CN102651441B - Composition for reflective film, light-emitting component and manufacture method thereof for light-emitting component - Google Patents
Composition for reflective film, light-emitting component and manufacture method thereof for light-emitting component Download PDFInfo
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- CN102651441B CN102651441B CN201210041065.1A CN201210041065A CN102651441B CN 102651441 B CN102651441 B CN 102651441B CN 201210041065 A CN201210041065 A CN 201210041065A CN 102651441 B CN102651441 B CN 102651441B
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- light
- emitting component
- reflectance coating
- composition
- coating
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- 239000013464 silicone adhesive Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical compound [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 description 1
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
- H01L33/44—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 coatings, e.g. passivation layer or anti-reflective coating
- H01L33/46—Reflective coating, e.g. dielectric Bragg reflector
-
- 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
- H01L2933/0025—Processes relating to coatings
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Led Device Packages (AREA)
- Paints Or Removers (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The light-emitting component of the present invention, possesses the reflectance coating of the light that luminescent layer, light-transmitting substrate and reflection are sent by luminescent layer successively, and described reflectance coating contains metal nanoparticle.Described light-emitting component and then can possess the strengthening membrane containing binding agent.
Description
Technical field
The present invention relates to the composition for reflective film for light-emitting component, by this for the reflectance coating group of light-emitting component
The light-emitting component of compound manufacture and the manufacture method of light-emitting component.More particularly, it relates to possess luminescent layer, light transmission successively
The reflectance coating of light that substrate and reflection are sent by luminescent layer, possess the reflecting layer effectively reflecting the light sent by luminescent layer
Light-emitting component and the manufacture method of light-emitting component.
Background technology
In recent years, light-emitting component, LED light source the most therein, with high brightness etc., are used in various field.Especially
It is owing to being capable of White LED light source, in the purposes such as backlight being therefore used for ligthing paraphernalia, liquid crystal display.
In order to improve the brightness etc. of LED light source further, ground more effectively utilizing the luminescence from LED element
Studying carefully, disclose a kind of LED light source, this LED light source has substrate, is mounted in the LED element supported on substrate and containing fluorescent agent
Sealant, possesses the luminous plating Ag electrode film of reflection LED element between substrate and LED element, has on plating Ag electrode film
There is titanium thin film (patent documentation 1).
In this LED light source, by arranging reflective coating between substrate and LED element, reflection carrys out self-luminous body effectively
Light and increase luminous intensity.Wherein, Ag thin film and titanium thin film are formed by galvanoplastic and vacuum film formation.
Generally, mention galvanoplastic and be envisioned that miscellaneous operation, the generation of waste liquid, mention vacuum film formation, in order to maintain
The vacuum film formation apparatus large-scale with operating, needs the biggest cost.In above-mentioned LED light source, owing to only having plating Ag electrode film, meeting
Produce heat deterioration, light deterioration, it is therefore desirable to titanium thin film and it needs to and with galvanoplastic and vacuum film formation.
Additionally, this invention is to possess the reflectance coating of the light that luminescent layer, light-transmitting substrate and reflection are sent by luminescent layer successively
Light-emitting component be object, between luminescent layer and light-transmitting substrate, there is not reflectance coating.In this composition, owing to generally only having
Plating Ag electrode film, can produce heat deterioration, light deterioration, it is therefore desirable to and with galvanoplastic and vacuum film formation.
Patent documentation 1: Japanese Unexamined Patent Publication 2009-231568 publication
Summary of the invention
The present invention is to solve the problems referred to above as problem.It is an object of the invention to, it is provided that sent out by light-emitting component by reflection
The light gone out and the thin film forming method improving the reflectance coating with electrode effect, can suppress the heat due to reflectance coating and environment band
The deterioration that comes and make that manufacturing process is easy, greatly improve the light-emitting component of operating cost and the manufacture method of light-emitting component.
The reflectance coating for light-emitting component that the present invention relates to be solved above-mentioned problem by techniques illustrated below scheme is used
Compositions, for the reinforcement film composition of light-emitting component and light-emitting component.
1st scheme of the present invention is the composition for reflective film for light-emitting component, for possessing luminescent layer, printing opacity successively
Property substrate and the light-emitting component of the reflectance coating of light that sent by luminescent layer of reflection, composition for reflective film contains metallic nanoparticle
Son.
2nd scheme of the present invention is the composition for reflective film for light-emitting component that above-mentioned 1st scheme relates to, Jin Erhan
There is additive.
3rd scheme of the present invention is the composition for reflective film for light-emitting component that above-mentioned 1st or the 2nd scheme relates to,
And then containing disperse medium.
4th scheme of the present invention is the reinforcement film composition for light-emitting component, for possessing luminescent layer, printing opacity successively
Property the reflectance coating of light that sent by luminescent layer of substrate, reflection and the light-emitting component of strengthening membrane, strengthen film composition and contain bonding
Agent.
5th scheme of the present invention is the reinforcement film composition for light-emitting component that above-mentioned 4th scheme relates to, wherein,
And then containing one or both in silica-based particle, silicate particles, metallic or metal oxide particle
Above microgranule or flaky particles.
6th scheme of the present invention is light-emitting component, possesses luminescent layer, light-transmitting substrate and reflection successively and is sent by luminescent layer
The reflectance coating of light, reflectance coating contains metal nanoparticle.
7th scheme of the present invention is the light-emitting component that above-mentioned 6th scheme relates to, described reflectance coating and then containing additive.
8th scheme of the present invention is the light-emitting component that above-mentioned 6th or the 7th scheme relates to, and then possesses strengthening membrane, has successively
Standby described luminescent layer, described light-transmitting substrate, described reflectance coating and described strengthening membrane, described strengthening membrane contains binding agent.
9th scheme of the present invention is the light-emitting component that above-mentioned 8th scheme relates to, wherein, described strengthening membrane so containing choosing
One or more microgranule in silica-based particle, silicate particles, metallic or metal oxide particle
Or flaky particles.
10th scheme of the present invention is the light-emitting component that in the above-mentioned 6th～the 9th, either a program relates to, and described reflectance coating can lead to
Cross wet coating method manufacture.
11st scheme of the present invention is the light-emitting component that above-mentioned 8th or the 9th scheme relates to, and described strengthening membrane is coated with by wet type
Cloth method manufactures.
12nd scheme of the present invention is the light-emitting component that in the above-mentioned 6th～the 11st, either a program relates to, described reflectance coating
Thickness is 0.05～1.0 μm.
13rd scheme of the present invention is the manufacture method of light-emitting component, wherein, utilizes wet on light-transmitting substrate
After the method coating composition for reflective film containing metal nanoparticle and additive, by burning till or solidifying to form reflectance coating,
The opposing face of the reflectance coating of light-transmitting substrate forms luminescent layer.
In the manufacture method of above-mentioned light-emitting component, it is possible to use the reflectance coating formation group for light-emitting component of the present invention
Compound.
The manufacture method that 14th scheme is the light-emitting component that above-mentioned 13rd scheme relates to of the present invention, is forming above-mentioned reflection
After film, before formation luminescent layer, and then utilize the wet coating method coating strengthening membrane group containing binding agent on the reflecting film
After compound, by burning till or solidifying to form strengthening membrane.
In the manufacture method of above-mentioned light-emitting component, it is possible to use the strengthening membrane formation group for light-emitting component of the present invention
Compound.
According to the reflectance coating formation compositions for light-emitting component of the present invention, by metal nanoparticle, even if being
The light-emitting component of high-output power, it is also possible to improve thermostability, corrosion resistance, it is provided that the heat produced by luminescent layer can be suppressed
Or the high life light-emitting component of the deterioration of reflectance coating that environment brings.This reflectance coating can be used for various light source, is particularly well-suited to LED
Light source.Additionally, this reflectance coating can be manufactured by wet coating method, therefore manufacturing process is easy, can be with low cost manufacture.This
Outward, according to the present invention it is possible to provide thermostability, the higher light-emitting component of corrosion resistance.
According to the light-emitting component of the present invention, the adaptation of light-transmitting substrate and luminescent layer can be improved, improve light-emitting component
Reliability.
Additionally, possess the light-emitting component of the present invention of strengthening membrane, thermostability, corrosion resistance are high, and suppression is produced by luminescent layer
Heat or the deterioration of reflectance coating that brings of environment, the life-span is high.
The manufacture method of the light-emitting component according to the present invention, can obtain thermostability, corrosion resistance height with low cost easily
Light-emitting component.
Accompanying drawing explanation
Fig. 1 is the sectional view of an example of the light-emitting component representing the present invention.
Fig. 2 is the sectional view of preferably one example of the light-emitting component representing the present invention.
