CN108864707A - Curability silicone resin component, optical semiconductor sealing material and optical semiconductor device - Google Patents
Curability silicone resin component, optical semiconductor sealing material and optical semiconductor device Download PDFInfo
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- CN108864707A CN108864707A CN201810433048.XA CN201810433048A CN108864707A CN 108864707 A CN108864707 A CN 108864707A CN 201810433048 A CN201810433048 A CN 201810433048A CN 108864707 A CN108864707 A CN 108864707A
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- silicone resin
- resin component
- optical semiconductor
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 51
- 230000003287 optical effect Effects 0.000 title claims abstract description 50
- 229920002050 silicone resin Polymers 0.000 title claims abstract description 50
- 239000003566 sealing material Substances 0.000 title claims description 22
- 239000000203 mixture Substances 0.000 claims abstract description 54
- 239000000463 material Substances 0.000 claims abstract description 49
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 33
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 29
- 150000001875 compounds Chemical class 0.000 claims abstract description 23
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 17
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 12
- 150000001451 organic peroxides Chemical class 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 9
- 125000003118 aryl group Chemical group 0.000 claims abstract description 8
- 239000004615 ingredient Substances 0.000 claims description 124
- 229910052799 carbon Inorganic materials 0.000 claims description 34
- -1 siloxane unit Chemical group 0.000 claims description 32
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 11
- 125000005843 halogen group Chemical group 0.000 claims description 9
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 8
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims 6
- 239000000758 substrate Substances 0.000 abstract description 24
- 230000007797 corrosion Effects 0.000 abstract description 8
- 238000005260 corrosion Methods 0.000 abstract description 8
- 150000001721 carbon Chemical group 0.000 description 26
- 229910052697 platinum Inorganic materials 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- 239000007789 gas Substances 0.000 description 11
- 239000002253 acid Substances 0.000 description 10
- 238000007259 addition reaction Methods 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 10
- 238000002156 mixing Methods 0.000 description 10
- 230000004888 barrier function Effects 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 8
- 230000000704 physical effect Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 7
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 238000006459 hydrosilylation reaction Methods 0.000 description 5
- NAWXUBYGYWOOIX-SFHVURJKSA-N (2s)-2-[[4-[2-(2,4-diaminoquinazolin-6-yl)ethyl]benzoyl]amino]-4-methylidenepentanedioic acid Chemical compound C1=CC2=NC(N)=NC(N)=C2C=C1CCC1=CC=C(C(=O)N[C@@H](CC(=C)C(O)=O)C(O)=O)C=C1 NAWXUBYGYWOOIX-SFHVURJKSA-N 0.000 description 4
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 230000000536 complexating effect Effects 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
- 239000011347 resin Substances 0.000 description 4
- 0 CCC(C)(C)N(C)*C Chemical compound CCC(C)(C)N(C)*C 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 125000005641 methacryl group Chemical group 0.000 description 2
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 239000011224 oxide ceramic Substances 0.000 description 2
- 229910052574 oxide ceramic Inorganic materials 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 125000003944 tolyl group Chemical group 0.000 description 2
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- 125000005023 xylyl group Chemical group 0.000 description 2
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 description 1
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- IKEHOXWJQXIQAG-UHFFFAOYSA-N 2-tert-butyl-4-methylphenol Chemical compound CC1=CC=C(O)C(C(C)(C)C)=C1 IKEHOXWJQXIQAG-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 206010018612 Gonorrhoea Diseases 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 125000002521 alkyl halide group Chemical group 0.000 description 1
- 229940045985 antineoplastic platinum compound Drugs 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000004218 chloromethyl group Chemical group [H]C([H])(Cl)* 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- VWWMOACCGFHMEV-UHFFFAOYSA-N dicarbide(2-) Chemical compound [C-]#[C-] VWWMOACCGFHMEV-UHFFFAOYSA-N 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 150000002148 esters Chemical group 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 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 1
- NYMPGSQKHIOWIO-UHFFFAOYSA-N hydroxy(diphenyl)silicon Chemical compound C=1C=CC=CC=1[Si](O)C1=CC=CC=C1 NYMPGSQKHIOWIO-UHFFFAOYSA-N 0.000 description 1
- NOKUWSXLHXMAOM-UHFFFAOYSA-N hydroxy(phenyl)silicon Chemical compound O[Si]C1=CC=CC=C1 NOKUWSXLHXMAOM-UHFFFAOYSA-N 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 125000005386 organosiloxy group Chemical group 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 150000003058 platinum compounds Chemical class 0.000 description 1
- 229920001921 poly-methyl-phenyl-siloxane Polymers 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- RWRDJVNMSZYMDV-UHFFFAOYSA-L radium chloride Chemical class [Cl-].[Cl-].[Ra+2] RWRDJVNMSZYMDV-UHFFFAOYSA-L 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 125000005425 toluyl group Chemical group 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
Abstract
The problem to be solved by the present invention is that providing a kind of curability silicone resin component, it can obtain a kind of solidfied material, the adhesiveness of the solidfied material and the substrate for being equipped with optical semiconductor improves, and the curability silicone resin component can prevent the corrosion for the metal electrode being formed on substrate.To solve the above-mentioned problems, the present invention is a kind of curability silicone resin component, which is characterized in that contains following compositions：(A) the straight-chain organopolysiloxane indicated by following formula (1), the R in formula (1)1Indicate aliphatic unsaturated group, R2Indicate the monovalent hydrocarbon without aliphatic unsaturated bond, R3Indicate alkyl, R4Indicate aryl, a and b are the integers for meeting a >=0, b > 0, b/ (a+b) >=0.5；(B) the organohydrogensiloxanes compound indicated by following formula (2)；(C) organic peroxide；And (D) platinum group metal catalyst.
