CN107541075A - Heat molten type organopolysiloxane composition, fluorophor sheet material and semiconductor devices - Google Patents
Heat molten type organopolysiloxane composition, fluorophor sheet material and semiconductor devices Download PDFInfo
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- CN107541075A CN107541075A CN201710894231.5A CN201710894231A CN107541075A CN 107541075 A CN107541075 A CN 107541075A CN 201710894231 A CN201710894231 A CN 201710894231A CN 107541075 A CN107541075 A CN 107541075A
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- 239000000463 material Substances 0.000 title claims abstract description 75
- 239000000203 mixture Substances 0.000 title claims abstract description 67
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 60
- 239000004065 semiconductor Substances 0.000 title claims abstract description 17
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 60
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 59
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 48
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 47
- 239000010703 silicon Substances 0.000 claims abstract description 46
- 239000004593 Epoxy Substances 0.000 claims abstract description 19
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910020388 SiO1/2 Inorganic materials 0.000 claims abstract description 10
- 229910020487 SiO3/2 Inorganic materials 0.000 claims abstract description 10
- 238000006459 hydrosilylation reaction Methods 0.000 claims abstract description 6
- 229910020447 SiO2/2 Inorganic materials 0.000 claims abstract description 5
- 229920005989 resin Polymers 0.000 claims description 24
- 239000011347 resin Substances 0.000 claims description 24
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 23
- -1 Methyl Chemical group 0.000 claims description 20
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 17
- 238000007711 solidification Methods 0.000 claims description 16
- 230000008023 solidification Effects 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 5
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 238000000465 moulding Methods 0.000 abstract description 2
- 238000010792 warming Methods 0.000 description 16
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 15
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 15
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 238000009835 boiling Methods 0.000 description 11
- 239000002253 acid Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 10
- 238000003756 stirring Methods 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000010410 layer Substances 0.000 description 7
- 229910052697 platinum Inorganic materials 0.000 description 7
- 230000007935 neutral effect Effects 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 238000000638 solvent extraction Methods 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- HAURRGANAANPSQ-UHFFFAOYSA-N cis-2,4,6-Trimethyl-2,4,6-triphenylcyclotrisiloxane Chemical compound O1[Si](C)(C=2C=CC=CC=2)O[Si](C)(C=2C=CC=CC=2)O[Si]1(C)C1=CC=CC=C1 HAURRGANAANPSQ-UHFFFAOYSA-N 0.000 description 5
- 239000012044 organic layer Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000007259 addition reaction Methods 0.000 description 4
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YBHBEZSZXFLQMW-UHFFFAOYSA-N [dimethoxy(phenyl)silyl]methanamine Chemical compound CO[Si](CN)(OC)C1=CC=CC=C1 YBHBEZSZXFLQMW-UHFFFAOYSA-N 0.000 description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002683 reaction inhibitor Substances 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- UHUUYVZLXJHWDV-UHFFFAOYSA-N trimethyl(methylsilyloxy)silane Chemical compound C[SiH2]O[Si](C)(C)C UHUUYVZLXJHWDV-UHFFFAOYSA-N 0.000 description 3
- WGLLSSPDPJPLOR-UHFFFAOYSA-N 2,3-dimethylbut-2-ene Chemical group CC(C)=C(C)C WGLLSSPDPJPLOR-UHFFFAOYSA-N 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 2
- DIESBVMVWAXZIE-UHFFFAOYSA-N C(C)O[SiH3].CC=C Chemical compound C(C)O[SiH3].CC=C DIESBVMVWAXZIE-UHFFFAOYSA-N 0.000 description 2
- 125000003342 alkenyl group Chemical group 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- JEWCZPTVOYXPGG-UHFFFAOYSA-N ethenyl-ethoxy-dimethylsilane Chemical compound CCO[Si](C)(C)C=C JEWCZPTVOYXPGG-UHFFFAOYSA-N 0.000 description 2
- 229920001558 organosilicon polymer Polymers 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000032258 transport Effects 0.000 description 2
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 description 1
- PXJZCBUXFVZSLL-UHFFFAOYSA-N CO[SiH2]OC.C=CC Chemical compound CO[SiH2]OC.C=CC PXJZCBUXFVZSLL-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
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- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002118 epoxides Chemical class 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
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- 238000005470 impregnation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
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- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000005487 naphthalate group Chemical group 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000002940 palladium Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003283 rhodium Chemical class 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004577 thatch Substances 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to organosilicon technical field, is related to a kind of heat molten type organopolysiloxane composition, fluorophor sheet material and semiconductor devices, including：(A) R is included1 3SiO1/2Unit, R2 2SiO2/2Unit and R3SiO3/2The branched molecular structure organopolysiloxane of unit；(B1) there is the organopolysiloxane of straight-chain molecular structure, and the both ends of strand respectively block containing a silicon hydrogen；(B2) R is included4 3SiO1/2Unit and R5SiO3/2The branched molecular structure organopolysiloxane of unit, containing at least one with the silicon hydrogen-based of silicon bonding and at least one phenyl in the component (B2)；(C) there is vinyl and the organopolysiloxane of epoxy radicals, and contain average at least one and the vinyl of silicon bonding and at least one epoxy radicals in a molecule；(D) catalyst needed for hydrosilylation.The present invention is not only solid at 25 DEG C, and surface viscosity is low, can be melted by heating, further curing molding, obtained fluorophor sheet material have excellent adhesive property afterwards.
