CN105518104A - Wavelength conversion sheet, sealed optical semiconductor element and optical semiconductor element device - Google Patents
Wavelength conversion sheet, sealed optical semiconductor element and optical semiconductor element device Download PDFInfo
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- CN105518104A CN105518104A CN201480048721.8A CN201480048721A CN105518104A CN 105518104 A CN105518104 A CN 105518104A CN 201480048721 A CN201480048721 A CN 201480048721A CN 105518104 A CN105518104 A CN 105518104A
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- wavelength conversion
- optical semiconductor
- conversion sheet
- fluor
- resin
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- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- H01L33/483—Containers
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Abstract
A wavelength conversion sheet which is characterized by being formed of a phosphor resin composition that contains a silicone resin, organic particles and a phosphor. This wavelength conversion sheet is also characterized in that the organic particles have a refractive index of 1.45-1.60.
Description
Technical field
The present invention relates to wavelength conversion sheet, encapsulation optical semiconductor and optical semiconductor device, specifically, relate to for the wavelength conversion sheet of optical applications, encapsulation optical semiconductor and optical semiconductor device.
Background technology
At present, as the light-emitting device that can send high-octane light, there will be a known white light semiconductor device.
White light semiconductor device possesses the optical semiconductor that such as sends blue light and makes blue light (wavelength) be converted to the packaged material of sodium yellow optical-semiconductor element encapsulation, by the such as colour mixture such as blue and yellow is realized the luminescence of white.
As the packaged material of such white light semiconductor device, propose such as containing the light sheets semiconductor sealing material of silicone resin, fluor and silica dioxide granule (such as with reference to following patent documentation 1.)。
Prior art document
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 2011-228525 publication
Summary of the invention
the problem that invention will solve
But light sheets semiconductor sealing material can produce the large unfavorable condition of the deviation of the colourity of the light through packaged material.Its result, the white light sent from optical semiconductor device produces uneven color.
The object of the invention is to, the wavelength conversion sheet of the deviation that can suppress colourity, encapsulation optical semiconductor and optical semiconductor device are provided.
for the scheme of dealing with problems
The feature of wavelength conversion sheet of the present invention is, is formed by the fluor resin combination containing silicone resin, organic granular and fluor, and the specific refractory power of aforementioned organic granular is 1.45 ~ 1.60.
In addition, in wavelength conversion sheet of the present invention, the ratio that contains of the aforementioned organic granular in aforementioned wavelength conversion sheet is suitably 10 ~ 25 quality %.
In addition, in wavelength conversion sheet of the present invention, the aforementioned organic granular in aforementioned wavelength conversion sheet and the total of aforementioned phosphors are suitably 15 ~ 70 quality % containing ratio.
In addition, in wavelength conversion sheet of the present invention, at least one material that aforementioned organic granular is suitable for by being selected from the group that is made up of acrylic resin, acrylicstyrene system resin and phenylethylene resin series is formed.
In addition, in wavelength conversion sheet of the present invention, aforementioned phosphors is suitable for containing CaAlSiN
3: Eu fluor.
In addition, the feature of optical semiconductor of the present invention is, the above-mentioned wavelength conversion sheet possessing optical semiconductor and configure in opposite directions with aforementioned optical semiconductor.
In addition, the feature of optical semiconductor device of the present invention is to possess: substrate, the optical semiconductor being installed on aforesaid base plate and the above-mentioned wavelength conversion sheet configured in opposite directions with aforementioned optical semiconductor.
the effect of invention
Wavelength conversion sheet of the present invention contains the organic granular that specific refractory power is 1.45 ~ 1.60, therefore, compared with the situation containing other additive, can suppress the deviation of colourity.
In addition, optical semiconductor and optical semiconductor device possess wavelength conversion sheet of the present invention, therefore, it is possible to send uniform (uneven color is few) white light.
Accompanying drawing explanation
Figure 1A ~ Figure 1B of Fig. 1 is the process picture sheet of the operation of the embodiment represented for the manufacture of wavelength conversion sheet of the present invention, Figure 1A represent prepare the operation of peeling base, operation that Figure 1B represents stacked wavelength conversion sheet.
Fig. 2 A ~ Fig. 2 D of Fig. 2 represents that the wavelength conversion sheet of use shown in Figure 1B is to manufacture the operation of an embodiment of optical semiconductor device of the present invention, and Fig. 2 A represents encapsulated layer lamination process, Fig. 2 B represents arrangement step, Fig. 2 C represents packaging process, Fig. 2 D represents stripping process.
Fig. 3 A ~ Fig. 3 E of Fig. 3 represents that the wavelength conversion sheet of use shown in Figure 1B is to manufacture the operation of the variation of optical semiconductor device, and Fig. 3 A represents encapsulated layer lamination process, Fig. 3 B represents arrangement step, Fig. 3 C represents packaging process, Fig. 3 D represents the 2nd stripping process, Fig. 3 E represents installation procedure.
Fig. 4 represents other embodiment (optical semiconductor device possesses the embodiment of housing) of optical semiconductor device of the present invention.
Fig. 5 represents the vertical view of the measuring method that the deviation for illustration of colourity is evaluated.
Embodiment
In Fig. 1, using on the upside of paper as upside (the 1st side, direction, thickness direction side), using on the downside of paper as downside (the 1st direction opposite side, thickness direction opposite side).For the accompanying drawing beyond Fig. 1, also with the direction of Fig. 1 for benchmark.
[wavelength conversion sheet]
Wavelength conversion sheet of the present invention is formed as sheet by the fluor resin combination containing silicone resin, organic granular and fluor.
Silicone resin such as can list the silicone resin of the transparency used as the packaged material for encapsulating optical semiconductor, can use known or commercially available resin.As silicone resin, such as, can list 2 elementary reaction curable resins, 1 elementary reaction curable resin.
2 elementary reaction curable resins can have 2 kinds of reaction mechanisms, in the reaction in the 1st stage, carry out B rank (semicure) from A scalariform state, then, in the reaction in the 2nd stage, carry out C rank (solidifying completely) from B scalariform state.That is, 2 elementary reaction curable resins are the heat-curing resin that can become B scalariform state under the heating condition of appropriateness.Wherein, 2 elementary reaction curable resins also can become C scalariform state by strong heating from A scalariform state quickly and not maintain B scalariform state.It should be noted that, B scalariform state is the state that heat-curing resin is between liquid A scalariform state and completely crued C scalariform state, is solidification and gelation is carried out slightly, compressive modulus of elasticity is less than the Young's modulus of C scalariform state semisolid or solid state.
1 elementary reaction curable resin has a kind of reaction mechanism, by the reaction in the 1st stage, can carry out C rank (solidifying completely) from A scalariform state.It should be noted that, 1 elementary reaction curable resin comprises following heat-curing resin, namely, described heat-curing resin is in the reaction way in the 1st stage, it reacts stopping, can becoming B scalariform state, by further heating thereafter from A scalariform state, the reaction in the 1st stage restarts, and can carry out C rank (solidifying completely) from B scalariform state.That is, this heat-curing resin is the heat-curing resin that can form B scalariform state.On the other hand, 1 elementary reaction curable resin comprises following heat-curing resin, that is, described heat-curing resin carries out C rank (solidifying completely) from A scalariform state quickly and can not carry out controlling, namely can not becoming B scalariform state in the mode stopped the reaction way in 1 stage.
As silicone resin, specifically, by such as condensation/addition reaction curing type silicone resin combination, containing heteroatoms modified organic silicone resin composition, addition reaction curing type silicone resin combination, form containing the organosilicon resin composition such as organosilicon resin composition, thermoplastic heat curable silicone resin composition of inorganic oxide.
Organosilicon resin composition can be used alone, or also can combinationally use.
In organosilicon resin composition, from the viewpoint of the deviation of the transparency, weather resistance, thermotolerance, photostabilization, suppression colourity, preferably list addition reaction curing type silicone resin combination, condensation/addition reaction curing type silicone resin combination, more preferably list addition reaction curing type silicone resin combination.
Addition reaction curing type silicone resin combination is 1 elementary reaction curable resin, such as, containing containing thiazolinyl polysiloxane, containing hydrogenated silylation polysiloxane and hydrosilylation catalysts.
In molecule, 2 more than alkenyls and/or cycloalkenyl group is contained containing thiazolinyl polysiloxane.Containing thiazolinyl polysiloxane specifically, represent with a following average group accepted way of doing sth (1).
An average group accepted way of doing sth (1):
R
1 aR
2 bSiO
(4-a-b)/2
(in formula, R
1represent the alkenyl of carbon number 2 ~ 10 and/or the cycloalkenyl group of carbon number 3 ~ 10.R
2represent that 1 valency alkyl of the carbon number 1 ~ 10 not replacing or replace (wherein, does not comprise alkenyl and cycloalkenyl group.)。A is more than 0.05 and less than 0.50, b is more than 0.80 and less than 1.80.)