Detailed description of the invention
Below based on embodiment, the present invention is specifically described.And, unless % particularly shows, otherwise except number
It is quality % outside being worth intrinsic situation.
[for the composition for reflective film of light-emitting component]
The feature of the composition for reflective film for light-emitting component (hereinafter referred to as composition for reflective film) of the present invention exists
In, it is the light-emitting component of the reflectance coating for possessing the light that luminescent layer, light-transmitting substrate and reflection are sent by luminescent layer successively
Composition for reflective film, composition for reflective film contains metal nanoparticle.
Metal nanoparticle to the composition for reflective film after burning till or solidifying, i.e. to reflectance coating give sent by luminescent layer
The reflexive of light.As metal nanoparticle, can enumerate selected from silver, gold, platinum, palladium, ruthenium, nickel, copper, stannum, indium, zinc, ferrum, chromium
Form with one or more the mixing composition in manganese or alloy, the most silver-colored from the viewpoint of reflexive, electric conductivity,
Gold.The mean diameter of metal nanoparticle is preferably 10～50nm.Wherein, mean diameter uses BET by specific area measuring
Method is measured.Such as, in specific area measuring, it is possible to use Quantachrome Instruments's
QUANTACHROME AUTOSORB-1.The shape of metal nanoparticle is preferably ball from the viewpoint of dispersibility, reflexive
Shape, tabular.
Composition for reflective film, from the viewpoint of the adaptation of reflectance coating, reflexive, preferably comprises additive.As adding
Add thing, from the viewpoint of reflexive, adaptation, more preferably contain selected from organic polymer, metal-oxide, metallic hydrogen oxidation
At least one in thing, organo-metallic compound and silicone oil.
As the organic polymer as additive, from the viewpoint of reflexive, it is preferably selected from polyvinylpyrrolidine
At least one in ketone, the copolymer of polyvinylpyrrolidone and water-soluble cellulose.Copolymerization as polyvinylpyrrolidone
Thing, can enumerate PVP-methacrylate copolymer, PVP-styrol copolymer, PVP-vinyl acetate copolymer etc..This
Outward, as water-soluble cellulose, the fibers such as hydroxypropyl methylcellulose, methylcellulose, hydroxyethylmethyl-cellulose can be enumerated
Element ether.
As the metal-oxide as additive, be preferably containing selected from aluminum, silicon, titanium, zirconium, chromium, manganese, ferrum, cobalt, nickel,
The oxide of at least one in silver, copper, zinc, molybdenum, stannum, indium and antimony or composite oxides.Composite oxides, the most permissible
Enumerate ITO (Indium Tin Oxide, tin-doped indium oxide), ATO (the Antimony-doped Tin containing above-mentioned metal
Oxide, antimony-doped tin oxide), IZO (Indium-doped Zinc Oxide, indium doping zinc oxide), AZO (Aluminum-
Doped Zinc Oxide, aluminium-doped zinc oxide) etc..
As the metal hydroxides as additive, be preferably containing selected from aluminum, silicon, titanium, zirconium, chromium, manganese, ferrum, cobalt,
The hydroxide of at least one in nickel, silver, copper, zinc, molybdenum, stannum, indium and antimony.
As the organo-metallic compound as additive, be preferably containing selected from silicon, titanium, zirconium, chromium, manganese, ferrum, cobalt, nickel,
The hydrolysate of the metallic soap of at least one, metal complex, metal alkoxide or metal alkoxide in silver, copper, zinc, molybdenum and stannum.Example
As, as metallic soap, chromium acetate, formic acid manganese, ferric citrate, cobaltous formate, nickel acetate, Itrol., copper acetate, lemon can be enumerated
Lemon acid copper, tin acetate, zinc acetate, zinc oxalate, acetic acid molybdenum etc..Additionally, as metal complex, zinc acetylacetonate can be enumerated and joins
Compound, acetylacetone,2,4-pentanedione chromic compound, acetylacetone,2,4-pentanedione nickel complex etc..Additionally, as metal alkoxide, can enumerate isopropyl titanate,
Methyl silicate, isocyanatopropyl trimethoxy silane, TSL 8330 etc..
As the silicone oil as additive, it is possible to use pure silicon oil (Straight silicone oil) and modified silicon oil
Both.As modified silicon oil, the part at the side chain of polysiloxanes and then can be used to import the silicone oil (side of organic group
Chain), polysiloxanes two ends import organic groups silicone oil (two tip type), in two ends of polysiloxanes appoint
The side that anticipates imports the silicone oil (single tip type) of organic group and is imported with at the part of side chain and two ends of polysiloxanes
The silicone oil (side chain two tip type) of machine group.Responding property silicone oil and non-reactive silicone oil in modified silicon oil, can use simultaneously
These two kinds of additives as the present invention.And, reactive silicone oil represents amino-modified silicone oil, epoxy-modified silicone oil, carboxyl
Modified silicon oil, carbinol-modified silicone oil, sulfhydryl modified silicone oil and xenogenesis functional group modification (epoxy radicals, amino, polyether-based) silicone oil, non-
Reactive silicone oil represents that polyether modified silicon oil, methyl styrene base modified silicon oil, alkyl modified silicon oil, higher fatty acids are ester modified
Silicone oil, fluorine richness silicone oil and hydrophilic special modified silicon oil.
Additionally, from the viewpoint of coating, composition for reflective film preferably comprises disperse medium.Disperse medium relative to
All disperse medium 100 mass %, containing more than the water more than 1 mass %, more than preferably 2 mass % and 2 mass %, preferably 3
Solvent compatible with water more than quality %, such as alcohols are suitable.Such as, when disperse medium only comprises water and alcohols, contain
Contain the alcohols of 98 mass % when having the water of 2 mass %, during alcohols containing 2 mass %, contain the water of 98 mass %.Further
Ground, disperse medium, the protection molecule being i.e. chemically modified surfaces of metal nanoparticles contain hydroxyl (-OH) or carbonyl (-C
=O) in either or both.Relative to whole disperse medium 100 mass %, the content of water is preferably more than 1 mass %.
During this is because the content of water is less than 2 mass %, it is difficult to sinter at low temperatures and combined by wet coating method coating reflectance coating
The film that thing obtains.And it is because causing the reflectance reduction of the reflectance coating after burning till.It addition, hydroxyl (-OH) is if containing
In the protective agent that the metal nanoparticles such as Nano silver grain are chemically modified, then the dispersion stabilization of composition for reflective film
Excellence, also has effective effect to the low-temperature sintering of film.Additionally, carbonyl (-C=O) is if containing to Nano silver grain etc.
In the protective agent that metal nanoparticle is chemically modified, the most in the same manner as described above, the dispersion stabilization of composition for reflective film
Excellence, also has effective effect to the low-temperature sintering of film.As the solvent compatible with water used in disperse medium, preferably
For alcohols.Wherein, as above-mentioned alcohols, more preferably use selected from methanol, ethanol, propanol, butanol, ethylene glycol, propylene glycol, two sweet
One or more in alcohol, glycerol, isobornyl hexanol and erithritol.
Relative to composition for reflective film 100 mass parts of removing disperse medium, if metal nanoparticle 75 mass parts
Below then preferred, if more than 80 mass parts the most more preferably from the viewpoint of reflexive.If additionally, below 95 mass parts,
Then from the viewpoint of the adaptation of reflectance coating preferably, if more than 80 mass parts the most more preferably.And, if wanting reflectance coating is composed
When giving electric conductivity, relative to reflectance coating 100 mass parts, metal nanoparticle is preferably more than 75 mass parts, more preferably 80 matter
More than amount part.
Relative to composition for reflective film 100 mass parts, from the viewpoint of coating, preferred disperse medium is 50～99
Mass parts.
Additionally, composition for reflective film is according to the composition used, it is preferably added to low resistance agent (low opposing), water-soluble
Property cellulose derivative.As low resistance agent, more preferably selected from cobalt, ferrum, indium, nickel, lead, stannum, titanium and the inorganic acid salt of zinc
And one or more in acylate.Such as nickel acetate and the mixture of iron chloride, naphthalene acid zinc, tin octoate can be enumerated
Mixture etc. with mixture, indium nitrate and the mixture of lead acetate, acetoacetate titanium and the cobalt octoate of antimony chloride.Relative to
Composition for reflective film, preferably less than resistance agent are 0.2～15 mass parts.Water-soluble cellulose derivative is non-ionic surface
Activating agent, compared with other surfactant, even if adding on a small quantity, the ability of monodisperse metal nanoparticles is the most high, additionally,
By the interpolation of water-soluble cellulose derivative, the reflexive of the reflectance coating of formation also can be improved.Spread out as water-soluble cellulose
Biology, can enumerate hydroxypropyl cellulose, hydroxypropyl methylcellulose etc..Relative to composition for reflective film 100 mass parts, preferably
Water-soluble cellulose derivative is 0.2～5 mass parts.