Description
Technical field
The invention belongs to organosilicon technical field, more particularly to a kind of heat molten type organopolysiloxane composition, fluorophor
Sheet material and semiconductor devices.
Background technology
The basic structural unit of organosilicon polymer is made up of silica chain link, and side chain is then various with other by silicon atom
Organic group is connected.Compared with other high polymer materials, organosilicon polymer has following outstanding properties：1. weatherability, organic
The main chain of silicon product is-Si-O-, has heat endurance more more preferable than other high polymer materials and resistance to irradiation and weather-proof energy
Power, there is longer service life under natural environment.2. electrical insulation properties, organosilicon product all has good electrical insulating property
Can, before its dielectric loss, proof voltage, Inverter fed motor, specific volume resistance and surface resistivity etc. rank in insulating materials
Thatch, and their electric property is influenceed very little by temperature and frequency.Therefore, based on above-mentioned good combination property, as
One kind of organosilicon product, organopolysiloxane are widely used in LED light volt industry.
Generally, fluorophor sheet material includes fluorophor and resin, and fluorophor is scattered in into the liquid tree for sealed LED chip
In fat, LED chip is packaged using fluorophor sheet material, the LED that various performances are improved can be obtained.
In recent years, in order to improve LED manufacturing process, it is solid or semisolid encapsulating material at room temperature to develop,
For example, the silicone resin sheet formed using silicon composition progress semi-solid preparation, said composition include the organosilicon of vinyl
Resin, the organic siliconresin containing silicon hydrogen, and the catalyst needed for hydrosilylation.Utilize encapsulation made of said composition
Material has certain practicality, improves the performance of LED, still, the encapsulating material there is also it is certain the problem of, for example,
The encapsulating material has surface viscosity at 25 DEG C, is unfavorable for depositing and transports, and fluorophor sheet material is bonded solidification with LED chip
Afterwards, cohesive force is poor between fluorophor sheet material and LED chip.
The content of the invention
The technical problems to be solved by the invention are：There is surface at 25 DEG C for fluorophor sheet material of the prior art
Viscosity, after solidification is bonded with LED chip, the technical problem of cohesive force difference between fluorophor sheet material and LED chip, there is provided Yi Zhongre
Molten type organopolysiloxane composition, fluorophor sheet material and semiconductor devices.
In order to solve the above technical problems, the embodiment of the present invention provides a kind of heat molten type organopolysiloxane composition, it is described
Composition includes：
(A) R is included1 3SiO1/2Unit, R2 2SiO2/2Unit and R3SiO3/2The organic poly- silica of branched molecular structure of unit
Alkane, R1、R2And R3Methyl, vinyl or phenyl are each independently selected from, is contained in the organopolysiloxane average at least one
Vinyl and at least one phenyl with silicon bonding, the molar fraction of the phenyl group are more than 10%；
(B1) there is the organopolysiloxane of straight-chain molecular structure, and the both ends of strand respectively block containing a silicon hydrogen,
With the group of silicon bonding it is methyl, phenyl or vinyl on molecular backbone；
(B2) R is included4 3SiO1/2Unit and R5SiO3/2The branched molecular structure organopolysiloxane of unit, R4And R5Each
Independently selected from methyl, vinyl or phenyl, containing at least one and silicon hydrogen-based of silicon bonding and at least in the component (B2)
One phenyl；
Wherein, the weight content ratio relation of the component (B1) and the component (B2) is w1:W2=10:90-50:
50；
(C) there is vinyl and the organopolysiloxane of epoxy radicals, and contain average at least one and silicon in a molecule
The vinyl of bonding and at least one epoxy radicals；
(D) catalyst needed for hydrosilylation.
Alternatively, the component (C) have following average unit formulas be,
[Me2ViSiO1/2]a1[PhMeSiO2/2]b1[R6MeSiO2/2]c1
Wherein, the Me is methyl, Ph is phenyl, Vi is vinyl and R6ForAnd 0.1<a1<
0.5,0.3<b1<0.8,0.1<c1<0.5.
Alternatively, the content of the vinyl in the component (C) is 0.1-0.5mol/100g, the content of the epoxy radicals
For 0.05-0.50mol/100g.
Alternatively, the quality of the component (C) accounts for the 0.5%-5.0% of the gross mass of the composition.
Alternatively, it is 0.1-0.5mol/100g with the content of the vinyl of silicon bonding described in the component (A).
Alternatively, in the hydrogen atom and the component (A) with silicon bonding in the component (B1) and the component (B2)
The ratio between the molal weight of vinyl sum be 0.9-2.0.
Alternatively, the component (A) has following average unit formulas,
[PhSiO3/2]a2[Me2ViSiO1/2]b2[MeViSiO2/2]c2,
Wherein Me is methyl, Ph is phenyl and Vi is vinyl, and 0.3<a2<0.8,0.1<b2<0.5,0.1<c2<0.3.
Alternatively, the component (B1) has following average unit formulas,
[R7MeSiO2/2]a3[Me2HSiO1/2]2,
Wherein Me is methyl, R7It is hydrogen atom for phenyl or cyclohexyl and H, and 0<a3<100.
Alternatively, the component (B2) has following average unit formulas,
[PhSiO3/2]a4[Me2HSiO1/2]b4,
Wherein Me is methyl, Ph is phenyl and H is hydrogen atom, and 0.3<a4<1,0<b4<0.6.