As R in formula (1)
1the alkenyl represented, such as, can list: the alkenyl of the carbon numbers 2 ~ 10 such as vinyl, allyl group, propenyl, butenyl, pentenyl, hexenyl, heptenyl, octenyl.As R
1the cycloalkenyl group represented, such as, can list: the cycloalkenyl group of the carbon number such as cyclohexenyl, norbornene 3 ~ 10.
As R
1, preferably list alkenyl, more preferably list the alkenyl of carbon number 2 ~ 4, preferably list vinyl further.
R
1the thiazolinyl represented is the group of identical type or multiple group.
R
2the 1 valency alkyl represented is 1 valency alkyl of the carbonatoms 1 ~ 10 not replacing or replace except alkenyl and cycloalkenyl group.
As unsubstituted 1 valency alkyl, can list: the alkyl of the carbon numbers 1 ~ 10 such as such as methyl, ethyl, propyl group, sec.-propyl, butyl, isobutyl-, sec-butyl, the tertiary butyl, amyl group, hexyl, amyl group, heptyl, octyl group, 2-ethylhexyl, nonyl, decyl, the cycloalkyl of the carbon numbers 3 ~ 6 such as such as cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, the aryl of the carbon numbers 6 ~ 10 such as such as phenyl, tolyl, naphthyl, the such as aralkyl of the carbon number 7 ~ 8 such as benzyl, benzyl ethyl.Preferably list the aryl of the alkyl of carbon number 1 ~ 3, carbon number 6 ~ 10, more preferably list methyl and/or phenyl.
On the other hand, 1 valency alkyl of the replacement hydrogen atom that can list in above-mentioned unsubstituted 1 valency alkyl is substituted with a substituent and the group obtained.
Alternatively base, can list halogen atom, the such as glycidyl ethers etc. such as such as chlorine atom.
1 valency alkyl alternatively, specifically can list 3-chloropropyl, glycidoxypropyl group etc.
1 valency alkyl can be any number of for what do not replace and replace, preferably do not replace.
R
2the 1 valency alkyl represented can be the alkyl of identical type or multiple alkyl.Preferably list methyl and/or phenyl, more preferably list combinationally using of methyl and phenyl.
A is preferably more than 0.10 and less than 0.40.
B is preferably more than 1.5 and less than 1.75.
Weight-average molecular weight containing thiazolinyl polysiloxane is such as more than 100, is preferably more than 500, in addition, such as, is less than 10000, is preferably less than 5000.Weight-average molecular weight containing thiazolinyl polysiloxane is the scaled value based on polystyrene standard by gel permeation chromatography.
Suitable method preparation can be utilized containing thiazolinyl polysiloxane, in addition, also can use commercially available product.
In addition, containing thiazolinyl polysiloxane can be identical type containing thiazolinyl polysiloxane or multiple containing thiazolinyl polysiloxane.
Containing hydrogenated silylation polysiloxane such as contains more than 2 hydrosilyl groups (SiH yl) in molecule.Containing hydrogenated silylation polysiloxane specifically represents with a following average group accepted way of doing sth (2).
An average group accepted way of doing sth (2):
H
cR
3 dSiO
(4-c-d)/2
(in formula, R
3represent that 1 valency alkyl of the carbon number 1 ~ 10 not replacing or replace (wherein, does not comprise alkenyl and/or cycloalkenyl group.)。C is more than 0.30 and less than 1.0, d is more than 0.90 and less than 2.0.)
In formula (2), R
31 valency alkyl of the carbon number 1 ~ 10 not replacing or replace represented can exemplify the R with formula (1)
2the alkyl that the 1 valency alkyl of the carbon number 1 ~ 10 not replacing or replace represented is identical.Preferably list 1 valency alkyl of unsubstituted carbon number 1 ~ 10, more preferably list the aryl of the alkyl of carbon number 1 ~ 10, carbon number 6 ~ 10, preferably list methyl and/or phenyl further.
C is preferably less than 0.5.
D is preferably more than 1.3 and less than 1.7.
The weight-average molecular weight of containing hydrogenated silylation polysiloxane is such as more than 100, is preferably more than 500, in addition, such as, is less than 10000, is preferably less than 5000.The weight-average molecular weight of containing hydrogenated silylation polysiloxane is the scaled value based on polystyrene standard by gel permeation chromatography.
Containing hydrogenated silylation polysiloxane can utilize suitable method to prepare, and in addition, also can use commercially available product.
In addition, containing hydrogenated silylation polysiloxane can be the containing hydrogenated silylation polysiloxane of identical type or multiple containing hydrogenated silylation polysiloxane.
In an above-mentioned average group accepted way of doing sth (1) and an average group accepted way of doing sth (2), preferred R
2and R
3at least any one alkyl comprise phenyl, more preferably R
2and R
3two kinds of hydrocarbon all comprise phenyl.It should be noted that, R
2and R
3at least any one alkyl comprises phenyl time, addition reaction curing type silicone resin combination is regarded as phenyl system organosilicon resin composition.This phenyl system organosilicon resin composition is the 1 elementary reaction curable resin that can become B scalariform state.
On the other hand, R
2and R
3when two kinds of hydrocarbon are methyl, addition reaction curing type silicone resin combination is regarded as methyl system organosilicon resin composition.Methyl system organosilicon resin composition is the 1 elementary reaction curable resin that can not become B scalariform state.
The compounding ratio of containing hydrogenated silylation polysiloxane adjusts as follows: be such as more than 1/30 containing the alkenyl of thiazolinyl polysiloxane and the mole number of cycloalkenyl group relative to the ratio (mole number of the mole number/hydrosilyl groups of alkenyl and cycloalkenyl group) of the mole number of the hydrosilyl groups of containing hydrogenated silylation polysiloxane, be preferably more than 1/3, be such as less than 30/1 in addition, be preferably less than 3/1.
As long as the material (addition catalyst) that hydrosilylation catalysts improves for making the speed of response of the hydrosilylation reactions (hydrosilyl groups addition) containing the alkenyl of thiazolinyl polysiloxane and/or the hydrosilyl groups of cycloalkenyl group and containing hydrogenated silylation polysiloxane, just be not particularly limited, such as, can list metal catalyst.As metal catalyst, can list: platinum catalyst, such as palladium catalyst, the such as rhodium catalysts etc. such as such as platinum black, platinum chloride, Platinic chloride, platinum-alkene complex, platinum-carbonylcomplex, platinum-acetylacetic ester.
The compounding ratio of hydrosilylation catalysts is in the amount of metal of metal catalyst (being specially atoms metal), relative to containing thiazolinyl polysiloxane and containing hydrogenated silylation polysiloxane, take quality as standard, for such as more than 1.0ppm, in addition, be such as below 10000ppm, preferably below 1000ppm, more preferably below 500ppm.
Addition reaction curing type silicone resin combination will be by preparing so that aforementioned proportion is compounding containing thiazolinyl polysiloxane, containing hydrogenated silylation polysiloxane and hydrosilylation catalysts.
Above-mentioned addition reaction curing type silicone resin combination is prepared into A rank (liquid) state by compounding uses containing thiazolinyl polysiloxane, containing hydrogenated silylation polysiloxane and hydrosilylation catalysts.
The hydrosilylation addition reaction containing the alkenyl of thiazolinyl polysiloxane and/or the hydrosilyl groups of cycloalkenyl group and containing hydrogenated silylation polysiloxane is there is in phenyl system organosilicon resin composition by the heating of desired condition, thereafter, hydrosilylation addition reaction stops for the time being.Thereby, it is possible to become B rank (semicure) state from A scalariform state.Afterwards, by the heating of further desired condition, above-mentioned hydrosilylation addition reaction restarts, thus completes.Thereby, it is possible to become C rank (solidifying completely) state from B scalariform state.
It should be noted that, when phenyl system organosilicon resin composition is in B rank (semicure) state, be solid state.In addition, the phenyl system organosilicon resin composition of this B scalariform state can have thermoplasticity and Thermocurable concurrently.That is, the phenyl system organosilicon resin composition on B rank is by after heating temporarily plasticizing, solidifies completely.
On the other hand, in above-mentioned methyl system organosilicon resin composition, there is the hydrosilylation addition reaction of alkenyl and/or cycloalkenyl group and hydrosilyl groups, do not occur stoppingly to promote reaction, thus complete.Thereby, it is possible to become C rank (solidifying completely) state from A scalariform state.Methyl system organosilicon resin composition uses commercially available product.As commercially available product, such as can list ELASTOSIL series (wackerasahikaseisiliconeco., ltd. manufacture, be specially the methyl system organosilicon resin compositions such as ELASTOSILLR7665), KER series (Shin-EtsuChemicalCo., Ltd. manufacture) etc.
