CN106486586B - Light emitting device and method for manufacturing the same - Google Patents
Light emitting device and method for manufacturing the same Download PDFInfo
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- CN106486586B CN106486586B CN201510532841.1A CN201510532841A CN106486586B CN 106486586 B CN106486586 B CN 106486586B CN 201510532841 A CN201510532841 A CN 201510532841A CN 106486586 B CN106486586 B CN 106486586B
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- 238000000034 method Methods 0.000 title description 17
- 238000004519 manufacturing process Methods 0.000 title description 2
- 239000000463 material Substances 0.000 claims abstract description 112
- 239000011241 protective layer Substances 0.000 claims abstract description 37
- 238000002360 preparation method Methods 0.000 claims abstract description 27
- UMVBXBACMIOFDO-UHFFFAOYSA-N [N].[Si] Chemical group [N].[Si] UMVBXBACMIOFDO-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000010410 layer Substances 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims description 118
- 239000000843 powder Substances 0.000 claims description 70
- 239000010408 film Substances 0.000 claims description 58
- 238000004020 luminiscence type Methods 0.000 claims description 52
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 30
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 20
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 17
- 229910017464 nitrogen compound Inorganic materials 0.000 claims description 17
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000003054 catalyst Substances 0.000 claims description 15
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 14
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
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- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
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- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 8
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
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- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
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- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 5
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- PNJWIWWMYCMZRO-UHFFFAOYSA-N 4-penten-2-one Chemical compound CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 4
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- 229910003087 TiOx Inorganic materials 0.000 claims description 4
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- 239000002253 acid Substances 0.000 claims description 4
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- 229910052681 coesite Inorganic materials 0.000 claims description 4
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- 229910052814 silicon oxide Inorganic materials 0.000 claims description 4
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- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 claims description 4
- 125000005270 trialkylamine group Chemical group 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- 229910052844 willemite Inorganic materials 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 3
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- 229910052802 copper Inorganic materials 0.000 claims description 3
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- 239000004793 Polystyrene Substances 0.000 claims 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052746 lanthanum Inorganic materials 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 claims 1
- 150000002902 organometallic compounds Chemical class 0.000 claims 1
- 238000000576 coating method Methods 0.000 description 17
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- 239000011248 coating agent Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
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- 239000000084 colloidal system Substances 0.000 description 4
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- 238000007790 scraping Methods 0.000 description 4
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
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- 150000002602 lanthanoids Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
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- 238000005829 trimerization reaction Methods 0.000 description 2
- 229920000297 Rayon Polymers 0.000 description 1
- UBMXAAKAFOKSPA-UHFFFAOYSA-N [N].[O].[Si] Chemical compound [N].[O].[Si] UBMXAAKAFOKSPA-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- H01L33/505—Wavelength conversion elements characterised by the shape, e.g. plate or foil
-
- 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
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Luminescent Compositions (AREA)
- Led Device Packages (AREA)
Abstract
The invention discloses a light-emitting device and a preparation method thereof, wherein the light-emitting device comprises: a first light emitting unit; the second light-emitting unit covers the first light-emitting unit and comprises a fluorescent material film and a protective layer; the protective layer is located on the fluorescent material film, the protective layer is a silicon nitrogen material layer, and the tolerance temperature of the light-emitting device exceeds 320 ℃.
Description
Technical field
The present invention is to be prepared about a kind of light emitting device by novel fluorescent material coating method, espespecially a kind of
Light emitting device with excellent durability, weatherability, resistance to scraping and firm photoluminescent property.
Background technique
In recent years, because light emitting diode (LED) has few luminous efficiency height, power consumption, long service life and component size
The advantages that small, is widely used in various light emitting devices.However, there is light emitting diode heat dissipation, luminance shortage and brightness to pass
The problems such as subtracting, and white light can not be directly inspired, therefore, attempt to develop efficient white light LEDs there are many research, to take
For existing lighting apparatus.
The white light LEDs of mainstream at present, using blue LED chip cooperation yellow light YAG fluorescent powder body, with as
White light source.Although the continuity of spectral wavelength distribution is not so good as sunlight, and coloured with white light produced by this complementary colours principle
Color uneven situation, therefore color saturation is lower.Accordingly, the white light source generated by this method can only be used to simply illuminate,
And it cannot be widely applied to people's livelihood illumination market.In addition, also using ultraviolet light-emitting diodes chip cooperation feux rouges, green light,
And blue light three-color phosphor can be mixed into white light by the trichromatic light mixing mechanism of red blue green.
Currently, the light emitting diode for forming capable of emitting white light is packaged using following methods.Firstly, according to predetermined colour temperature scale
Take more than one fluorescent powder of a proper proportion.Then, fluorescent powder is added to resin (such as: silica resin or epoxy resin)
And stir, be dispersed in fluorescent powder can in resin.Then, the resin for being dispersed with fluorescent powder is mixed with curing agent, with point
The high viscosity colloid 102 for being dispersed with fluorescent powder is covered in LED chip 101 by glue machine, and drying and encapsulation procedure can be made one
It is stamped the white light LEDs element 10 of solid state fluorescence colloid, as shown in Figure 1.However, obtained white light LEDs element, due to fluorescent powder
External form specific gravity and size it is irregular, therefore solid state fluorescence colloid is easy and to lead to colour temperature not because of fluorescent powder material property disunity
The problems such as quasi- uneven with light mixing.
