CN107541076A - High heat-resisting organopolysiloxane composition and semiconductor devices - Google Patents
High heat-resisting organopolysiloxane composition and semiconductor devices Download PDFInfo
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- CN107541076A CN107541076A CN201710894234.9A CN201710894234A CN107541076A CN 107541076 A CN107541076 A CN 107541076A CN 201710894234 A CN201710894234 A CN 201710894234A CN 107541076 A CN107541076 A CN 107541076A
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- 239000000203 mixture Substances 0.000 title claims abstract description 77
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 70
- 239000004065 semiconductor Substances 0.000 title claims abstract description 11
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 60
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 27
- 239000010703 silicon Substances 0.000 claims abstract description 26
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 26
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 23
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 18
- 238000007711 solidification Methods 0.000 claims abstract description 16
- 230000008023 solidification Effects 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 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 abstract description 8
- 230000000903 blocking effect Effects 0.000 claims abstract description 5
- 238000006459 hydrosilylation reaction Methods 0.000 claims abstract description 5
- 230000001737 promoting effect Effects 0.000 claims abstract description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 13
- -1 Hydride siloxane Chemical class 0.000 claims description 11
- 230000003287 optical effect Effects 0.000 claims description 10
- 229910020447 SiO2/2 Inorganic materials 0.000 claims description 9
- 229910020485 SiO4/2 Inorganic materials 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 4
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- 239000002253 acid Substances 0.000 description 11
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- 238000000638 solvent extraction Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
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- 239000002585 base Substances 0.000 description 8
- 238000004073 vulcanization Methods 0.000 description 8
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- 230000033228 biological regulation Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 238000007259 addition reaction Methods 0.000 description 5
- 125000003342 alkenyl group Chemical group 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 5
- 238000012935 Averaging Methods 0.000 description 4
- YBHBEZSZXFLQMW-UHFFFAOYSA-N [dimethoxy(phenyl)silyl]methanamine Chemical compound CO[Si](CN)(OC)C1=CC=CC=C1 YBHBEZSZXFLQMW-UHFFFAOYSA-N 0.000 description 4
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- UHUUYVZLXJHWDV-UHFFFAOYSA-N trimethyl(methylsilyloxy)silane Chemical compound C[SiH2]O[Si](C)(C)C UHUUYVZLXJHWDV-UHFFFAOYSA-N 0.000 description 4
- 241000218202 Coptis Species 0.000 description 3
- 235000002991 Coptis groenlandica Nutrition 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 239000011324 bead Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- AHUXYBVKTIBBJW-UHFFFAOYSA-N dimethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)C1=CC=CC=C1 AHUXYBVKTIBBJW-UHFFFAOYSA-N 0.000 description 3
- 229920001558 organosilicon polymer Polymers 0.000 description 3
- 239000002683 reaction inhibitor Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- WGLLSSPDPJPLOR-UHFFFAOYSA-N 2,3-dimethylbut-2-ene Chemical group CC(C)=C(C)C WGLLSSPDPJPLOR-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 150000003961 organosilicon compounds Chemical class 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000011265 semifinished product Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- CGMFKBXPQJJHBR-UHFFFAOYSA-N [SiH3]O[SiH](C=C)C=C Chemical compound [SiH3]O[SiH](C=C)C=C CGMFKBXPQJJHBR-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 201000009310 astigmatism Diseases 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- SJJCABYOVIHNPZ-UHFFFAOYSA-N cyclohexyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)C1CCCCC1 SJJCABYOVIHNPZ-UHFFFAOYSA-N 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- ZLNAFSPCNATQPQ-UHFFFAOYSA-N ethenyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)C=C ZLNAFSPCNATQPQ-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
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- 239000011256 inorganic filler Substances 0.000 description 1
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- 239000001023 inorganic pigment Substances 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
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- 238000012986 modification Methods 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
- 230000035699 permeability Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 150000003283 rhodium Chemical class 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Silicon Polymers (AREA)
Abstract
The present invention relates to organosilicon technical field, is related to a kind of high heat-resisting organopolysiloxane composition and semiconductor devices, including：(A1) there is the organopolysiloxane of branched molecular structure, component (A1) average unit formula is [PhSiO3/2]a1[Me2ViSiO1/2]b1；(A2) there is the organopolysiloxane of straight-chain molecular structure, and the both ends of strand are respectively selected from methyl, phenyl or cyclohexyl by the group on an ethenyl blocking, molecular backbone with silicon bonding, the molar fraction of phenyl is less than 30%；(B) there are the poly- Organhydridosiloxaneresins containing the average at least one and hydrogen atom of silicon bonding and at least one phenyl in a molecule, the molar fraction of phenyl is less than 40%；(C) dosage is enough the hydrosilylation catalysts for promoting the composition solidification.The present invention does not only have excellent cold-resistant thermal impact, resistance to cure time is long and moisture resistance is good, and also excellent heat resistance and high amount of light.