Description
Technical field
The present invention relates to a kind of curability silicone resin component, the optical semiconductors being made of the composition to seal
Material has used optical semiconductor device obtained by the solidfied material of the optical semiconductor sealing material.
Background technique
The composition of the LED lamp known as optical semiconductor device is as follows：It is close using what is be made of transparent resin
Closure material, to seal the LED element being installed on substrate.As the sealing material to seal this LED, it was widely used in the past
The composition of epoxy resin substrate (referring for example to patent document 1).
However, in the sealing material of epoxy resin substrate, in recent years because the miniaturization with semiconductor package body is with LED's
High brightness and the short wavelengthization of calorific value increase and light, cause to be easy to happen rupture and xanthochromia, thus reliability is caused to reduce.
Therefore, from the viewpoint with excellent heat resistance, used silicon-ketone composition as sealing material.Especially addition
Reaction-curable silicone resin component, due to that can be solidified in the short time by heating, productivity is good, is suitable as
The sealing material of LED (referring for example to patent document 2).
However, metal in LED substrate and the sealing material being made of the solidfied material of addition reaction curing type silicon-ketone composition
The adhesiveness of material is simultaneously insufficient, thus removing is easy to happen between substrate and the solidfied material of the silicon-ketone composition.
In addition, silicon-ketone composition in general gas permeability is excellent, therefore it is easy to be influenced by from external environment.If
LED lamp is exposed among the sulphur compound in atmosphere and exhaust gas etc., then sulphur compound etc. can penetrate the solidification of silicon-ketone composition
Object, and with the metal electrode on the substrate that is sealed by the solidfied material of time corrosion, especially silver electrode, and make its change
It is black.
Existing technical literature
Patent document
Patent document 1：Japanese Unexamined Patent Publication 2000-198930 bulletin；
Patent document 2：Japanese Unexamined Patent Publication 2004-292714 bulletin.
Summary of the invention
Problem to be solved by the invention
The present invention is completed in view of the above-mentioned facts, its purpose is to provide a kind of curability silicone resin component,
It can obtain a kind of solidfied material, and the adhesiveness of the solidfied material and the substrate for being equipped with optical semiconductor improves, and institute
The corrosion for the metal electrode being formed on substrate can be prevented by stating curability silicone resin component.In addition, the purpose of the present invention
It is to provide a kind of optical semiconductor sealing material being made of the composition, and there is optical semiconductor sealing
The optical semiconductor device of the solidfied material of material.
The technical solution solved the problems, such as
To solve the above-mentioned problems, in accordance with the invention it is possible to provide a kind of curability silicone resin component, feature exists
In containing following compositions：
(A) the straight-chain organopolysiloxane indicated by following formula (1),
R in formula (1)1Each independently represent the aliphatic unsaturated group of carbon atom number 2~10, R2Table each independently
Show without aliphatic unsaturated bond and the monovalent hydrocarbon of carbon atom number 1~12 that can be substituted with halogen atoms, R3Respectively solely
On the spot indicate the alkyl of carbon atom number 1~8, R4Each independently represent the aryl of carbon atom number 6~10, a and b be meet a >=
0, the integer of b > 0, b/ (a+b) >=0.5, and putting in order for each siloxane unit is arbitrary；
(B) by following formula (2) indicate organohydrogensiloxanes compound, and the amount of (B) ingredient be by (B) at
Point SiH radix total amount/{ total amount of the aliphatic unsaturation bond number of (A) ingredient } indicate molar ratio become 0.2~5.0
Amount,
In formula (2), R5Indicate hydrogen atom or methyl, R6Indicate the bivalent hydrocarbon radical of carbon atom number 1~12, R7Each independently
Indicate without aliphatic unsaturated bond and the monovalent hydrocarbon of carbon atom number 1~12 that can be substituted with halogen atoms, n is 0,1,
Any one numerical value in 2；
(C) organic peroxide, 100 mass parts of total amount relative to (A) ingredient are 0.01~5 mass parts；And
(D) platinum group metal catalyst, relative to the total quality of (A) ingredient and (B) ingredient, with platinum group
Mass conversion be 0.1~1000ppm.
If it is this curability silicone resin component, then a kind of solidfied material, the solidfied material and installation can be obtained
There is the adhesiveness of the substrate of optical semiconductor to improve, and the curability silicone resin component can prevent from being formed in base
The corrosion of metal electrode on plate.
In addition, being at this time preferably aforementioned R2And R7It is phenyl or methyl.
If it is containing with such R2And R7(A) ingredient and (B) ingredient composition, then can obtain one kind
Adhesiveness and the further excellent solidfied material of gas barrier property.
In addition, being preferably at this time, aforementioned (A) ingredient is the organopolysiloxane indicated by following formula (3),
If it is the curability silicone resin component of this (A) ingredient is contained, then can obtain a kind of adhesiveness and
The further excellent solidfied material of gas barrier property, and the solidfied material of high rigidity can be become, therefore preferably.
In addition, being preferably at this time, aforementioned (B) ingredient is the organohydrogensiloxanes compound indicated by following formula (4),
If it is the curability silicone resin component of this (B) ingredient is contained, then can obtain a kind of adhesiveness and
The further excellent solidfied material of gas barrier property, and the solidfied material of high rigidity can be become, therefore preferably.