In order to reinforce fixed fluorescence blob of viscose and prevent from causing LED element impaired because aqueous vapor is penetrated into, will generally cover once again
Transparent organic silicon glue or epoxide-resin glue are sprayed on solid state fluorescence colloid.However, under long-time operation, organic silica gel or ring
Oxygen resin glue often has the generation of phenomena such as yellow or fragmentation, can not still prevent aqueous vapor or impurity from penetrating into LED element, cause the effect that shines
Rate reduces even integral member failure.Also, organosilicon glue-line or epoxy glue layer is not high to the tolerance of temperature (is only capable of fitting
For about 150 DEG C or less), therefore environment temperature must be taken into consideration in using LED element when, is greatly lowered the application value of LED.Therefore,
Need to develop at present it is a kind of with excellent durability, weatherability, resistance to scraping light emitting device, this light emitting device simultaneously has simultaneously
The characteristics such as even light mixing, refractive index be good, to which the application value of white light emitting device can be significantly increased.
Summary of the invention
The main object of the present invention provide it is a kind of with excellent durability, weatherability, resistance to scraping light emitting device,
It is composed of the first luminescence unit and the second luminescence unit, wherein fluorescent material closely pastes the first luminescence unit, and this
The light emitting device of invention has that even light mixing, refractive index are good, go out the medium characteristic of luminous intensity collection.
To reach above-mentioned purpose, light emitting device of the invention is completed via a kind of novel fluorescent material coating method,
Include the following steps: that (A) disperses a fluorescent material in one second solvent, to form a fluorescent material solution；(B) by one
One luminescence unit is placed in a container, and injects a third solvent, and the third solvent covers the surface of first luminescence unit；
(C) one the 4th solvent is injected into the third solvent, to form one the 5th solvent；(D) by the fluorescent material solution be added to this
Five solvents, to form a fluorescent material film in the 5th solvent surface；(E) the 5th solvent in the container is removed, this is made
Fluorescent material film is formed in the first luminescence unit surface；(F) in forming a protective layer on the fluorescent material film；And
(G) heat treatment is formed with first luminescence unit of the protective layer；Wherein, which is a silicon nitride material layer, and obtained
The tolerable temperature of the light emitting device is at 320 DEG C or more.
In step (D), the 5th solvent is the combination of third solvent and the 4th solvent, and the 5th is formed in step (C)
The rear standing of solvent 0~30 minute, preferably 5~20 minutes, more preferably 5~10 minutes, will the middle phosphor formed of step (A)
Expect that solution is placed in the 5th solvent, and then fluorescent material film can be made well to be formed in the first luminescence unit surface.
In step (E) afterwards and before step (F), can further include a step (E1): drying is formed with the fluorescent material film
The substrate, remain in the second solvent on first luminescence unit to remove.Also, after step (G), a step can be further included
Suddenly (G1): repeating the step (A) accordingly, can be formed to step (G) with forming multiple fluorescent material films and multiple protective layers
The fluorescent material film and the protective layer being arranged alternately.The usually intellectual of having can be according to actually required in the art
Light mixing mechanism, and determine the fluorescent material film quantity of setting.
In fluorescent material coating method of the invention, the second solvent, third solvent and the 4th solvent have no it is specifically limited,
As long as meeting following conditions: third solvent specific gravity is greater than the second solvent and the 4th solvent.It is described in detail, when third is added in the 4th solvent
When solvent forms five solvents, second will form temporary interface with the 4th solvent, and time of repose be more than about 30 minutes with
Afterwards, this interface can disappear, i.e., the 4th solvent is thoroughly mixed with third solvent.Preferably, second solvent, the third solvent and
4th solvent can be each independently selected from by: water, methanol, ethyl alcohol, propyl alcohol, butanol, isopropanol, acetone, butanone, normal butane,
Pentane, n-hexane, normal heptane, ethyl acetate, butyl acetate, ether, glycol dimethyl ether (DME), methylene chloride (DCM),
Dimethylformamide (DMF), tetrahydrofuran (THF), n-methyl-2-pyrrolidone (NMP), 3- methoxy propyl fine (MPN) and its
Set composed by mixture；So the invention is not limited thereto.Second preferred solvents are normal butane or isopropanol, the third solvent
Preferably ethyl acetate and the 4th preferred solvents are that ether or 3- methoxy propyl are fine (MPN).
The present invention separately provides a kind of light emitting device, is made of the above method, which includes: one first luminous single
Member；And one second luminescence unit, it is covered on first luminescence unit, and second luminescence unit includes that a fluorescent material is thin
Film and a protective layer, wherein the protective layer is located on the fluorescent material film, which is a silicon nitride material layer, and the hair
The tolerable temperature of electro-optical device is more than 320 DEG C.