Within the scope without prejudice to the object of the present invention, and then as required, composition for reflective film can coordinate antioxidation
Agent, levelling agent, thixotropic agent, implant, Stress Release agent, other additive etc..
[reinforcement film composition]
Reinforcement film composition (hereinafter referred to as strengthening film composition) for light-emitting component is sent out for being used for possessing successively
The strengthening membrane combination of the reflectance coating of the light that photosphere, light-transmitting substrate, reflection are sent by luminescent layer and the light-emitting component of strengthening membrane
Thing, strengthens film composition and contains binding agent.Strengthening film composition and can form strengthening membrane, this external reflectance coating has emptying aperture
Time, penetrate into reflectance coating, contain binding agent at the emptying aperture of reflectance coating and/or the interface of reflectance coating and increasing reflective transparent film, permissible
Improve the dhering strength of the intensity of reflectance coating itself or reflectance coating and increasing reflective transparent film.
Binding agent preferably comprises the polymer being irradiated by ultraviolet, heat or heating after uv irradiation and solidify
Any in the organic system of type binding agent or inorganic system base material, or the inorganic system base material of non-polymeric binding agent
One or both.The organic system base material of polymer type adhesive preferably comprises selected from acrylic compounds, epoxies, polyurethane
One or more in the polymer of class, acroleic acid polyurethane class, propylene oxide acids, cellulose family and type siloxane.
As acrylic adhesives, interpolation Photoepolymerizationinitiater initiater in acrylic monomer can be used, to this mixture
Irradiation ultraviolet radiation (UV), carries out photopolymerization and the acrylic polymer that obtains.As acrylic monomer, can enumerate and be selected from
1,6-hexanediyl ester, trimethylolpropane trimethacrylate, neopentylglycol diacrylate, tetramethylol methane four
Acrylate, two (trimethylolpropane) tetraacrylate, 1,9-nonanediol diacrylate, tripropylene glycol diacrylate
One or more single in ester, epoxidation cyamelide triacrylate and tetramethylol methane tetraacrylate
Monomer or mix monomer.In these monomers, preferably add MIBK (methyl iso-butyl ketone (MIBK)), PGME (1-methoxy-2-propanol),
PGMEA (propylene glycol methyl ether acetate) equal solvent.Wherein, if the common organic solvents of above-mentioned monomer can be dissolved, then may be used
With use ethanol, methanol, benzene,toluene,xylene, NMP (N-Methyl pyrrolidone), acrylonitrile, acetonitrile, THF (oxolane),
Ethyl acetate, MEK (butanone), DEGMBE, butyl carbitol acetate, butyl cellosolve, butyl cellosolve second
Acid esters, carbitol, diethylene glycol monoethyl ether acetate, IPA (isopropanol), acetone, DMF (dimethylformamide), DMSO
(dimethyl sulfoxide), piperidines, phenol etc..Additionally, as Photoepolymerizationinitiater initiater, can enumerate 1-hydroxy-cyclohexyl-phenyl-one,
2-hydroxy-2-methyl-1-phenyl-1 propane-1-ketone, 2-hydroxyl-1-[4-[4-(2-hydroxy-2-methyl-propiono)-benzyl]-
Phenyl]-2-methyl-propan-1-ketone, 1-[4-(2-hydroxyl-oxethyl)-phenyl]-2-hydroxy-2-methyl-1-propane-1-ketone etc..
Acrylic monomer, can with above-mentioned arbitrary solvent dilution, be adjusted to viscosity easy to apply and use.Relative to acrylic compounds
Monomer 100 mass parts, adds the Photoepolymerizationinitiater initiater of 0.1～30 mass parts.This is because, relative to acrylic monomer 100
Mass parts, the addition of Photoepolymerizationinitiater initiater becomes insufficient, if more than 30 mass parts, solidifying less than solidification during 0.1 mass parts
Film (strengthening membrane) variable color or residual stress and cause closely sealed bad.So, in acrylic monomer, solvent and photopolymerization are added
Initiator, is stirred, and the mixture obtained is as the substrate liquid strengthening film composition.And, in acrylic monomer
Add solvent and Photoepolymerizationinitiater initiater, be stirred, in the case of the mixed liquor that obtains is uneven, it is also possible to be heated up to 40 DEG C of left sides
Right.
As epoxy adhesive, interpolation solvent in epoxylite can be used to be stirred, add in this mixed liquor
Be heating and curing agent, is stirred obtaining mixed liquor, heats obtained mixed liquor and the epoxide polymer that obtains.Make
For epoxylite, biphenyl type epoxy resin, cresol novolak epoxy, bisphenol A type epoxy resin, bisphenol-f type can be enumerated
Epoxy resin, naphthalene type epoxy resin etc..Additionally, as solvent, BCA (butyl carbitol acetate), ECA (two can be enumerated
Glycol monoethyl ether acetate), BC (DEGMBE) etc..Wherein, if typically having of above-mentioned epoxylite can be dissolved
Machine solvent, then can use ethanol, methanol, benzene,toluene,xylene, PGME (1-methoxy-2-propanol), PGMEA (propylene glycol
Methyl ether acetate), NMP (N-Methyl pyrrolidone), MIBK (methyl iso-butyl ketone (MIBK)), acrylonitrile, acetonitrile, THF (tetrahydrochysene furan
Mutter), ethyl acetate, MEK (butanone), DEGMBE, butyl carbitol acetate, butyl cellosolve, the molten fibre of butyl
Agent acetas, carbitol, diethylene glycol monoethyl ether acetate, IPA (isopropanol), acetone, DMF (dimethylformamide),
DMSO (dimethyl sulfoxide), piperidines, phenol etc..Further, as thermal curing agents, can enumerate 2-ethyl-4-methylimidazole,
Boron fluoride monoethanolamine, DICY (dicyandiamide), diethyl amino propyl amine, isophorone diamine, diaminodiphenyl-methane,
Piperidines, 2,4,6-tri--(dimethylaminomethyl) phenol, 2-methylimidazole, hexahydrophthalic anhydride, 7,11-18 carbon two
Alkene-1,18-bis-carbohydrazide etc..Epoxylite, can with above-mentioned arbitrary solvent dilution, be adjusted to viscosity easy to apply and make
With.Relative to epoxylite 100 mass parts, add thermal curing agents 0.5～20 mass parts.This is because, relative to epoxies
Resin 100 mass parts, when the addition of thermal curing agents is less than 0.5 mass parts, solidification becomes insufficient, if more than 20 mass parts,
Then solidfied material (strengthening membrane) is produced big internal stress, cause adaptation bad.So, in epoxylite, solvent is added
And thermal curing agents, it being stirred, the mixture obtained is as the substrate liquid strengthening film composition.And, to epoxylite
Middle interpolation solvent, is stirred, in the case of the mixed liquor that obtains is uneven, it is also possible to be heated up to about 40 DEG C.
Cellulose family binding agent can be stirred, in this mixed liquor by adding solvent in cellulosic polymer
Add gelatin, be stirred obtaining mixed liquor, obtained mixed liquor heated and obtains.It is polymerized as cellulose family
Thing, can enumerate the hydroxypropyl cellulose as water-soluble cellulose derivative, hydroxypropyl methylcellulose, methylcellulose, hydroxyl
Ethylmethylcellulose etc..Additionally, as solvent, IPA (isopropanol), ethanol, methanol, PGME (propylene glycol list first can be enumerated
Ether), PGMEA (propylene glycol methyl ether acetate), MIBK (methyl iso-butyl ketone (MIBK)), acetone etc..Cellulosic polymer, Ke Yiyong
Above-mentioned arbitrary solvent dilution, it is adjusted to viscosity easy to apply and uses.Relative to cellulosic polymer 100 mass parts, add
Add gelatin 0.1～20 mass parts.This is because, relative to cellulosic polymer 100 mass parts, if the addition of gelatin is less than
0.1 mass parts or more than 20 mass parts, then can not get being suitable for the viscosity of coating.So, in cellulosic resin, solvent is added
And gelatin, it being stirred, the mixture obtained is as the substrate liquid strengthening film composition.And, to cellulosic polymer
Middle interpolation solvent and gelatin, be heated up to about 30 DEG C and be stirred, thus mixed liquor becomes uniform.