In addition, being preferably at this time, aforementioned (C) ingredient is the organic peroxide indicated by following formula (5),
If it is this (C) ingredient, then composition of the invention can be certainly promoted to solidify.
In addition, the present invention provides a kind of optical semiconductor sealing material, it is to be combined by said curing property silicone resin
Object is constituted.
Curability silicone resin component of the invention can obtain a kind of solidfied material, the solidfied material and be equipped with light half
The adhesiveness of the substrate of conductor element improves, and the curability silicone resin component can prevent from being formed on substrate
The corrosion of metal electrode, therefore the use of optical semiconductor sealing material can be suitable as.
In addition, the present invention provides a kind of optical semiconductor device, which is characterized in that have optical semiconductor, with to close
Seal the solidfied material of the aforementioned optical semiconductor sealing material of the optical semiconductor.
This optical semiconductor device has used optical semiconductor sealing material of the invention, can become high reliablity
Optical semiconductor device.
The effect of invention
Curability silicone resin component of the invention, by having both using organic peroxide the vulcanization carried out
(vulcanization) addition reaction and carried out using platinum group metal catalyst, thus with photosemiconductor member is equipped with
The adhesiveness of the substrate of part is good, and has the effect of preventing from being formed in the corrosion of the metal electrode on substrate.This light half
Conductor device has the solidification for the optical semiconductor sealing material being made of curability silicone resin component of the invention
The optical semiconductor of object sealing can become the optical semiconductor device of high reliablity.
Detailed description of the invention
Fig. 1 is the figure of the adhesive test testing piece made using the composition obtained in embodiment, comparative example.
Description of symbols
11,12 aluminium oxide ceramic substrate；
The solidfied material of 13 curability silicone resin components.
Specific embodiment
It is that the present inventor is studied in order to achieve the above objectives and attentively as a result, finding a kind of curability silicone resin group
Object is closed, containing following (A)~(D) ingredient, when using the curability silicone resin component as the close of optical semiconductor
Closure material comes substrate and the silicon-ketone composition to seal this optical semiconductor in use, being equipped with optical semiconductor
Solidfied material can bond securely, be further able to prevent from being formed in the corrosion of the metal electrode, especially silver electrode on substrate,
And a kind of optical semiconductor device of high reliability can be obtained, the optical semiconductor device has used the curability silicone tree
Oil/fat composition, thereby completing the present invention.Hereinafter, explaining curability silicone resin component of the invention, photosemiconductor in detail
Component seal material and optical semiconductor device.
That is, the present invention provides a kind of curability silicone resin component, which is characterized in that contain following compositions：
(A) the straight-chain organopolysiloxane indicated by following formula (1),
R in formula (1)1Each independently represent the aliphatic unsaturated group of carbon atom number 2~10, R2Table each independently
Show without aliphatic unsaturated bond and the monovalent hydrocarbon of carbon atom number 1~12 that can be substituted with halogen atoms, R3Respectively solely
On the spot indicate the alkyl of carbon atom number 1~8, R4Each independently represent the aryl of carbon atom number 6~10, a and b be meet a >=
0, the integer of b > 0, b/ (a+b) >=0.5, and putting in order for each siloxane unit is arbitrary；
(B) by following formula (2) indicate organohydrogensiloxanes compound, and the amount of (B) ingredient be by (B) at
Point SiH radix total amount/{ total amount of the aliphatic unsaturation bond number of (A) ingredient } indicate molar ratio become 0.2~5.0
Amount,
In formula (2), R5Indicate hydrogen atom or methyl, R6Indicate the bivalent hydrocarbon radical of carbon atom number 1~12, R7Each independently
Indicate without aliphatic unsaturated bond and the monovalent hydrocarbon of carbon atom number 1~12 that can be substituted with halogen atoms, n is 0,1,
Any one numerical value in 2；
(C) organic peroxide, 100 mass parts of total amount relative to (A) ingredient are 0.01~5 mass parts；And
(D) platinum group metal catalyst, relative to the total quality of (A) ingredient and (B) ingredient, with platinum group
Mass conversion be 0.1~1000ppm.
[(A) ingredient]
(A) ingredient is the straight-chain organopolysiloxane indicated by following formula (1),
R in formula (1)1Each independently represent the aliphatic unsaturated group of carbon atom number 2~10, R2Table each independently
Show without aliphatic unsaturated bond and the monovalent hydrocarbon of carbon atom number 1~12 that can be substituted with halogen atoms, R3Respectively solely
On the spot indicate the alkyl of carbon atom number 1~8, R4Each independently represent the aryl of carbon atom number 6~10, a and b be meet a >=
0, the integer of b > 0, b/ (a+b) >=0.5, and putting in order for each siloxane unit is arbitrary.
(A) ingredient is the organopolysiloxane with following straight-chain molecule structures：Main chain is by duplicate two organosilicon
Oxygen alkane unit is constituted, and two end of strand is closed by three organosiloxies.
(A) ingredient is oily, and viscosity is preferably in the range of 10~100000000mPas, especially preferably 200
In the range of~10000mPss.If it is 100000000mPas hereinafter, not having to then worry exceedingly to be used as soft segment (soft
Segment it) plays a role and the hardness of solidfied material reduces, and workability is excellent, therefore preferably.In addition, viscosity is to utilize
23 DEG C of the measured value that rotational viscometer measures.In addition, a and b are the integers for meeting a >=0, b > 0, b/ (a+b) >=0.5, by a
The degree of polymerization indicated with the total amount of b is preferably numerical value in the range of (A) ingredient meets above-mentioned range of viscosities.
