CN105609599B - A kind of encapsulating material and its method for packaging white LED for blue chip - Google Patents
A kind of encapsulating material and its method for packaging white LED for blue chip Download PDFInfo
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- CN105609599B CN105609599B CN201610088997.XA CN201610088997A CN105609599B CN 105609599 B CN105609599 B CN 105609599B CN 201610088997 A CN201610088997 A CN 201610088997A CN 105609599 B CN105609599 B CN 105609599B
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- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 title claims abstract description 16
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 79
- 229910020440 K2SiF6 Inorganic materials 0.000 claims abstract description 25
- 239000003292 glue Substances 0.000 claims abstract description 13
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005266 casting Methods 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- 238000005245 sintering Methods 0.000 claims description 17
- 239000002994 raw material Substances 0.000 claims description 15
- 229910052681 coesite Inorganic materials 0.000 claims description 12
- 229910052906 cristobalite Inorganic materials 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 229910052682 stishovite Inorganic materials 0.000 claims description 12
- 229910052905 tridymite Inorganic materials 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 229910003443 lutetium oxide Inorganic materials 0.000 claims description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 7
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012286 potassium permanganate Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims description 6
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 238000009877 rendering Methods 0.000 abstract description 37
- 238000005286 illumination Methods 0.000 abstract description 8
- 229910004074 SiF6 Inorganic materials 0.000 description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 229910052799 carbon Inorganic materials 0.000 description 11
- 238000005538 encapsulation Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000007873 sieving Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 241001062009 Indigofera Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007850 degeneration Effects 0.000 description 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers 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 having potential barriers 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/55—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing beryllium, magnesium, alkali metals or alkaline earth metals
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/57—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing manganese or rhenium
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/61—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing fluorine, chlorine, bromine, iodine or unspecified halogen elements
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers 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 having potential barriers 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
- H01L33/502—Wavelength conversion materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers 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 having potential barriers 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
- H01L33/502—Wavelength conversion materials
- H01L33/504—Elements with two or more wavelength conversion materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/0041—Processes relating to semiconductor body packages relating to wavelength conversion elements
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
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- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Luminescent Compositions (AREA)
- Led Device Packages (AREA)
Abstract
The invention discloses a kind of encapsulating material and its method for packaging white LED for blue chip, the encapsulating materials, by 10~30% green emitting phosphor of weight percent weight, 0.5~7.5% red fluorescence powder, 0.1~10%K2SiF6:Mn4+Powder and the casting glue of surplus are made, and packaging method includes：By green emitting phosphor, red fluorescence powder and K2SiF6:Mn4+Powder is uniformly mixed with casting glue, and then even application is packaged on blue chip, obtains white light LEDs, in the case of being basically unchanged ensureing white light LEDs luminous efficiency, improves the special colour rendering index R9 of white light.Encapsulating material and method can effectively improve the special colour rendering index R9 of white light, improve the color saturation of white light, while keep good luminous efficiency so that white light LEDs are in the good application prospect in the fields such as show window illumination, reading lighting, medical illumination.
Description
Technical field
The present invention relates to the encapsulating material fields of light source, and in particular to a kind of encapsulating material for blue chip and its white
Light LED encapsulation method.
Background technology
Colour rendering index is evaluation index of the light source to the coloration ability of object.Colour rendering index be divided into general colour rendering index and
Special colour rendering index, general colour rendering index are that light source refers to the special colour developing of 8 kinds of samples of colour as defined in International Commission on Illumination
Several average value, the medium standard color sample of eight kinds of chromas of R1~R8.This 8 kinds of samples of colour are selected from Munsell colour scale, comprising various
Representational tone, they have medium chroma and lightness.Special colour rendering index is light source to a certain selected standard color
The colour rendering index of sample.International Commission on Illumination also replenishes regulations in addition to 8 kinds of tinctorial patterns that regulation calculates general colour rendering index
Calculate the sample of colour of special colour rendering index, R9~R15 red, yellow, green, blue, the colour of skin of American-European young women, leaf green, Asia
The colour of skin of continent young women.