Description
Technical field
The invention belongs to organosilicon technical field, more particularly to a kind of high heat-resisting organopolysiloxane composition and partly lead
Body device.
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-, is had than other high polymer materials preferably resistance to irradiation and weather-proof ability, under natural environment
With longer service life.2. electrical insulation properties, organosilicon product all has good electrical insulation capability, its dielectric damage
Consumption, proof voltage, Inverter fed motor, specific volume resistance and surface resistivity etc. come out at the top in insulating materials, and they
Electric property influenceed very little by temperature and frequency.Therefore, based on above-mentioned good combination property, as organosilicon polymer
One kind, organopolysiloxane is widely used in LED light volt industry.
Generally, LED packaging part includes light-emitting component and LED support, and the light-emitting component is fixed on the LED support
On, the LED support is generally made up of metallic matrix, and silver coating is provided with the metallic matrix, and the silver coating is used for
To the optically focused or astigmatism of light-emitting component light.Organopolysiloxane composition is coated on the light-emitting component and LED support
On silver coating, and solidified, that is, be basically completed the encapsulation to LED.
In the prior art, LED can produce heat in use, the work(used with single packaging of LED
Rate more and more higher, caused heat is increasing during use, and the organopolysiloxane heat resistance in existing LED compared with
Difference, cause the phenomenon that LED is easily cracking or even peels off, influence the service life of LED；It is in addition, existing organic poly-
The light transmittance of siloxanes is poor, and organopolysiloxane is coated on the light-emitting component of LED, causes the amount of light of LED not
It is high.
The content of the invention
The technical problems to be solved by the invention are：It is poor and go out for LED packaging part heat resistance of the prior art
The not high technical problem of light quantity, there is provided a kind of high heat-resisting organopolysiloxane composition and semiconductor devices.
In order to solve the above technical problems, the invention provides a kind of high heat-resisting organopolysiloxane composition, the height
Heat-resisting organopolysiloxane composition includes：
(A1) there is the organopolysiloxane of branched molecular structure, the component (A1) has following averaging unit molecules
Formula：
[PhSiO3/2]a1[Me2ViSiO1/2]b1,
Wherein Ph is phenyl, and Me is methyl, and Vi is vinyl, and 0.4<a1<3,0.2<b1<0.8；
(A2) have straight-chain molecular structure organopolysiloxane, and the both ends of strand respectively by an ethenyl blocking, point
Methyl, phenyl or cyclohexyl are selected from sub- main chain with the group of silicon bonding, the molar fraction of the phenyl is less than 30%；
Wherein, the component (A1) and the weight content ratio relation of the component (A2) are w1:W2=90:10-50:
50；
(B) have in a molecule containing it is average it is at least one with the hydrogen atom of silicon bonding and at least one phenyl it is poly-
Organhydridosiloxaneresins, the molar fraction of the phenyl are less than 40%；
(C) dosage is enough the hydrosilylation catalysts for the organopolysiloxane composition solidification for promoting the height heat-resisting.
Alternatively, the molar fraction of phenyl is 20%-25% in the component (A2).
Alternatively, the molar fraction of phenyl is 25%-35% in the component (B).
Alternatively, the component (A2) has following average unit formulas：
[RMeSiO2/2]a2[Me2ViSiO1/2]2,
Wherein R is phenyl or cyclohexyl, and Me is methyl, and Vi is vinyl, and 0<a2<100.
Alternatively, the molar content of the hydrogen atom with silicon bonding in the component (B) is 0.2-0.8mol/100g, institute
The molecular weight for stating component (B) is less than 1500.
Alternatively, the content of component (A2) medium vinyl is 0.05-1.0mol/100g.
Alternatively, in the hydrogen atom and the component (A1) and the component (A2) with silicon bonding in the component (B)
The ratio between the molal weight of vinyl sum be 0.9-2.0.
Alternatively, the weight ratio of the weight sum of the component (A1) and the component (A2) and the component (B) is 90:
10-10:90。
Alternatively, described (B) has following average unit formulas：
[PhSiO3/2]a3[SiO4/2]b3[Ph2SiO2/2]c3[Me2HSiO1/2]d3,
Wherein Ph is phenyl, and Me is methyl, and H is hydrogen atom, and a3=0 or 1, b3=0 or 1,0<c3<10,1<d3<5.
Alternatively, the heat-resisting organopolysiloxane composition of the height is under solid state, in 25 DEG C of temperature, humidity 60%
Tensile strength under the conditions of RH is 2-10Mpa, elongation at break 10%-100%, refractive index 1.47-1.54.