In light emitting device of the invention, the thickness of first luminescence unit and second luminescence unit has no special limit
System, and the overall thickness of first luminescence unit and second luminescence unit is between 105 μm to 225 μm, preferably extremely in 120 μm
Between 210 μm.In addition, light emitting device of the invention has a non-uniform surface, therefore the appearance of light emitting device is out-of-flatness
Plate structure.
In light emitting device of the invention and preparation method thereof, which may include: shown at least one Formulas I
Silicon-nitrogen compound, one first solvent and a catalyst,
Wherein n is positive integer, preferably between 4 to 3000, more preferably between 4 to 300；And the silicon nitrification
The number-average molecular weight of object is 150 to 150,000 gram/mole, preferably 10, between 000 to 15,000 gram/mole.
Wherein, there is high-adhesiveness and high temperature resistant with high rigidity, to substrate after silicon-nitrogen compound heat treatment, even if
Under conditions of about 300 DEG C of temperatures above, still consolidated by the silicon nitride material layer that silicon-nitrogen compound, the first solvent and catalyst are formed
And there is not phenomena such as yellow, cracking, protect fluorescent material film and avoid the situation of fluorescent powder removing.In addition, the silicon nitrogen
Compound can mix a nanometer materials, be at least one selected from by TiO2、SiO2、ZnO、ZrO、Y2O3、Al2O3、CoO、MnO2、
Set composed by PbO, NiO, CuO and its compound, the partial sizes of the nanometer materials can be between 5nm between 500nm, can
Modulation Refractive Index of Material and light transmittance promote light mixing effect and light extraction efficiency.
Wherein, which is the solvent of anhydrous state, is at least one selected from by dimethylbenzene, toluene, ethyl alcohol, first
Collection composed by alcohol, isopropanol, ethylene glycol, butyl acetate, ethyl acetate, dibasic ester (Dibasic ester) and petroleum ether
It closes；Preferably dibasic ester and methanol mixture.In addition, the catalyst be the miscellaneous cyclic compound of N-, one-alkylamine, di-alkyl amine,
Trialkylamine, organic acid, inorganic acid, peroxide, metal carboxylate, vinyl acetone acid misfit object, metal or organic metal
Compound；The miscellaneous cyclic compound of preferably N- or metal carboxylate.The usually intellectual of having can be according to selection in the art
Silicon-nitrogen compound, the properties such as hardness, mobility needed for considering protective layer and select appropriate solvent and catalyst.By silicon nitrification
The silicon nitride material layer that object, the first solvent and catalyst are formed penetrates into the hole between fluorescent material film and substrate compared with Canon, consolidates glimmering
The luminescent properties of luminescent material.
In light emitting device of the invention and preparation method thereof, which may include a fluorescent powder, preferably can be more
Including a ball-type carrier；In the case where the fluorescent material includes the fluorescent powder and the ball-type carrier, fluorescent powder can be covered
Ball-type carrier surface；Fluorescent powder may be included in ball-type carrier inside；Or part fluorescent powder covering ball-type carrier surface, and portion
Fluorescent powder is divided to be contained in ball-type carrier inside.Meanwhile the material of ball-type carrier can be SiOx, TiOx, PS, PMMA or trimerization
Melamine resin.The material of fluorescent powder can be general known fluorescent powder, such as: selected from by ZnO, ZrO2、PbO、Y2O3、Y2O2、
Zn2SiO4、Y3Al5O12、Y3(AlGa)5O12Y2SiO5、LaOCl、InBO3、ZnGa2O4、ZnS、PbS、CdS、CaS、SrS、
ZnxCd1-xS、Y2O2S, AlN and Gd2O2The compound gathered composed by S, and can more be mixed as the compound of fluorescent powder
Miscellaneous at least one selected from by Cu, Ag, Eu, Yb, La, Cl, Tb, Al, Ce, Er, Zn, Mn and other lanthanide series (Pr, Pm, Sm, Ho,
Er set element composed by).Furthermore the partial size of ball-type carrier is preferably between 10 μm to 100 μm, more preferably extremely between 25 μm
Between 50 μm；And the partial size of fluorescent powder is preferably between 5 μm to 50 μm, more preferably between 10 μm to 25 μm.Therefore, by
It is uniform in fluorescent material partial size and property, and uniform fluorescent material film can be formed in substrate surface.
In light emitting device of the invention and preparation method thereof, the first luminescence unit can be any LED chip or LED element
Semi-finished product, preferably one is formed with the blue light epi-wafer of epitaxial layer, a packed LED chip (face-up chip), a vertical LED
Chip (vertical chip) or a flip LED chip.
In light emitting device of the invention and preparation method thereof, the protective layer is using coating common in the art
Method is formed on the fluorescent material film, such as spin-coating method, stick coating method, scraper coating, rolling method, spraying coating, bristle apply
Method, dipping coating etc..Therefore, fluorescent material film can be stable on substrate and be not easy to be stripped, at the same adjustment be coated with it is glimmering
The refractive index of the substrate of luminescent material.
