
Fluorescent material=1:0.05:0.001.
The red green of above-mentioned gained is answered using XRF (FLS8900, Edinburgh, Britain Instruments company)
Close fluorescent glass to be measured, the transmitting spectrogram of gained is as shown in Figure 4.The fluorometric investigation result of embodiment 3 illustrates composite fluorescence
The transmitting spectrogram of glass is a broadband, and emission peak 600nm, the transmitting spectrogram intensity of embodiment 3 is less than embodiment 2 and 1
Emissive porwer.
Embodiment 4
A kind of white light LEDs red green composite fluorescence glass, it includes host glass, red fluorescence powder and green fluorescence
Powder；Described host glass is mainly by R2O、ZnO、B2O3、SiO2It is prepared with the raw material of R'O components, wherein R2O is Na2O,
R'O is BaO；Specific glass ingredient (molar fraction)：
The red fluorescence powder is Ca1-xSrxAlSiN3:Eu2+(Ca1-x Srx)2Si5N8:Eu2+, 0≤x≤1 is described
Green emitting phosphor is Lu3-xYxAl5O12:Ce3+, 0≤x≤1；
Wherein, the mass ratio of host glass, red fluorescence powder and green emitting phosphor is glass dust：Red fluorescence powder：Green
Fluorescent material=1:0.05:0.002.
The red green of above-mentioned gained is answered using XRF (FLS8900, Edinburgh, Britain Instruments company)
Fluorescent glass is closed to be measured.The fluorometric investigation result of embodiment 4 illustrates that the transmitting spectrogram of composite fluorescence glass is a broadband, hair
It is 600nm to penetrate peak value, and the transmitting spectrogram intensity of embodiment 4 is less than the emissive porwer of embodiment 3,2 and 1.
Embodiment 5
A kind of white light LEDs red green composite fluorescence glass, it includes host glass, red fluorescence powder and green fluorescence
Powder；Described host glass is mainly by R2O、ZnO、B2O3、SiO2It is prepared with the raw material of R'O components, wherein R2O is Na2O,
R'O is BaO；Specific glass ingredient (molar fraction)：
The red fluorescence powder is Ca1-xSrxAlSiN3:Eu2+(Ca1-x Srx)2Si5N8:Eu2+, 0≤x≤1 is described
Green emitting phosphor is Lu3-xYxAl5O12:Ce3+, 0≤x≤1；
Wherein, the mass ratio of host glass, red fluorescence powder and green emitting phosphor is glass dust：Red fluorescence powder：Green
Fluorescent material=1:0.05:0.008.
The red green of above-mentioned gained is answered using XRF (FLS8900, Edinburgh, Britain Instruments company)
Fluorescent glass is closed to be measured.The fluorometric investigation result of embodiment 5 illustrates that the transmitting spectrogram of composite fluorescence glass is a broadband, hair
It is 600nm to penetrate peak value, and the transmitting spectrogram intensity of embodiment 5 is less than the emissive porwer of embodiment 4.
Embodiment 6
A kind of white light LEDs red green composite fluorescence glass, it includes host glass, red fluorescence powder and green fluorescence
Powder；Described host glass is mainly by R2O、ZnO、B2O3、SiO2It is prepared with the raw material of R'O components, wherein R2O is Na2O,
R'O is BaO；Specific glass ingredient (molar fraction)：
Melted after raw material is well mixed, fusion temperature is 900 DEG C, is incubated 3 hours, obtains glass metal, glass metal falls
Enter in cold water, carry out water quenching cooling, obtain residuite glass；Glass grinds, with red fluorescence powder and green emitting phosphor group
Into composite phosphor uniformly mixed according to mass ratio, sintered in Muffle furnace, sintering temperature is 400 DEG C, and sintering time is
10min, then start to anneal in glass transformation temperature, cool to 20 DEG C, 5-10 DEG C/h of rate of temperature fall, produce white light LEDs use
Red green composite fluorescence glass.
Wherein described red fluorescence powder is Ca1-xSrxAlSiN3:Eu2+(Ca1-x Srx)2Si5N8:Eu2+, 0≤x≤1,
The green emitting phosphor is Lu3-xYxAl5O12:Ce3+, 0≤x≤1；
Wherein, the mass ratio of host glass, red fluorescence powder and green emitting phosphor is glass dust：Red fluorescence powder：Green
Fluorescent material=1:0.05:0.003.