Condensation/addition reaction curing type silicone resin combination is 2 elementary reaction curable resins, specifically can list: such as Japanese Unexamined Patent Publication 2010-265436 publication, the 1st ~ 8th condensation/addition reaction curing type silicone resin combination recorded in Japanese Unexamined Patent Publication 2013-187227 publication etc., such as Japanese Unexamined Patent Publication 2013-091705 publication, Japanese Unexamined Patent Publication 2013-001815 publication, Japanese Unexamined Patent Publication 2013-001814 publication, Japanese Unexamined Patent Publication 2013-001813 publication, the organosilicon resin composition etc. containing cage modle eight polysilsesquioxane recorded in Japanese Unexamined Patent Publication 2012-102167 publication etc.It should be noted that, condensation/addition reaction curing type silicone resin combination is solid state, has thermoplasticity and Thermocurable concurrently.
The ratio that contains of the silicone resin in fluor resin combination is such as more than 25 quality %, preferably more than 35 quality %, in addition, such as, is below 70 quality %, is preferably below 50 quality %.
The specific refractory power of silicone resin is such as more than 1.35, is preferably more than 1.40, in addition, is such as less than 1.65, preferably less than 1.60.The specific refractory power of silicone resin utilizes Abbérefractometer to calculate.It should be noted that, the specific refractory power of silicone resin calculates with the form of the specific refractory power of solid state (complete solid state).
As the material of organic granular, such as, thermoplastic resin can be listed.Specifically, can list: acrylic resin, phenylethylene resin series, acrylicstyrene system resin, silicon-type resin, polycarbonate-based resin, benzoguanamine system resin, polyolefin-based resins, polyester based resin, polyamide series resin, polyimide system resin etc.
Such organic granular can be used alone or also can combinationally use.
Wherein, from the viewpoint of light diffusing, availability, preferably list acrylic resin, phenylethylene resin series, acrylicstyrene system resin.
Acrylic resin poly-(methyl) acrylate for obtaining by making the monomer polymerization containing (methyl) acrylate (acrylate and/or methacrylic ester).Such as can list poly-(methyl) methyl acrylate, poly-(methyl) ethyl propenoate, poly-(methyl) propyl acrylate, poly-(methyl) butyl acrylate, (methyl) methyl acrylate-(methyl) ethyl acrylate copolymer etc.
Phenylethylene resin series is such as by styrenic that the monomer polymerization made containing styrenic monomers obtains.As phenylethylene resin series, such as, polystyrene, poly alpha methylstyrene etc. can be listed.
The acrylicstyrene based copolymer of acrylicstyrene system resin for obtaining by making the monomer polymerization containing (methyl) acrylate and styrenic monomers.As acrylicstyrene system resin, such as, can list (methyl) acrylate-styrene multipolymer, (methyl) ethacrylate-styrene multipolymer, (methyl) ethacrylate-styrene multipolymer etc.
It should be noted that, aforesaid propylene acid resin, phenylethylene resin series, acrylicstyrene system resin also can for the multipolymers containing the co-polymerized monomer except acrylic monomer and styrenic monomers.As co-polymerized monomer, preferably list (methyl) vinylformic acid, vinyl cyanide, ethene, divinyl.These co-polymerized monomers can be used alone or combinationally use two or more.
These organic granulars can be cross-linked.That is, crosslinked acrylic resin, cross-linked acrylic acid-phenylethylene resin series, cross-linked styrene system resin is preferably listed.
In addition, organic granular is particulate state, and its shape is not particularly limited, such as, can list roughly spherical, roughly writing board shape, roughly aciculiform shape etc.
The median size (mean value of maximum length) of organic granular is such as more than 1 μm, is preferably more than 5 μm, in addition, for such as less than 100 μm, preferably less than 20 μm, is more preferably less than 10 μm, more preferably less than 9 μm.
When especially using addition reaction curing type silicone resin combination (preferably not there is the methyl system organosilicon resin composition of phenyl), the median size of particularly preferred organic granular is more than 6 μm and less than 9 μm, most preferably is more than 7 μm and less than 9 μm.In addition, when using condensation/addition reaction curing type silicone resin combination (preferred phenyl system organosilicon resin composition), the median size of particularly preferred organic granular is more than 5 μm and less than 7 μm.
When the median size of organic granular is in above-mentioned scope, the deviation of the colourity of wavelength conversion sheet can be suppressed further.The median size of organic granular utilizes particle size distribution device to measure.
The specific refractory power of organic granular is more than 1.45, is preferably more than 1.48.In addition, specific refractory power is less than 1.60, is preferably less than 1.55, is more preferably less than 1.53, more preferably less than 1.50.The specific refractory power of organic granular utilizes Abbérefractometer to calculate.
When the specific refractory power of organic granular is below above-mentioned lower limit, the light diffusion effect that organic granular brings is low, fully can not suppress the deviation of the colourity of wavelength conversion sheet.On the other hand, the specific refractory power of organic granular exceedes above-mentioned in limited time upper, and the refringence of silicone resin and organic granular becomes greatly, has the worry that light transmission reduces.
As these organic granulars, specifically can list: the SSX series (specific refractory power 1.49, crosslinked polymethylmethacrylaparticles particle), SBX series (specific refractory power 1.59, crosslinked polystyrene particle), MSX series (specific refractory power 1.495 ~ 1.595, copolymer of methyl methacrylatestyrene cross-linked particles), MB series (specific refractory power 1.49, poly methyl methacrylate particle), BMX series (specific refractory power 1.49, cross-linked poly-methyl methacrylate butyl ester particle) etc. of Sekisui Plastics Co., Ltd..
The specific refractory power of silicone resin and the specific refractivity of organic granular are such as more than 0.04, are preferably more than 0.05, in addition, such as, are less than 0.20, are preferably less than 0.12, more preferably less than 0.10.Thereby, it is possible to suppress the deviation of the colourity of wavelength conversion sheet further.
The true specific gravity of organic granular is such as more than 1.00, is preferably more than 1.10, in addition, is such as less than 1.50, preferably less than 1.30.
The ratio that contains of the organic granular in fluor resin combination is such as more than 5 quality %, preferably more than 10 quality %, is more preferably more than 15 quality %, in addition, for such as below 30 quality %, be preferably below 25 quality %, be more preferably below 20 quality %.Thereby, it is possible to the deviation of the colourity suppressing organic granular to cause further.
Fluor be have wavelength Conversion function particle and for for the known fluor of optical semiconductor device, such as, can list: blue light can be converted to the yellow fluorophor of sodium yellow, blue light can be converted to the red-emitting phosphors of red light, blue light can be converted to the known fluor such as the green-emitting phosphor of green light.
As yellow fluorophor, can list: such as Y
3al
5o
12: Ce (YAG (yttrium aluminum garnet): Ce), Tb
3al
3o
12: Ce) etc. Ce (TAG (terbium aluminium garnet): there is the oxynitride fluor etc. such as carbuncle type fluor, such as the Ca-α-SiAlON of garnet crystal structure.Preferably list YAG:Ce.
As red-emitting phosphors, such as, CaAlSiN can be listed
3: Eu (CASN), CaSiN
2: the nitride phosphors etc. such as Eu.From the viewpoint of acquisition easiness, preferably list CASN.
As green-emitting phosphor, such as, Lu can be listed
3al
5o
12: the carbuncle type fluor such as Ce (LuAG: ruthenium aluminium garnet).
In such fluor, preferably list the combination of independent yellow fluorophor or red-emitting phosphors and green-emitting phosphor.
Such fluor can be used alone or also can combinationally use.
In addition, fluor is particulate state, and its shape is not particularly limited, such as, can list roughly spherical, roughly writing board shape, roughly aciculiform shape etc.
In addition, the median size (mean value of maximum length) of fluor is such as more than 0.1 μm, is preferably more than 0.2 μm, is more preferably more than 1 μm, in addition, for such as less than 500 μm, be preferably less than 200 μm, be more preferably less than 50 μm.The median size of phosphor particle utilizes particle size distribution device to measure.
The compounding corresponding optical semiconductor of fluor is with the suitable adjustment of the mode becoming white through the light of wavelength conversion sheet, the ratio that contains of the fluor in fluor resin combination is such as more than 5 quality %, preferably more than 10 quality %, in addition, be such as below 65 quality %, preferably below 50 quality %.
When fluor is the combination of red-emitting phosphors and green-emitting phosphor, for them containing ratio, relative to green-emitting phosphor 100 mass parts, red-emitting phosphors be more than more than such as 1 mass parts, preferably 5 mass parts, in addition, for below such as 50 mass parts, be preferably below 30 mass parts.
In addition, in fluor resin combination, organic granular and the total of aforementioned phosphors are such as more than 15 quality %, preferably more than 20 quality % containing ratio, in addition, are such as below 70 quality %, preferably below 60 quality %.
Fluor resin combination also can contain inorganic particle.