In above-mentioned formula (1), R1It is each independently as the fat of the carbon atom numbers such as vinyl, allyl, acetenyl 2~10
Race's unsaturated group, the preferably alkenyl of carbon atom number 2~6, especially preferably vinyl.
R2As long as being each independently without aliphatic unsaturated bond and the carbon atom number 1 that can be substituted with halogen atoms
~12 monovalent hydrocarbon, is not particularly limited, it can be cited for example that, methyl, ethyl, propyl, butyl, amyl, hexyl, heptyl etc.
Alkyl；The naphthenic base such as cyclopenta, cyclohexyl；The aryl such as phenyl, tolyl, xylyl, naphthalene；The virtues such as benzyl, phenethyl
Alkyl；Alkylhalide groups such as chloromethyl, 3- chloropropyl etc.；Preferably carbon atom number 1~10 unsubstituted or replace through halogen one
Valency alkyl, especially preferably methyl or phenyl.
R3Be each independently the alkyl of carbon atom number 1~8, can enumerate, methyl, ethyl, propyl, butyl, amyl, oneself
Base, heptyl, octyl.The preferably alkyl of carbon atom number 1~4, more preferably methyl.
R4It is each independently the aryl of carbon atom number 6~10, can be enumerated, phenyl, tolyl, xylyl, naphthalene
Deng preferably phenyl.
It as the specific example of (A) ingredient, can enumerate, the closing of two terminal methyl group phenyl vinyl siloxy of strand is poly-
Diphenyl siloxane, two end diphenylacetylene siloxy of strand close polydiphenylsiloxane, two end first of strand
Base phenyl vinyl siloxy closes polymethylphenylsiloxane, two end diphenylacetylene siloxy of strand closes poly- first
Base phenyl siloxane etc.；(A) individually one kind, which can be used, in ingredient also can be used together two kinds or more.
Especially preferably, aforementioned (A) ingredient is the organopolysiloxane indicated by following formula (3).
[(B) ingredient]
(B) ingredient is the organohydrogensiloxanes compound indicated by following formula (2), has methylacryloyl or acryloyl
Base.In addition, the hydrogen atom (i.e. SiH yl) in a molecule of this (B) ingredient with 1 or more with silicon atom bond, it can be with (A)
The aliphatic unsaturated group of ingredient carries out hydrosilylation (hydrosilylation) reaction, plays a role as crosslinking agent.
In addition, carry out radical crosslinking by the organic peroxide using (C) ingredient, solidfied material can be assigned high adhesion with
Gas barrier property.(B) individually one kind, which can be used, in ingredient also can be used together two kinds or more.
In formula (2), R5Indicate hydrogen atom or methyl, R6Indicate the bivalent hydrocarbon radical of carbon atom number 1~12, R7Each independently
Indicate without aliphatic unsaturated bond and the monovalent hydrocarbon of carbon atom number 1~12 that can be substituted with halogen atoms, n is 0,1,
Any one numerical value in 2.
R in ester moiety6Bivalent hydrocarbon radical carbon atom number be 1~12, especially preferably carbon atom number be 1~4.
R7Each independently represent without aliphatic unsaturated bond and can be substituted with halogen atoms carbon atom number 1~
12 monovalent hydrocarbon can be enumerated and above-mentioned R2Identical monovalent hydrocarbon, especially preferably phenyl or methyl.
Especially preferably, aforementioned (B) ingredient is the organohydrogensiloxanes compound indicated by following formula (4).
(B) blended amount of ingredient is by { total amount of the SiH radix of (B) ingredient }/{ aliphatic unsaturated bond of (A) ingredient
Several total amounts } indicate molar ratio become 0.2~5.0 amount, preferably 0.5~2.0.When lower than 0.2 or more than 5.0, hand over
Join emptying thin or superfluous (B) to play a role at branch as soft segment, to become the reason of hardness reduces.
[(C) ingredient]
(C) curing agent (catalyst) that ingredient is made of organic peroxide, can make curability silicone of the invention
Resin combination hardens silicone rubber or resin is made.Promote acryloyl group and methacryl by addition (C) ingredient
The polymerization of base, to help to improve bonding force and gas barrier property.
As organic peroxide, it can be cited for example that, benzoyl peroxide, peroxidized t-butyl perbenzoate, peroxidating
O-methyl-benzene formyl, peroxidating are to toluyl, di-t-butyl peroxide, dicumyl peroxide, bis- (t-butyl peroxy of 1,1-
Base) -3,3,5- trimethyl-cyclohexane, 1,1- bis- (t-butylperoxy) hexamethylene, two (tert-butyl mistake of 2,5- dimethyl -2,5-
Oxygroup) hexane, 2,5- dimethyl -2,5 two (t-butylperoxy) hexin, 1,6- be bis- (to toluyl groups peroxy ketonic oxygen
Base) hexane, two (4- methyl benzoyl peroxy) hexa-methylene double manganese esters etc., list can be used in these organic peroxides
It is solely a kind of to use two kinds of combination of the above.
Especially preferably, (C) ingredient is the organic peroxide indicated by following formula (5).
(C) additive amount of ingredient is effective quantity (so-called catalytic amount), the organopolysiloxane relative to (A) ingredient
100 mass parts of total amount are 0.01~5 mass parts, preferably 0.05~3 mass parts of blending.