Embodiment 7
A kind of white light LEDs red green composite fluorescence glass, it includes host glass, red fluorescence powder and green fluorescence
Powder；Described host glass is mainly by R2O、ZnO、B2O3、SiO2It is prepared with the raw material of R'O components, wherein R2O is Na2O,
R'O is BaO；Specific glass ingredient (molar fraction)：
Melted after raw material is well mixed, fusion temperature is 900 DEG C, is incubated 3 hours, obtains glass metal, glass metal falls
Enter in cold water, carry out water quenching cooling, obtain residuite glass；Glass grinds, with red fluorescence powder and green emitting phosphor group
Into composite phosphor uniformly mixed according to mass ratio, sintered in Muffle furnace, sintering temperature is 700 DEG C, and sintering time is
50min, then start to anneal in glass transformation temperature, cool to 20 DEG C, 5-10 DEG C/h of rate of temperature fall, produce white light LEDs use
Red green composite fluorescence glass.
Wherein described red fluorescence powder is Ca1-xSrxAlSiN3:Eu2+(Ca1-x Srx)2Si5N8:Eu2+, 0≤x≤1,
The green emitting phosphor is Lu3-xYxAl5O12:Ce3+, 0≤x≤1；
Wherein, the mass ratio of host glass, red fluorescence powder and green emitting phosphor is glass dust：Red fluorescence powder：Green
Fluorescent material=1:0.05:0.003.
Embodiment 8
A kind of white light LEDs red green composite fluorescence glass, it includes host glass, red fluorescence powder and green fluorescence
Powder；Described host glass is mainly by R2O、ZnO、B2O3、SiO2It is prepared with the raw material of R'O components, wherein R2O is Na2O,
R'O is BaO；Specific glass ingredient (molar fraction)：
Melted after raw material is well mixed, fusion temperature is 1200 DEG C, is incubated 1 hour, obtains glass metal, glass metal falls
Enter in cold water, carry out water quenching cooling, obtain residuite glass；Glass grinds, with red fluorescence powder and green emitting phosphor group
Into composite phosphor uniformly mixed according to mass ratio, sintered in Muffle furnace, sintering temperature is 400 DEG C, and sintering time is
50min, then start to anneal in glass transformation temperature, cool to 20 DEG C, 5-10 DEG C/h of rate of temperature fall, produce white light LEDs use
Red green composite fluorescence glass.
Wherein described red fluorescence powder is Ca1-xSrxAlSiN3:Eu2+(Ca1-x Srx)2Si5N8:Eu2+, 0≤x≤1,
The green emitting phosphor is Lu3-xYxAl5O12:Ce3+, 0≤x≤1；
Wherein, the mass ratio of host glass, red fluorescence powder and green emitting phosphor is glass dust：Red fluorescence powder：Green
Fluorescent material=1:0.05:0.003.
Embodiment 9
A kind of white light LEDs red green composite fluorescence glass, it includes host glass, red fluorescence powder and green fluorescence
Powder；Described host glass is mainly by R2O、ZnO、B2O3、SiO2It is prepared with the raw material of R'O components, wherein R2O is Na2O,
R'O is BaO；Specific glass ingredient (molar fraction)：
Melted after raw material is well mixed, fusion temperature is 1200 DEG C, is incubated 1 hour, obtains glass metal, glass metal falls
Enter in cold water, carry out water quenching cooling, obtain residuite glass；Glass grinds, with red fluorescence powder and green emitting phosphor group
Into composite phosphor uniformly mixed according to mass ratio, sintered in Muffle furnace, sintering temperature is 700 DEG C, and sintering time is
10min, then start to anneal in glass transformation temperature, cool to 20 DEG C, 5-10 DEG C/h of rate of temperature fall, produce white light LEDs use
Red green composite fluorescence glass.
Wherein described red fluorescence powder is Ca1-xSrxAlSiN3:Eu2+(Ca1-x Srx)2Si5N8:Eu2+, 0≤x≤1,
The green emitting phosphor is Lu3-xYxAl5O12:Ce3+, 0≤x≤1；
Wherein, the mass ratio of host glass, red fluorescence powder and green emitting phosphor is glass dust：Red fluorescence powder：Green
Fluorescent material=1:0.05:0.003.