Present invention also offers a kind of semiconductor devices, the semiconductor devices includes light-emitting component and fixed described luminous
The support of element, wherein, the heat-resisting organopolysiloxane composition of height of the present invention is coated with the light-emitting component
Solidfied material.
The high heat-resisting organopolysiloxane composition and its semiconductor devices of solidification provided according to embodiments of the present invention,
Not only there is excellent cold-resistant thermal impact, resistance to cure time is long and moisture resistance is good, but also there is excellent heat resistance and height
Amount of light.
Brief description of the drawings
Fig. 1 is the semiconductor packages diagrammatic cross-section that one embodiment of the invention provides.
Reference in specification is as follows：
1st, LED support；2nd, light-emitting component；3rd, electrode；4th, joint line；5th, high heat-resisting organopolysiloxane composition is consolidated
Change body.
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 referred to as vinyl, and Me is referred to as methyl, and Ph is referred to as phenyl, and R is referred to as phenyl or ring
Hexyl.
The present invention provides a kind of high heat-resisting organopolysiloxane composition, including：
(A1) there is the organopolysiloxane of branched molecular structure, the component (A1) has following averaging unit molecules
Formula：
[PhSiO3/2]a1[Me2ViSiO1/2]b1,
Wherein Ph is phenyl, and Me is methyl, and Vi is vinyl, and 0.4<a1<3,0.2<b1<0.8；
(A2) have straight-chain molecular structure organopolysiloxane, and the both ends of strand respectively by an ethenyl blocking, point
Methyl, phenyl or cyclohexyl are selected from sub- main chain with the group of silicon bonding, the molar fraction of the phenyl is less than 30%；
Wherein, the component (A1) and the weight content ratio relation of the component (A2) are w1:W2=90:10-50:
50；
(B) have in a molecule containing it is average it is at least one with the hydrogen atom of silicon bonding and at least one phenyl it is poly-
Organhydridosiloxaneresins, the molar fraction of the phenyl are less than 40%；
(C) dosage is enough the hydrosilylation catalysts for promoting the composition solidification.
Wherein, the component (A1) is one of main component of the present composition, vinyl and group in this component
Being reacted to each other with the hydrogen atom of silicon bonding in point (B), forms cross-bond, and solidified.The molecular structure of component (A1) is
Branched molecular structure, and contain average at least one and the vinyl of silicon bonding and at least one phenyl in a molecule.Institute
It is MT structures to state branched molecular structure, and MT structures refer to containing R3SiO1/2And RSiO3/2Siloxy units, wherein R can be with
For Me, Vi or Ph group.
The average unit formula that the component (A1) has is：
[PhSiO3/2]a1[Me2ViSiO1/2]b1,
Wherein Ph is phenyl, and Me is methyl, and Vi is vinyl, and 0.4<a1<3,0.2<b1<0.8；In component (A1) only
Contain R3SiO1/2And RSiO3/2Siloxy units, and at the both ends of the strand by R3SiO1/2Siloxy units are sealed
End, molecule middle-of-chain pass through branched RSiO3/2Siloxy units connect, in the strand, no R2SiO2/2First silicon
Oxyalkyl units, component (A1) have completely branched molecular structure, make the organopolysiloxane composition with excellent
Also there is excellent heat resistance and high amount of light while cold-resistant thermal impact, resistance to cure time are long, moisture resistance is good.
For example, component (A1) may include following average unit formula as representative：
[PhSiO3/2]0.4[Me2ViSiO1/2]0.9；
[PhSiO3/2]0.8[Me2ViSiO1/2]2.0。
In order to further control the refractive index of firming body that the present composition obtains, the molar fraction of the phenyl is preferred
More than 30%.Component (A1) is solid at ambient temperature, such as component (A1) exists at 25 DEG C in the form of solid.
The component (A2) is one of main component of the present composition, the vinyl in this component and component (B)
In reacted to each other with the hydrogen atom of silicon bonding, form cross-bond, and solidified.The molecular structure of component (A2) is straight chain molecule
Structure, and the both ends of strand are respectively selected from methyl, phenyl, ring by the group on an ethenyl blocking, molecular backbone with silicon bonding
Hexyl；In order to which its heat resistance and amount of light can be improved while the refractive index of firming body of present composition acquisition is controlled,
The molar fraction of the phenyl is less than 30%.Further to improve the heat resistance and light extraction of the firming body that the present composition obtains
Measure, the molar fraction of phenyl is preferably 20%-25% in the component (A2).
When the molar fraction of phenyl is more than 30% in component (A2), the firming body of manufactured organopolysiloxane composition
Heat resistance is poor, using the poor heat resistance of LED made of the organopolysiloxane composition, causes to apply organopolysiloxane group
Easily cracking or the peeling of the luminescent element surface of compound, influence the service life of LED；Meanwhile the amount of light of the LED is not
Height, the intensity of illumination of LED is have impact on, reduce the optical property of LED.