Using has the polyurethane binding of Thermocurable polyurethane resin to prepare as follows.First, make with trihydroxy methyl third
The polyol compound such as alkane or neopentyl glycol be representative polyol component with toluene di-isocyanate(TDI) (TDI), diphenyl-methane
The polyisocyanate compounds reaction of the excess that isocyanates (MDI) etc. are representative, thus obtain end containing active isocyanate
The polyurethane prepolymer of base.Then, this end polyurethane prepolymer containing active isocyanate base is made and with methylphenol as generation
The block agents such as the phenols of table, the lactams with β-butyrolactam as representative or the oximes with methyl ethyl ketoxime as representative are anti-
Should.As solvent, ketone, alkyl benzene, cellosolve class, esters, alcohols etc. can be used.As the concrete example of ketone, Ke Yiju
Go out acetone, butanone etc., as the concrete example of alkyl benzene, benzene, toluene etc. can be enumerated.Additionally, concrete as cellosolve
Example, can enumerate methyl cellosolve, butyl cellosolve etc., as the concrete example of esters, can enumerate butyl cellosolve acetate,
Butyl acetates etc., as the concrete example of alcohols, can enumerate isopropanol, butanol etc..On the other hand, as thermal curing agents (reaction
Agent), polyamine can be used.As the concrete example of polyamine, N-octyl group-N-aminopropyl-N '-aminopropyl the third two can be enumerated
Amine, N-lauryl-N-aminopropyl-N '-aminopropyl propane diamine, N-myristyl-N-aminopropyl-N '-aminopropyl third
Diamidogen, N-octyl group-N-aminopropyl-N ', N '-two (aminopropyl) propane diamine etc..To making above-mentioned polyol component and Carbimide.
The end that ester compounds reaction the obtains polyurethane prepolymer containing active isocyanate base implements the block utilizing block agent to carry out
Change, thus make block polyisocyanate.The Carbimide. that the amino that polyamine has has relative to this block polyisocyanate
The equivalent proportion of ester group is preferably about 1 (scopes of 0.7～1.1).If this is because, the amino that polyamine has is relative to block
The equivalent proportion of the NCO that polyisocyanate has is less than 0.7 or more than 1.1, then in block polyisocyanate and polyamine
A side increase, reaction becomes insufficient, therefore becomes to solidify insufficient.Polyether polyols with reduced unsaturation, can be with above-mentioned the most molten
Dilution agent, it is adjusted to viscosity easy to apply and uses.
As acroleic acid polyurethane class binding agent, containing urethane acrylate quasi-oligomer, can enumerate and pass through ultraviolet
Line (UV) irradiate solidification, purple light UV-3310B or purple light UV-6100B (Japan synthesis society system), EBECRYL4820 or
The acrylic acid such as EBECRYL284 (ダ ィ セ Le サ ィ テ ッ Network society system), U-4HA or UA-32P (chemical industry society of Xin Zhong village system) gather
Urethane base polymer.And, it is added as needed on Photoepolymerizationinitiater initiater (the such as 1-hydroxy-cyclohexan that acrylate apoplexy due to endogenous wind uses
Base-phenyl ketone, 2-hydroxy-2-methyl-1-phenyl-propan-1-ketone etc.), such that it is able to improve curable.Additionally, as molten
Agent, can use ketone, alkyl benzene, cellosolve class, esters, alcohols etc..As the concrete example of ketone, acetone, first can be enumerated
Ethyl ketones etc., as the concrete example of alkyl benzene, can enumerate benzene, toluene etc..As the concrete example of cellosolve class, first can be enumerated
Base cellosolve, butyl cellosolve etc., as the concrete example of esters, can enumerate butyl cellosolve acetate, butyl acetate etc., makees
For the concrete example of alcohols, isopropanol, butanol etc. can be enumerated.Relative to acroleic acid polyurethane base polymer 100 mass parts, according to
Need to add Photoepolymerizationinitiater initiater in the range of 0.1～30 mass parts.This is because, the addition of Photoepolymerizationinitiater initiater is less than
During 0.1 mass parts, solidification becomes insufficient, if more than 30 mass parts, then the internal stress of backplate strengthening membrane increases, and becomes
Adaptation is bad.Additionally, acroleic acid polyurethane class monomer, easy to apply gluing can be adjusted to above-mentioned arbitrary solvent dilution
Degree uses.
As propylene oxide acids binding agent, propylene oxide acids polymers can be used.As epoxy acrylic Type of Collective
Thing, can enumerate bisphenol-a epoxy acrylate (the NK ォ リ go EA-1020 of chemical industry society of such as Xin Zhong village), 1,6-oneself
Glycol diglycidyl ether diacrylate (the NK ォ リ go EA-5521 of chemical industry society of such as Xin Zhong village) etc..Additionally,
ネ ォ Port one Le 8318 of ュ ピ カ society of Japan, ネ ォ Port one Le 8355 etc. can also be used.As solvent, ketone can be used
Class, alkyl benzene, cellosolve class, esters, alcohols etc..As the concrete example of ketone, acetone, butanone etc. can be enumerated, as
The concrete example of alkyl benzene, can enumerate benzene, toluene etc..As the concrete example of cellosolve class, methyl cellosolve, fourth can be enumerated
Base cellosolves etc., as the concrete example of esters, can enumerate butyl cellosolve acetate, butyl acetate etc., as the tool of alcohols
Style, can enumerate isopropanol, butanol etc..As required, thermal curing agents, light can be added in Epoxy Acrylates polymer
Polymerization initiator.Then, by thermal curing agents, Photoepolymerizationinitiater initiater, carry out being heating and curing or UV solidification, or after UV solidifies
It is heating and curing.Additionally, Epoxy Acrylates polymer, can with above-mentioned arbitrary solvent dilution, be adjusted to easy to apply
Viscosity use.
As Silicone Adhesives, siloxane type polymers can be used.As siloxane type polymers, can enumerate poly-
Dimethyl siloxane, poly-methylhydrogensiloxane, PSI etc..Additionally, as type siloxane depicted herein
Polymer, it is possible to use both pure silicon oil (Straight silicone oil) and modified silicon oil.As modified silicon oil, can
With so use polysiloxanes side chain a part import organic group silicone oil (side chain type), polysiloxanes two end
End imports the silicone oil (two tip type) of organic group, the silicon of any one party importing organic group in two ends of polysiloxanes
Oil (single tip type) and import silicone oil (side chain two end of organic group in the part of side chain of polysiloxanes and two ends
Type) etc..Responding property silicone oil and non-reactive silicone oil in modified silicon oil, it is possible to use these both sides.And, reactive silicone oil represents
Amino-modified silicone oil, epoxy-modified silicone oil, Carboxyl Modified Polydimethylsiloxane, carbinol-modified silicone oil, sulfhydryl modified silicone oil or xenogenesis official's energy
Modified (epoxy radicals, amino, the polyether-based) silicone oil of group, non-reactive silicone oil represents that polyether modified silicon oil, methyl styrene base are modified
Silicone oil, alkyl modified silicon oil, high-grade aliphatic ester modified silicon oil, fluorine richness silicone oil or hydrophilic special modified silicon oil.Additionally, conduct
Solvent, can use ketone, alkyl benzene, cellosolve class, esters, alcohols etc..As the concrete example of ketone, can enumerate acetone,
Butanone etc..As the concrete example of alkyl benzene, benzene, toluene etc. can be enumerated.Additionally, as the concrete example of cellosolve class, can
To enumerate methyl cellosolve, butyl cellosolve etc..As the concrete example of esters, butyl cellosolve acetate, acetic acid can be enumerated
Butyl ester etc..As the concrete example of alcohols, isopropanol, butanol etc. can be enumerated.As required, can add in siloxane type polymers
Be heating and curing agent, Photoepolymerizationinitiater initiater, even if but be added without in the case of thermal curing agents film also solidifies, it is not necessary to thermal curing agents.
Additionally, siloxane type polymers, can with above-mentioned arbitrary solvent dilution, be adjusted to viscosity easy to apply and use.
The inorganic system base material of polymer type adhesive preferably comprises selected from metallic soap, metal complex, metal alkoxide
With one or more in the hydrolysate of metal alkoxide.The inorganic system base material of these polymer type adhesives is for passing through
Heating is changed to the material of inorganic system base material from organic system.I.e., it is possible to there is inorganic system base material by burning till formation
The film of character.And, the metal contained in the hydrolysate of above-mentioned metallic soap, metal complex, metal alkoxide or metal alkoxide is excellent
Elect as in aluminum, silicon, titanium, zirconium and stannum one or more.As above-mentioned metallic soap, chromium acetate, formic acid can be enumerated
Manganese, ferric citrate, cobaltous formate, nickel acetate, Itrol., copper acetate, copper citrate, tin acetate, zinc acetate, zinc oxalate, acetic acid
Molybdenum etc..As metal complex, acetylacetone,2,4-pentanedione Zn complex, acetylacetone,2,4-pentanedione chromic compound, nickel acetylacetonate cooperation can be enumerated
Thing etc..As metal alkoxide, isopropyl titanate, methyl silicate, isocyanatopropyl trimethoxy silane, aminopropyl three can be enumerated
Ethoxysilane etc..