Embodiment 10
A kind of white light LEDs red green composite fluorescence glass, it includes host glass, red fluorescence powder and green fluorescence
Powder；Described host glass is mainly by R2O、ZnO、B2O3、SiO2It is prepared with the raw material of R'O components, wherein R2O is Na2O,
R'O is BaO；Specific glass ingredient (molar fraction)：
Melted after raw material is well mixed, fusion temperature is 1200 DEG C, is incubated 3 hours, obtains glass metal, glass metal falls
Enter in cold water, carry out water quenching cooling, obtain residuite glass；Glass grinds, with red fluorescence powder and green emitting phosphor group
Into composite phosphor uniformly mixed according to mass ratio, sintered in Muffle furnace, sintering temperature is 700 DEG C, and sintering time is
50min, then start to anneal in glass transformation temperature, cool to 20 DEG C, 5-10 DEG C/h of rate of temperature fall, produce white light LEDs use
Red green composite fluorescence glass.
Wherein described red fluorescence powder is Ca1-xSrxAlSiN3:Eu2+(Ca1-x Srx)2Si5N8:Eu2+, 0≤x≤1,
The green emitting phosphor is Lu3-xYxAl5O12:Ce3+, 0≤x≤1；
Wherein, the mass ratio of host glass, red fluorescence powder and green emitting phosphor is glass dust：Red fluorescence powder：Green
Fluorescent material=1:0.05:0.003.
Present invention disclosed above preferred embodiment is only intended to help and illustrates the present invention.Preferred embodiment is not detailed
All details are described, it is only described embodiment also not limit the invention.Obviously, according to the content of this specification,
It can make many modifications and variations.This specification is chosen and specifically describes these embodiments, is to preferably explain the present invention
Principle and practical application so that skilled artisan can be best understood by and utilize the present invention.The present invention is only
Limited by claims and its four corner and equivalent.
Claims (10)
1. a kind of white light LEDs red green composite fluorescence glass, it is characterised in that include host glass, red fluorescence powder and green
Color fluorescent material；The host glass is mainly by R2O、ZnO、B2O3、SiO2It is prepared with the raw material of R'O components, wherein each component
It is calculated as by molar fraction：R2O 5-20% molar fractions, ZnO 10-30% molar fractions, B2O320-50% molar fractions,
SiO20-20% molar fractions, R'O 0-20% molar fractions.
A kind of 2. white light LEDs according to claim 1 red green composite fluorescence glass, it is characterised in that the R2O is selected
From Li2O、Na2O or K2More than one in O.
A kind of 3. white light LEDs according to claim 1 red green composite fluorescence glass, it is characterised in that the R'O choosings
From in MgO, CaO, SrO or BaO more than one.
A kind of 4. white light LEDs according to claim 1 red green composite fluorescence glass, it is characterised in that the SiO2's
Molar fraction is 1-18%.
5. a kind of white light LEDs according to claim 1 red green composite fluorescence glass, it is characterised in that the R'O's
Molar fraction is 1-18%.
A kind of 6. white light LEDs according to claim 1 red green composite fluorescence glass, it is characterised in that the red
Fluorescent material is Ca1-xSrxAlSiN3:Eu2+(Ca1-x Srx)2Si5N8:Eu2+, wherein 0≤x≤1, its excitation wavelength is 450-
470nm, its launch wavelength are 600-670nm.
A kind of 7. white light LEDs according to claim 1 red green composite fluorescence glass, it is characterised in that the green
Fluorescent material is Lu3-xYxAl5O12:Ce3+, wherein 0≤x≤1, its excitation wavelength is 450-470nm, and its launch wavelength is 500-
570nm。
8. a kind of white light LEDs red green composite fluorescence method for glass preparation, it is characterised in that methods described includes following step
Suddenly：
(1) weighed by following molar fraction：R2O 5-20% molar fractions, ZnO 10-30% molar fractions, B2O320-50%
Molar fraction, SiO20-20% molar fractions, R'O 0-20% molar fractions, wherein, R2O、ZnO、B2O3、SiO2Distinguish with R'O
From raw material R2CO3, ZnO, H3BO3, SiO2, R'CO3；
(2) by the raw material R2CO3, ZnO, H3BO3, SiO2, R'CO3Being melted after well mixed, fusion temperature is 900 DEG C-
1200 DEG C, 1-3 hours are incubated, obtain glass metal；
(3) glass metal is poured into cold water, carries out water quenching cooling, obtain residuite glass；
(4) by glass grinds, the composite phosphor formed with red fluorescence powder and green emitting phosphor uniformly mixes according to mass ratio
Close, sintered in Muffle furnace, sintering temperature is 400 DEG C -700 DEG C, sintering time 10-50min, then in glass transformation temperature
Start to anneal, cool to 20 DEG C, 5-10 DEG C/h of rate of temperature fall, produce white light LEDs red green composite fluorescence glass.