With the development of LED technology, the application field of white light LEDs is also from spies such as large screen display, Landscape Lighting, indicator lights
The fields such as room lighting, medical illumination are gradually stepped into kind light source applications field, and light efficiency, the colour rendering index of light source seem more and more heavier
It will.But the light efficiency of current white light LEDs is mutually restricted with colour rendering index, it is difficult to reach very high requirement simultaneously.Current evaluation light
The colour rendering in source only considers the color fidelity of object, and there is no the color saturations for considering object, have ignored high saturation color
The special colour rendering index R9 of colour rendering index R9-R14, particularly saturated red are particularly important to the visual evaluation of colour rendering quality.
Color saturation but has large effect for measurement effect in practical application, if this is because simply to preceding 8 low saturations
Or the colour rendering index of medium saturation is averagely obtained general colour rendering index, it is possible to obtain a high Ra value, but it is practical
On it is poor to the color representation of high saturation color, it is impossible to reflect true color effect.
At present, white light LEDs mostly excite yellow fluorescent powder using blue chip, but lead to white light due to lacking red color light component
The problems such as the colour temperature of LED is higher, luminous efficiency is relatively low, colour rendering index is low, therefore available blue chip excited blue-green fluorescent powder
Add red fluorescence powder, to achieve the purpose that reduce colour temperature, improve colour rendering index.But the general colour rendering index (Ra) of these schemes exists
Between 80-90, special colour rendering index (R9) is but still very low so that the color saturation of white light is inadequate, comprehensive colour rendering index compared with
It is low, it is unable to reach and requires application requirement.
Current red fluorescence powder wavelength generally in 630-670nm, if you need to improve the light efficiency of white light, is needed wavelength blue shift
To 605-630nm or so.
Invention content
It is low to solve white light LEDs special colour rendering index, lead to problems such as color developing effect poor, the present invention provides one kind to be used for
The encapsulating material and its method for packaging white LED of blue chip, the encapsulating material by green emitting phosphor (510-530nm) with
A certain amount of K is added in the combination of red fluorescence powder (620-640nm)2SiF6:Mn4+Powder, the packaging method can ensure in vain
In the case that light LED luminous efficiencies are basically unchanged, the special colour rendering index R9 of white light is improved, so as to which the colour developing for improving white light refers to
Number.
A kind of encapsulating material for blue chip is made of the raw material of following weight percent weight：
The present invention is used for the encapsulating material of blue chip, blue chip (460nm) is packaged, by green fluorescence
Powder (510-530nm) in the combination of red fluorescence powder (620-640nm) with adding in a certain amount of K2SiF6:Mn4+Powder.K2SiF6:
Mn4+Powder realizes wavelength in the feux rouges of 631nm under blue light excitation, the wide only 3nm of half-wave, can effectively improve the R9 values of white light, from
And improve the synthesis colour rendering index of white light.The blue chip of encapsulating material encapsulation can ensure that white light LEDs luminous efficiency is basic
In the case of constant, the special colour rendering index R9 of white light is improved, so as to improve the colour rendering index of white light.
The green emitting phosphor is Lu2.98Al5O12:0.02Ce3+。
The red fluorescence powder is Sr2Si5N8:Eu2+。
The prior art can be used in casting glue, and the casting glue can be one or both of epoxy resin, silica gel etc., pass through
One-step optimization is epoxy resin.
Further preferably, the encapsulating material for blue chip is made of the raw material of following weight percent weight：
A kind of method for packaging white LED of encapsulating material using for blue chip, includes the following steps：
By green emitting phosphor (500~540nm, preferably 520nm), red fluorescence powder (600~660nm, preferably 630nm) and
K2SiF6:Mn4+Powder is uniformly mixed with casting glue, and then even application is at blue chip (430~490nm, preferably 460nm)
On, it is packaged, obtains white light LEDs.