On the other hand, as the inorganic system base material of non-polymeric binding agent, SiO can be enumerated2Bonding agent.Should
SiO2Bonding agent can make as an example as shown below.First, while stirring, HCl is dissolved in pure water, prepares HCl
Aqueous solution.Then, being mixed with ethanol by tetraethoxysilane, after adding above-mentioned HCl/water solution in this mixed liquor, heating is carried out
Reaction.Thus, SiO is made2Bonding agent.Additionally, non-polymeric binding agent preferably comprise selected from metallic soap, metal complex,
One in metal alkoxide, the hydrolysate of metal alkoxide, halogenated silanes class, 2-alkoxyethanol, beta-diketon and alkyl acetates
Or it is two or more.Containing collosol and gel in the hydrolysate of this metal alkoxide.And, above-mentioned metallic soap, metal complex, metal alcohol
The metal contained in the hydrolysate of salt or metal alkoxide is preferably selected from one or more in aluminum, silicon, titanium, zirconium and stannum.
As metallic soap, chromium acetate, formic acid manganese, ferric citrate, cobaltous formate, nickel acetate, Itrol., copper acetate, Fructus Citri Limoniae can be enumerated
Acid copper, tin acetate, zinc acetate, zinc oxalate, acetic acid molybdenum etc., as metal complex, can enumerate acetylacetone,2,4-pentanedione Zn complex, second
Acyl acetone chromic compound, acetylacetone,2,4-pentanedione nickel complex etc., as metal alkoxide, can enumerate isopropyl titanate, methyl silicate, isocyanide
Acid propyl trimethoxy silicane, aminopropyltriethoxywerene werene etc..As halogenated silanes class, chlorosilane, bromine silicon can be enumerated
Alkane, silicon fluoride etc..As 2-alkoxyethanol, 2-methyl cellosolve, cellosolvo, butoxy ethanol can be enumerated
Deng.As beta-diketon, 2 can be enumerated, 4-pentanedione, 1,3-diphenylpropane-1，3-dione etc..As alkyl acetates, permissible
Enumerate ethylene glycol monomethyl ether acetate, propylene glycol methyl ether acetate etc..
Additionally, strengthen film composition can containing in silane coupler, aluminum coupling agent and titanium coupling agent one or
Two or more.Reinforcement film composition, by containing silane coupler, aluminum coupling agent etc., can improve strengthening membrane further to instead
Penetrate the adaptation of film.Therefore, after 1 piece of light-transmitting substrate forms multiple luminescent layer, by cutting from reflectance coating side at printing opacity
Property substrate on form slot segmentation, use when being divided into the operation of each light-emitting component, strengthening membrane can be suppressed to peel off from reflectance coating.
Can be containing selected from silicon dioxide granule, silicate particles, metallic or metal additionally, strengthen film composition
One or more microgranule in oxide particle or flaky particles.Such as, strengthening film composition can be containing being selected from
One or both in silica sol, aerosil particle, silicon dioxide granule, mica particle and montmorillonite particle
Above microgranule or flaky particles.Silica sol is SiO2Or the colloid of its hydrate, mean diameter is 1～100nm, excellent
Elect 5～50nm as, not there is certain structure.Aerosil particle by silicon chloride gasify, in the flame of high temperature in
Under gas phase state oxidized and generate, mean diameter is 1～50nm, preferably 5～30nm.Silicon dioxide granule is mean diameter
It it is 1～100nm, preferably 5～the particle of 50nm.Mica particle be the mean diameter prepared by synthetic method be 10～50000nm
Particle, preferred average diameter is 1～20 μm and flaky particles that average thickness is 10～100nm.Montmorillonite particle is to have
The face consisted of ionic bond etc. is with the ion exchangeable laminar silicic acid of the overlapping abreast crystalline texture of the most weak bonding force
The one of salt compound, be mean diameter be the particle of 10～100000nm, preferred average diameter is 1～20 μm and averagely thick
Degree is the flaky particles of 10～100nm.Strengthen film composition by containing silica sol, aerosil particle
Deng, the hardness of strengthening membrane can be increased further.Therefore, after forming separating tank by cutting, i.e. use air knife etc. to remove residual
Overlap (バ リ) on this separating tank or precipitate, owing to mar proof and the resistance to impact of strengthening membrane are good, will not lack and add
Edge part in the separating tank of strong film.Relative to strengthen film composition 100 mass parts, their addition be preferably 0.1～
30 mass parts, more preferably 0.2～20 mass parts.It is difficult to obtain effect, on the other hand, if more than 30 during less than 0.1 mass parts
Mass parts, then adaptation easily reduces.And, in the present invention, the mean diameter of each particle and each microgranule measures as follows.Use laser
Diffraction/scattering formula particle size distribution device (hole field makes made, model: LA-950) measures, and particle diameter benchmark is with number form
Calculated 50% mean diameter (D50).Utilize the individual base that this laser diffraction/scattering formula particle size distribution device obtains
The value of quasi-mean diameter, and by scanning electron microscope (Hitachi's Ha ィ テ Network ノ ロ ジ mono-ズ system, model: S-4300SE
And S-900) substantially uniform to mean diameter during arbitrary 50 particles actual measurement particle diameter in the image observed.Additionally, it is above-mentioned flat
The average diameter of flat particle and average thickness, the average diameter of aftermentioned each flat microgranule and average thickness enter the most as described above
Row measures.
And, the scope of 1～100nm that the mean diameter of silica sol is defined to be due to, less than colloid during 1nm
Unstable and easily condense, if more than 100nm, particle diameter is big, will not form dispersion liquid.Additionally, by aerosil particle, two
Silicon oxide particle, mica particle, montmorillonite particle be equally sized to above-mentioned scope be due to, these sizes can obtain
Particle size, or in order to make them be not more than the size range of the thickness of the film of lower floor (reflectance coating).
Further, strengthening film composition and can contain microgranule or flat microgranule, this microgranule or flat microgranule contain choosing
One or more metal in gold, platinum, palladium, ruthenium, nickel, copper, stannum, indium, zinc, ferrum, chromium, manganese and aluminum or these gold
The oxide belonged to.The mean diameter of these microgranules is set as 1～50000nm, preferably 100～the scope of 5000nm.Flat microgranule
Average diameter be preferably 1～50000nm, the average thickness of flat microgranule is preferably 100～20000nm.Strengthening membrane combines
Thing, can imparting flexibility further to strengthening membrane by the microgranule containing gold, platinum etc. or flat microgranule.Therefore, during cutting, i.e.
Make strengthening membrane is produced stress, utilize ductility that strengthening membrane has and malleability can discharge stress.Wherein, by the microgranule of metal
Being equally sized to above-mentioned scope is owing to the size of obtained microgranule is defined, by the dimension limitation of the flat microgranule of metal
It is owing to forming the size range not over reflectance coating thickness for above-mentioned scope.The addition of these microgranules or flat microgranule is excellent
Elect 0.1～30 mass parts, more preferably 0.2～20 mass parts as.This is because, be difficult to obtain effect when being less than 0.1 mass parts,
On the other hand, if more than 30 mass parts, adaptation is the most easily reduced.Additionally, metal or the microgranule of metal-oxide or flat microgranule
In content be defined to more than 70 mass %, preferably 80～100 scopes of mass %.During this is because, be less than 70 mass %, add
The processability of strong film reduces.
Within the scope without prejudice to the object of the present invention, and then as required, strengthen film composition and can coordinate antioxidation
Agent, levelling agent, thixotropic agent, Stress Release agent, other additive etc..
[light-emitting component]
The light-emitting component of the present invention possesses the reflection of the light that luminescent layer, light-transmitting substrate and reflection are sent by luminescent layer successively
Film, it is characterised in that reflectance coating contains metal nanoparticle.
Fig. 1 represents the sectional view of an example of light-emitting component.Light-emitting component 1 possess successively reflectance coating 10, light-transmitting substrate 20,
Luminescent layer 30.Generally, reflectance coating 10 utilizes adhesive linkage 50 to engage with supporting substrate 60, forms desired wiring at luminescent layer 30
After, sealed by sealing material 40.