A kind of 9. white light LEDs according to claim 8 red green composite fluorescence method for glass preparation, it is characterised in that
The mass ratio of glass dust described in step (4) and the composite phosphor is 1:0.001-1:0.1, the red fluorescence powder and institute
The mass ratio for stating green emitting phosphor is 1:1-1:30.
A kind of 10. white light LEDs according to claim 8 red green composite fluorescence method for glass preparation, it is characterised in that
The R2O is selected from Li2O、Na2O or K2More than one in O, the R'O in MgO, CaO, SrO or BaO more than one.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710823250.9A CN107365070A (en) | 2017-09-13 | 2017-09-13 | A kind of white light LEDs red green composite fluorescence glass and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710823250.9A CN107365070A (en) | 2017-09-13 | 2017-09-13 | A kind of white light LEDs red green composite fluorescence glass and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107365070A true CN107365070A (en) | 2017-11-21 |
Family
ID=60302787
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710823250.9A Pending CN107365070A (en) | 2017-09-13 | 2017-09-13 | A kind of white light LEDs red green composite fluorescence glass and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107365070A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107973527A (en) * | 2018-01-04 | 2018-05-01 | 上海应用技术大学 | A kind of preparation method of double layer phosphor |
| CN108455846A (en) * | 2018-04-02 | 2018-08-28 | 上海应用技术大学 | A kind of fluorescent glass of composite phosphor and its preparation method and application |
| CN110156326A (en) * | 2018-02-11 | 2019-08-23 | 天津理工大学 | Fluorescent glass ceramics based on glass powder with low melting point and preparation method thereof |
| CN110360469A (en) * | 2019-07-17 | 2019-10-22 | 上海应用技术大学 | A kind of full spectral laser based on fluorophor |
| CN110698073A (en) * | 2019-11-19 | 2020-01-17 | 温州大学新材料与产业技术研究院 | Full-spectrum borosilicate fluorescent glass and preparation method thereof |
| CN112645592A (en) * | 2020-12-23 | 2021-04-13 | 温州大学 | Preparation and application of efficient adjustable composite fluorescent glass material |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101471417A (en) * | 2007-12-27 | 2009-07-01 | 丰田合成株式会社 | Method for manufacturing glass plate containing fluophor and method for manufacturing light-emitting device |
| CN101643315A (en) * | 2009-08-10 | 2010-02-10 | 武汉理工大学 | Low-melting-point fluorescent glass for white light LED and preparation method thereof |
| CN103137835A (en) * | 2011-12-01 | 2013-06-05 | 弘大贸易股份有限公司 | Method of enhancing color rendering index of a white led |
| CN104087290A (en) * | 2014-07-15 | 2014-10-08 | 江苏罗化新材料有限公司 | Method for preparing nitride red phosphor |
| CN104130776A (en) * | 2014-07-15 | 2014-11-05 | 江苏罗化新材料有限公司 | Non-hydrogenous reducing preparation method for nitride red fluorescent powder |
| CN104282827A (en) * | 2013-07-04 | 2015-01-14 | 三星电子株式会社 | Wavelength conversion structure, apparatus comprising wavelength conversion structure, and related methods of manufacturing |
| CN106800371A (en) * | 2017-01-25 | 2017-06-06 | 上海应用技术大学 | A kind of high thermal conductivity coefficient borosilicate fluorescent glass material and preparation method thereof |
-
2017
- 2017-09-13 CN CN201710823250.9A patent/CN107365070A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101471417A (en) * | 2007-12-27 | 2009-07-01 | 丰田合成株式会社 | Method for manufacturing glass plate containing fluophor and method for manufacturing light-emitting device |
| CN101643315A (en) * | 2009-08-10 | 2010-02-10 | 武汉理工大学 | Low-melting-point fluorescent glass for white light LED and preparation method thereof |
| CN103137835A (en) * | 2011-12-01 | 2013-06-05 | 弘大贸易股份有限公司 | Method of enhancing color rendering index of a white led |
| CN104282827A (en) * | 2013-07-04 | 2015-01-14 | 三星电子株式会社 | Wavelength conversion structure, apparatus comprising wavelength conversion structure, and related methods of manufacturing |
| CN104087290A (en) * | 2014-07-15 | 2014-10-08 | 江苏罗化新材料有限公司 | Method for preparing nitride red phosphor |
| CN104130776A (en) * | 2014-07-15 | 2014-11-05 | 江苏罗化新材料有限公司 | Non-hydrogenous reducing preparation method for nitride red fluorescent powder |