The green emitting phosphor is Lu2.98Al5O12:0.02Ce3+, the preparation method includes：According to stoichiometry
Compare Lu2.98Al5O12:0.02Ce3+, weigh Lu2O3Powder, Al2O3、CeO2It is placed in agate to grind in alms bowl, be uniformly mixed, using full of also
Primordial Qi atmosphere carries out high temperature sintering, and calcination temperature is 900~1400 DEG C, and the time is 2~6h, is made annealing treatment, obtained after sintering
Lu2.98Al5O12:0.02Ce3+Fluorescent powder.It advanced optimizes, calcination temperature is 1000 DEG C, calcination time 3h.
The red fluorescence powder is Sr2Si5N8:Eu2+, the preparation method includes：With SrCO3、SiO2、Si3N4、
Eu2O3For raw material, according to stoichiometric ratio Sr2Si5N8:Eu2+It weighs, and uniformly mixed raw material will be passed through under reducing atmosphere
Be warming up to 1400~1600 DEG C, react 5~9h, it is to be sintered it is complete after made annealing treatment, obtain Sr2Si5N8:Eu2+Fluorescent powder.System
Standby Sr2Si5N8:Eu2+The calcination temperature of fluorescent powder is 1400~1600 DEG C, reacts 5~9h, advanced optimizes and be for calcination temperature
1500 DEG C, reaction time 6h.
The K2SiF6:Mn4+Raw powder's production technology includes：According to K2SiF6:Mn4+Stoichiometric ratio, by SiO2It puts
Enter HF/KMnO4In aqueous solution, standing obtains K2SiF6:Mn4+。
The prior art, such as GaN, InGaN can be used in the blue chip, and it can be GaN chips to advanced optimize.
The reducing atmosphere can be nitrogen or nitrogen and hydrogen mixture, advanced optimize as nitrogen and hydrogen mixture, i.e., by volume hundred
Divide the N than 95%2With 5% H2Composition.
The degeneration processing is carried out in Muffle furnace, and sintering temperature is 400 DEG C~600, and the time is 1~3h, into one
Step, sintering temperature are 500 DEG C, time 2h, and the carbon calcined because of high temperature carbon shirt-circuiting furnace to bring can be mainly removed by low-temperature sintering
The impurity such as powder improve the purity of sample.
The present invention adds in K in the encapsulation of red fluorescence powder, green emitting phosphor and blue chip2SiF6:Mn4+Powder can be effective
Ground improves the colour rendering index of white light LEDs, improves the lighting quality of LED, plays important propulsion to the development of LED light illumination and makees
With.
Compared with prior art, the invention has the advantages that：
By adding in a certain amount of K in the present invention2SiF6:Mn4+Powder applies together with red fluorescence powder and green emitting phosphor
It applies and is packaged on blue chip, the colour developing of saturation feux rouges can be effectively improved under the premise of preferable luminous efficiency is kept
Index R9, and and then improve the colour rendering index of white light, solve at present that white light LEDs occur in blue chip encapsulation technology on the market
The problem of red area colour developing is insufficient.Meanwhile packaged type using the present invention, white light LEDs can be reduced in a certain range
Colour temperature makes the light that LED is sent out that people be allowed to feel more warm.The powder that the present invention uses mainly has Lu2.98Al5O12:0.02Ce3+
Fluorescent powder, Sr2Si5N8:Eu2+Fluorescent powder and K2SiF6:Mn4+Powder, three kinds of powders have stable physical property, can be when long
Between energy radiation lower keep good optical property.And preparation process is simple used by three kinds of powders, of low cost, tool
There is good market value.In the present invention, new fluorescent powder packaging method can effectively improve the special colour rendering index of white light
R9, improves the color saturation of white light, while keeps good luminous efficiency so that white light LEDs shine in show window illumination, reading
The fields such as bright, medical illumination have a good application prospect.