Accordingly, through fluorescent material coating method of the invention, phosphor that can be uniform by property with easy processing procedure
Material film is formed on substrate, and silicon nitrogen protective layer is formed on fluorescent material film, and then produces even light mixing, folding
It is good while there is the light emitting device of excellent durability to penetrate rate, it is existing to there will not be yellow or deterioration etc. even across long-time operation
As occurring, it effectively prevent aqueous vapor or impurity to penetrate into light emitting device, stablizes the luminous efficiency for maintaining device.
Detailed description of the invention
Fig. 1 is the schematic diagram of existing light emitting diode.
Fig. 2A to 2H is that the fluorescent material of the embodiment of the present invention 1 is coated on the flow chart of substrate surface.
Specific embodiment
Illustrate embodiments of the present invention below by way of particular specific embodiment, the personage for being familiar with this skill can be by this theory
Other advantages and efficacy of the present invention can be easily understood for bright book disclosure of that.The present invention also can be different specific by other
Embodiment is implemented or is applied, and the various details in this specification also can not depart from this hair for different viewpoints and application
Various modifications and change are carried out under bright spirit.
The present invention provides it is a kind of with excellent durability, weatherability, resistance to scraping light emitting device, shone by first
Unit and the second luminescence unit are composed, and wherein fluorescent material closely pastes the first luminescence unit, and of the invention are shone
Device has that even light mixing, refractive index are good, go out the medium characteristic of luminous intensity collection.
Light emitting device of the invention is completed via a kind of novel fluorescent material coating method, including the following steps: (A)
It disperses a fluorescent material in one second solvent, to form a fluorescent material solution；(B) one first luminescence unit is placed in one
Container, and a third solvent is injected, and the third solvent covers the surface of first luminescence unit；(C) one the 4th solvent is infused
Enter the third solvent, to form one the 5th solvent；(D) the fluorescent material solution is added to the 5th solvent, in the 5th
Solvent surface forms a fluorescent material film；(E) the 5th solvent in the container is removed, the fluorescent material film is formed in
The first luminescence unit surface；(F) in forming a protective layer on the fluorescent material film；And (G) heat treatment is formed with the guarantor
First luminescence unit of sheath；Wherein, which is a silicon nitride material layer, and the tolerable temperature of the light emitting device obtained
At 320 DEG C or more.
In step (D), the 5th solvent is the combination of third solvent and the 4th solvent, and the 5th is formed in step (C)
The rear standing of solvent 0~30 minute, preferably 5~20 minutes, more preferably 5~10 minutes, will the middle phosphor formed of step (A)
Expect that solution is placed in the 5th solvent, and then fluorescent material film can be made well to be formed in the first luminescence unit surface.
In step (E) afterwards and before step (F), can further include a step (E1): drying is formed with the fluorescent material film
The substrate, remain in the second solvent on first luminescence unit to remove.Also, after step (G), a step can be further included
Suddenly (G1): repeating the step (A) accordingly, can be formed to step (G) with forming multiple fluorescent material films and multiple protective layers
The fluorescent material film and the protective layer being arranged alternately.The usually intellectual of having can be according to actually required in the art
Light mixing mechanism, and determine the fluorescent material film quantity of setting.
In fluorescent material coating method of the invention, the second solvent, third solvent and the 4th solvent have no it is specifically limited,
As long as meeting following conditions: third solvent specific gravity is greater than the second solvent and the 4th solvent.It is described in detail, when third is added in the 4th solvent
When solvent forms five solvents, second will form temporary interface with the 4th solvent, and time of repose be more than about 30 minutes with
Afterwards, this interface can disappear, i.e., the 4th solvent is thoroughly mixed with third solvent.Preferably, second solvent, the third solvent and
4th solvent can be each independently selected from by: water, methanol, ethyl alcohol, propyl alcohol, butanol, isopropanol, acetone, butanone, normal butane,
Pentane, n-hexane, normal heptane, ethyl acetate, butyl acetate, ether, glycol dimethyl ether (DME), methylene chloride (DCM),
Dimethylformamide (DMF), tetrahydrofuran (THF), n-methyl-2-pyrrolidone (NMP), 3- methoxy propyl fine (MPN) and its
Set composed by mixture；So the invention is not limited thereto.Second preferred solvents are normal butane or isopropanol, the third solvent
Preferably ethyl acetate and the 4th preferred solvents are that ether or 3- methoxy propyl are fine (MPN).
The present invention separately provides a kind of light emitting device, is made of the above method, which includes: one first luminous single
Member；And one second luminescence unit, it is covered on first luminescence unit, and second luminescence unit includes that a fluorescent material is thin
Film and a protective layer, wherein the protective layer is located on the fluorescent material film, which is a silicon nitride material layer, and the hair
The tolerable temperature of electro-optical device is more than 320 DEG C.