Fig. 2 represents the sectional view of preferably one example of light-emitting component.If light-emitting component 2 possesses strengthening membrane 12, reflectance coating successively
11, substrate 21, luminescent layer 31, then by strengthening membrane 12, can improve the thermostability of reflectance coating 11, corrosion resistance, and then permissible
Improve in the adaptation of light-transmitting substrate and reflectance coating, suppression cutting action that reflectance coating 11 is from the stripping of substrate 21, the most preferably.
And, if strengthening membrane 12 is containing binding agent, can be manufactured by wet coating method, even if therefore it is further preferred that but pass through vacuum
Membrane formation process etc. manufacture and also are able to improve the thermostability of reflectance coating 11, corrosion resistance.In the composition shown in Fig. 2, strengthening membrane 12 leads to
Cross adhesive linkage 51 and engage with supporting substrate 61, after luminescent layer 31 forms desired wiring, seal by sealing material 41.
<reflectance coating>
Reflectance coating is reflected through the light of the luminescent layer of matrix.Reflectance coating contains metal nanoparticle, and then preferably comprises and add
Add thing.Metal nanoparticle, additive are described above.
Relative to nesa coating 100 mass parts, the content ratio of additive is preferably 0.1～25 mass parts, more preferably
It is 0.2～10 mass parts.If more than 0.1 mass parts, then good, if below 25 mass parts with the bonding force of nesa coating
Film when being then not likely to produce film forming is uneven.
From the viewpoint of reflexive, electric conductivity, the thickness of reflectance coating is preferably 0.05～1.0 μm, more preferably 0.1～
0.5μm。
If the average diameter being present in the pore in the face of the light-transmitting substrate side of reflectance coating is below 100nm, mean depth
It is 30/μm for below 100nm, number density2, then, in the range of wavelength 380～780nm, theoretical reflectance rate can be reached
The high diffuse-reflectance rate of more than 80%, it is advantageous to.Usual reflectance spectrum shows, at long wavelength side, the project that reflectance is high, short wavelength
The project that side display reflectance is low.If the average diameter of pore moves to more than 100nm, the then flex point starting to reduce due to reflectance
Longer wavelength side, it is impossible to obtaining good reflectance, therefore preferred average diameter is below 100nm.If additionally, pore is average
The degree of depth more than 100nm, then increases due to the slope (gradient) of reflectance spectrum, can not get good reflectance, and therefore pore is average
The degree of depth is preferably below 100nm.If the number density of pore is more than 30/μm2, then due to the reflectance reduction of long wavelength side,
Less than good reflectance, therefore the number density of pore is preferably 30/μm2Below.
<strengthening membrane>
Strengthening membrane improves thermostability and the corrosion resistance of reflectance coating, and suppression uses cutting in the manufacturing process of light-emitting component
Time the stripping of reflectance coating.Strengthening membrane contains binding agent, and binding agent is described above.
Such as, when containing the binding agent of polymerization species, it is also possible to containing selected from acrylic polymer, epoxies polymerization
Thing, polyurethane polymer, acroleic acid polyurethane base polymer, propylene oxide acids polymers, cellulosic polymer and silicon
One or more in oxygen alkanes polymer.Further, it is also possible to the inorganic system base material containing polymeric adhesives
Or the inorganic system base material of non-polymeric species binding agent.
Additionally, as to strengthening shown in film composition explanation, it is also possible to containing selected from silica-based particle, silicate grain
One or more microgranule in son, metallic or metal oxide particle or flaky particles.
From the viewpoint of thermostability, corrosion resistance, the thickness of strengthening membrane is preferably 0.01～0.5 μm, more preferably
0.01～0.2 μm.
[manufacture method of light-emitting component]
The manufacture method of the light-emitting component of the present invention is characterised by, is coated with by wet coating method on light-transmitting substrate
After composition for reflective film containing metal nanoparticle and additive, utilize and burn till or solidify to form reflectance coating, in light transmission
The opposing face of the reflectance coating of substrate forms luminescent layer.
First, on light-transmitting substrate, contain metal nanoparticle by wet coating method coating, preferably comprise additive
Composition for reflective film.Coating herein, is preferably 0.05～1.0 μm with the thickness after burning till, more preferably 0.1～0.5 μ
The mode of m is carried out.Then, by this film at temperature 120～350 DEG C, preferably 150～250 DEG C, be dried 5～60 minutes, preferably
15～40 minutes.It is thusly-formed reflectance coating.
If light-transmitting substrate can form luminescent layer, without particular limitation of, but from the viewpoint of light transmission, exothermicity,
It is preferably sapphire substrate.
Composition for reflective film can pass through paint mixer, ball mill, sand mill, centrifugal grinding mills, triple-roller mill (three
This ロ one Le) etc. according to common method mix desired composition, and disperse light transmission binding agent, according to circumstances dispersed transparent conduction
Property particle etc. manufactures.It is of course also possible to manufactured by common stirring operation.And, if mixing is except metallic nanoparticle
After composition outside son, mix, then from the homogenizing that is easy to get with the disperse medium containing additionally the most scattered metal nanoparticle
Composition for reflective film from the viewpoint of preferably.
Wet coating method is preferably spraying process, point gum machine rubbing method (デ ィ ス ペ Application サ mono-U one テ ィ Application グ method), spin coating
Any one in method, knife coating, slot coated method, ink-jet application method, screen painting method, flexographic printing process or mold rubbing method
Kind, but it is not limited to this, available all of method.
Spraying process is to make composition for reflective film nebulize by compressed air and coat on light-transmitting substrate or right
The method that dispersion itself carries out pressurizeing and nebulizes and coat on light-transmitting substrate, point gum machine rubbing method for example be by by
Composition for reflective film is injected in syringe and presses the piston of this syringe and carrys out the minute nozzle discharge from syringe front end
Dispersion, coats the method on light-transmitting substrate.Spin-coating method is reflectance coating combination of dripping on the light-transmitting substrate rotated
Thing, is at water by its centrifugal force to the method for this composition for reflective film dripped of light-transmitting substrate circumferential expansion, knife coating
Square being upwards movably disposed the front end with scraper separates the light-transmitting substrate of predetermined gap, to than this scraper closer to upstream
Supply composition for reflective film on the light-transmitting substrate of side, make the method that light-transmitting substrate moves horizontally towards downstream.Slit
Rubbing method is the method making composition for reflective film flow out from narrow slit and coat light-transmitting substrate, ink-jet application method
It is composition for reflective film to be filled in the print cartridge of commercially available ink-jet printer, light-transmitting substrate carries out ink jet printing
Method.Screen painting method is to utilize yarn to indicate material as pattern, is combined by reflectance coating by the domain picture being made thereon
Thing is transferred to the method for light-transmitting substrate.Flexographic printing process is not make the composition for reflective film investing in version be attached directly to
Photosensitiveness substrate, and being by once from the transfer of version to film, and the utilization being transferred back to light-transmitting substrate from film is anti-
Penetrate the printing process of the water proofing property of film composition.Mold rubbing method is to be used by the reflectance coating in manifold distribution supply to mould
Compositions, by slit extrusion on thin film, the method that the surface of the light-transmitting substrate advanced is coated.Mold rubbing method
There are slotted coating method or slidingtype coating method, curtain coating mode.
Finally, will there is the light-transmitting substrate of reflective coating film in an atmosphere or the inert gas atmosphere such as nitrogen or argon
In, preferably at 130～250 DEG C, more preferably holding 5～60 minutes at a temperature of 180～220 DEG C, preferably holding 15～40 points
Clock burns till.And, when binding agent is by reactions such as hydrolysis, can solidify at lower temperatures.
Make the scope that firing temperature is 130～250 DEG C with the light-transmitting substrate of film be due to, during less than 130 DEG C,
The bad problem that solidification is insufficient is produced in reflectance coating.If additionally, more than 250 DEG C, then so-called low temperature process will not be produced
Advantage in production, i.e. causing manufacturing cost to increase, productivity ratio declines.Further, it is that owing to luminescent layer compares, To Be Protected from Heat, because burning till work
Sequence and luminous efficiency decline.
Make the scope that firing time is 5～60 minutes with the light-transmitting substrate of film be due to, firing time is less than
During lower limit, reflectance coating produces binding agent and burns till insufficient bad problem.If firing time exceedes higher limit, then manufacture
Cost increases to more than necessity and productivity ratio declines, and, there is the bad problem that the luminous efficiency of luminescent layer declines.
The opposing face of the reflectance coating at light-transmitting substrate is formed the method for luminescent layer without particular limitation of, can be known
Metalorganic chemical vapor deposition method (MOCVD), hydride gas phase epitaxial growth method (HVPE), molecular beam epitaxial growth method
(MBE) method such as.