Inorganic particle is compounded in fluor resin combination as required in order to improve film-forming properties.As inorganic particle, can list: such as silicon-dioxide (SiO
2), talcum (Mg
3(Si
4o
10) (HO)
2), aluminum oxide (Al
2o
3), boron oxide (B
2o
3), calcium oxide (CaO), zinc oxide (ZnO), strontium oxide (SrO), magnesium oxide (MgO), zirconium white (ZrO
2), barium oxide (BaO), weisspiessglanz (Sb
2o
3) etc. oxide compound, such as aluminium nitride (AlN), silicon nitride (Si
3n
4) etc. the particles of inorganic material such as nitride (inorganics).Preferably list oxide compound, more preferably list silicon-dioxide.
The median size (mean value of maximum length) of inorganic particle is such as more than 1nm, preferably more than 5nm, in addition, for such as less than 30 μm, preferably less than 10 μm, is more preferably less than 5 μm, more preferably less than 0.1 μm.The median size of inorganic particle utilizes particle size distribution device to measure.
The specific refractory power of inorganic particle is such as more than 1.35, is preferably more than 1.40, in addition, is such as less than 1.65, preferably less than 1.60.The specific refractory power of inorganic particle utilizes Abbérefractometer to calculate.
Especially when fluorescencer composition contains phenyl system organosilicon resin composition, preferably containing inorganic particle.Thereby, it is possible to improve the viscosity of fluorescencer composition, improve film-forming properties, therefore, it is possible to obtain the wavelength conversion sheet containing phenyl system silicone resin that inhibit the deviation of colourity more reliably.
When fluor resin combination contains inorganic particle, the ratio that contains of the inorganic particle in fluor resin combination is such as more than 0.1 quality %, preferably more than 0.5 quality %, in addition, is such as below 10 quality %, preferably below 5 quality %.
And then, in above-mentioned fluor resin combination, as required, the known additives such as silane coupling agent, anti-aging agent, properties-correcting agent, tensio-active agent, dyestuff, pigment, anti-blushing agent, UV light absorber can be added with the ratio be applicable to.
When preparing fluor resin combination, silicone resin, organic granular, fluor and the inorganic particle added as required and additive are coordinated with above-mentioned compounding ratio, and mixes.
As mixing condition, temperature is such as more than 10 DEG C, is preferably more than 15 DEG C, in addition, is such as less than 40 DEG C, preferably less than 35 DEG C.
In addition, fluor resin combination carries out deaeration as required after its preparation.
As defoaming method, such as, can list known defoaming methods such as stirring deaeration, vacuum deaerator (vacuum defoamation), evacuation and centrifugal degassing, ultrasonic deaeration.
The viscosity of fluor resin combination is such as more than 1000mPas, preferably more than 2000mPas at such as 25 DEG C, is preferably below 50000mPas, is more preferably below 30000mPas.
The viscosity of fluor resin combination is less than above-mentioned in limited time lower, sometimes plasticity or processibility insufficient.On the other hand, exceed above-mentioned in limited time upper, there is following situation: before stacked organosilicon resin composition carries out flaking, to utilize in the bubble removal step of fluor resin combination (coating liquid) stirring etc. and carry out bubble cannot vagus escape, bubble enters optical semiconductor device, produces the unfavorable condition in the color shift of optical semiconductor device, reliability test.
[manufacture method of wavelength conversion sheet]
With reference to Fig. 1, the method manufacturing wavelength conversion sheet 1 is described.
The manufacture method of wavelength conversion sheet 1 possesses such as preparatory process (with reference to Figure 1A), wavelength conversion sheet lamination process (with reference to Figure 1B).Below, each operation is described in detail.
(preparatory process)
In preparatory process, first, as shown in Figure 1A, peeling base 2 is prepared.
Peeling base 2 is as the surface of wavelength conversion sheet 1 being carried out to the screening glass of covering protection, the coated substrate use of wavelength conversion sheet 1.
Peeling base 2, in order to until protect wavelength conversion sheet 1 during utilizing wavelength conversion sheet 1 to encapsulate optical semiconductor 5, and is strippingly pasted onto the back side of wavelength conversion sheet 1.Namely, peeling base 2 is following flexible thin films by resin formation: when the outbound/conveying/keeping of wavelength conversion sheet 1, stacked in the mode at the back side covering wavelength conversion sheet 1, before will using wavelength conversion sheet 1, peeling base 2 can be peeled off from the back side of wavelength conversion sheet 1 in the mode bending to roughly U-shaped.That is, peeling base 2 only comprises flexible thin film.In addition, the binding face of flexible thin film can carry out lift-off processing as required.
As peeling base 2, be not particularly limited, can list: the peel plate such as resin sheet, such as sheet glass such as such as polyester film (such as pet film), polycarbonate film, polyolefin film (such as polyethylene film, polypropylene film), polystyrene film, acrylic film, silicone resin film, fluorine resin film.
It should be noted that, for the surface (forming the face of wavelength conversion sheet 1 side) of peeling base 2, in order to improve the separability from wavelength conversion sheet 1, can lift-off processing be implemented as required.
The thickness of peeling base 2 is not particularly limited, and when resin sheet, from the viewpoint of such as treatability, cost, is such as 20 ~ 100 μm, when peel plate, is such as 0.5 ~ 10mm.
(wavelength conversion sheet lamination process)
In wavelength conversion sheet lamination process, as shown in Figure 1B, wavelength conversion sheet 1 is layered in the upper surface of peeling base 2.
Specifically, such as, fluor resin combination is such as coated on the upper surface of peeling base 2, then makes fluor resin composition.
As coating process, such as, can list the known coating processes such as applicator coating, cast coat, rotary coating, roller coat.
As the curing of fluor resin combination, the kind according to silicone resin is suitably determined, such as, can list heating.
As heating condition, temperature is such as more than 70 DEG C, is preferably more than 90 DEG C, in addition, is such as less than 150 DEG C, preferably less than 130 DEG C.Time is such as more than 1 minute, is preferably more than 3 minutes, in addition, is such as less than 30 minutes, preferably less than 15 minutes.
Thus, at the stacked wavelength conversion sheet 1 of the upper surface of peeling base 2.
By above operation, manufacture wavelength conversion sheet 1.
Wavelength conversion sheet 1 is preferably formed with the form of the fluor resin combination of C scalariform state (complete solid state).
It should be noted that, when fluor resin combination containing the silicone resin that can become B scalariform state is heating and curing, 2 stepwise heatings can be passed through, C scalariform state is become after maintaining for some time with B scalariform state, in addition, also can make C scalariform state by 1 stepwise heating and not maintain B scalariform state.
Wavelength conversion sheet 1 has writing board shape, specifically, has the thickness of regulation, extends, have smooth surface and the smooth back side along the prescribed direction orthogonal with aforementioned thicknesses direction.In addition, wavelength conversion sheet 1 is not light-emitting device but light-emitting device parts, be parts for the manufacture of light-emitting device, and it containing LED and the substrate carrying LED, specifically, is not formed by fluor resin combination.With the circulation of the form of independent parts, be available equipment in industry.
It should be noted that, when silicone resin contains phenyl system organosilicon resin composition, in the reaction (reaction of C rankization) of phenyl system organosilicon resin composition, the hydrosilyl groups addition reaction containing the alkenyl of thiazolinyl polysiloxane and/or the hydrosilyl groups of cycloalkenyl group and containing hydrogenated silylation polysiloxane is promoted further.Thereafter, the hydrosilyl groups of alkenyl and/or cycloalkenyl group or containing hydrogenated silylation polysiloxane disappears, and hydrosilyl groups addition reaction terminates, and thus, obtains the phenyl system organosilicon resin composition on C rank, i.e. cured article (product).
Above-mentioned cured article represents with a following average group accepted way of doing sth (3).
An average group accepted way of doing sth (3):
R
5 eSiO
(4-e)/2
(in formula, R
5represent that the 1 valency alkyl comprising the carbon number 1 ~ 10 not replacing or replace of phenyl (wherein, does not comprise alkenyl and cycloalkenyl group.)。E is more than 1 and less than 3.)
As R
51 valency alkyl of the carbon number 1 ~ 10 not replacing or replace represented, can illustrate the R with formula (1)
2the 1 valency alkyl of the carbon number 1 ~ 10 not replacing or replace represented and the R of formula (2)
3the group that the 1 valency alkyl of the carbon number 1 ~ 10 not replacing or replace represented is identical.Preferably list the aryl of unsubstituted 1 valency alkyl, the alkyl more preferably listing carbon number 1 ~ 10, carbon number 6 ~ 10, preferably list combinationally using of phenyl and methyl further.
E is preferably more than 1 and less than 3.
In addition, the R of an average group accepted way of doing sth (3) for cured article
5in being more than 30 % by mole containing ratio, being preferably more than 35 % by mole of phenyl, in addition, be less than 55 % by mole, preferably less than 50 % by mole.
The thickness of wavelength conversion sheet 1 is such as more than 10 μm, is preferably more than 50 μm, in addition, is such as less than 1000 μm, preferably less than 500 μm.
The difference R of the maxima and minima of the deviation of the chrominance C IEx of wavelength conversion sheet 1, i.e. chrominance C IEx is such as less than 0.0150, is preferably less than 0.0100, is more preferably less than 0.0070 in the scope of the thickness less than 5 μm of wavelength conversion sheet 1.The measuring method of the deviation of colourity will be described in an embodiment.