Description of the drawings
Fig. 1 is the white-light LED fluorescence spectrogram obtained in embodiment 1 (i.e. comparative example 1)；
Fig. 2 is the white-light LED fluorescence spectrogram obtained in embodiment 2；
Fig. 3 is the white-light LED fluorescence spectrogram obtained in embodiment 3；
Fig. 4 is the white-light LED fluorescence spectrogram obtained in embodiment 4；
Fig. 5 is the white-light LED fluorescence spectrogram obtained in embodiment 5 (i.e. comparative example 2).
Specific embodiment
Embodiment 1 (as a comparison case 1)
LuAG (520nm) green emitting phosphors and 0.036g of 0.255g is applied on blue chip (460nm)
Sr2Si5N8:Eu2+Red fluorescence powder (630nm), is packaged.
1) according to stoichiometric ratio Lu2.98Al5O12:0.02Ce3+, precise Lu2O3Powder, Al2O3、CeO2It is placed in agate
It grinds in alms bowl, is uniformly mixed, is moved in crucible after sieving, using full of reducing atmosphere (percent by volume 95%N2, 5%H2)
High temperature carbon shirt-circuiting furnace carries out high temperature sintering (1000 DEG C, 3h), is made annealing treatment (500 DEG C, 2h) after sintering in Muffle furnace is put into,
Obtain the high Lu of purity2.98Al5O12:0.02Ce3+Fluorescent powder (i.e. LuAG green emitting phosphors).
2) with SrCO3、SiO2、Si3N4、Eu2O3For raw material, according to stoichiometric ratio Sr2Si5N8:Eu2+It weighs, and will pass through
Uniformly mixed raw material is put into high temperature carbon shirt-circuiting furnace, in reducing atmosphere (percent by volume 95%N2, 5%H2) under be warming up to 1500
DEG C reaction 6h.It is to be sintered it is complete after be put into Muffle furnace and suffered and made annealing treatment (500 DEG C, 2h), obtain Sr2Si5N8:Eu2+Fluorescence
Powder.
3) Lu that precise 0.255g is prepared2.98Al5O12:0.02Ce3+Fluorescent powder, 0.036g are prepared into
Sr2Si5N8:Eu2+Fluorescent powder is uniformly mixed with the casting glue of 1g, and then even application is on the surface of blue chip (460nm), into
Row encapsulation.
Embodiment 2
LuAG (520nm) green emitting phosphors and 0.036g of 0.255g is applied on blue chip (460nm)
Sr2Si5N8:Eu2+Red fluorescence powder (630nm), then add the K of 0.01g2SiF6:Mn4+Red fluorescence powder (630nm), is sealed
Dress.
1) according to stoichiometric ratio Lu2.98Al5O12:0.02Ce3+, precise Lu2O3Powder, Al2O3、CeO2It is placed in agate
It grinds in alms bowl, is uniformly mixed, is moved in crucible after sieving, using full of reducing atmosphere (percent by volume 95%N2, 5%H2)
High temperature carbon shirt-circuiting furnace carries out high temperature sintering, and calcination temperature is 1000 DEG C, time 3h.It anneals in Muffle furnace is put into after sintering
It handles (500 DEG C, 2h), obtains the high Lu of purity2.98Al5O12:0.02Ce3+Fluorescent powder (i.e. LuAG green emitting phosphors).
2) with SrCO3、SiO2、Si3N4、Eu2O3For raw material, according to stoichiometric ratio Sr2Si5N8:Eu2+It weighs, and will pass through
Uniformly mixed raw material is put into high temperature carbon shirt-circuiting furnace, in reducing atmosphere (percent by volume 95%N2, 5%H2) under be warming up to 1500
DEG C, react 6h.It is to be sintered it is complete after be put into Muffle furnace and suffered and made annealing treatment (500 DEG C, 2h), obtain Sr2Si5N8:Eu2+Fluorescence
Powder.