In order to further improve the reactivity of the component (A2) and the component (B), the content of the alkenyl is preferred
For 0.05-1.0mol/100g, the content of alkenyl within this range makes the crosslink density of composition because will not too high or mistake
It is low and cause that system easily ftractures or gas permeability is too high.The present invention is not limited especially viscosity of the component (A2) at 25 DEG C
System, preferably 10-10000mPas, viscosity composition within this range have preferable ductility simultaneously application property compared with
It is good.
In order to further improve the heat resistance and amount of light of the firming body of present composition acquisition, the component
(A2) it can be following average unit formulas：
[RMeSiO2/2]a2[Me2ViSiO1/2]2,
Wherein Me is methyl, R is phenyl or cyclohexyl, Vi are vinyl, and 0<a2<10.
In the present invention, the component (A1) and the weight content ratio relation of the component (A2) are w1:W2=90:10-
50:50。
The component (B) is one of main component of the present composition, and the component (B) has to be contained in a molecule
There are the poly- Organhydridosiloxaneresins of the averagely at least one and hydrogen atom of silicon bonding and at least one phenyl, mole of the phenyl
Fraction is less than 40%, the composition that the component (B) in the content range is formed with other components of the invention, after it solidifies
With excellent heat resistance and high amount of light.Further to improve the heat resistance for the firming body that the present composition obtains and going out
Light quantity, the molar fraction of phenyl is preferably 25%-35% in the component (B).
When the molar fraction of phenyl is more than 40%, the heat resistance of the firming body of the organopolysiloxane composition of synthesis compared with
Difference, using the poor heat resistance of LED made of the organopolysiloxane composition, cause the hair for applying organopolysiloxane composition
Easily cracking or the peeling of optical element surface, influence the service life of LED；Meanwhile the amount of light of the LED is not high, have impact on
The intensity of illumination of LED, reduce the optical property of LED.
In the present invention, the hydrogen atom molar content in the component (B) with silicon bonding is preferably 0.2-0.8mol/100g,
Molecular weight is preferably less than 1500, the composition that the component (B) in the content range is formed with other components of the invention,
It has excellent thermal shock after solidifying, resistance to cure time is long and moisture resistance is good.
As one of the preferred embodiment of the present invention, (B) has following average unit formulas：
[PhSiO3/2]a3[SiO4/2]b3[Ph2SiO2/2]c3[Me2HSiO1/2]d3,
Wherein Ph is phenyl, and Me is methyl, and H is hydrogen atom, and a3=0 or 1, b3=0 or 1,0<c3<10,1<d3<5.
For example, the component (B) may include but be not limited to following molecular structural formula as representative：
[PhSiO3/2]1[Ph2SiO2/2]6[Me2HSiO1/2]3,
[SiO4/2]1[Ph2SiO2/2]8[Me2HSiO1/2]4,
Wherein Ph is phenyl, and Me is methyl, and H is hydrogen atom.
In the present invention, component (C) is to promote the alkenyl and the hydrogen of the silicon bonding in component (B) in component (A1) and (A2)
The catalyst of hydrosilylation reactions occurs for atom.In other words, component (C) 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 or 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 (C) is not particularly limited, it is used
Amount need to be enough to promote said composition curing reaction.
In the high heat-resisting organopolysiloxane composition of the present invention, component (D) addition reaction inhibitor is may also include, its
Effect is to extend the Storage period of the high heat-resisting organopolysiloxane composition 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 (D) are not particularly limited, and this area can be used routinely to suppress
Agent, addition can be added optionally, for example, component (D) is ethynylcyclohexanol in the present invention, addition be component (A1),
(A2) and (B) gross weight 0.05%.
In the present invention, the preparation method of component (A1), (A2), (B), (C) and (D) is not particularly limited, this can be used
Field usual manner prepares, or commercially available.
In the present invention, the content ratio relation of the component (A1), (A2) and component (B) is not particularly limited, such as
The weight ratio of component (A1), (A2) and component (B) 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 hydrogen atom with silicon bonding in component (B) and the second in component (A1) and (A2)
Enough reactions, such as the hydrogen atom with silicon bonding in component (B) and the second in component (A1) and (A2) occur for alkenyl
The ratio between molal weight of alkenyl sum is preferably 0.9-2.0.
, can be by the way that necessary component (A1), (A2) and component (B), (C) be mixed in the present invention, and optionally addO-on therapy
(D) and other additives such as inorganic filler or pigment etc., so as to prepare high heat-resisting organopolysiloxane composition.