In light emitting device of the invention, the thickness of first luminescence unit and second luminescence unit has no special limit
System, and the overall thickness of first luminescence unit and second luminescence unit is between 105 μm to 225 μm, preferably extremely in 120 μm
Between 210 μm.In addition, light emitting device of the invention has a non-uniform surface, therefore the appearance of light emitting device is out-of-flatness
Plate structure.
In light emitting device of the invention and preparation method thereof, which may include: shown at least one Formulas I
Silicon-nitrogen compound, one first solvent and a catalyst,
Wherein n is positive integer, preferably between 4 to 3000, more preferably between 4 to 300；And the silicon nitrification
The number-average molecular weight of object is 150 to 150,000 gram/mole, preferably 10, between 000 to 15,000 gram/mole.
Wherein, there is high-adhesiveness and high temperature resistant with high rigidity, to substrate after silicon-nitrogen compound heat treatment, even if
Under conditions of about 300 DEG C of temperatures above, still consolidated by the silicon nitride material layer that silicon-nitrogen compound, the first solvent and catalyst are formed
And there is not phenomena such as yellow, cracking, protect fluorescent material film and avoid the situation of fluorescent powder removing.In addition, the silicon nitrogen
Compound can mix a nanometer materials, be at least one selected from by TiO2、SiO2、ZnO、ZrO、Y2O3、Al2O3、CoO、MnO2、
Set composed by PbO, NiO, CuO and its compound, the partial sizes of the nanometer materials can be between 5nm between 500nm, can
Modulation Refractive Index of Material and light transmittance promote light mixing effect and light extraction efficiency.
Wherein, which is the solvent of anhydrous state, is at least one selected from by dimethylbenzene, toluene, ethyl alcohol, first
Collection composed by alcohol, isopropanol, ethylene glycol, butyl acetate, ethyl acetate, dibasic ester (Dibasic ester) and petroleum ether
It closes；Preferably dibasic ester and methanol mixture.In addition, the catalyst be the miscellaneous cyclic compound of N-, one-alkylamine, di-alkyl amine,
Trialkylamine, organic acid, inorganic acid, peroxide, metal carboxylate, vinyl acetone acid misfit object, metal or organic metal
Compound；The miscellaneous cyclic compound of preferably N- or metal carboxylate.The usually intellectual of having can be according to selection in the art
Silicon-nitrogen compound, the properties such as hardness, mobility needed for considering protective layer and select appropriate solvent and catalyst.By silicon nitrification
The silicon nitride material layer that object, the first solvent and catalyst are formed penetrates into the hole between fluorescent material film and substrate compared with Canon, consolidates glimmering
The luminescent properties of luminescent material.
In light emitting device of the invention and preparation method thereof, which may include a fluorescent powder, preferably can be more
Including a ball-type carrier；In the case where the fluorescent material includes the fluorescent powder and the ball-type carrier, fluorescent powder can be covered
Ball-type carrier surface；Fluorescent powder may be included in ball-type carrier inside；Or part fluorescent powder covering ball-type carrier surface, and portion
Fluorescent powder is divided to be contained in ball-type carrier inside.Meanwhile the material of ball-type carrier can be SiOx, TiOx, PS, PMMA or trimerization
Melamine resin.The material of fluorescent powder can be general known fluorescent powder, such as: selected from by ZnO, ZrO2、PbO、Y2O3、Y2O2、
Zn2SiO4、Y3Al5O12、Y3(AlGa)5O12Y2SiO5、LaOCl、InBO3、ZnGa2O4、ZnS、PbS、CdS、CaS、SrS、
ZnxCd1-xS、Y2O2S, AlN and Gd2O2The compound gathered composed by S, and can more be mixed as the compound of fluorescent powder
Miscellaneous at least one selected from by Cu, Ag, Eu, Yb, La, Cl, Tb, Al, Ce, Er, Zn, Mn and other lanthanide series (Pr, Pm, Sm, Ho,
Er set element composed by).Furthermore the partial size of ball-type carrier is preferably between 10 μm to 100 μm, more preferably extremely between 25 μm
Between 50 μm；And the partial size of fluorescent powder is preferably between 5 μm to 50 μm, more preferably between 10 μm to 25 μm.Therefore, by
It is uniform in fluorescent material partial size and property, and uniform fluorescent material film can be formed in substrate surface.
In light emitting device of the invention and preparation method thereof, the first luminescence unit can be any LED chip or LED element
Semi-finished product, preferably one is formed with the blue light epi-wafer of epitaxial layer, a packed LED chip (face-up chip), a vertical LED
Chip (vertical chip) or a flip LED chip.
In light emitting device of the invention and preparation method thereof, the protective layer is using coating common in the art
Method is formed on the fluorescent material film, such as spin-coating method, stick coating method, scraper coating, rolling method, spraying coating, bristle apply
Method, dipping coating etc..Therefore, fluorescent material film can be stable on substrate and be not easy to be stripped, at the same adjustment be coated with it is glimmering
The refractive index of the substrate of luminescent material.