3) according to K2SiF6:Mn4+Stoichiometric ratio, by SiO2It is put into HF/KMnO4In aqueous solution, stood at 25 DEG C of room temperature
It can obtain required K2SiF6:Mn4+。
4) the above-mentioned Lu being prepared of accurate weighing 0.255g2.98Al5O12:0.02Ce3+Fluorescent powder, 0.036g
Sr2Si5N8:Eu2+The K of fluorescent powder and 0.01g2SiF6:Mn4+Powder is uniformly mixed with the casting glue of 1g, and then even application is in indigo plant
The surface of optical chip, is packaged.
Fig. 1, Fig. 2 are respectively embodiment 1 (i.e. comparative example 1) and the fluorescence spectra of the white light LEDs obtained by embodiment 2.
As seen from the figure, K is added in the encapsulation technology of Xiang Hong, green fluorescence powder coating blue-light LED chip2SiF6:Mn4+Powder can have
Effect ground improves the colour rendering index of the saturation feux rouges R9 of white light LEDs, improves the red light region ratio that white light LEDs are sent out, Jin Erti
The high colour rendering index of white light LEDs.
Embodiment 3
LuAG (520nm) green emitting phosphors and 0.036g of 0.255g is applied on blue chip (460nm)
Sr2Si5N8:Eu2+Red fluorescence powder (630nm), then add the K of 0.04g2SiF6:Mn4+Red fluorescence powder (630nm), is sealed
Dress.
1) according to stoichiometric ratio Lu2.98Al5O12:0.02Ce3+, precise Lu2O3Powder, Al2O3、CeO2It is placed in agate
It grinds in alms bowl, is uniformly mixed, is moved in crucible after sieving, using full of reducing atmosphere (percent by volume 95%N2, 5%H2)
High temperature carbon shirt-circuiting furnace carries out high temperature sintering, and calcination temperature is 1000 DEG C, time 3h.It anneals in Muffle furnace is put into after sintering
It handles (500 DEG C, 2h), obtains the high Lu of purity2.98Al5O12:0.02Ce3+Fluorescent powder (i.e. LuAG green emitting phosphors).
2) with SrCO3、SiO2、Si3N4、Eu2O3For raw material, according to stoichiometric ratio Sr2Si5N8:Eu2+It weighs, and will pass through
Uniformly mixed raw material is put into high temperature carbon shirt-circuiting furnace, in reducing atmosphere (percent by volume 95%N2, 5%H2) under be warming up to 1500
DEG C, react 6h.It is to be sintered it is complete after be put into Muffle furnace and suffered and made annealing treatment (500 DEG C, 2h), obtain Sr2Si5N8:Eu2+Fluorescence
Powder.
3) according to K2SiF6:Mn4+Stoichiometric ratio, by SiO2It is put into HF/KMnO4In aqueous solution, stood at 25 DEG C of room temperature
It can obtain required K2SiF6:Mn4+。
4) Lu that precise 0.255g is prepared2.98Al5O12:0.02Ce3+The Sr of fluorescent powder, 0.036g2Si5N8:
Eu2+The K of fluorescent powder and 0.04g2SiF6:Mn4+Powder is uniformly mixed with the casting glue of 1g, and then even application is in blue chip
The surface of (460nm), is packaged.
Embodiment 4
LuAG (520nm) green emitting phosphors and 0.036g of 0.255g is applied on blue chip (460nm)
Sr2Si5N8:Eu2+Red fluorescence powder (630nm), then add the K of 0.08g2SiF6:Mn4+Red fluorescence powder (630nm), is sealed
Dress.
1) according to stoichiometric ratio Lu2.98Al5O12:0.02Ce3+, precise Lu2O3Powder, Al2O3、CeO2It is placed in agate
It grinds in alms bowl, is uniformly mixed, is moved in crucible after sieving, using full of reducing atmosphere (percent by volume 95%N2, 5%H2)
High temperature carbon shirt-circuiting furnace carries out high temperature sintering, and calcination temperature is 1000 DEG C, time 3h.It anneals in Muffle furnace is put into after sintering
It handles (500 DEG C, 2h), obtains the high Lu of purity2.98Al5O12:0.02Ce3+Fluorescent powder (i.e. LuAG green emitting phosphors).