In the present invention, there is provided a kind of semiconductor devices, including the support of light-emitting component and the fixed light-emitting component, will be upper
State the heat-resisting organopolysiloxane composition of mixed height to be coated on the support of the light-emitting component, solidified.Solidification
Time and temperature can change, for example, 0.5-2 hour can be kept to carry out one-step solidification at 60 DEG C -100 DEG C first, then
Kept for 2-4 hour carry out secondary solidification at 150 DEG C -200 DEG C.The drawing formed under the conditions of 25 DEG C of temperature, humidity 60%RH
It is 2-10Mpa to stretch intensity, and elongation at break 10%-100%, refractive index is 1.47-1.54 firming body.By contrast, often
The organopolysiloxane composition of rule is difficult to be formed thermal shock, resistance to vulcanization and moisture resistance and keeps consolidating for above-mentioned superperformance
Compound, and there is the advantages of excellent heat resistance and high amount of light.
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.
Synthetic example 1
By phenyltrimethoxysila,e 840g, reaction bulb is put into, and is cooled to 20 DEG C, the dilute of pH=8 is added dropwise in 60 minutes
Alkali lye 400.0g, stirred after dripping off 1 hour, then add acid regulation acid-base value to pH=5, tetramethyl divinyl disiloxane
160g continues backflow 60 minutes, adds solvent extraction, divides and goes sour water layer, and neutral pH is arrived in organic layer washing, pours into flask, vacuum water
Pump is evaporated under reduced pressure concentration, removal of solvent under reduced pressure and low-boiling point material, obtains following averaging unit structural resin：
(PhSiO3/2)0.631[(CH3)2(CH2=CH) SiO1/2]0.21 (A1-1)
The component is the organosilicon polysiloxane that viscosity is 80000mPas at 25 DEG C, and the molar fraction of phenyl is
41.43%, and vinyl molar content is 0.2mol/100g.
Synthetic example 2
By phenyltrimethoxysila,e 860g, reaction bulb is put into, and is cooled to 20 DEG C, the dilute of pH=8 is added dropwise in 60 minutes
Alkali lye 400.0g, stirred after dripping off 1 hour, then add acid regulation acid-base value to pH=5, tetramethyl divinyl disiloxane
140g continues backflow 60 minutes, adds solvent extraction, divides and goes sour water layer, and neutral pH is arrived in organic layer washing, pours into flask, vacuum water
Pump is evaporated under reduced pressure concentration, removal of solvent under reduced pressure and low-boiling point material, obtains following structural resin：
(PhSiO3/2)0.645[(CH3)2(CH2=CH) SiO1/2]0.18 (A1-2)
The component is the organosilicon polysiloxane that viscosity is 120000mPas at 25 DEG C, and the molar fraction of phenyl is
43.12%, and vinyl molar content is 0.18mol/100g.
Synthetic example 3
By phenyltrimethoxysila,e 600g and methylvinyldimethoxysilane 100g, reaction bulb is put into, and cool down
PH=8 sig water 400.0g is added dropwise in 20 DEG C, 60 minutes, stir 1 hour after dripping off, then add acid adjust acid-base value to
PH=5, tetramethyl divinyl disiloxane 140g continue backflow 60 minutes, add solvent extraction, divide and remove sour water layer, organic layer
Neutral pH is washed, pours into flask, vacuum pump is evaporated under reduced pressure concentration, removal of solvent under reduced pressure and low-boiling point material, obtained following
Structural resin：
(PhSiO3/2)0.42[MeViSiO2/2]0.13[Me2ViSiO1/2]0.3 (A1-3)
The component is the organosilicon polysiloxane that viscosity is 12000mPas at 25 DEG C, and the molar fraction of phenyl is
41.43%, and vinyl molar content is 0.25mol/100g.
Synthetic example 4
By aminomethyl phenyl dimethoxysilane 182g, reaction bulb is put into, and is cooled to 20 DEG C, pH=8 is added dropwise in 60 minutes
Sig water 100.0g, stir 1 hour after dripping off, then add acid regulation acid-base value to pH=5, the silicon of tetramethyl divinyl two
Oxygen alkane 186g continues backflow 60 minutes, adds solvent extraction, divides and goes sour water layer, and neutral pH is arrived in organic layer washing, pours into flask, very
Empty water pump is evaporated under reduced pressure concentration, removal of solvent under reduced pressure and low-boiling point material, obtains following structural resin：
[MePhSiO2/2]1[Me2ViSiO1/2]2 (A2-1)
The component is the organosilicon polysiloxane that viscosity is 5mPas at 25 DEG C, and the molar fraction of phenyl is 14.2%,
And vinyl molar content is 0.62mol/100g.