Embodiment 1
Fig. 2A to Fig. 2 H is that the fluorescent material of the embodiment of the present invention 1 is coated on the step schematic diagram of substrate surface.
[preparing fluorescent powder solution]
Firstly, taking fluorescent powder as a fluorescent material, using about 15 μm of Y of partial size2O3:La3+、YAG:La3+And
The mixture of CdSe:ZnS.By adjusting the ratio of various fluorescent powders, after blue light-emitting diode excites, this fluorescent powder can
Light mixing is carried out in its surface and issues white light.
Then, fluorescent powder 210 is mixed in the second solvent 211 with polymolecularity, it is molten obtains fluorescent powder mixing
Liquid, wherein fluorescent powder weight percent in the second solvent is 20wt%, as shown in Figure 2 A.Here, using normal butane as
Two solvents.
[forming fluorescent powder film]
As shown in Figure 2 B, take one first luminescence unit 20, and place it in 24 bottom of a container, wherein this first shine
Unit is a flip LED chip, then, third solvent 23 is injected in container 24, here, using pure water as third solvent.
Then, as shown in Figure 2 C, the 4th solvent 25 is reinjected in container 24, and the 4th solvent adding amount is the 1wt% of third solvent.
When third solvent 23 is added in the 4th solvent 25, a temporary interface 27 is formed between third solvent 23 and the 4th solvent 25, the
Three solvents 23 and the 4th solvent 25 form the 5th solvent 26, here, using ether as the 4th solvent.Then, it is molten to form the 5th
Agent 26 stands 5 minutes, fluorescent powder mixed solution shown in Fig. 2A is placed in 26 surface of the 5th solvent, due to as third solvent 23
The specific gravity of ethyl acetate be higher than the normal butane as the second solvent 211, therefore the fluorescent powder 210 in fluorescent material solution can arrange
On the surface thereof, one first fluorescent powder film 21 is formed, as shown in Figure 2 D.
Then, the 5th solvent 26 is removed from container 24, make the first fluorescent powder film 21 in 20 surface of light emitting device at
Type, as shown in Figure 2 E.Then, container 24 is placed in equipment for drying (not shown), to evaporate removing residual solvent.To
After drying completely, then first fluorescent powder film 21 for being formed in 20 surface of light emitting device can be obtained, as shown in Figure 2 F.
[forming protective layer]
A silicon nitrogen material solution is prepared, the silicon-nitrogen compound structure such as Formula Il used mixes solvent with dibasic ester, methanol
(solvent is again than 1: 1), Metal Palladium catalyst (weight ratio 0.5wt%) and nanoscale TiO2(partial size 20nm, weight ratio 1wt%) is mixed
It closes.
After mixing, with method of spin coating by silicon nitrogen material solution coating on the first fluorescent powder film 21, and formed
One first protective layer 22, as shown in Figure 2 G.After standing, by the first hair with the first fluorescent powder film 21 and the first protective layer 22
Light unit 20 carries out heat treatment 10 seconds to 1 hour, then is made annealing treatment, then completes the light emitting devices surface of the present embodiment, can
The material layers such as inorganic silicon oxygen, silicon nitrogen oxygen or silicon nitrogen are formed, and the apparatus surface is non-uniform surface.In Fig. 2 G, first is glimmering
The group of light powder film 21 and the first protective layer 22 is combined into the second luminescence unit 30.In this, the first luminescence unit 20 and second shines
The overall thickness of unit 30 is 115 μm.The usually intellectual of having can be according to the silicon nitrogen material SOLUTION PROPERTIES of preparation in the art
And select suitable curing mode.
Therefore, above-mentioned formation it is firm and have water oxygen resistant silicon nitride material layer, fixed fluorescent powder layer can be strengthened, through it is too long when
Between work down phenomena such as not having yellow or deteriorating, can prevent aqueous vapor from penetrating into and cause LED chip impaired, substrate is avoided to send out
Light efficiency deterioration, and can high temperature resistant more than 320 degree DEG C or more.By the flip obtained above for being coated with fluorescent powder film
LED chip, after pilot is bright, the color temperature of mixed light issued is 5400K.
Also, the more repeatable above-mentioned steps as shown in Fig. 2 B to Fig. 2 G etc., being formed has multilayered fluorescent powder film and more
The composite construction of layer protective film interaction setting, as illustrated in figure 2h, in the second fluorescent powder can be sequentially formed on the first protective layer 22 again
Film 21 ', the second protective layer 22 ', third fluorescent powder film 21 " and third protective layer 22 ", in this way, be formed by fluorescence
Powder film light mixing effect can reach expected colour temperature and color rendering.In Fig. 2 H, the first protective layer 22, the second fluorescent powder film
The group of 21 ', second protective layer 22 ', third fluorescent powder film 21 " and third protective layer 22 " is combined into the second luminescence unit 30 '.In
This, the overall thickness of the first luminescence unit 20 and the second luminescence unit 30 ' is 145 μm.Also, protective layer replaces with fluorescent powder film
Setting, can effective district every those fluorescent powder films, if film made of different phosphor material powders need to be arranged, being separated by with protective layer can
It avoids each fluorescent powder film from mutually mixing/interference, influences required light mixing effect.