In addition, this wavelength conversion sheet 1 is by being that the organic granular of 1.45 ~ 1.60 and the fluor resin combination of fluor are formed containing silicone resin, specific refractory power.Therefore, the organic granular light that can make to incide wavelength conversion sheet 1 inside from optical semiconductor 5 is effectively and equably in wavelength conversion sheet 1 internal divergence.Its result, can make the evenness of the light through wavelength conversion sheet 1, can suppress the deviation of colourity.
[manufacture method of optical semiconductor device]
Below, with reference to Fig. 2 A ~ Fig. 2 D to using above-mentioned wavelength conversion sheet 1 to encapsulate optical semiconductor 5 thus the method manufacturing optical semiconductor device 8 is described.
The manufacture method of optical semiconductor device 8 possesses such as encapsulated layer lamination process (with reference to Fig. 2 A), arrangement step (with reference to Fig. 2 B), packaging process (with reference to Fig. 2 C) and stripping process (with reference to Fig. 2 D).Below each operation is described in detail.
(encapsulated layer lamination process)
In encapsulated layer lamination process, first, as shown in Figure 2 A, the one side (face of not stacked peeling base 2) of the stacked wavelength conversion sheet 1 obtained in FIG of encapsulated layer 3 is made.
Encapsulated layer 3 is formed by potting resin composition, such potting resin composition comprises the known transparent resins buried underground and encapsulate for optical semiconductor, as transparent resins, can also list: the thermoplastic resins etc. such as heat-curing resin, such as acrylic resin, styrene resin, polycarbonate resin, polyolefin resin such as such as silicone resin (above-mentioned), epoxy resin, urethane resin.
Wherein, consider from weather resistance, thermotolerance and sunproof viewpoint, preferably list silicone resin.
As the method forming encapsulated layer 3 on wavelength conversion sheet 1, such as, can list following method: the method directly forming encapsulated layer 3 on wavelength conversion sheet 1; After the first-class formation encapsulated layer 3 of other peeling base, by laminating machine, thermo-compressed etc., this encapsulated layer 3 is transferred to the method etc. of wavelength conversion sheet 1 from described peeling base.
It should be noted that, when potting resin composition contains heat-curing resin, encapsulated layer 3 is heated, make the encapsulated layer 3 formed by potting resin composition become B scalariform state (semi-cured state).
As heating condition, temperature is such as more than 50 DEG C, is preferably more than 80 DEG C, in addition, for such as less than 150 DEG C, preferably less than 140 DEG C, heat-up time is such as more than 1 minute, is preferably more than 5 minutes, in addition, is such as less than 100 minutes, preferably less than 15 minutes.It should be noted that, whether encapsulated layer 3 is that B scalariform state suitably can set according to the kind of heat-curing resin.
Thus, the wavelength Conversion case chip 4 possessing wavelength conversion sheet 1 and stacked encapsulated layer 3 is thereon obtained.
(arrangement step)
In arrangement step, as shown in Figure 2 B, the substrate 7 and wavelength Conversion case chip 4 that are provided with optical semiconductor 5 are configured in opposite directions.That is, with optical semiconductor 5 and encapsulated layer 3 aspectant mode, substrate 7 and wavelength Conversion case chip 4 are configured in opposite directions.
Substrate 7 such as comprises insulated substrate.It should be noted that, be formed with the conductive pattern (not shown) comprising electrode on the surface of substrate 7.
Optical semiconductor 5 such as sending the element (being specially blue led) of blue light, is installed on substrate 7.Optical semiconductor 5 wire-bonded is connected to the electrode (not shown) of substrate 7.It should be noted that, during wire-bonded connects, be electrically connected by the electrode (not shown) of lead-in wire 6 (with reference to dotted line) by the terminal (not shown) being arranged at the upper surface of optical semiconductor 5 and the upper surface that is arranged at substrate 7.
It should be noted that, optical semiconductor 5 also can be installed on substrate 7 (with reference to solid line) by flip-chip.
(packaging process)
In packaging process, as shown in Figure 2 C, the encapsulated layer 3 embedded light semiconductor element 5 of wavelength Conversion case chip 4 is utilized.It should be noted that, when optical semiconductor 5 wire-bonded is connected to substrate 7, optical semiconductor 5 and lead-in wire 6 are buried underground.
Specifically, encapsulated layer 3 hot pressing is made to be connected to substrate 7.Preferably flat board compacting is carried out to wavelength Conversion case chip 4 and substrate 7.
As thermo-compressed condition, temperature is such as 80 ~ 220 DEG C, and pressure is such as 0.01 ~ 1MPa, and the press time is such as 1 ~ 10 minute.
By this thermo-compressed, upper surface and side and the packed layer 3 that goes between of optical semiconductor 5 cover.That is, optical semiconductor 5 and lead-in wire are embedded in encapsulated layer 3.
In addition, the packed layer 3 of upper surface of the substrate 7 exposed from optical semiconductor 5 covers.
Thus, wavelength Conversion case chip 4 is adhered to optical semiconductor 5 and substrate 7.
In addition, by this thermo-compressed, when potting resin composition contains heat-curing resin, encapsulated layer 3 becomes C scalariform state (complete solid state) respectively.
(stripping process)
In stripping process, as shown in the dotted line of Fig. 2 C and Fig. 2 D, peeling base 2 is peeled off from wavelength Conversion case chip 4.
Thus, the optical semiconductor device 8 encapsulating optical semiconductor 5 with encapsulated layer 3 is obtained.
In addition, when optical semiconductor 5 is blue led, obtain the optical semiconductor device 8 as white light emitting device.
That is, optical semiconductor device 8 possesses: substrate 7, is installed on the optical semiconductor 5 of substrate 7, is formed at the encapsulated layer 3 for encapsulating optical semiconductor 5 on substrate 7, and the wavelength conversion sheet 1 be formed on encapsulated layer 3 configured in opposite directions with optical semiconductor 5.
In addition, by utilizing this wavelength Conversion case chip 4 to encapsulate optical semiconductor 5, the deviation of the colourity of the white light sent from optical semiconductor device 8 can be suppressed, seeing the white that uneven color is few.
[variation]
In variation, give identical reference marks to the component same with an above-mentioned embodiment and operation, description is omitted.
In above-mentioned embodiment, as shown in Figure 2 C, wavelength Conversion case chip 4 is utilized to encapsulate the optical semiconductor 5 being installed on substrate 7, but such as also can as shown in Figure 3 C, the optical semiconductor 5 being not yet installed on substrate 7 to being supported by support chip 9 encapsulates.
In this variation, the manufacture method of optical semiconductor device 8 possesses such as: encapsulated layer lamination process (with reference to Fig. 3 A), arrangement step (with reference to Fig. 3 B), packaging process (with reference to Fig. 3 C), the 1st stripping process (dotted line with reference to Fig. 3 C), the 2nd stripping process (with reference to Fig. 3 D) and installation procedure (Fig. 3 E).Below, each operation is described in detail.
(encapsulated layer lamination process)
Encapsulated layer lamination process is same with the encapsulated layer lamination process of above-mentioned embodiment.
(arrangement step)
In preparatory process, as shown in Figure 3 B, configure in opposite directions by support chip 9 and by the optical semiconductor 5 that support chip 9 supports with wavelength Conversion case chip 4.That is, with optical semiconductor 5 and encapsulated layer 3 aspectant mode, support chip 9 and wavelength Conversion case chip 4 are configured in opposite directions.
Support chip 9 possesses back up pad 10 and is layered in the bonding coat 11 of upper surface of back up pad 10.
Back up pad 10, in the tabular extended along direction, face, is arranged on the bottom of support chip 9, is formed as overlooking roughly identical with support chip 9 shape.Back up pad 10 is formed by the mechanically resistant material that can not stretch along direction, face, specifically, as such material, can list: the metals such as oxide compound, such as stainless steel, the such as silicon etc. such as such as silicon oxide (quartz etc.), aluminum oxide.The thickness of back up pad 10 is such as 0.1 ~ 2mm.
Bonding coat 11 is formed at the whole upper surface of back up pad 10.As the jointing material for the formation of bonding coat 11, such as, can list the pressure adhesive such as acrylic pressure sensitive caking agent, silicon-type pressure adhesive.In addition, also can be irradiated stripping film (be specially the middle active energy beams recorded such as Japanese Unexamined Patent Publication 2005-286003 publication and irradiate stripping film) etc. by the active energy beam that such as bounding force reduces by the irradiation of active energy beam and form bonding coat 11.The thickness of bonding coat 11 is such as 0.1 ~ 1mm.
When preparing support chip 9, such as, back up pad 10 and bonding coat 11 are fitted.It should be noted that, also can utilize and first prepare back up pad 10, then the varnish prepared by above-mentioned jointing material and solvent compounding as required coated back up pad 10, as required bonding coat 11 is directly laminated in back up pad 10 by the coating process etc. that solvent distillation is removed afterwards.