[(D) ingredient]
(D) ingredient is platinum group metal catalyst, can promote the hydrosilylation addition of (A) ingredient Yu (B) ingredient
Reaction.As the platinum group metal catalyst of (D) ingredient, as long as the fat with silicon atom bond in (A) ingredient can be promoted
The hydrosilylation addition reaction of SiH base in race's unsaturated group and (B) ingredient, can be used any catalyst, and can make
It also can be used together two kinds or more with independent one kind.
As (D) ingredient, it can be cited for example that following platinum group metal compounds：The platinums group metal such as platinum, palladium, rhodium；Alternatively, chlorine
The modified chloroplatinic acid of platinic acid, alcohol；The complex of chloroplatinic acid and olefines, vinylsiloxane or acetylide；Four (triphens
Base phosphine) palladium, three (triphenylphosphine) radium chlorides etc.；But especially preferably platinum compounds.
(D) blended amount of ingredient is the effective quantity as hydrosilylation catalysts, relative to (A) ingredient and (B) ingredient
Total quality, with the mass conversion of platinum group in the range of 0.1~1000ppm, preferably 1~500ppm's
In range.
[other compositions]
In curability silicone resin component of the invention, in order to assign desired property, can blend dyestuff, pigment,
The added materials such as fire retardant.For example, 2,6- bis- can be blended in order to inhibit coloring, gonorrhoea, oxidative degradation for being cured object etc.
Antioxidant well known to tert-butyl-4-methyl-Phenol etc..In addition, can blend and be obstructed to assign the resistance for light deterioration
Amine (hindered amine) is the light stabilizers such as stabilizer；In order to improve bonding force, it is (silane coupled bonding agent can be blended
Agent).
Further, as needed, in order to improve the intensity of solidfied material, point with aliphatic unsaturated group can be blended
The inorganic fillers such as branch shape organopolysiloxane and fumed silica.In addition, in order to ensure service life, can blend with
Lower addition reaction controlling agent：3- methyl-1-dodecyne-3- alcohol, 1- ethynylcyclohexanol, 3,5- dimethyl-1- hexin-3- alcohol
Deng.
In addition, the condition of cure about curability silicone resin component of the invention, there is no particular restriction, but usually excellent
It is selected as being set as the heating condition of 60~180 DEG C, 1~5 hour.
The present invention provides a kind of optical semiconductor sealing material, is by curability silicone resin component of the invention
It constitutes.Curability silicone resin component of the invention can obtain a kind of solidfied material, the solidfied material with light be installed partly lead
The adhesiveness of the substrate of volume elements part improves, and the curability silicone resin component can prevent the gold being formed on substrate
Belong to the corrosion of electrode, therefore the use of optical semiconductor sealing material can be suitable as.
In addition, the OTR oxygen transmission rate of the solidfied material for the 1mm thickness for solidifying composition of the invention and obtaining, preferably
1000cc/m2It is following.
In addition, the moisture-vapor transmission of the solidfied material for the 1mm thickness for solidifying composition of the invention and obtaining, preferably
12g/m2It is following.
If it is the solidfied material with such OTR oxygen transmission rate and moisture-vapor transmission, even if then LED lamp is exposed to
Among sulphur compound and exhaust gas in atmosphere etc., without the metal electrode for worrying to corrode with the time on substrate, especially
Silver electrode and make its blackening.
In addition, the present invention provides a kind of optical semiconductor device, which is characterized in that have optical semiconductor, with to close
Seal the solidfied material of the aforementioned optical semiconductor sealing material of the optical semiconductor.This optical semiconductor device has used this
The optical semiconductor sealing material of invention can become the optical semiconductor device of high reliablity.
In addition, curability silicone resin component of the invention can obtain a kind of solidfied material that the transparency is high.With quilt
The optical semiconductor device of the optical semiconductors such as LED of the high solidfied material sealing of this transparency, can will be by photosemiconductor member
The light efficiency that part issues is directed to outside well.
[embodiment]
Hereinafter, showing embodiment and comparative example, to specifically describe the present invention, but the present invention is not limited to following implementations
Example.
(embodiment 1)
Equably mix the organopolysiloxane indicated as 100 mass parts of (A) ingredient of the invention by above-mentioned formula (3)
(viscosity 1500mPas), the organohydrogensiloxanes that are indicated by above-mentioned formula (4) of 25 mass parts as (B) ingredient of the invention
Compound and 0.1 mass parts ethynylmethyl decyl carbitol as addition reaction controlling agent.(in addition, in above-mentioned composition
{ total amount of the SiH radix of (B) ingredient }/{ total amount of the aliphatic unsaturation bond number of (A) ingredient } molar ratio be 0.9.)
In this regard, mixing following component to obtain composition：0.4 mass parts 1,1-, bis- (uncle as (C) ingredient of the invention
Butyl peroxy) hexamethylene；It is in such a way that platinum content becomes 1 mass % using by following formula as (D) ingredient of the invention
(6) organopolysiloxane indicated is by the complexing of chloroplatinic acid and 1,3- divinyl -1,1,3,3- tetramethyl disiloxane
Object is diluted and is obtained, and the amount of (D) ingredient is the total quality relative to (A), (B) ingredient, is become with the mass conversion of platinum
The amount of 10ppm.The physical property of this composition is as shown in table 1.