Alternatively, the composition is under solid state, at 25 DEG C of temperature, the tensile strength under the conditions of humidity 60%RH
For 2-10Mpa, elongation at break 10%-100%, refractive index 1.47-1.55, hardness D30-D70.
The present invention also provides a kind of fluorophor sheet material, including fluorophor and resin, the fluorophor are scattered in the resin
Liquid form in, the resin be the heat molten type organopolysiloxane composition solidfied material.
The present invention also provides a kind of semiconductor devices, including the support of light-emitting component and the fixed light-emitting component, described
The fluorophor sheet material is posted on light-emitting component.
Had an advantageous effect in that according to embodiment provided by the invention：Compared with prior art, heat provided by the invention
Molten type organopolysiloxane composition, is existed using fluorophor sheet material and its semiconductor devices, said composition made of said composition
It is solid at 25 DEG C, surface viscosity is low, can be melted by heating, afterwards further curing molding.Heated by said composition
After fluorophor sheet material is pasted onto LED chip made of the characteristic of fusing, there is excellent cohesive force, and it at 25 DEG C, surface is glued
Property it is low, storage and transport it is all very convenient.
Brief description of the drawings
Fig. 1 is the schematic diagram that the fluorophor sheet material that one embodiment of the invention provides is affixed on LED chip.
Reference in specification is as follows：
1st, the fluorophor sheet material containing heat molten type organopolysiloxane composition after solidifying；2nd, LED chip；3rd, electrode；
4th, circuit substrate；
Embodiment
In order that technical problem solved by the invention, technical scheme and beneficial effect are more clearly understood, below in conjunction with
Drawings and Examples, the present invention is described in further detail.It should be appreciated that specific embodiment described herein is only
To explain the present invention, it is not intended to limit the present invention.
In describing below, Vi is vinyl, and H is hydrogen atom, and Me is methyl, and Ph is phenyl, R6For epoxy radicals, R7For phenyl
Or cyclohexyl.
A kind of heat molten type organopolysiloxane composition provided by the invention, the composition include：
(A) R is included1 3SiO1/2Unit, R2 2SiO2/2Unit and R3SiO3/2The organic poly- silica of branched molecular structure of unit
Alkane, R1、R2And R3Methyl, vinyl or phenyl are each independently selected from, is contained in the organopolysiloxane average at least one
Vinyl and at least one phenyl with silicon bonding, the molar fraction of the phenyl group are more than 10%；
(B1) there is the organopolysiloxane of straight-chain molecular structure, and the both ends of strand respectively block containing a silicon hydrogen,
With the group of silicon bonding it is methyl, phenyl or vinyl on molecular backbone；
(B2) R is included4 3SiO1/2Unit and R5SiO3/2The branched molecular structure organopolysiloxane of unit, R4And R5Each
Independently selected from methyl, vinyl or phenyl, containing at least one and silicon hydrogen-based of silicon bonding and at least in the component (B2)
One phenyl；
Wherein, the weight content ratio relation of the component (B1) and the component (B2) is w1:W2=10:90-50:
50；
(C) there is the organosilicon polysiloxane of vinyl and epoxy radicals, and in a molecule containing it is average it is at least one with
The vinyl of silicon bonding and at least one epoxy radicals；
(D) catalyst needed for hydrosilylation.
Wherein, the component (A) is one of main component of the present composition, vinyl and component in this component
(B1) being reacted to each other with the hydrogen atom of silicon bonding and in component (B2), forms cross-bond, and solidified.Component (A) is bag
Include R1 3SiO1/2Unit, R2 2SiO2/2Unit and R3SiO3/2The branched molecular structure organopolysiloxane of unit, organic poly- silicon
Contain average at least one and the vinyl of silicon bonding and at least one phenyl in oxygen alkane；Wherein R1、R2And R3Select independently of one another
From methyl, vinyl or phenyl.In order to further control the refractive index of the firming body of present composition acquisition, the phenyl
Molar fraction is more than 10%.
As one of the preferred embodiment of the present invention, (A) has following average unit formulas,
[PhSiO3/2]a2[Me2ViSiO1/2]b2[PhViSiO2/2]c2,
Wherein Me is methyl, Ph is phenyl and Vi is vinyl, and 0.3<a2<0.8,0.1<b2<0.5,0.1<c2<0.3.
In order to further improve the reactivity of the component (A) and component (B1) and component (B2), in the component (A)
Content with the vinyl of silicon bonding is 0.1-0.5mol/100g.
In the present invention, component (A) is solid at 25 DEG C, organic poly- silica that the component (A) is formed with other components
The solidfied material of alkane composition is solid in 25 DEG C of conditions, the solidfied material surface tack free of composition, is made using said composition
Fluorophor sheet material, it is also solid in 25 DEG C of conditions, fluorophor sheet material surface tack free, and fluorophor sheet material is being stored and transported
It is more simple and convenient when defeated.
The component (B1) is one of main component of the present composition, the hydrogen atom with silicon bonding in this component
Reacted to each other with the vinyl in component (A), form cross-bond, and solidified.The molecular structure of component (B1) is straight chain point
Minor structure, the both ends of strand respectively block containing a silicon hydrogen, and the group on molecular backbone with silicon bonding can be methyl, phenyl
Or vinyl, the phenyl molar fraction in component (B1) are preferably greater than 10%, the molecular weight of component (B1) is preferably 1500.
As one of the preferred embodiment of the present invention, (B1) has following average unit formulas,
[R7MeSiO2/2]a3[Me2HSiO1/2]2,
Wherein Me is methyl, R7It is hydrogen atom for phenyl or cyclohexyl and H, and 0<a3<100.