Synthetic example 5
Aminomethyl phenyl dimethoxysilane 546g is added dropwise in pH=5 water, 20 DEG C hydrolyze 60 minutes, add tetramethyl
Divinyl disiloxane 186g continues backflow 60 minutes, adds KOH, regulation reaction system to pH=8, continues 60 points of backflow
Clock, acid adding are adjusted to pH=5-7, add solvent extraction, branch vibration layer, and neutral pH is arrived in organic layer washing, pours into flask, and 70 DEG C are returned
Stream 60 minutes, vacuum pump are evaporated under reduced pressure concentration, removal of solvent under reduced pressure and low-boiling point material, obtain following structural resin：
(PhMeSiO2/2)3[(CH3)2(CH2=CH) SiO1/2]2 (A2-2)
The component is the organosilicon polysiloxane that viscosity is 50mPas at 25 DEG C, and the molar fraction of phenyl is 25%,
And vinyl molar content is 0.3mol/100g.
Synthetic example 6
Cyclohexylmethyldimethoxysilane 800g is added dropwise in pH=5 water, 20 DEG C hydrolyze 60 minutes, add tetramethyl
Base divinyl disiloxane 200g continues backflow 60 minutes, adds KOH, regulation reaction system to pH=8, continues 60 points of backflow
Clock, acid adding are adjusted to pH=5-7, add solvent extraction, branch vibration layer, and neutral pH is arrived in organic layer washing, pours into flask, and 70 DEG C are returned
Stream 60 minutes, vacuum pump are evaporated under reduced pressure concentration, removal of solvent under reduced pressure and low-boiling point material, obtain following structural resin：
(C6H11MeSiO2/2)6[(CH3)2(CH2=CH) SiO1/2]2 (A2-3)
The component is the organosilicon polysiloxane that viscosity is 1100mPas at 25 DEG C, and the molar fraction of cyclohexyl is
33%, and vinyl molar content is 0.21mol/100g.
Synthetic example 7
By aminomethyl phenyl dimethoxysilane 364g, reaction bulb is put into, and is cooled to 20 DEG C, pH=8 is added dropwise in 60 minutes
Sig water 100.0g, stir 1 hour after dripping off, then add acid regulation acid-base value to pH=5, tetramethyl disiloxane 134g
Continue backflow 60 minutes, add solvent extraction, divide and go sour water layer, neutral pH is arrived in organic layer washing, pours into flask, vacuum pump subtracts
Distillation and concentration, removal of solvent under reduced pressure and low-boiling point material are pressed, obtains following structural resin：
[MePhSiO2/2]2[Me2HSiO1/2]2 (B1)
The component is the organosilicon polysiloxane that viscosity is 15mPas at 25 DEG C, and the molar fraction of phenyl is 20%,
And silicon hydrogen molar content is 0.49mol/100g.
Synthetic example 8
By aminomethyl phenyl dimethoxysilane 182g and dimethoxydiphenylsilane 244g, reaction bulb is put into, and cool down
PH=8 sig water 100.0g is added dropwise in 20 DEG C, 60 minutes, stir 1 hour after dripping off, then add acid adjust acid-base value to
PH=5, tetramethyl disiloxane 134g continue backflow 60 minutes, add solvent extraction, divide and go sour water layer, and organic layer is washed in
Property pH, pour into flask, vacuum pump is evaporated under reduced pressure concentration, removal of solvent under reduced pressure and low-boiling point material, obtains following structural resin：
[MePhSiO2/2][Ph2SiO2/2][Me2HSiO1/2]2 (B2)
The component is the organosilicon polysiloxane that viscosity is 15mPas at 25 DEG C, and the molar fraction of phenyl is 30%,
And silicon hydrogen molar content is 0.427mol/100g.
Synthetic example 9
By tetraethyl orthosilicate 104g, after dimethoxydiphenylsilane 488g is well mixed, 1h is added dropwise to pH=3 water
In, maintain temperature to react 2h at 20 DEG C, add tetramethyl disiloxane 150g, 70 DEG C are warming up to after reacting 2h during dropwise addition
Reaction 180 minutes, near room temperature, solvent extraction is added, divide and go sour water layer, neutral pH, vacuum pump decompression are arrived in organic layer washing
Distillation and concentration, removal of solvent under reduced pressure and low-boiling point material, obtain following structural resin：
(Ph2SiO2/2)4[SiO4/2]1[(CH3)2HSiO1/2]4 (B3)
The component is the organo-silicon compound that viscosity is 500mPas at 25 DEG C, and the molar content of its hydrogen is
0.36mol/100g, phenyl molar fraction are 40%.