The thickness of support chip 9 is such as 0.2 ~ 6mm.
Then, optical semiconductor 5 is laminated in support chip 9.Specifically, the lower surface of optical semiconductor 5 is made to contact with the upper surface of bonding coat 11.
Thus, optical semiconductor 5 is configured (mounting) in support chip 9.That is, support chip 9 is made to support optical semiconductor 5.
(packaging process and the 1st stripping process)
As shown in Figure 3 C, packaging process and the 1st stripping process are identical with the packaging process of above-mentioned embodiment and stripping process respectively.
By packaging process and the 1st stripping process, obtain possessing optical semiconductor 5, for encapsulating the encapsulated layer 3 of optical semiconductor 5 and configuring in opposite directions with optical semiconductor 5 and be formed at the encapsulation optical semiconductor 12 of the wavelength conversion sheet 1 on encapsulated layer 3.It should be noted that, encapsulated layer 3 covers upper surface and the side of optical semiconductor 5.The lower surface of optical semiconductor 5 exposes from encapsulated layer 3, contacts with the upper surface of bonding coat 11.
(the 2nd stripping process)
In 2nd stripping process, as shown in the arrow of Fig. 3 D, encapsulation optical semiconductor 12 is peeled off from the upper surface of bonding coat 11.Specifically, when bonding coat 11 irradiates stripping film for active energy beam, active energy beam is irradiated to bonding coat 11.
Thus, obtain possessing optical semiconductor 5, for encapsulating the encapsulated layer 3 of optical semiconductor 5 and configuring in opposite directions with optical semiconductor 5 and be formed at the encapsulation optical semiconductor 12 of the wavelength conversion sheet 1 on encapsulated layer 3.
(installation procedure)
In installation procedure, as shown in FIGURE 3 E encapsulation optical semiconductor 12 is being installed on substrate 7 afterwards.Specifically, the electrode (not shown) of the terminal (not shown) with substrate 7 that are arranged at the lower surface of optical semiconductor 5 is connected, thus encapsulation optical semiconductor 12 flip-chip is installed on substrate 7.
Thus, the optical semiconductor device 8 possessing substrate 7, optical semiconductor 5, encapsulated layer 3 and wavelength conversion sheet 1 is manufactured.
Utilize the method, also can play action effect similar to the above.
In above-mentioned embodiment, as shown in Figure 2 C, optical semiconductor device 8 possesses: substrate 7, be installed on substrate 7 optical semiconductor 5, be formed on substrate 7 for the encapsulated layer 3 that encapsulates optical semiconductor 5 and the wavelength conversion sheet 1 be formed on encapsulated layer 3, although not diagram, such as optical semiconductor device 8 also can possess: substrate 7, the optical semiconductor 5 being installed on substrate 7 and the wavelength conversion sheet 1 for encapsulating optical semiconductor 5 be formed on substrate 7.That is, optical semiconductor device 8 can not possess encapsulated layer 3.
This optical semiconductor device 8 such as can manufacture as follows: on the substrate 7 being provided with optical semiconductor 5, known coating process is utilized to be coated with fluor resin combination in the mode becoming the thickness that can encapsulate optical semiconductor 5 (and lead-in wire 6), and solidify, manufacture thus.
In above-mentioned embodiment, as shown in Figure 3 D, encapsulation optical semiconductor 12 possesses: optical semiconductor 5, for the encapsulated layer 3 that encapsulates optical semiconductor 5 and the wavelength conversion sheet 1 be formed on encapsulated layer 3, although not diagram, such as, encapsulate optical semiconductor 12 and also can possess optical semiconductor 5 and the wavelength conversion sheet 1 for encapsulating optical semiconductor 5.That is, optical semiconductor device 8 also can not possess encapsulated layer 3.
This encapsulation optical semiconductor 12 such as can manufacture as follows: on the support chip 9 supporting optical semiconductor 5, known coating process is utilized to be coated with fluor resin combination in the mode becoming the thickness that can encapsulate optical semiconductor 5, and solidify, then, support chip 9 is peeled off, manufactures thus.
In above-mentioned embodiment, as shown in Figure 2 C, the mode that optical semiconductor device 8 does not possess to surround optical semiconductor 5 is configured in the housing on substrate 7, but such as shown in Figure 4, optical semiconductor device 8 also can possess housing 13.
The optical semiconductor device 8 of the embodiment of Fig. 4 possesses: substrate 7, the optical semiconductor 5 being installed on substrate 7, the housing 13 be formed on substrate 7, for the encapsulated layer 3 that encapsulates optical semiconductor 5 and the wavelength conversion sheet 1 be formed on encapsulated layer 3.
Housing 13 is overlooked in roughly shaped as frame shape, forms the roughly trapezoidal tubular that width upward narrows gradually.In addition, housing 13 configures across compartment of terrain with the mode and optical semiconductor 5 of surrounding optical semiconductor 5.
Encapsulated layer 3 is filled in housing 13.
Wavelength conversion sheet 1 is also formed at the medial end of the whole upper surface of encapsulated layer 3 and the upper surface of housing 13.
Embodiment
Embodiment and comparative example are below shown, more specific description is carried out to the present invention, but the present invention is not by any restriction of these examples.The numerical value of embodiment shown below can be replaced by the numerical value (i.e. higher limit or lower value) recorded in above-mentioned embodiment.
Embodiment 1
Silicone resin (LR7665 is added in disposable cup (disposalcup), addition reaction curing type silicone resin combination, wackerasahikaseisiliconeco., ltd. manufacture) 4.0g, YAG fluor (Y468, median size 17 μm, NemotoLumi-MaterialsCo., Ltd. manufacture) 4.0g and crosslinked polymethylmethacrylaparticles particle (SSX-108, organic granular, specific refractory power 1.49, median size 8 μm, Sekisui Plastics Co., Ltd. manufactures) 2.0g, after stirring 5 minutes with spatula, use stirrer/defoaming device (mazerustar again, KURABOINDUSTRIESLTD. manufacture) implement to stir deaeration in 3 minutes.Thus, wavelength conversion sheet composition (varnish) is prepared.The viscosity of wavelength conversion sheet composition is 19000mPas ~ 25000mPas.
On slide glass (length 76mm × width 52mm × thickness 1.2 ~ 1.5mm, Song Langxiaozi Industrial Co., Ltd manufacture), use applicator (YoshimitsuSeikiCo., Ltd., manufacture, " BakerapplicatorYBA type ", scale is adjusted to 2.2 ~ 2.8) the wavelength conversion sheet composition of coating preparation, such that length direction is 60mm, width is 52mm.
Then, slide glass is configured on hot plate, heats 5 minutes at 105 DEG C, thus, wavelength conversion sheet composition is solidified, manufacture wavelength conversion sheet (C rank, thickness 170 ~ 210 μm) (with reference to Fig. 5 described later).
Embodiment 2 ~ 13 and comparative example 1 ~ 3
Change into except the formula described in table 1 and table 2 except by the formula of wavelength conversion sheet composition, operate similarly to Example 1, manufacture wavelength conversion sheet (C rank, thickness 170 ~ 210 μm).
Embodiment 14 ~ 22 and comparative example 4
According to following synthesis example and preparation example, prepare phenyl system organosilicon resin composition A.This phenyl system organosilicon resin composition A is used to replace LR7665, the formula of wavelength conversion sheet composition is changed into the formula described in table 3, in addition, operate similarly to Example 1, manufacture wavelength conversion sheet (C rank, thickness 170 ~ 210 μm).
(synthesis example 1)
1 is dropped in the four-hole boiling flask being equipped with stirrer, reflux condensing tube, input port and thermometer, 3-divinyl-1,1,3,3-tetramethyl disiloxane 93.2g, water 140g, trifluoromethanesulfonic acid 0.38g and toluene 500g, mix, dripped the mixture of aminomethyl phenyl dimethoxysilane 729.2g and phenyltrimethoxysila,e 330.5g while stirring with 1 hour, reflux 1 hour thereafter.Then cool, lower floor's (water layer) is separated and removes, 3 washings are carried out to upper strata (toluene solution).Potassium hydroxide 0.40g is added, while water is removed limit backflow from water separator tube in the toluene solution through washing.After completing the removal of water, then reflux 5 hours, and cool.Thereafter, drop into acetic acid 0.6g and neutralize, then filter, the toluene solution obtained is washed 3 times.Thereafter, by concentrating under reduced pressure, obtain liquid containing thiazolinyl polysiloxane A.Containing the averaged unit formula of thiazolinyl polysiloxane A and an average group accepted way of doing sth as follows.