In order to further improve the reactivity of the component (A1) and component (B1) and component (B2), in the component (B1)
Hydrogen atom content with silicon bonding is 0.2-0.6mol/100g.
The component (B2) is one of main component of the present composition, the hydrogen atom with silicon bonding in this component
Reacted to each other with the vinyl in component (A), form cross-bond, and solidified.Component (B2) is to include R4 3SiO1/2Unit and
R5SiO3/2The branched molecular structure organopolysiloxane of unit, containing at least one with the silicon of silicon bonding in the component (B2)
Hydrogen-based and at least one phenyl；Wherein R4And R5It is each independently selected from methyl, vinyl or phenyl.In order to further control this
The refractive index for the firming body that inventive composition obtains, the molar fraction of the phenyl are preferably greater than 10%.
As one of the preferred embodiment of the present invention, (B1) has following average unit formulas,
[PhSiO3/2]a4[Me2HSiO1/2]b4,
Wherein Me is methyl, Ph is phenyl and H is hydrogen atom, and 0.3<a4<1,0<b4<0.6.
In order to further improve the reactivity of the component (A1) and component (B1) and component (B2), in the component (B2)
Be 0.2-0.5mol/100g with the hydrogen atom content of silicon bonding.
The component (C) is one of main component of the present composition, and component (C) has vinyl and epoxy radicals
Organosilicon polysiloxane, and contain average at least one and the vinyl of silicon bonding and at least one epoxy radicals in a molecule；
The component (C) for containing epoxide group can response type organic silicon rigidity-increasing stick, because it has the vinyl group of reactable,
Fluorophor sheet material is made in composition containing component (C), and is packaged into the solidification process of semiconductor devices, organosilicon thickening
Vinyl in agent component (C) participates in the reaction between said composition, component (C) final curing in the semiconductor device, is kept away
Exempt from hot setting or during semiconductor devices lights for a long time, the organic silicon rigidity-increasing stick occurs volatilizing or migrates and lose, so as to lead
Fluorophor sheet material declines with LED chip cohesive force after causing solidification；In other words, component (C) can make the fluorescence after solidification
There is excellent adhesive property between body sheet material and LED chip, its adhesive property will not be influenceed because of hot setting.
As one of the preferred embodiment of the present invention, (C) has following average unit formulas,
[Me2ViSiO1/2]a1[PhMeSiO2/2]b1[R6MeSiO2/2]c1
Wherein, the Me is methyl, Ph is phenyl, Vi is vinyl and R6ForAnd 0.1<a1<
0.5,0.3<b1<0.8,0.1<c1<0.5.
For example, the component (C) may include following molecular formula as representative：
[Me2ViSiO1/2]0.2[PhMeSiO2/2]0.5[R6MeSiO2/2]0.3。
Further to improve the solidfied material adhesive property under the high temperature conditions of the composition containing component (C), described group
The content of the vinyl divided in (C) is 0.1-0.5mol/100g, and the content of the epoxy radicals is 0.05-0.5mol/100g；Institute
State component (C) quality account for the composition gross mass 0.5%-5.0%.
In the present invention, component (D) is to promote the alkenyl and the hydrogen of component (B1) and the silicon bonding in (B2) in component (A)
The catalyst of hydrosilylation reactions occurs for atom.In other words, component (D) is to promote the catalyst of composition solidification.Wherein, originally
Catalyst type is not particularly limited for invention, the custom catalystses of this area, such as platinum-type catalyst, rhodium class catalyst
Or palladium class catalyst, the present invention are preferably platinum-type catalyst.Instantiation includes：Platinum black, chloroplatinic acid, chloroplatinic acid alcoholic solution,
Platinum-alkenylsiloxane complex, platinum-alkene complex etc., preferably platinum-alkenylsiloxane complex, the present invention use
Platinum catalyst with tetramethyl-ethylene base disiloxane as dentate.The dosage of component (D) is not particularly limited, it is used
Amount need to be enough to promote said composition curing reaction.
In the organopolysiloxane composition of the heat molten type of the present invention, component (E) addition reaction inhibitor is may also include, its
Effect is to extend the Storage period of the organopolysiloxane composition of the heat molten type of the present invention, and addition reaction inhibitor is a kind of
Material with temperature dependency, its inhibition is lost when heating to a certain extent rapidly, and it is anti-make it that solidification occurs for composition
Should.The species weight and addition of the addition reaction inhibitor of component (E) are not particularly limited, and this area can be used routinely to suppress
Agent, addition can be added optionally, for example, component (E) is ethynylcyclohexanol in the present invention, addition is component (A), (B1)
The 0.05% of (B2) gross weight.
In the present invention, the preparation method of component (A), (B1), (B2), (C), (D) and (E) is not particularly limited, can be adopted
Prepared with this area usual manner, or it is commercially available.
In the present invention, the content ratio relation of the component (A) and component (B1) and (B2) is not particularly limited, such as
Component (A) and component (B1), the weight ratio of (B2) can be 1:99-99:1, preferred weight ratio 90:10-10:90, more preferably
Weight ratio is 20:80-80:20.As long as meet the alkenyl atom in component (A) and in component (B1), (B2) and silicon bonding
Hydrogen atom occur enough reaction, such as in component (B1), (B2) with the hydrogen atom of silicon bonding with component (A)
The ratio between molal weight of alkenyl sum is preferably 0.9-2.0.