Thus, the manufacture method of the present invention is by using wet coating method, owing to can get rid of vacuum evaporation as much as possible
The vacuum technology such as method, sputtering method, therefore can more be manufactured inexpensively reflectance coating, can manufacture the present invention's with low cost easily
The light-emitting component that thermostability, corrosion resistance are high.And, when light-emitting component engages with other parts, if directly being welded by high temperature
Material Au-Sn solder bonds reflectance coating, then reflectance coating is likely corroded by Au-Sn solder, thus the most preferred.
If additionally, after forming reflectance coating, before formation luminescent layer, and then being contained by wet coating method coating on the reflecting film
After having the reinforcement film composition of binding agent, utilize and burn till or solidify to form strengthening membrane, then owing to luminescence can be improved further
The thermostability of element, corrosion resistance, and then suppress to use the stripping of reflectance coating when cutting in the manufacturing process of light-emitting component,
It is advantageous to.
The binding agent of strengthening membrane is as it has been described above, strengthen the manufacture method of film composition, wet coating method and reflectance coating use
Compositions is identical, simply in the case of strengthening film composition, is preferably 0.01～0.5 μm with the thickness after burning till, more excellent
The mode electing 0.01～0.2 μm as is carried out.Moreover, it is also possible to suitably select according to the kind of the binding agent strengthening film composition
Heating means or ultraviolet irradiation method for solidification.
And, add the particle of above-mentioned necessity, microgranule, flat microgranule etc. as in the substrate liquid strengthening film composition
Additive so that these additives are dispersed in the method in substrate liquid, can enumerate dispersion stirring etc. utilize the wing stir into
The shearing of dispersion, planet stirring or the triple-roller mill etc. of row disperses, includes the dispersion etc. utilizing pearl of ball mill or paint mixer.
The dispersion liquid of dispersing additive in said method solvent composition in advance in substrate liquid will be utilized further, it is also possible to use
The method carrying out mixing.Further, in the case of additive itself has become by the dispersion liquid of suitable solvent dispersion, remove
Outside said method, it is possible to use utilize the liquid mixing method that ultrasonic homogenizer or ultrasonic activation are carried out.
As it has been described above, by using wet coating method, can more be manufactured inexpensively nesa coating, can be easily with low
Cost manufactures thermostability, the higher light-emitting component of corrosion resistance.
[embodiment]
By the following examples the present invention is specifically described, but the present invention is not limited by them.
[embodiment 1]
First composition for reflective film is made.Following presentation production order.
<making of composition for reflective film>
Silver nitrate is dissolved in deionized water, prepares aqueous metal salt.Additionally, sodium citrate is dissolved in deionization
In water, preparation concentration is the sodium citrate aqueous solution of 26 mass %.In remaining the stream of nitrogen gas of 35 DEG C, to this sodium citrate
Aqueous solution it is directly added into granular ferrous sulfate and makes it dissolve, preparing and contain citrate ions with sub-with the mol ratio of 3: 2
The reducing agent aqueous solution of iron ion.
Then, while above-mentioned stream of nitrogen gas is maintained at 35 DEG C, in reducing agent aqueous solution, magnetic stirring apparatus is added
Stirrer, while stirring with the rotating speed 100rpm of stirrer, drip in this reducing agent aqueous solution above-mentioned aqueous metal salt,
Mix.Here, the concentration of each solution is adjusted so that aqueous metal salt to the addition of reducing agent aqueous solution is
Less than the 1/10 of the amount of reducing agent aqueous solution, thus, even if the aqueous metal salt of room temperature of dripping, also can keep reaction temperature
At 40 DEG C.Additionally, the mixing ratio of reducing agent aqueous solution Yu aqueous metal salt is adjusted so that the lemon of reducing agent aqueous solution
The mol ratio of lemon acid ion and ferrous ion is all 3 times relative to the total atom valence mumber of the metal ion in aqueous metal salt and rubs
You.Aqueous metal salt is after the end of dripping of reducing agent aqueous solution, and then continues stirring mixed liquor 15 minutes, thus, mixed
Close liquid internal generation Nano silver grain, thus obtain being dispersed with the silver nanoparticle dispersion liquid of Nano silver grain.Nano silver grain
The pH of dispersion liquid is 5.5, and the stoichiometry growing amount of the Nano silver grain in dispersion liquid is 5g/ liter.
The silver nanoparticle dispersion liquid obtained at room temperature is placed, and thus makes the Nano silver grain in dispersion liquid settle, logical
The condensation product crossing the decant Nano silver grain to having settled separates.Add in separated nano grain of silver subcondensation and go
Ionized water forms dispersion, after carrying out desalting processing by ultrafiltration, and nano grain of silver subcondensation and then carry out displacement with methanol and wash
Washing, the content making metal (silver-colored) is 50 mass %.Then, use centrifugal separator, adjust the centrifugal force of this centrifugal separator, right
The particle diameter bigger silver particles more than 100nm separates, thus, by the nano grain of silver in the range of primary particle size 10～50nm
The content of son is adjusted to and is averagely calculated as 71% according to number.That is, by according to the silver in the range of number average meter primary particle size 10～50nm
Nanoparticle is adjusted to 71% relative to the ratio shared by whole Nano silver grains 100%, obtains silver nanoparticle dispersion liquid.?
To Nano silver grain be chemically modified by the protective agent of sodium citrate.
Then, by the interpolation of the metal nanoparticle obtained 10 mass parts is mixed into mixing containing water, ethanol and methanol
Closing in solution 90 mass parts makes this metal nanoparticle disperse, and makes composition for reflective film.And, constitute reflectance coating combination
The metal nanoparticle of thing contains the metal nanoparticle of more than 75 mass %.
For composition for reflective film, formed reflective coating film on the glass substrate by spin-coating method, in nitrogen atmosphere 200
Burn till at DEG C 20 minutes, thus obtain the reflectance coating of thickness 200nm.Here, the mensuration of thickness is by utilizing Hitachi Ha ィ テ Network ノ
The cross-section that ロ ジ mono-ズ scanning electron microscope (SEM, device name: S-4300, SU-8000) is carried out measures.?
In other embodiment, comparative example, similarly measure thickness.
[embodiment 2]
After making silver nanoparticle dispersion liquid similarly to Example 1, by metal nanoparticle 10 mass that will obtain
Part adds to be mixed in mixed solution 90 mass parts containing water, ethanol and methanol makes this metal nanoparticle disperse, to this point
Dissipate in liquid to form ratio addition polyvinylpyrrolidone (PVP, the molecule of metal nanoparticle 96 mass parts, PVP 4 mass parts
Amount 360000), tin acetate, thus make composition for reflective film.And, constitute the metal nanoparticle of composition for reflective film
Containing metal nanoparticles more than 75 mass %.Then, carry out similarly to Example 1, obtain the reflection of thickness 100nm
Film.
[embodiment 3]
After making silver nanoparticle dispersion liquid similarly to Example 1, by metal nanoparticle 10 mass that will obtain
Part adds to be mixed in mixed solution 90 mass parts containing water, ethanol and methanol makes this metal nanoparticle disperse, to this point
Dissipate to form the ratio addition zinc acetate of metal nanoparticle 95 mass parts, zinc acetate 5 mass parts in liquid, thus make reflectance coating
Use compositions.Then, carry out similarly to Example 1, obtain the reflectance coating of thickness 200nm.
Then, reinforcement film composition is made.Following presentation production order.
<strengthening the making of film composition>
Using neopentylglycol diacrylate as starting monomer, at PGME 100cm3Middle dissolving 10g, adds 1-hydroxyl-ring
Hexyl-phenyl ketone 0.5g, is maintained at 50 DEG C, keeps 1 hour, synthesizing propylene acid resin while being stirred vigorously.Use ethanol dilution
This acrylic resin is 1 mass % to form solid component concentration, thus makes reinforcement film composition.
Reinforcement film composition film forming is made on the reflecting film with spin coater.Further, burn till at 150 DEG C 10 minutes,
Strengthened film.
[embodiment 4]
After making silver nanoparticle dispersion liquid similarly to Example 1, by metal nanoparticle 10 mass that will obtain
Part adds to be mixed in mixed solution 90 mass parts containing water, ethanol and methanol makes this metal nanoparticle disperse, to this point
Dissipate to form the ratio addition copper acetate of metal nanoparticle 95 mass parts, copper acetate 5 mass parts in liquid, thus make reflectance coating
Use compositions.Then, carry out similarly to Example 1, obtain the reflectance coating of thickness 150nm.