2) with SrCO3、SiO2、Si3N4、Eu2O3For raw material, according to stoichiometric ratio Sr2Si5N8:Eu2+It weighs, and will pass through
Uniformly mixed raw material is put into high temperature carbon shirt-circuiting furnace, in reducing atmosphere (percent by volume 95%N2, 5%H2) under be warming up to 1500
DEG C, react 6h.It is to be sintered it is complete after be put into Muffle furnace and suffered and made annealing treatment (500 DEG C, 2h), obtain Sr2Si5N8:Eu2+Fluorescence
Powder.
3) according to K2SiF6:Mn4+Stoichiometric ratio, by SiO2It is put into HF/KMnO4In aqueous solution, stood at 25 DEG C of room temperature
It can obtain required K2SiF6:Mn4+。
4) Lu that precise 0.255g is prepared2.98Al5O12:0.02Ce3+The Sr of fluorescent powder, 0.036g2Si5N8:
Eu2+The K of fluorescent powder and 0.08g2SiF6:Mn4+Powder is uniformly mixed with casting glue, and then even application is in blue chip
The surface of (460nm), is packaged.
Fig. 2, Fig. 3, Fig. 4 are respectively embodiment 2, embodiment 3, the fluorescence spectra of white light LEDs prepared by embodiment 4.
There is figure to can be seen that in a certain range with K2SiF6:Mn4+The increase of powder doping, the colour rendering index of white light LEDs are gradual
Raising.
Embodiment 5 (as a comparison case 2)
LuAG (520nm) green emitting phosphors of 0.255g and the K of 0.08g are applied on blue chip (460nm)2SiF6:
Mn4+Red fluorescence powder (630nm), is packaged.
LuAG (520nm) green emitting phosphors and 0.036g of 0.255g is applied on blue chip (460nm)
Sr2Si5N8:Eu2+Red fluorescence powder (630nm) applies, then adds the K of 0.01g2SiF6:Mn4+Red fluorescence powder (630nm), into
Row encapsulation.
1) according to stoichiometric ratio Lu2.98Al5O12:0.02Ce3+, precise Lu2O3Powder, Al2O3、CeO2It is placed in agate
It grinds in alms bowl, is uniformly mixed, is moved in crucible after sieving, high temperature sintering is carried out using the high temperature carbon shirt-circuiting furnace full of reducing atmosphere,
Calcination temperature is 1000 DEG C, time 3h.(500 DEG C, 2h) are made annealing treatment after sintering in Muffle furnace is put into, obtain purity
High Lu2.98Al5O12:0.02Ce3+Fluorescent powder.
2) according to K2SiF6:Mn4+Stoichiometric ratio, by SiO2It is put into HF/KMnO4In aqueous solution, being stood under room temperature can be with
Obtain required K2SiF6:Mn4+。
3) Lu that precise 0.255g is prepared2.98Al5O12:0.02Ce3+The K of fluorescent powder and 0.08g2SiF6:Mn4+
Powder is uniformly mixed with 1g casting glues, and then even application is packaged on the surface of LED chip.
Fig. 5 is the fluorescence spectra of the white light LEDs prepared by embodiment 5 (as a comparison case 2), its Fig. 4 is compared
It was found that K2SiF6:Mn4+The light that powder is emitted needs narrow-band light in red light region, if by K2SiF6:Mn4+Powder,
Green emitting phosphor is packaged with blue chip, and white light LEDs luminous intensity obtained is low, and colour rendering is poor.Therefore, K2SiF6:Mn4+
Powder play the role of in white light LEDs improve saturation feux rouges colour rendering index, and then solve white-light LED encapsulation in red light region not
The problem of sufficient.