, can be by the way that necessary component (A), (B1) and (B2) be mixed, then by the mixed solution and component in the present invention
(C) mixed with (D), and optionally addO-on therapy (E) and other additives for example fluorescent material, pigment, luminous flux auxiliary agent and
Heat-resistant agent etc., so as to prepare the organopolysiloxane composition of heat molten type.
In the present invention, phase that the heat molten type organopolysiloxane composition passes through component (A), (B1), (B2), (C) and (D)
Interaction, form it into the resin that 25 DEG C are solid, in this condition, the resin does not have surface viscosity, with temperature
Increase, at least more than the 100 DEG C resins for becoming melt fluidity, during it solidifies again, the resin shows excellent
Different adhesive property.Gone back using fluorophor sheet material made of above-mentioned characteristic and semiconductor devices in addition to the excellent properties with itself
There is the performance of above-mentioned heat molten type organopolysiloxane composition.
In the present invention, above-mentioned mixed composition and a certain amount of fluorophor are coated on poly- to benzene after well mixed
On naphthalate resin (PET) film, carry out precuring and fluorophor sheet material is made, the fluorophor can be fluorescent material
YAG-04；Then fluorophor sheet material is affixed on the light-emitting component of semiconductor devices, carries out secondary solidification, the light-emitting component leads to
The support crossed on semiconductor devices is fixed.Hardening time and temperature can change, for example, being coated with the composition and fluorescence first
PET film after powder YAG-04 can keep 10-60min to carry out precuring at 50 DEG C -80 DEG C, then by obtained phosphor plates
Material is affixed on light-emitting component and 2-4 hour is kept at 150 DEG C -200 DEG C, and secondary solidification is carried out under 0.5MPa pressure.Formed
Tensile strength under the conditions of 25 DEG C of temperature, humidity 60%RH is 2-10Mpa, elongation at break 10%-100%, refractive index
For 1.47-1.55, hardness is D30-D70 firming body.By contrast, the made firming body of conventional organopolysiloxane composition
It is difficult to form the solidfied material that tensile strength, elongation at break, refractive index and hardness keep above-mentioned superperformance, and and LED core
Piece has the advantages of splendid cohesive force.
With reference to embodiments, the present invention is described in further detail.It is it should be appreciated that described herein specific
Embodiment only to explain the present invention, is not intended to limit the present invention.
In describing below, Vi is referred to as vinyl, and Me is referred to as methyl, and Ph is referred to as phenyl, and H is referred to as hydrogen atom, and R refers to
On behalf of
Synthetic example 1
By phenyltrimethoxysila,e 1480g, vinyl list end socket 325.65g, methyl ethylene dimethoxy silane
198.35g；Reaction bulb is put into, and is cooled to 20 DEG C, pH=8 sig water 500.0g is added dropwise in 60 minutes, is warming up to after dripping off
50 DEG C are stirred 1 hour, continuation return stirring 1 hour, are then added acid regulation acid-base value to pH=7, are added solvent extraction, divide and go
Neutral pH is arrived in sour water layer, organic layer washing, pours into flask, and vacuum pump is evaporated under reduced pressure concentration, removal of solvent under reduced pressure and low boiling
Material, obtain following structural resin：
[PhSiO3/2]0.65[MeViSiO2/2]0.13[Me2ViSiO1/2]0.22 (A-1)
The organopolysiloxane that it is solid at 25 DEG C that the component, which is, phenyl content 53%, and vinyl molar content
For 0.300mol/100g.
Synthetic example 2
By phenyltrimethoxysila,e 1460g, vinyl list end socket 200g, aminomethyl phenyl dimethoxysilane 245g；Throw
Enter reaction bulb, and be cooled to 20 DEG C, pH=8 sig water 500.0g is added dropwise in 60 minutes, it is small that 50 DEG C of stirrings 1 are warming up to after dripping off
When, continuation return stirring 1 hour, then addition acid regulation acid-base value to pH=7, adds solvent extraction, divides and goes sour water layer, organic
Neutral pH arrive in layer washing, pours into flask, and vacuum pump, which is evaporated under reduced pressure, to be concentrated, removal of solvent under reduced pressure and low-boiling point material, obtain with
Lower structural resin：
[PhSiO3/2]0.72[Me2ViSiO1/2]0.15[MePhSiO2/2]0.13 (A-2)
The organopolysiloxane that it is solid at 25 DEG C that the component, which is, phenyl content 66%, and vinyl molar content
For 0.120mol/100g.
Synthetic example 3
Aminomethyl phenyl dimethoxysilane 271.65g, 1h are added dropwise in pH=3 water, temperature is maintained during dropwise addition
At 20 DEG C, 2h is reacted, adds tetramethyl disiloxane 100g, being warming up to 70 DEG C after reaction 2h reacts 180 minutes, is down to room temperature,
Solvent extraction is added, divides and goes sour water layer, neutral pH is arrived in organic layer washing, and vacuum pump is evaporated under reduced pressure concentration, removal of solvent under reduced pressure
And low-boiling point material, obtain following structural resin：
[PhMeSiO2/2]8[Me2HSiO1/2]2 (B1-1)
The component is the organopolysiloxane that viscosity is 40mPas at 25 DEG C, and the molar content of its hydrogen is 0.49mol/
100g, phenyl content 33%.