Synthetic example 10
By phenyltrimethoxysila,e 99g, after dimethoxydiphenylsilane 366g is well mixed, 1h is added dropwise to pH=3
Water in, during dropwise addition maintain temperature at 20 DEG C, react 2h, add tetramethyl disiloxane 120g, react 2h after be warming up to
70 DEG C are reacted 180 minutes, near room temperature, add solvent extraction, are divided and are gone sour water layer, and neutral pH, vacuum pump are arrived in organic layer washing
Concentration, removal of solvent under reduced pressure and low-boiling point material are evaporated under reduced pressure, obtains following structural resin：
(Ph2SiO2/2)3(PhSiO3/2)1[(CH3)2HSiO1/2]3 (B4)
The component is the organo-silicon compound that viscosity is 300mPas at 25 DEG C, and the molar content of its hydrogen is
0.32mol/100g, phenyl molar fraction are 43.75%.
Put into practice embodiment 1-4 and comparative example 1-5
Resin (A1-1) prepared by synthetic example 1-10, (A1-2), (A1-3), (A2-1), (A2-2), (A2-3),
(B1), (B2), (B3), (B4) and
(C) addition reaction catalyst：The octanol solution (platinum concentration 5wt%) of chloroplatinic acid；
(D) 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, there is provided one is fixed with the support of light-emitting component 2
1, wherein the light-emitting component 2 is connected by joint line 4 (being usually gold thread) with electrode 3, by the foregoing curable of the present invention
Organopolysiloxane composition 5 is coated on the support 1 for being fixed with light-emitting component 2, is solidified.
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 150 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.
【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.
【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 150 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.
【Resistance to vulcanization】
After obtained composition deaeration, the point on 1W PCT2835 semi-finished product (gold thread containing chip) after 150 DEG C of 2h that dehumidify
Glue, the 1h at 100 DEG C, then at 150 DEG C after 3h solidifications, by cradle hangs in the reagent bottle of the 1000ml equipped with 1g sulphur powders,
Toasted 5 hours at 80 DEG C, test the light decay of lamp bead.
【PCT2835 white light supports are moistureproof】
After obtained composition deaeration, on the PCT2835 semi-finished product (gold thread containing chip) of the 1W after 150 DEG C of 2h that dehumidify
Dispensing, the 1h at 100 DEG C, then lamp bead is placed in 60 DEG C, 52h under the conditions of 60%RH, put after taking-up after 3h solidifications at 150 DEG C
15-30min is put, five warm area Reflow Solderings is crossed, 270 DEG C of the highest temperature, crosses three times.
【Cold shock testing】
100 1W PCT2835 white light packaging bodies are placed in thermal shock case, each circulation is by -60 DEG C, keeping 15
Minute, at 125 DEG C, keep forming for 15 minutes, cycle alternation, dead lamp rate is recorded after 500cyc.
【Heat resistant test】
10 1W PCT2835 white light packaging bodies are placed in 120 DEG C of baking ovens and lighted, the light decay of 5 days test lamp beads.
Table 1
Note：Test by being expressed as √, test not by be expressed as ×.
Table 2
Note：Test by being expressed as √, test not by be expressed as ×.
Pass through Tables 1 and 2：
1. by comparing embodiment 1-2 and comparative example 1, phenyl in component (A2) in organopolysiloxane composition
When molar fraction is less than 30%, organopolysiloxane composition is all good in cold-resistant thermal shock resistance properties, resistance to vulcanization and humidity resistance
In the case of, its heat resistance and to go out optical property more preferable；By comparing embodiment 1 and 2, phenyl rubs in component (A2)
When your fraction is 25%, organopolysiloxane composition is in cold-resistant thermal shock resistance properties, resistance to vulcanization and all good feelings of humidity resistance
Under condition, its heat resistance and to go out optical property more preferable.
2. by comparing embodiment 1,3 and 4 and comparative example 2, phenyl in component (B) in organopolysiloxane composition
Molar fraction be less than 40% when, organopolysiloxane composition cold-resistant thermal shock resistance properties, it is resistance to vulcanization and humidity resistance it is all good
In the case of good, its heat resistance and to go out optical property more preferable；By comparing embodiment 1,3 and 4, component (B) in embodiment 3
Phenyl molar fraction be 30% when, organopolysiloxane composition is in cold-resistant thermal shock resistance properties, resistance to vulcanization and moisture resistance
Can it is all good in the case of, its heat resistance and to go out optical property more preferable.
3. by comparing embodiment 1-4 and comparative example 1-3, phenyl in component (A2) in organopolysiloxane composition
Molar fraction be less than 30% and component (B) in phenyl molar fraction be less than 40% when, organopolysiloxane composition is resistance to
In the case that thermal shock performance, resistance to vulcanization and humidity resistance are all good, its heat resistance and to go out optical property more preferable.