Averaged unit formula:
((CH
2＝CH)(CH
3)
2SiO
1/2)
0.15(CH
3C
6H
5SiO
2/2)
0.60(C
6H
5SiO
3/2)
0.25
An average group accepted way of doing sth:
(CH
2＝CH)
0.15(CH
3)
0.90(C
6H
5)
0.85SiO
1.05
That is, containing thiazolinyl polysiloxane A R
1for vinyl, R
2for methyl and phenyl, the above-mentioned average group accepted way of doing sth (1) of a=0.15, b=1.75 represents.
In addition, utilize gel permeation chromatography to contain the weight-average molecular weight of the polystyrene conversion of thiazolinyl polysiloxane A, result is 2300.
(synthesis example 2)
1 is dropped in the four-hole boiling flask being equipped with stirrer, reflux condensing tube, input port and thermometer, 3-divinyl-1,1,3,3-tetramethyl disiloxane 93.2g, water 140g, trifluoromethanesulfonic acid 0.38g and toluene 500g, mix, and drips the mixture of dimethoxydiphenylsilane 173.4g and phenyltrimethoxysila,e 300.6g while stirring with 1 hour, after dropping terminates, reflux 1 hour.Then cool, lower floor's (water layer) is separated and removes, 3 washings are carried out to upper strata (toluene solution).Potassium hydroxide 0.40g is added, while water is removed limit backflow from water separator tube in the toluene solution through washing.After completing the removal of water, then reflux 5 hours, and cool.Drop into acetic acid 0.6g to neutralize, then filter, the toluene solution obtained is washed 3 times.Thereafter, by concentrating under reduced pressure, obtain liquid containing thiazolinyl polysiloxane B.Containing the averaged unit formula of thiazolinyl polysiloxane B and an average group accepted way of doing sth as follows.
Averaged unit formula:
(CH
2＝CH(CH
3)
2SiO
1/2)
0.31((C
6H
5)
2SiO
2/2)
0.22(C
6H
5SiO
3/2)
0.47
An average group accepted way of doing sth:
(CH
2＝CH)
0.31(CH
3)
0.62(C
6H
5)
0.91SiO
1.08
That is, containing thiazolinyl polysiloxane B R
1for vinyl, R
2for the above-mentioned average group accepted way of doing sth (1) of methyl and phenyl, a=0.31, b=1.53 represents.
In addition, utilize gel permeation chromatography to contain the weight-average molecular weight of the polystyrene conversion of thiazolinyl polysiloxane B, result is 1000.
(synthesis example 3)
Dimethoxydiphenylsilane 325.9g, phenyltrimethoxysila,e 564.9g and trifluoromethanesulfonic acid 2.36g is dropped in the four-hole boiling flask being equipped with stirrer, reflux condensing tube, input port and thermometer, mix, add 1,1,3,3-tetramethyl disiloxane 134.3g, dripped acetic acid 432g with 30 minutes while stirring.After dropping terminates, stir the mixture while be warming up to 50 DEG C, react 3 hours.After being cooled to room temperature, add toluene and water, fully leave standstill after mixing, lower floor's (water layer) is separated and removes.Thereafter, carry out 3 washings to upper strata (toluene solution), then, concentrating under reduced pressure, obtains containing hydrogenated silylation polysiloxane C (linking agent C) thus.
Averaged unit formula and an average group accepted way of doing sth of containing hydrogenated silylation polysiloxane C are as follows.
Averaged unit formula:
(H(CH
3)
2SiO
1/2)
0.33((C
6H
5)
2SiO
2/2)
0.22(C
6H
5PhSiO
3/2)
0.45
An average group accepted way of doing sth:
H
0.33(CH
3)
0.66(C
6H
5)
0.89SiO
1.06
That is, containing hydrogenated silylation polysiloxane C R
3for the above-mentioned average group accepted way of doing sth (2) of methyl and phenyl, c=0.33, d=1.55 represents.
In addition, utilize the weight-average molecular weight of the polystyrene conversion of gel permeation chromatography containing hydrogenated silylation polysiloxane C, result is 1000.
(preparation example 1)
Will containing thiazolinyl polysiloxane A (synthesis example 1) 20g, containing thiazolinyl polysiloxane B (synthesis example 2) 25g, containing hydrogenated silylation polysiloxane C (synthesis example 3, linking agent C) 25g and platinum carbonylcomplex (trade(brand)name " SIP6829.2 ", Gelest company manufactures, platinum concentration 2.0 quality %) 5mg mixing, prepare phenyl system organosilicon resin composition (addition reaction curing type silicone resin combination, 1 elementary reaction curable resin of B scalariform state can be formed).
Comparative example 5
In disposable cup, add silicone resin (LR7665) 6.0g and YAG fluor (Y468) 4.0g, after stirring 5 minutes with spatula, then implement to stir deaeration in 3 minutes with stirrer/defoaming device.Thus, wavelength conversion layer composition (varnish) is prepared.
On slide glass, use the wavelength conversion layer composition of applicator coating preparation.
Then, slide glass is configured on hot plate, heats 5 minutes at 105 DEG C, thus wavelength conversion layer composition is solidified, form wavelength conversion sheet (thickness 200 μm).
Thus, the wavelength conversion sheet of comparative example 5 is obtained.
Comparative example 6
In disposable cup, add silicone resin (LR7665) 9.0g and crosslinked polymethylmethacrylaparticles particle (SSX-108) 1.0g, after stirring 5 minutes with spatula, then implement to stir deaeration in 3 minutes with stirrer/defoaming device.Thus, diffusion layer composition (varnish) is prepared.
Then, on the surface of the wavelength conversion sheet of comparative example 5, use the diffusion layer composition of applicator coating preparation.
Then, the wavelength conversion sheet being coated with diffusion layer composition is configured on hot plate, heats 5 minutes at 105 DEG C, thus diffusion layer composition is solidified, form diffusion layer (thickness 100 μm).
Thus, the wavelength conversion sheet possessing the comparative example 6 of 2 Rotating fields of wavelength conversion layer/diffusion layer is manufactured.
(evaluation of the specific refractory power of the solid state of silicone resin)
Respectively LR7665 and phenyl system organosilicon resin composition are measured to the specific refractory power of solid state.
Specifically, make LR7665 and phenyl system organosilicon resin composition A individually, namely at 100 DEG C, not carry out reaction in 1 hour (completely solidification, C rank) containing particle and fluor, obtain cured article.Then, with Abbérefractometer, obtained cured article is measured.
The specific refractory power of the cured article of LR7665, phenyl system organosilicon resin composition A is 1.42.
(alkyl (the R of the cured article obtained by phenyl system organosilicon resin composition A
5) in phenyl containing the mensuration of ratio)
Utilize
1h-NMR and
29si-NMR calculates by the alkyl (R of an average group accepted way of doing sth (3) being bonded directly to Siliciumatom in the cured article be obtained by reacting of phenyl system organosilicon resin composition A (the phenyl system organosilicon resin composition A namely not containing mineral filler)
5) in phenyl containing ratio (% by mole).
Specifically, making the phenyl system organosilicon resin composition A on A rank at 100 DEG C, carry out reaction in 1 hour (completely solidification, C rank) when not adding mineral filler, obtaining cured article (complete solid state).
Then, the cured article obtained is measured
1h-NMR and
29si-NMR, calculates the alkyl (R being bonded directly to Siliciumatom thus
5) in the ratio (% by mole) shared by phenyl.
Its result is 48 % by mole.
(evaluation of the deviation of colourity)
In each embodiment and each comparative example, as shown in Figure 5, using with the angle of preparing the slide glass 14 having wavelength conversion sheet 1 on the surface at a distance of the place of 3mm as reference point X.In the scope (inside of the dotted line of Fig. 5) of 70mm, in the width direction 35mm along its length from reference point X, measure colourity and the thickness of the wavelength conversion sheet of each embodiment and each comparative example with spacing 5mm.It should be noted that, chrominance C IEx utilizes determination of colority device (manufacture of DF-1000A, Otsuka Electronics Co., Ltd.) to measure, and thickness utilizes laser displacement gauge (LT-9030M, KEYENCECORPORATION manufacture) to measure.
Mark and draw the thickness measured in x-axis, mark and draw chrominance C IEx in y-axis.It should be noted that, in order to get rid of the impact of the light spilt, removing the determination data of each 15mm in length direction two ends.
Then, the difference (y-axis direction length) of the maxima and minima of chrominance C IEx is calculated respectively with the width unit of thickness 5 μm (x-axis direction).
Now, the scope (in the scope of thickness 195 ~ 200 μm in such as embodiment 1) of the thickness 5 μm selecting the difference of maxima and minima minimum, is shown in table 1 ~ table 3 by the difference R of the maxima and minima of the chrominance C IEs in this film thickness range.
It should be noted that, the poor R of comparative example 5 is 0.0170, and the poor R of comparative example 6 is 0.0190.
Table 1
Table 2
Table 3
It should be noted that, the numerical value in each composition of table 1 ~ table 3 represents mass fraction in case of no particular description.The details of the composition in table 1 ~ table 3 is as follows.