Synthetic example 4
Aminomethyl phenyl dimethoxysilane 271.65g, 1h are added dropwise in pH=3 water, temperature is maintained during dropwise addition
At 20 DEG C, 2h is reacted, adds vinyl double seal head 136g, being warming up to 70 DEG C after reaction 2h reacts 180 minutes, is down to room temperature, adds
Enter solvent extraction, point go sour water layer, neutral pH arrive in organic layer washing, and vacuum pump is evaporated under reduced pressure concentration, removal of solvent under reduced pressure with
Low-boiling point material, obtain following structural resin：
[PhMeSiO2/2]8[Me2ViSiO1/2]2 (B1-2)
The component is the organopolysiloxane that viscosity is 62mPas at 25 DEG C, and the molar content of its vinyl is
0.43mol/100g, phenyl content 33%.
Synthetic example 5
Phenyltrimethoxysila,e 500g, 1h are added dropwise in pH=3 water, temperature is maintained during dropwise addition at 20 DEG C,
2h is reacted, adds tetramethyl disiloxane 40g, being warming up to 70 DEG C after reaction 2h reacts 180 minutes, near room temperature, adds solvent
Extraction, divide and go sour water layer, neutral pH is arrived in organic layer washing, and vacuum pump is evaporated under reduced pressure concentration, removal of solvent under reduced pressure and low boiling
Material, obtain following structural resin：
[PhSiO3/2]0.81[Me2HSiO1/2]0.19 (B2-1)
The component is the organopolysiloxane that viscosity is 1700mPas at 25 DEG C, and the molar content of its hydrogen is
0.34mol/100g, phenyl content 40%.
Synthetic example 6
Phenyltrimethoxysila,e 500g, 1h are added dropwise in pH=3 water, temperature is maintained during dropwise addition at 20 DEG C,
2h is reacted, adds tetramethyl disiloxane 270g, being warming up to 70 DEG C after reaction 2h reacts 180 minutes, near room temperature, adds solvent
Extraction, divide and go sour water layer, neutral pH is arrived in organic layer washing, and vacuum pump is evaporated under reduced pressure concentration, removal of solvent under reduced pressure and low boiling
Material, obtain following structural resin：
[PhSiO3/2]0.39[Me2HSiO1/2]0.61 (B2-2)
The component is the organopolysiloxane that viscosity is 60mPas at 25 DEG C, and the molar content of its hydrogen is 0.68mol/
100g, phenyl content 20%.
Synthetic example 7
By trimethyl triphenyl cyclotrisiloxane 230g, (3- glycidoxypropyl groups) methyl dimethoxysilane 193g,
Vinyldimethylethoxysilane 100g, ethyl acetate 50g add flask, and the octanol of chloroplatinic acid is added dropwise after stirring dropwise
Solution (platinum concentration 5wt%), it is warming up to 80 DEG C and reacts 10 hours, be then evacuated to -0.095MPa, be then warming up to 170
DEG C vacuumize and to slough low-boiling point material, obtain following structural resin：
[Me2ViSiO1/2]0.23[PhMeSiO2/2]0.51[R6MeSiO2/2]0.26 (C-1)
Wherein, the R6For
The component is the organosilicon polysiloxane that viscosity is 50mPas at 25 DEG C, and the content of vinyl is 0.22mol/
100g, the content of epoxy radicals is 0.18mol/100g.
Synthetic example 8
By trimethyl triphenyl cyclotrisiloxane 300g, (3- glycidoxypropyl groups) methyl dimethoxysilane 96g, two
Methyl ethylene Ethoxysilane 120g, ethyl acetate 50g add flask, and the octanol that chloroplatinic acid is added dropwise after stirring dropwise is molten
Liquid (platinum concentration 5wt%), it is warming up to 80 DEG C and reacts 10 hours, be then evacuated to -0.095MPa, be then warming up to 170 DEG C
Vacuumize and slough low-boiling point material, obtain following structural resin：
[Me2ViSiO1/2]0.12[PhMeSiO2/2]0.62[R6MeSiO2/2]0.26 (C-2)
Wherein, the R6For
The component is the organosilicon polysiloxane that viscosity is 80mPas at 25 DEG C, and the content of vinyl is 0.26mol/
100g, the content of epoxy radicals is 0.09mol/100g.
Synthetic example 9
By trimethyl triphenyl cyclotrisiloxane 360g, (3- glycidoxypropyl groups) methyl dimethoxysilane 25g, two
Methyl ethylene Ethoxysilane 45g, ethyl acetate 50g add flask, and the octanol that chloroplatinic acid is added dropwise after stirring dropwise is molten
Liquid (platinum concentration 5wt%), it is warming up to 80 DEG C and reacts 10 hours, be then evacuated to -0.095MPa, be then warming up to 170 DEG C
Vacuumize and slough low-boiling point material, obtain following structural resin：
[Me2ViSiO1/2]0.08[PhMeSiO2/2]0.88[R6MeSiO2/2]0.04 (C-3)
Wherein, the R6For
The component is the organosilicon polysiloxane that viscosity is 80mPas at 25 DEG C, and the content of vinyl is 0.06mol/
100g, the content of epoxy radicals is 0.03mol/100g.