(in formula (6), putting in order for each siloxane unit is arbitrary)
(embodiment 2)
Equably mix the organic poly- silicon oxygen indicated as 100 mass parts of (A) ingredient of the invention by above-mentioned formula (3)
Alkane, as the organohydrogensiloxanes compound that is indicated by above-mentioned formula (4) of 12 mass parts of (B) ingredient of the invention and 20 mass
Part organohydrogensiloxanes compound indicated by following formula (7) (molar ratio of formula (4) and (7) is 1.0) and as addition reaction
0.1 mass parts ethynylmethyl decyl carbitol of controlling agent.(in addition, in above-mentioned composition { the SiH radix of (B) ingredient
Total amount }/the molar ratio of { total amount of the aliphatic unsaturation bond number of (A) ingredient } is 0.9.)
In this regard, mixing following component to obtain composition：0.4 mass parts 1,1-, bis- (uncle as (C) ingredient of the invention
Butyl peroxy) hexamethylene；It is in such a way that platinum content becomes 1 mass % using by above-mentioned formula as (D) ingredient of the invention
(6) organopolysiloxane indicated is by the complexing of chloroplatinic acid and 1,3- divinyl -1,1,3,3- tetramethyl disiloxane
Object is diluted and is obtained, and the amount of (D) ingredient is the total quality relative to (A), (B) ingredient, is become with the mass conversion of platinum
The amount of 10ppm.The physical property of this composition is as shown in table 1.
(embodiment 3)
Equably mix the organopolysiloxane indicated as 100 mass parts of (A) ingredient of the invention by following formula (8)
(viscosity 700mPas), the organohydrogensiloxanes that are indicated by above-mentioned formula (4) of 30 mass parts as (B) ingredient of the invention
Compound and 0.1 mass parts ethynylmethyl decyl carbitol as addition reaction controlling agent.(in addition, in above-mentioned composition
{ total amount of the SiH radix of (B) ingredient }/{ total amount of the aliphatic unsaturation bond number of (A) ingredient } molar ratio be 0.9.)
In this regard, mixing following component to obtain composition：0.8 mass parts 1,1-, bis- (uncle as (C) ingredient of the invention
Butyl peroxy) hexamethylene；It is in such a way that platinum content becomes 1 mass % using by above-mentioned formula as (D) ingredient of the invention
(6) organopolysiloxane indicated is by the complexing of chloroplatinic acid and 1,3- divinyl -1,1,3,3- tetramethyl disiloxane
Object is diluted and is obtained, and the amount of (D) ingredient is the total quality relative to (A), (B) ingredient, is become with the mass conversion of platinum
The amount of 10ppm.The physical property of this composition is as shown in table 1.
(embodiment 4)
Equably mix the organopolysiloxane indicated as 100 mass parts of (A) ingredient of the invention by following formula (9)
(viscosity 2000mPas), the organohydrogensilicon oxygen that is indicated by above-mentioned formula (4) of 20.9 mass parts as (B) ingredient of the invention
Hydride compounds and 0.1 mass parts ethynylmethyl decyl carbitol as addition reaction controlling agent.(in addition, above-mentioned composition
In { total amount of the SiH radix of (B) ingredient }/{ total amount of the aliphatic unsaturation bond number of (A) ingredient } molar ratio be 0.9.)
In this regard, mixing following component to obtain composition：0.8 mass parts 1,1-, bis- (uncle as (C) ingredient of the invention
Butyl peroxy) hexamethylene；It is in such a way that platinum content becomes 1 mass % using by above-mentioned formula as (D) ingredient of the invention
(6) organopolysiloxane indicated is by the complexing of chloroplatinic acid and 1,3- divinyl -1,1,3,3- tetramethyl disiloxane
Object is diluted and is obtained, and the amount of (D) ingredient is the total quality relative to (A), (B) ingredient, is become with the mass conversion of platinum
The amount of 10ppm.The physical property of this composition is as shown in table 1.
(comparative example 1)
Composition is obtained using method same as Example 1 other than not adding (C) ingredient for embodiment 1.
The physical property of this composition is as shown in table 1.
(comparative example 2)
Equably mix as (A) ingredient 100 mass parts indicated by following formula (3) organopolysiloxane, instead of (B)
Organohydrogensiloxanes compound that 22 mass parts of ingredient are indicated by following formula (10) and as the 0.1 of addition reaction controlling agent
Mass parts ethynylmethyl decyl carbitol.(in addition, { by the SiH base for the organohydrogensiloxanes compound that following formula (10) indicate
Several total amounts }/the molar ratio of { total amount of the aliphatic unsaturation bond number of (A) ingredient } is 0.9.)
In this regard, mixing following component to obtain composition：0.8 mass parts 1,1-, bis- (t-butyl peroxy as (C) ingredient
Base) hexamethylene；It is to indicate organic poly- using by following formula (10) in such a way that platinum content becomes 1 mass % as (D) ingredient
By chloroplatinic acid and 1, the complex compound of 3- divinyl -1,1,3,3- tetramethyl disiloxanes is diluted and is obtained siloxanes, described
(D) amount of ingredient is the total quality relative to (A) ingredient and the organopolysiloxane indicated by following formula (10), with the matter of platinum
Amount conversion becomes the amount of 10ppm.The physical property of this composition is as shown in table 1.
(comparative example 3)
(viscosity is the organopolysiloxane that equably mixing replaces 74 mass parts of (A) ingredient to be indicated by following formula (11)
5000mPas) and 26 mass parts indicated by following average formulas (12) silicone resin, as 4.8 mass parts of (B) ingredient
By the organohydrogensiloxanes compound of above-mentioned formula (4) expression and as 0.1 mass parts ethynylmethyl of addition reaction controlling agent
Decyl carbitol.(in addition, { total amount of the SiH radix of (B) ingredient }/organopolysiloxane that indicated by following formula (11) and
By following average formulas (12) indicate silicone resin aliphatic unsaturation bond number total amount molar ratio be 0.9.)