Then, it is used as to strengthen the SiO of film composition2Bonding agent is prepared as follows.Use 500cm3Glass system four neck burn
Bottle, adds the tetraethoxysilane of 140g and the ethanol of 140g, while stirring, 60% nitric acid of 1.7g is dissolved in 120g's
In pure water and disposably add, then, react at 50 DEG C 3 hours, thus prepare the SiO being used as to strengthen film composition2In conjunction with
Agent.
Make transparent conductive film composition film forming with spin-coating method on the reflecting film, burn till at 160 DEG C 30 minutes, thus
Nesa coating to thickness 100nm.
[embodiment 5～6,17]
In addition to forming the composition of table 1 record, thickness, carry out similarly to Example 4, make embodiment 5～6,17.
And, the SiO used in embodiment 52Bonding agent uses the SiO used in embodiment 42Bonding agent.
[embodiment 7～16,18～20]
In addition to forming the composition of table 1 record, thickness, carry out similarly to Example 3, make embodiment 7～16,18
～20.Here, the acrylic compounds used in reinforcement film composition uses neopentylglycol diacrylate, epoxies uses
Bisphenol A type epoxy resin, uses methylcellulose in cellulose family, use diphenylmethane isocyanate and first in polyurethanes
Base phenol.
[embodiment 21]
In addition to forming the composition of table 1 record, thickness, carry out similarly to Example 2, make embodiment 21.And,
The SiO used in the present embodiment2Bonding agent uses the SiO used in embodiment 42Bonding agent.
[comparative example 1]
The Ag films of thickness 100nm is formed on the glass substrate by the sputtering method of vacuum film formation.
[comparative example 2]
Formed the Ag films of thickness 100nm by sputtering method on the glass substrate, and then form thickness by sputtering method
The titanium thin film of 30nm.
[mensuration of reflectance]
For embodiment 1～21, the evaluation of the reflectance of comparative example 1～2, by ultraviolet-uisible spectrophotometer and integration
The combination of ball, the diffuse-reflectance rate of the reflectance coating under mensuration wavelength 450nm.Additionally, the condition of 200 DEG C, 1000 hours is carried out at heat
Reason test, at hydrogen sulfide 10ppm, temperature 25 DEG C, relative humidity 75%RH, is carried out as corrosion resistance under conditions of 504 hours
The sulfuration test of test, measures the reflectance after each test.Table 1 represents their result.
[adaptation evaluation]
For adaptation evaluation, by the method according to tape test (JIS K-5600), to the reality after mensuration reflectance
Execute example 2, embodiment 5, by closely sealed for adhesive tape to film and when peeling off, peel off or the degree of crimped configuration according to the film formed, with
Excellent, pass, three levels of failing are evaluated.By in adhesive tape side non-adhesive film formation, only have the feelings that are stripped of jointing tape
Condition as excellent, using the stripping being contaminated with jointing tape and formed the situation of state that the photoelectric conversion layer of base material exposes as and
Lattice, situation about being exposed on the whole surface on the photoelectric conversion layer surface making formation base material due to the stripping of jointing tape is as too late
Lattice.Embodiment 2 is for passing, and embodiment 5 is excellent.
[table 1]
As shown in Table 1, in embodiment 1, embodiment 2, the reflectance after initial stage, heat treatment is high, the reflection after sulfuration test
Rate is also about 30%.On the other hand, though the reflectance height at comparative example 1 initial stage made by sputtering method, heat treatment
After deterioration big, the reflectance after sulfuration test is greatly reduced, is 14%.In addition understand, in embodiment 3～21, initial stage, Re Chu
Reflectance after reason, after sulfuration test is the highest, and thermostability and corrosion resistance are the highest, to due to the luminescence of high-output power
It is also the light-emitting component that deterioration is few that the temperature that layer causes raises.On the other hand, the comparative example 2 made by sputtering method, sulfuration
Reflectance after test is low, be 65%.
The light-emitting component of the present invention possesses the reflectance coating containing metal nanoparticle between light-transmitting substrate and luminescent layer,
Even if being thus the light-emitting component of high-output power, it is also possible to improve thermostability, corrosion resistance, can suppress due to by luminescent layer
The deterioration of the reflectance coating that the heat produced or environment bring.This reflectance coating can utilize wet coating method to make, and therefore can make system
Make operation easy, low cost.Additionally, between luminescent layer and reflectance coating and then possess the electrically conducting transparent containing light transmission binding agent
Film, therefore can improve thermostability, light resistance further, be highly useful.
Claims (2)
1. the manufacture method of a light-emitting component, it is characterised in that utilize wet coating method coating to contain on light-transmitting substrate
After the composition for reflective film of metal nanoparticle and additive, it is dried at 150～350 DEG C, and by burning till or solidifying shape
Becoming reflectance coating, the opposing face at the reflectance coating of light-transmitting substrate forms luminescent layer,
After forming reflectance coating, before formation luminescent layer, and then wet coating method coating is utilized to contain on described reflectance coating
After the reinforcement film composition of binding agent, by burning till or solidifying to form strengthening membrane,
Described reinforcement film composition contains selected from silica sol, silicon dioxide granule, mica particle and montmorillonite particle
In one or more microgranule or flaky particles.
The manufacture method of light-emitting component the most according to claim 1, wherein, described silicon dioxide granule is gas phase titanium dioxide
Silicon particle.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011-037725 | 2011-02-23 | ||
| JP2011037725A JP5741810B2 (en) | 2011-02-23 | 2011-02-23 | REFLECTIVE FILM COMPOSITION FOR LIGHT EMITTING ELEMENT, LIGHT EMITTING ELEMENT, AND METHOD FOR PRODUCING LIGHT EMITTING ELEMENT |
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| CN102651441A CN102651441A (en) | 2012-08-29 |
| CN102651441B true CN102651441B (en) | 2016-09-21 |
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| Country | Link |
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| JP (1) | JP5741810B2 (en) |
| KR (1) | KR101739149B1 (en) |
| CN (1) | CN102651441B (en) |
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| JP6094617B2 (en) * | 2015-03-31 | 2017-03-15 | ウシオ電機株式会社 | Fluorescent light source device |
| CN106756714B (en) * | 2016-11-30 | 2018-12-28 | 佛山市高明区诚睿基科技有限公司 | A kind of preparation method of the stainless steel material with surface insulation layer |
| CN114664993A (en) * | 2022-03-25 | 2022-06-24 | 安徽三安光电有限公司 | Reflection structure, light emitting diode and manufacturing method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101803037A (en) * | 2007-09-12 | 2010-08-11 | 三菱综合材料株式会社 | Composite membrane for super straight solar cell, process for producing the composite membrane for super straight solar cell, composite membrane for substraight solar cell, and process for producing the composite membrane for substraight solar cell |
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| JPH09298313A (en) * | 1996-04-30 | 1997-11-18 | Rohm Co Ltd | Semiconductor light emitting element and manufacture thereof |
| JP2003327870A (en) * | 2002-03-07 | 2003-11-19 | Sumitomo Osaka Cement Co Ltd | Coating for forming metal reflection film and metal reflection film using the coating and article having the film |
| JP4352687B2 (en) * | 2002-11-26 | 2009-10-28 | パナソニック電工株式会社 | Method for manufacturing light emitting device |
| JP2007324062A (en) * | 2006-06-02 | 2007-12-13 | Fujifilm Corp | End face light emission type light emitting device |
| JP4851953B2 (en) * | 2007-02-07 | 2012-01-11 | 株式会社日立製作所 | Optical member |
| JP5169389B2 (en) * | 2007-04-19 | 2013-03-27 | 三菱マテリアル株式会社 | Method for manufacturing conductive reflective film |
| JP2010123605A (en) * | 2008-11-17 | 2010-06-03 | Seiko Instruments Inc | Light-emitting device and method of manufacturing the same |
| EP2407980B1 (en) * | 2009-07-21 | 2019-01-23 | Nichia Corporation | Method for producing conductive material, conductive material obtained by the same method, electronic device containing the conductive material, and light-emitting device |
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- 2012-02-20 KR KR1020120017069A patent/KR101739149B1/en active IP Right Grant
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| CN101803037A (en) * | 2007-09-12 | 2010-08-11 | 三菱综合材料株式会社 | Composite membrane for super straight solar cell, process for producing the composite membrane for super straight solar cell, composite membrane for substraight solar cell, and process for producing the composite membrane for substraight solar cell |
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| Publication number | Publication date |
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| KR101739149B1 (en) | 2017-06-08 |
| CN102651441A (en) | 2012-08-29 |
| KR20120096891A (en) | 2012-08-31 |
| JP2012175007A (en) | 2012-09-10 |
| TWI537346B (en) | 2016-06-11 |
| JP5741810B2 (en) | 2015-07-01 |
| TW201247792A (en) | 2012-12-01 |
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