Synthetic example 10
Trimethyl triphenyl cyclotrisiloxane 300g, Vinyldimethylethoxysilane 180g, ethyl acetate 50g are added
Enter flask, the octanol solution (platinum concentration 5wt%) of chloroplatinic acid is added dropwise after stirring dropwise, it is small to be warming up to 80 DEG C of reactions 10
When, -0.095MPa is then evacuated to, 170 DEG C is then warming up to and vacuumizes and slough low-boiling point material, obtain following structure tree
Fat：
[Me2ViSiO1/2]0.3[PhMeSiO2/2]0.7 (C-4)
The component is the organosilicon polysiloxane that viscosity is 72mPas at 25 DEG C, and the content of vinyl is 0.40mol/
100g。
Synthetic example 11
By trimethyl triphenyl cyclotrisiloxane 300g, (3- glycidoxypropyl groups) methyl dimethoxysilane 120g,
Ethyl acetate 50g adds flask, and the octanol solution (platinum concentration 5wt%) of chloroplatinic acid is added dropwise after stirring dropwise, is warming up to
80 DEG C are reacted 10 hours, are then evacuated to -0.095MPa, are then warming up to 170 DEG C and are vacuumized and slough low-boiling point material, obtain
Following structural resin：
[PhMeSiO2/2]0.80[R6MeSiO2/2]0.20 (C-5)
Wherein, the R6For
The component is the organosilicon polysiloxane that viscosity is 96mPas at 25 DEG C, and the content of epoxy radicals is 0.14mol/
100g。
Put into practice embodiment 1-6 and comparative example 1-5
Resin (A-1) (A-2) (B1-1) (B1-2) (B2-1) (B2-2) (C-1) (C- prepared by synthetic example 1-11
2) (C-3) (C-4) (C-5) and
(D) addition reaction catalyst：The octanol solution (platinum concentration 5wt%) of chloroplatinic acid；
(E) inhibitor：2- phenyl -3- butyne-2-alcohols.
(each composition is counted in parts by weight) is mixed according to the combination shown in Tables 1 and 2, obtains the present composition.
Semiconductor devices LED shown in Fig. 1 encapsulates in the following way, by the organic poly- silicon of above-mentioned heat molten type of the present invention
Silicone compositions add a certain amount of fluorescent material, stir, are coated on after evacuation and centrifugal degassing in PET film, heated precuring
Fluorophor sheet material 1 is made afterwards, by obtained fluorophor sheet material by way of heating, pressurizeing, pastes and is containing electrode 3 and circuit
In the LED chip 2 of substrate 4, secondary solidification is carried out, the semiconductor devices LED that can be lighted is made.
Obtained each physical and chemical performance of composition is evaluated and tested by following methods.Result is recorded in Tables 1 and 2.
【Hardness】
After obtained composition deaeration, 10g is taken to keep 1h at 100 DEG C, then at 160 DEG C after 3h solidifications, at 25 DEG C,
Three point measurement hardness numbers are taken using shore D type hardness tester meters under conditions of 60%RH, and record average value.
【Tensile strength and elongation at break】
After obtained composition deaeration, the thin slice of 2mm left and right thicknesses, the 1h at 100 DEG C, then at 160 DEG C are prepared
After 3h solidifications, piece is processed into dumbbell shaped, at 25 DEG C, its stretching is tested by force using universal testing machine under conditions of 60%RH
Degree and elongation at break.
【Refractive index】
After obtained composition deaeration, the thin slice of 2mm left and right thicknesses, the 1h at 100 DEG C, then at 150 DEG C are prepared
After 3h solidifications, the composition after solidification is placed on Abbe refractometer and tests its refractive index.
【Surface viscosity】
Fluorophor sheet material is made in obtained composition, after 80 DEG C are placed 30min, is cooled to 25 DEG C, is tested with hand glimmering
The surface viscosity of body of light sheet material.
【Caking property】
Fluorophor sheet material is made in obtained composition, after fitting in LED chip, is installed on after placing 3h at 160 DEG C
The LED component that can be lighted.The method that tweezers impregnation is used under the conditions of 25 DEG C, to evaluate and test the fluorophor sheet material and LED core after solidification
The caking property of piece.
Table 1
Remarks：
Wherein, 00 to be expressed as performance excellent, and zero is expressed as that performance is good, and △ is expressed as poor performance.
Table 2
Remarks：
Wherein, 00 to be expressed as performance excellent, and zero is expressed as that performance is good, and △ is expressed as poor performance.
Pass through Tables 1 and 2：
1st, by comparing embodiment 1,3 and 5, the content of component (C) medium vinyl is 0.1-0.5mol/100g, ring
When the content of epoxide is 0.05-0.5mol/100g, by made from fluorophor sheet material ratio embodiment 5 made from embodiment 1 and 3
The surface viscosity and caking property of fluorophor sheet material are more preferable.
2nd, by comparing embodiment 1,2 and 6, the quality of component (C) accounts for the 0.5- of the gross mass of the composition
When 5.0%, than the surface viscosity of fluorophor sheet material made from embodiment 6 and glued by fluorophor sheet material made from embodiment 1-2
Knot property is more preferable.
3rd, by comparing embodiment 1,3 and 5 and comparative example 4-5, vinyl and epoxy radicals are contained simultaneously in component (C)
When, the surface viscosity of fluorophor sheet material made from ratio 4-5 is compared by fluorophor sheet material made from embodiment 1,3 and 5 and glued
Knot property is more preferable.
4th, by comparing embodiment 1 and comparative example 1, the average unit formula of component (A) is [PhSiO3/2]a2
[Me2ViSiO1/2]b2[MeViSiO2/2]c2, and 0.3<a2<0.8,0.1<b2<0.5,0.1<c2<When 0.3, made by embodiment 1
It is more preferable that the fluorophor sheet material obtained compares the surface viscosity of fluorophor sheet material and caking property made from ratio 1.