| CN106800371A (en) * | 2017-01-25 | 2017-06-06 | 上海应用技术大学 | A kind of high thermal conductivity coefficient borosilicate fluorescent glass material and preparation method thereof |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107973527A (en) * | 2018-01-04 | 2018-05-01 | 上海应用技术大学 | A kind of preparation method of double layer phosphor |
| CN110156326A (en) * | 2018-02-11 | 2019-08-23 | 天津理工大学 | Fluorescent glass ceramics based on glass powder with low melting point and preparation method thereof |
| CN108455846A (en) * | 2018-04-02 | 2018-08-28 | 上海应用技术大学 | A kind of fluorescent glass of composite phosphor and its preparation method and application |
| CN110360469A (en) * | 2019-07-17 | 2019-10-22 | 上海应用技术大学 | A kind of full spectral laser based on fluorophor |
| CN110360469B (en) * | 2019-07-17 | 2023-06-20 | 上海应用技术大学 | Full spectrum laser device based on fluorophor |
| CN110698073A (en) * | 2019-11-19 | 2020-01-17 | 温州大学新材料与产业技术研究院 | Full-spectrum borosilicate fluorescent glass and preparation method thereof |
| CN110698073B (en) * | 2019-11-19 | 2022-05-13 | 温州大学新材料与产业技术研究院 | Full-spectrum borosilicate fluorescent glass and preparation method thereof |
| CN112645592A (en) * | 2020-12-23 | 2021-04-13 | 温州大学 | Preparation and application of efficient adjustable composite fluorescent glass material |
| CN112645592B (en) * | 2020-12-23 | 2022-07-05 | 温州大学 | Preparation and application of efficient adjustable composite fluorescent glass material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107365070A (en) | A kind of white light LEDs red green composite fluorescence glass and preparation method thereof | |
| CN101643315B (en) | Low-melting-point fluorescent glass for white light LED and preparation method thereof | |
| CN100412156C (en) | Strontium silicate-based phosphor, fabrication method thereof, and led using the phosphor | |
| CN104726101B (en) | White light LEDs single-substrate white launches fluorophosphate fluorescent material and preparation method | |
| CN103031127B (en) | Orange fluorescent powder and preparation method thereof, and electric light source made of fluorescent powder | |
| CN101314519A (en) | Rare earth doping luminescent glass for white radiation LED and producing thereof | |
| CN108570323B (en) | Lithium strontium phosphate phosphor and preparation method thereof | |
| US9647180B2 (en) | Glass-phosphor composite containing rare-earth ion and light-emitting diode including same | |
| CN108558213A (en) | Fluorescent glass ceramic material, method for manufacturing same, and light emitting device including same | |
| CN107879623B (en) | Red luminescent glass ceramic for white light LED and preparation method thereof | |
| CN108753296A (en) | A kind of red emitting material and its preparation method and application that can be excited by near ultraviolet or blue chip | |
| CN107500529B (en) | YAG fluorescent glass, preparation method thereof and application thereof in white light LED | |
| CN110395913B (en) | Preparation method of fluorescent glass with layered arrangement structure for full-spectrum LED | |
| CN105347677B (en) | A kind of photic white light glass and its preparation technology | |
| CN108455846A (en) | A kind of fluorescent glass of composite phosphor and its preparation method and application | |
| CN106587636B (en) | A kind of low melting point transparent glass-ceramics and its preparation method and application | |
| CN110484251B (en) | Phosphor-aluminum acid strontium lithium sodium phosphor and preparation method thereof | |
| CN104377294B (en) | A kind of light-emitting device | |
| CN106698933A (en) | Transparent glass ceramic with low melting point as well as preparation method and application of transparent glass ceramic | |
| CN107827354B (en) | Red fluorescent glass and preparation method and application thereof | |
| CN108641715B (en) | A kind of fluorine gallic acid barium sodium red light material and preparation method thereof for white light LEDs | |
| CN107936968B (en) | Mn: YAG fluorescent powder preparation method, Mn: YAG (yttrium aluminum garnet) sandwich fluorescent glass as well as preparation method and application thereof | |
| CN102092952A (en) | Transparent glass ceramic with tunable light emitting colors and preparation technique thereof | |
| CN104910916B (en) | A kind of glow color adjustable New Phosphorus lime stone structure light-emitting material and application thereof | |
| CN103672450A (en) | Light emitting device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171121 |