Claims (6)
1. a kind of method for packaging white LED, which is characterized in that using the encapsulating material for blue chip, include the following steps：
By green emitting phosphor, red fluorescence powder and K2SiF6:Mn4+Powder is uniformly mixed with casting glue, and then even application is in blue light
It on chip, is packaged, obtains white light LEDs；
The encapsulating material for blue chip is made of the raw material of following weight percent weight：
The green emitting phosphor is Lu2.98Al5O12:0.02Ce3+；
The red fluorescence powder is Sr2Si5N8:Eu2+。
2. method for packaging white LED according to claim 1, which is characterized in that the casting glue is epoxy resin, silicon
One or both of glue.
3. method for packaging white LED according to claim 1, which is characterized in that the green emitting phosphor is
Lu2.98Al5O12:0.02Ce3+, preparation method includes：According to stoichiometric ratio Lu2.98Al5O12:0.02Ce3+, weigh Lu2O3Powder
Body, Al2O3、CeO2It is placed in agate to grind in alms bowl, be uniformly mixed, carry out high temperature sintering using full of reducing atmosphere, calcination temperature is
900~1400 DEG C, the time is 2~6h, is made annealing treatment after sintering, obtains Lu2.98Al5O12:0.02Ce3+Fluorescent powder.
4. method for packaging white LED according to claim 1, which is characterized in that the red fluorescence powder is
Sr2Si5N8:Eu2+, preparation method includes：With SrCO3、SiO2、Si3N4、Eu2O3For raw material, according to stoichiometric ratio Sr2Si5N8:
Eu2+It weighs, and 1400~1600 DEG C will be warming up under reducing atmosphere by uniformly mixed raw material, react 5~9h, it is to be sintered
It is made annealing treatment after complete, obtains Sr2Si5N8:Eu2+Fluorescent powder.
5. method for packaging white LED according to claim 3 or 4, which is characterized in that the reducing atmosphere for nitrogen or
Nitrogen and hydrogen mixture；
The annealing is carried out in Muffle furnace, and sintering temperature is 400 DEG C~600, and the time is 1~3h.
6. method for packaging white LED according to claim 1, which is characterized in that the K2SiF6:Mn4+The preparation of powder
Method includes：According to K2SiF6:Mn4+Stoichiometric ratio, by SiO2It is put into HF/KMnO4In aqueous solution, standing obtains K2SiF6:
Mn4+。
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| CN101939857A (en) * | 2008-02-07 | 2011-01-05 | 三菱化学株式会社 | Semiconductor light emitting device, backlight, color image display device and phosphor to be used for them |
| CN102986044A (en) * | 2010-10-15 | 2013-03-20 | 三菱化学株式会社 | White light emitting device and lighting device |
| CN104781942A (en) * | 2012-11-01 | 2015-07-15 | 皇家飞利浦有限公司 | LED-based device with wide color gamut |
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| CN101719531A (en) * | 2008-10-09 | 2010-06-02 | 夏普株式会社 | Semiconductor light-emitting device as well as image display and liquid crystal display employing the same |
| CN102986044A (en) * | 2010-10-15 | 2013-03-20 | 三菱化学株式会社 | White light emitting device and lighting device |
| CN104781942A (en) * | 2012-11-01 | 2015-07-15 | 皇家飞利浦有限公司 | LED-based device with wide color gamut |
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Address after: Hangzhou City, Zhejiang province 310018 Xiasha Higher Education Park source Street No. 258 Patentee after: China University of Metrology Address before: 310018 Hangzhou, Zhejiang, Jianggan District province Xiasha Higher Education Park, No. 258 source street Patentee before: China Institute of Metrology |
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Application publication date: 20160525 Assignee: NINGBO SUNPU OPTO CO., LTD. Assignor: China University of Metrology Contract record no.: X2019330000043 Denomination of invention: Packaging material for blue chip and white LED packaging method Granted publication date: 20180629 License type: Common License Record date: 20191111 |