[embodiment 2]
The production method of the present embodiment is as described in Example 1.In addition to fluorescent powder used in the present embodiment use partial size for
The nanosphere that 25 μm and material are PMMA is used as ball-type carrier, and fluorescent powder is using about 5 μm of partial size of Y2O3:La3+、YAG:La3 +And the mixture of CdSe:ZnS, and the mixture of fluorescent powder is contained in ball-type carrier inside.In addition, being done using isopropanol
For the second solvent, and using 3- methoxy propyl fine (MPN) as the 4th solvent.Therefore, in the present embodiment be made be coated with it is glimmering
The flip LED chip of light powder film, after pilot is bright, the color temperature of mixed light issued is 5700K.
Above-described embodiment is illustrated only for facilitating explanation, and the interest field that the present invention is advocated certainly should be special to apply
Subject to described in sharp range, not just the above examples.
Claims (33)
1. a kind of light emitting device, comprising:
One first luminescence unit；And
One second luminescence unit is covered on first luminescence unit, and second luminescence unit includes that a fluorescent material is thin
Film and a protective layer；
Wherein, which is located on the fluorescent material film, which is a silicon nitride material layer, and the light emitting device is resistance to
It is 320 DEG C or more by temperature；Wherein, which includes: silicon-nitrogen compound shown at least one Formulas I and a catalyst,
Wherein n is positive integer, and the number-average molecular weight of the silicon-nitrogen compound is 150 to 150,000 gram/mole.
2. light emitting device as described in claim 1, wherein the overall thickness of first luminescence unit and second luminescence unit is situated between
Between 105 μm to 225 μm.
3. light emitting device as described in claim 1 has a non-uniform surface.
4. light emitting device as described in claim 1, wherein the silicon nitride material layer includes: one first solvent.
5. light emitting device as described in claim 1, wherein the silicon-nitrogen compound is to mix a nanometer materials, is at least
One selected from by TiO2、SiO2、ZnO、ZrO、Y2O3、Al2O3、CoO、MnO2, collection composed by PbO, NiO, CuO and its compound
It closes.
6. light emitting device as claimed in claim 5, wherein the partial size of the nanometer materials is between 5nm between 500nm.
7. light emitting device as claimed in claim 4, wherein first solvent is at least one selected from by dimethylbenzene, toluene, second
Alcohol, methanol, isopropanol, ethylene glycol, butyl acetate, ethyl acetate, dibasic ester (Dibasic ester) and petroleum ether institute group
At set.
8. light emitting device as described in claim 1, wherein the catalyst is the miscellaneous cyclic compound of N-, one-alkylamine, di-alkyl
Amine, trialkylamine, organic acid, inorganic acid, peroxide, metal carboxylate, vinyl acetone acid misfit object, metal or organic gold
Belong to compound.
9. light emitting device as described in claim 1, wherein first luminescence unit is that a blue light for being formed with epitaxial layer builds core
Piece, a packed LED chip (face-up chip), a vertical LED chip (vertical chip) or a flip LED chip
(flip chip)。
10. light emitting device as described in claim 1, wherein the fluorescent material includes a ball-type carrier and a fluorescent powder.
11. light emitting device as claimed in claim 10, wherein the fluorescent powder covers the ball-type carrier surface or is contained in this
Ball-type carrier inside.
12. light emitting device as claimed in claim 10, wherein the material of the ball-type carrier be SiOx, TiOx, PS, PMMA or
Melamine resin, and the range of X is between 0.5~2.
13. light emitting device as claimed in claim 10, wherein the fluorescent powder is at least one selected from by ZnO, ZrO2、PbO、
Y2O3、Y2O2、Zn2SiO4、Y3Al5O12、Y3(AlGa)5O12Y2SiO5、LaOCl、InBO3、ZnGa2O4、ZnS、PbS、CdS、CaS、
SrS、ZnxCd1-xS、Y2O2S、AlN、Gd2O2The compound gathered composed by S, and X is between 0.5 to 2.
14. light emitting device as claimed in claim 13, wherein this compound doped at least one selected from by Cu, Ag, Eu, Yb, La,
The element gathered composed by Cl, Tb, Al, Ce, Er, Zn, Mn, Pr, Pm, Sm, Ho and Er.
15. light emitting device as claimed in claim 10, wherein the partial size of the ball-type carrier is between 10 μm to 100 μm.
16. light emitting device as claimed in claim 10, wherein the partial size of the fluorescent powder is between 5 μm to 50 μm.
17. light emitting device as described in claim 1, wherein second luminescence unit includes multiple fluorescent material films and multiple
Protective layer, wherein the fluorescent material film is arranged alternately with the protective layer.