In this regard, mixing following component to obtain composition：0.8 mass parts 1,1-, bis- (t-butyl peroxy as (C) ingredient
Base) hexamethylene；It is to indicate organic poly- using by following formula (13) in such a way that platinum content becomes 1 mass % as (D) ingredient
By chloroplatinic acid and 1, the complex compound of 3- divinyl -1,1,3,3- tetramethyl disiloxanes is diluted and is obtained siloxanes, described
(D) amount of ingredient is relative to the organopolysiloxane indicated by following formula (11), the silicone indicated by following average formulas (12)
The total quality of resin and (B) ingredient becomes the amount of 10ppm with the mass conversion of platinum.The physical property of this composition is as shown in table 1.
(comparative example 4)
(viscosity is the organopolysiloxane that equably mixing replaces 100 mass parts of (A) ingredient to be indicated by above-mentioned formula (6)
700mPas), the organohydrogensiloxanes compound that is indicated by above-mentioned formula (4) as 6.3 mass parts of (B) ingredient and as adding
At 0.1 mass parts ethynylmethyl decyl carbitol of reaction controlling agent.(in addition, { total amount of the SiH radix of (B) ingredient }/
The molar ratio of { total amount of the aliphatic unsaturation bond number of the organopolysiloxane indicated by above-mentioned formula (6) } is 0.9.)
In this regard, mixing following component to obtain composition：0.8 mass parts 1,1-, bis- (t-butyl peroxy as (C) ingredient
Base) hexamethylene；It is to indicate organic poly- using by above-mentioned formula (6) in such a way that platinum content becomes 1 mass % as (D) ingredient
By chloroplatinic acid and 1, the complex compound of 3- divinyl -1,1,3,3- tetramethyl disiloxanes is diluted and is obtained siloxanes, described
(D) amount of ingredient is the total quality relative to the organopolysiloxane and (B) ingredient that are indicated by above-mentioned formula (6), with the matter of platinum
Amount conversion becomes the amount of 10ppm.The physical property of this composition is as shown in table 1.
It carries out with the following methods, to evaluate the composition obtained in embodiment and comparative example, the results are shown in Table 1.In table 1
The characteristic shown is the value measured at 23 DEG C.
[appearance]
Visually to observe the appearance of each composition.
[refractive index]
The digital refractometer RX-9000 α manufactured using ATAGO company, come the wavelength of each composition when measuring 25 DEG C
The refractive index of 589nm.
[hardness]
Curability silicone resin component is heated 2 hours by the heated air circulation type baking oven using 150 DEG C, to make thickness
The solidfied material for spending 2mm makes manufactured D type hardness tester meter using upper island for the solidfied material, and comes according to JIS K6253
Measure hardness.
[adhesiveness (adhesive strength)]
Make adhesive test testing piece as shown in Figure 1.That is, with 2 piece aluminum oxide ceramic substrate, 11,12 (KDS corporation
Make, width 25mm × depth 50mm × thickness 1mm) end overlapping 10mm as clamp the curability obtained of 1mm thickness
The mode of silicone resin component carries out, and by being heated 2 hours with 150 DEG C, to make the curability silicone resin component
Solidification, and make by being cured property silicone resin component solidfied material 13 bonding (bond area be 25mm × 10mm=
250mm2) 2 piece aluminum oxide ceramic substrates constitute testing piece.Using cupping machine, (Shimadzu Seisakusho Ltd. is manufactured
AUTOGRAPH), with tensile speed 50mm/ minutes by the aluminium oxide ceramic substrate 11 of this testing piece, 12 respective ends toward phase
Opposite direction (arrow direction of Fig. 1) stretches, and finds out the adhesive strength (MPa) of per unit area.
[OTR oxygen transmission rate test]
Curability silicone resin component is heated 3 hours by the heated air circulation type baking oven using 150 DEG C, to make thickness
The solidfied material for spending 1mm, measure made solidfied material OTR oxygen transmission rate (manufacture of illinois instruments company
PARMEATION ANALYZER 8001)。
[moisture-vapor transmission test]
Curability silicone resin component is heated 3 hours by the heated air circulation type baking oven using 150 DEG C, to make thickness
The solidfied material for spending 1mm, measure made solidfied material moisture-vapor transmission (manufacture of SYSTECH illinois company
LYSSY L80-5000)。
[table 1]
By the Examples 1 to 4 of table 1 it is found that if using curability silicone resin component of the invention, confirming can
Obtain bonding force and the excellent solidfied material of gas barrier property.
On the other hand, it does not add the comparative example 1 of (C) ingredient, used without acryloxy or methacryl
The organohydrogensiloxanes compound of oxygroup come replace the comparative example 2 of (B) ingredient of the invention and used do not have be bonded to silicon original
In the straight-chain organopolysiloxane of aryl on son and the comparative example 3 of branch-like polysiloxanes, bonding force and gas barrier property are bright
It is aobvious poorer than embodiment.In addition, as a result gas barrier property is more worse than embodiment in the low comparative example 4 of the phenyl content of (A) ingredient.
In addition, the present invention is not limited to above-mentioned embodiments.Above embodiment is to illustrate, as long as having and this hair
The substantially identical composition of the technical idea recorded in bright claims and the technical solution for playing same function and effect, all
It is included in technical scope of the invention.