LR7665: trade(brand)name " ELASTOSILLR7665 ", addition reaction curing type silicone resin combination (methyl system organosilicon resin composition, can not become 1 elementary reaction curable resin of B scalariform state), wackerasahikaseisiliconeco., ltd. manufacture
Crosslinked methyl methacrylate particle: " SSX-108 ", organic granular, specific refractory power 1.49, median size 8 μm, Sekisui Plastics Co., Ltd. manufacture
Crosslinked methyl methacrylate particle: " SSX-105 ", organic granular, specific refractory power 1.49, median size 5 μm, Sekisui Plastics Co., Ltd. manufacture
Crosslinked methyl methacrylate particle: " SSX-106 ", organic granular, specific refractory power 1.49, median size 6 μm, Sekisui Plastics Co., Ltd. manufacture
Crosslinked methyl methacrylate particle: " SSX-110 ", organic granular, specific refractory power 1.49, median size 10 μm, Sekisui Plastics Co., Ltd. manufacture
Crosslinked methyl methacrylate particle: " SSX-108LXE ", organic granular, specific refractory power 1.545, median size 8 μm, Sekisui Plastics Co., Ltd. manufacture
Crosslinked methyl methacrylate particle: " XX-227AA ", organic granular, specific refractory power 1.525, median size 8 μm, Sekisui Plastics Co., Ltd. manufacture
Silica dioxide granule: " 3sdc ", specific refractory power 1.45, median size 3.4 μm, Deuki Kagaku Kogyo Co., Ltd manufacture
Organic silicon granule: " Tospearl2000B ", specific refractory power 1.42, median size 6.0 μm, MomentivePerformanceMaterialsInc. manufacture
AEROSIL particle: " R976S ", specific refractory power 1.46, median size 7nm, Evonik company manufacture
YAG fluor: " Y468 ", YAG:Ce, median size 17 μm, NemotoLumi-MaterialsCo., Ltd. manufacture
LuAG fluor: " LP-6956 ", Lu3Al
5o
12: Ce, median size 15 μm, LWB company manufacture
CASN fluor: " ER6238 ", CaAlSiN
3: Eu, median size 15 μm, Intematix company manufacture
It should be noted that, foregoing invention provides as illustrative embodiment of the present invention, and it is only illustrate, and being not construed as limiting property is explained.The variation of the present invention that it will be apparent to those skilled in the art is included in the protection domain of claim.
utilizability in industry
Wavelength conversion sheet of the present invention, encapsulation optical semiconductor and optical semiconductor device can be applied to various Industrial products, such as, may be used for the optical applications etc. such as white light semiconductor device.
description of reference numerals
1 wavelength conversion sheet
5 optical semiconductors
7 substrates
8 optical semiconductor devices
12 encapsulation optical semiconductors
Claims (7)
1. a wavelength conversion sheet, is characterized in that, is formed by the fluor resin combination containing silicone resin, organic granular and fluor,
The specific refractory power of described organic granular is 1.45 ~ 1.60.
2. wavelength conversion sheet according to claim 1, is characterized in that, the described organic granular in described wavelength conversion sheet containing ratio be 10 ~ 25 quality %.
3. wavelength conversion sheet according to claim 1, is characterized in that, the described organic granular in described wavelength conversion sheet and the total of described fluor are 15 ~ 70 quality % containing ratio.
4. wavelength conversion sheet according to claim 1, is characterized in that, described organic granular is formed by least one material be selected from the group that is made up of acrylic resin, acrylicstyrene system resin and phenylethylene resin series.
5. wavelength conversion sheet according to claim 1, is characterized in that, described fluor contains CaAlSiN
3: Eu fluor.
6. an optical semiconductor device, is characterized in that, possesses:
Substrate;
Optical semiconductor, it is installed on described substrate; With
Wavelength conversion sheet, itself and described optical semiconductor configure in opposite directions, are formed by the fluor resin combination containing silicone resin, organic granular and fluor, and the specific refractory power of described organic granular is 1.45 ~ 1.60.
7. encapsulate an optical semiconductor, it is characterized in that possessing:
Optical semiconductor; With
Wavelength conversion sheet, itself and described optical semiconductor configure in opposite directions, are formed by the fluor resin combination containing silicone resin, organic granular and fluor, and the specific refractory power of described organic granular is 1.45 ~ 1.60.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2013185474 | 2013-09-06 | ||
| JP2013-185474 | 2013-09-06 | ||
| JP2014167786A JP2015073084A (en) | 2013-09-06 | 2014-08-20 | Wavelength conversion sheet, sealed optical semiconductor, and optical semiconductor element device |
| JP2014-167786 | 2014-08-20 | ||
| PCT/JP2014/072343 WO2015033824A1 (en) | 2013-09-06 | 2014-08-26 | Wavelength conversion sheet, sealed optical semiconductor element and optical semiconductor element device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105518104A true CN105518104A (en) | 2016-04-20 |
Family
ID=52628301
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201480048721.8A Pending CN105518104A (en) | 2013-09-06 | 2014-08-26 | Wavelength conversion sheet, sealed optical semiconductor element and optical semiconductor element device |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JP2015073084A (en) |
| KR (1) | KR20160055141A (en) |
| CN (1) | CN105518104A (en) |
| TW (1) | TW201513409A (en) |
| WO (1) | WO2015033824A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113207302A (en) * | 2018-12-18 | 2021-08-03 | 松下知识产权经营株式会社 | Wavelength conversion member, optical device, projector, and method for manufacturing wavelength conversion member |
| CN113917776A (en) * | 2020-07-09 | 2022-01-11 | 中强光电股份有限公司 | Wavelength conversion device and projection device |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6018608B2 (en) * | 2014-08-08 | 2016-11-02 | 日東電工株式会社 | Sealing sheet, manufacturing method thereof, optical semiconductor device, and sealing optical semiconductor element |
| JP6925100B2 (en) | 2015-05-21 | 2021-08-25 | 日亜化学工業株式会社 | Light emitting device |
| WO2017006942A1 (en) * | 2015-07-06 | 2017-01-12 | 株式会社朝日ラバー | Cell-holding container and cell culture method using same |
| JP2019514201A (en) | 2016-04-18 | 2019-05-30 | オスラム オプト セミコンダクターズ ゲゼルシャフト ミット ベシュレンクテル ハフツングＯｓｒａｍ Ｏｐｔｏ Ｓｅｍｉｃｏｎｄｕｃｔｏｒｓ ＧｍｂＨ | Method of manufacturing optoelectronic component, and optoelectronic component |
| KR102171639B1 (en) * | 2016-12-27 | 2020-10-29 | 한국전자기술연구원 | LED mounted display and manufacturing method thereof |
| JP6823262B2 (en) * | 2017-03-15 | 2021-02-03 | ミツミ電機株式会社 | Optical module manufacturing method and optical module |
| US10570333B2 (en) * | 2017-05-23 | 2020-02-25 | Osram Opto Semiconductors Gmbh | Wavelength conversion element, light emitting device and method for producing a wavelength conversion element |
| KR102158183B1 (en) * | 2019-09-16 | 2020-09-21 | 한국전자기술연구원 | LED mounted display and manufacturing method thereof |
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| US11114594B2 (en) * | 2007-08-24 | 2021-09-07 | Creeled, Inc. | Light emitting device packages using light scattering particles of different size |
| JP5324114B2 (en) * | 2008-03-27 | 2013-10-23 | リンテック株式会社 | Manufacturing method of light emitting module sheet, light emitting module sheet |
| JP5766411B2 (en) * | 2010-06-29 | 2015-08-19 | 日東電工株式会社 | Phosphor layer and light emitting device |
| JP5286393B2 (en) * | 2011-07-29 | 2013-09-11 | シャープ株式会社 | LIGHT EMITTING ELEMENT, LIGHT EMITTING DEVICE, AND LIGHT EMITTING ELEMENT MANUFACTURING METHOD |
-
2014
- 2014-08-20 JP JP2014167786A patent/JP2015073084A/en active Pending
- 2014-08-26 KR KR1020167005624A patent/KR20160055141A/en not_active Application Discontinuation
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113207302A (en) * | 2018-12-18 | 2021-08-03 | 松下知识产权经营株式会社 | Wavelength conversion member, optical device, projector, and method for manufacturing wavelength conversion member |
| CN113207302B (en) * | 2018-12-18 | 2023-07-14 | 松下知识产权经营株式会社 | Wavelength conversion member, optical device, projector, and method for manufacturing wavelength conversion member |
| CN113917776A (en) * | 2020-07-09 | 2022-01-11 | 中强光电股份有限公司 | Wavelength conversion device and projection device |
| US11640107B2 (en) | 2020-07-09 | 2023-05-02 | Coretronic Corporation | Wavelength conversion device and projection device |
Also Published As
| Publication number | Publication date |
|---|---|
| TW201513409A (en) | 2015-04-01 |
| WO2015033824A1 (en) | 2015-03-12 |
| JP2015073084A (en) | 2015-04-16 |
| KR20160055141A (en) | 2016-05-17 |
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