18. a kind of preparation method of light emitting device, including the following steps:
(A) it disperses a fluorescent material in one second solvent, to form a fluorescent material solution；
(B) one first luminescence unit is placed in a container, and injects a third solvent, and the third solvent covers this and first shines
The surface of unit；
(C) one the 4th solvent is injected into the third solvent, to form one the 5th solvent；
(D) the fluorescent material solution is added to the 5th solvent, to form a fluorescent material film in the 5th solvent surface；
(E) the 5th solvent in the container is removed, the fluorescent material film is made to be formed in the first luminescence unit surface；
(F) in forming a protective layer on the fluorescent material film；And
(G) heat treatment is formed with first luminescence unit of the protective layer；
Wherein, which is a silicon nitride material layer, and the tolerable temperature of the light emitting device obtained is at 320 DEG C or more；Wherein,
The silicon nitride material layer includes: silicon-nitrogen compound shown at least one Formulas I and a catalyst,
Wherein n is positive integer, and the number-average molecular weight of the silicon-nitrogen compound is 150 to 150,000 gram/mole；The fluorescent material
Including a ball-type carrier and a fluorescent powder, the partial size of the fluorescent powder is between 5 μm to 50 μm.
19. the preparation method of light emitting device as claimed in claim 18, wherein the silicon nitride material layer includes: one first solvent.
20. the preparation method of light emitting device as claimed in claim 18, wherein the silicon-nitrogen compound is to mix a nanoscale material
Material is at least one selected from by TiO2、SiO2、ZnO、ZrO、Y2O3、Al2O3、CoO、MnO2, PbO, NiO, CuO and its compound
Composed set.
21. the preparation method of light emitting device as claimed in claim 20, wherein the partial size of the nanometer materials between 5nm extremely
Between 500nm.
22. the preparation method of light emitting device as claimed in claim 19, wherein first solvent is at least one selected from by diformazan
Collection composed by benzene, toluene, ethyl alcohol, methanol, isopropanol, ethylene glycol, butyl acetate, ethyl acetate, dibasic ester and petroleum ether
It closes.
23. the preparation method of light emitting device as claimed in claim 18, wherein the catalyst is the miscellaneous cyclic compound of N-, one-alkane
Base amine, di-alkyl amine, trialkylamine, organic acid, inorganic acid, peroxide, metal carboxylate, vinyl acetone acid misfit object,
Metal or organo-metallic compound.
24. the preparation method of light emitting device as claimed in claim 18, wherein in step (E) afterwards and before step (F), more
Including a step (E1): dry first luminescence unit for being formed with the fluorescent material film.
25. the preparation method of light emitting device as claimed in claim 18 further includes a step (G1) after step (G): repeating
The step (A) is to step (G), to form multiple fluorescent material films and multiple protective layers.
26. the preparation method of light emitting device as claimed in claim 18, wherein it is second molten to be greater than this for the specific gravity of the third solvent
The specific gravity of agent and the 4th solvent.
27. the preparation method of light emitting device as claimed in claim 18, wherein the fluorescent powder covers the ball-type carrier surface
Or it is contained in the ball-type carrier inside.
28. the preparation method of light emitting device as claimed in claim 18, wherein the material of the ball-type carrier be SiOx, TiOx,
PS, PMMA or melamine resin.
29. the preparation method of light emitting device as claimed in claim 18, wherein the fluorescent powder be at least one selected from by ZnO,
ZrO2、PbO、Y2O3、Y2O2、Zn2SiO4、Y3Al5O12、Y3(AlGa)5O12Y2SiO5、LaOCl、InBO3、ZnGa2O4、ZnS、PbS、
CdS、CaS、SrS、ZnxCd1-xS、Y2O2S、AlN、Gd2O2The compound gathered composed by S, and X is between 0.5 to 2.
30. the preparation method of light emitting device as claimed in claim 29, wherein the compound be doping at least one selected from by Cu,
The element gathered composed by Ag, Eu, Yb, La, Cl, Tb, Al, Ce, Er, Zn, Mn, Pr, Pm, Sm, Ho and Er.
31. the preparation method of light emitting device as claimed in claim 18, wherein the partial size of the ball-type carrier is between 10 μm to 100
Between μm.
32. the preparation method of light emitting device as claimed in claim 18, wherein second solvent, the third solvent and this
Four solvents are to be each independently selected from by water, methanol, ethyl alcohol, propyl alcohol, butanol, isopropanol, acetone, butanone, normal butane, positive penta
Alkane, n-hexane, normal heptane, ethyl acetate, butyl acetate, ether, glycol dimethyl ether (DME), methylene chloride (DCM), diformazan
Base formamide (DMF), tetrahydrofuran (THF), n-methyl-2-pyrrolidone (NMP), 3- methoxy propyl fine (MPN) and its mixing
Set composed by object.
33. the preparation method of light emitting device as claimed in claim 18, wherein first luminescence unit is formed with epitaxy for one
The blue light epi-wafer of layer, a packed LED chip (face-up chip), a vertical LED chip (vertical chip) one cover
Brilliant LED chip (flip chip).
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