Claims (13)
1. a kind of curability silicone resin component, which is characterized in that contain following compositions：
(A) the straight-chain organopolysiloxane indicated by following formula (1),
R in formula (1)1Each independently represent the aliphatic unsaturated group of carbon atom number 2~10, R2It each independently represents not
With aliphatic unsaturated bond and the monovalent hydrocarbon of carbon atom number 1~12 that can be substituted with halogen atoms, R3Each independently
Indicate the alkyl of carbon atom number 1~8, R4The aryl of carbon atom number 6~10 is each independently represented, a and b are to meet a >=0, b >
0, the integer of b/ (a+b) >=0.5, and putting in order for each siloxane unit is arbitrary；
(B) the organohydrogensiloxanes compound indicated by following formula (2), and the amount of (B) ingredient is by { (B) ingredient
The total amount of SiH radix }/{ total amount of the aliphatic unsaturation bond number of (A) ingredient } indicate molar ratio become 0.2~5.0 amount,
In formula (2), R5Indicate hydrogen atom or methyl, R6Indicate the bivalent hydrocarbon radical of carbon atom number 1~12, R7It each independently represents
Without aliphatic unsaturated bond and the monovalent hydrocarbon of carbon atom number 1~12 that can be substituted with halogen atoms, n is in 0,1,2
Any one numerical value；
(C) organic peroxide, 100 mass parts of total amount relative to (A) ingredient are 0.01~5 mass parts；And
(D) platinum group metal catalyst, relative to the total quality of (A) ingredient and (B) ingredient, with the matter of platinum group
Amount is scaled 0.1~1000ppm.
2. curability silicone resin component as described in claim 1, wherein the R2And R7It is phenyl or methyl.
3. curability silicone resin component as described in claim 1, wherein (A) ingredient is indicated by following formula (3)
Organopolysiloxane,
4. curability silicone resin component as claimed in claim 2, wherein (A) ingredient is indicated by following formula (3)
Organopolysiloxane,
5. curability silicone resin component as described in claim 1, wherein (B) ingredient is indicated by following formula (4)
Organohydrogensiloxanes compound,
6. curability silicone resin component as claimed in claim 2, wherein (B) ingredient is indicated by following formula (4)
Organohydrogensiloxanes compound,
7. curability silicone resin component as claimed in claim 3, wherein (B) ingredient is indicated by following formula (4)
Organohydrogensiloxanes compound,
8. curability silicone resin component as claimed in claim 4, wherein (B) ingredient is indicated by following formula (4)
Organohydrogensiloxanes compound,
9. such as curability silicone resin component described in any item of the claim 1 to 8, wherein (C) ingredient is under
The organic peroxide of formula (5) expression is stated,
10. a kind of optical semiconductor sealing material is by curability silicone tree described in any item of the claim 1 to 8
Oil/fat composition is constituted.
11. a kind of optical semiconductor sealing material is by curability silicone resin component structure as claimed in claim 9
At.
12. a kind of optical semiconductor device, which is characterized in that there is optical semiconductor and to seal the photosemiconductor member
The solidfied material of the optical semiconductor sealing material described in any one of claim 10 of part.
13. a kind of optical semiconductor device, which is characterized in that there is optical semiconductor and to seal the photosemiconductor member
The solidfied material of optical semiconductor sealing material described in the claim 11 of part.
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| JP2017-094122 | 2017-05-10 | ||
| JP2017094122A JP6751370B2 (en) | 2017-05-10 | 2017-05-10 | Curable silicone resin composition, optical semiconductor element sealing material, and optical semiconductor device |
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| CN108864707A true CN108864707A (en) | 2018-11-23 |
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| JP (1) | JP6751370B2 (en) |
| KR (1) | KR102421335B1 (en) |
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| JP7296748B2 (en) * | 2019-03-08 | 2023-06-23 | 信越化学工業株式会社 | Resin composition for wafer-level optical semiconductor device, and optical semiconductor device |
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| JP6072663B2 (en) * | 2013-10-15 | 2017-02-01 | 信越化学工業株式会社 | An optical semiconductor device comprising a heat curable conductive silicone composition, a conductive adhesive comprising the composition, a conductive die bond material comprising the composition, and a cured product of the die bond material. |
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| KR101835941B1 (en) * | 2015-10-19 | 2018-03-08 | 삼성에스디아이 주식회사 | Composition for encapsulating organic light emitting diode device and organic light emitting diode display using prepared the same |
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- 2017-05-10 JP JP2017094122A patent/JP6751370B2/en active Active
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- 2018-05-04 KR KR1020180051642A patent/KR102421335B1/en active IP Right Grant
- 2018-05-08 CN CN201810433048.XA patent/CN108864707B/en active Active
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| US4201808A (en) * | 1978-06-12 | 1980-05-06 | Union Carbide Corporation | Radiation curable silicone release compositions |
| US4675346A (en) * | 1983-06-20 | 1987-06-23 | Loctite Corporation | UV curable silicone rubber compositions |
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| CN108864707B (en) | 2021-03-09 |
| KR102421335B1 (en) | 2022-07-18 |
| JP2018188585A (en) | 2018-11-29 |
| JP6751370B2 (en) | 2020-09-02 |
| TW201905092A (en) | 2019-02-01 |
| KR20180123973A (en) | 2018-11-20 |
| TWI752226B (en) | 2022-01-11 |
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