5th, by comparing embodiment 2 and comparative example 2, the average unit formula of component (B1) is [RMeSiO2/2]a3
[Me2HSiO1/2]2, and 0<a3<When 100, fluorophor sheet material made from ratio 2 is compared by fluorophor sheet material made from embodiment 2
Surface viscosity and caking property it is more preferable.
6th, it is by comparing embodiment 3 and comparative example 1, the average unit formula of component (B2)
[PhSiO3/2]a4[Me2HSiO1/2]b4, and 0.3<a4<1,0<b4<When 0.6, pass through fluorophor made from embodiment 3
Sheet material is more preferable than the surface viscosity of fluorophor sheet material and caking property made from comparative example 3.
7th, by comparing embodiment 1-6 and comparative example 1-5, after can obtaining inviscid precuring by the present invention
Fluorophor sheet material, hardness is high after being heating and curing, and tensile strength and elongation at break integrated data are more excellent, by using this containing glimmering
Body of light sheet material, there is provided a kind of fluorophor sheet material with high bonding force, which is used as, to be fitted in LED chip.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (12)
- A kind of 1. heat molten type organopolysiloxane composition, it is characterised in that including：(A) R is included1 3SiO1/2Unit, R2 2SiO2/2Unit and R3SiO3/2The branched molecular structure organopolysiloxane of unit, R1、 R2And R3Methyl, vinyl or phenyl are each independently selected from, contains average at least one and silicon key in the organopolysiloxane The vinyl of conjunction and at least one phenyl, the molar fraction of the phenyl group are more than 10%；(B1) there is the organopolysiloxane of straight-chain molecular structure, and the both ends of strand respectively block containing a silicon hydrogen, molecule With the group of silicon bonding it is methyl, phenyl or vinyl on main chain；(B2) R is included4 3SiO1/2Unit and R5SiO3/2The branched molecular structure organopolysiloxane of unit, wherein, R4And R5Each Independently selected from methyl, vinyl or phenyl, containing at least one and silicon hydrogen-based of silicon bonding and at least in the component (B2) One phenyl；Wherein, the weight content ratio relation of the component (B1) and the component (B2) is w1:W2=10:90-50:50；(C) there is vinyl and the organopolysiloxane of epoxy radicals, and contain average at least one and silicon bonding in a molecule Vinyl and at least one epoxy radicals；(D) catalyst needed for hydrosilylation.
- 2. heat molten type organopolysiloxane composition according to claim 1, it is characterised in that the component (C) has Following average unit formulas are,[Me2ViSiO1/2]a1[PhMeSiO2/2]b1[R6MeSiO2/2]c1Wherein, the Me is methyl, Ph is phenyl, Vi is vinyl and R6ForAnd 0.1<a1<0.5, 0.3<b1<0.8,0.1<c1<0.5.
- 3. heat molten type organopolysiloxane composition according to claim 1, it is characterised in that in the component (C) The content of vinyl is 0.1-0.5mol/100g, and the content of the epoxy radicals is 0.05-0.50mol/100g.
- 4. heat molten type organopolysiloxane composition according to claim 1, it is characterised in that the matter of the component (C) Amount accounts for the 0.5%-5% of the gross mass of the composition.
- 5. heat molten type organopolysiloxane composition according to claim 1, it is characterised in that in the component (A) Content with the vinyl of silicon bonding is 0.1-0.5mol/100g.
- 6. heat molten type organopolysiloxane composition according to claim 1, it is characterised in that the component (B1) and institute It is 0.9- to state the ratio between molal weight of vinyl sum in the hydrogen atom and the component (A) with silicon bonding in component (B2) 2.0。
- 7. heat molten type organopolysiloxane composition according to claim 1, it is characterised in that the component (A) has Following average unit formulas,[PhSiO3/2]a2[Me2ViSiO1/2]b2[MeViSiO2/2]c2,Wherein Me is methyl, Ph is phenyl and Vi is vinyl, and 0.3<a2<0.8,0.1<b2<0.5,0.1<c2<0.3.
- 8. heat molten type organopolysiloxane composition according to claim 1, it is characterised in that the component (B1) has Following average unit formulas,[R7MeSiO2/2]a3[Me2HSiO1/2]2,Wherein Me is methyl, R7It is hydrogen atom for phenyl or cyclohexyl and H, and 0<a3<100.
- 9. heat molten type organopolysiloxane composition according to claim 1, it is characterised in that the component (B2) has Following average unit formulas,[PhSiO3/2]a4[Me2HSiO1/2]b4,Wherein Me is methyl, Ph is phenyl and H is hydrogen atom, and 0.3<a4<1,0<b4<0.6.
- 10. heat molten type organopolysiloxane composition according to claim 1, it is characterised in that the composition is solid Under change state, at 25 DEG C of temperature, the tensile strength under the conditions of humidity 60%RH is 2-10Mpa, elongation at break 10%- 100%, refractive index 1.47-1.55, hardness D30-D70.
- 11. a kind of fluorophor sheet material, including fluorophor and resin, the fluorophor are scattered in the liquid form of the resin, Characterized in that, the resin is the solidification of the heat molten type organopolysiloxane composition described in claim any one of 1-10 Thing.
- 12. semiconductor devices made of fluorophor sheet material according to claim 11, it is characterised in that the semiconductor device Part includes the support of light-emitting component and the fixed light-emitting component, and the fluorophor sheet material is posted on the light-emitting component.
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