4. by comparing embodiment 1 and comparative example 4-5, the average list of component (A1) in organopolysiloxane composition
First molecular formula is [PhSiO3/2]a1[Me2ViSiO1/2]b1, and 0.4<a1<3,0.2<b1<When 0.8, organopolysiloxane composition
In the case where cold-resistant thermal shock resistance properties, resistance to vulcanization and humidity resistance are all good, its heat resistance and to go out optical property more preferable.
5. from embodiment 1-4 and comparative example 1-5, the averaging unit of component (A1) is divided in organopolysiloxane composition
Minor is [PhSiO3/2]a1[Me2ViSiO1/2]b1, and 0.4<a1<3,0.2<b1<0.8, the molar fraction of phenyl in component (A2)
When less than 30% and in component (B), the molar fraction of phenyl is less than 40%, hardness height, refractive index after being heating and curing
Good, tensile strength and elongation at break integrated data are more excellent, resistance to cure time is long, cold-resistant thermal shock resistance properties is good, humidity resistance is good,
Good Heat-resistance and amount of light height and the composition that can apply to 1W PCT2835 white light supports in LED encapsulation.
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 (11)
- A kind of 1. high heat-resisting organopolysiloxane composition, it is characterised in that including：(A1) there is the organopolysiloxane of branched molecular structure, the component (A1) has following average unit formulas：[PhSiO3/2]a1[Me2ViSiO1/2]b1,Wherein Ph is phenyl, and Me is methyl, and Vi is vinyl, and 0.4<a1<3,0.2<b1<0.8；(A2) there is the organopolysiloxane of straight-chain molecular structure, and the both ends of strand are respectively by an ethenyl blocking, molecule master Methyl, phenyl or cyclohexyl are selected from chain with the group of silicon bonding, the molar fraction of the phenyl is less than 30%；Wherein, the component (A1) and the weight content ratio relation of the component (A2) are w1:W2=90:10-50:50；(B) have in a molecule containing it is average it is at least one with the hydrogen atom of silicon bonding and at least one phenyl it is poly- organic Hydride siloxane, the molar fraction of the phenyl are less than 40%；(C) dosage is enough the hydrosilylation catalysts for the organopolysiloxane composition solidification for promoting the height heat-resisting.
- 2. the heat-resisting organopolysiloxane composition of height according to claim 1, it is characterised in that in the component (A2) The molar fraction of phenyl is 20%-25%.
- 3. the heat-resisting organopolysiloxane composition of height according to claim 1, it is characterised in that in the component (B) The molar fraction of phenyl is 25%-35%.
- 4. the heat-resisting organopolysiloxane composition of height according to claim 1, it is characterised in that component (A2) tool There are following average unit formulas：[RMeSiO2/2]a2[Me2ViSiO1/2]2,Wherein R is phenyl or cyclohexyl, and Me is methyl, and Vi is vinyl, and 0<a2<100.
- 5. the heat-resisting organopolysiloxane composition of height according to claim 1, it is characterised in that in the component (B) The molar content of the hydrogen atom with silicon bonding be 0.2-0.8mol/100g, the molecular weight of the component (B) is less than 1500.
- 6. the heat-resisting organopolysiloxane composition of height according to claim 1, it is characterised in that in the component (A2) The content of vinyl is 0.05-1.0mol/100g.
- 7. the heat-resisting organopolysiloxane composition of height according to claim 1, it is characterised in that in the component (B) Be with the ratio between the hydrogen atom of silicon bonding and the molal weight of vinyl sum in the component (A1) and the component (A2) 0.9-2.0。
- 8. the heat-resisting organopolysiloxane composition of height according to claim 1, it is characterised in that the component (A1) and The weight sum of the component (A2) is 90 with the weight ratio of the component (B):10-10:90.
- 9. the heat-resisting organopolysiloxane composition of height according to claim 1, it is characterised in that under (B) has State average unit formula：[PhSiO3/2]a3[SiO4/2]b3[Ph2SiO2/2]c3[Me2HSiO1/2]d3,Wherein Ph is phenyl, and Me is methyl, and H is hydrogen atom, and a3=0 or 1, b3=0 or 1,0<c3<10,1<d3<5.
- 10. the heat-resisting organopolysiloxane composition of height according to claim 1, it is characterised in that the height is heat-resisting For organopolysiloxane composition under solid state, the tensile strength under the conditions of 25 DEG C of temperature, humidity 60%RH is 2- 10Mpa, elongation at break 10%-100%, refractive index 1.47-1.54.
- 11. a kind of semiconductor devices, including the support of light-emitting component and the fixed light-emitting component, it is characterised in that the hair The solidfied material for the high heat-resisting organopolysiloxane composition being coated with optical element described in claim any one of 1-10.
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Application publication date: 20180105 |