TWI621665B - 可硬化性聚矽氧組合物、其硬化產品、及光半導體裝置 - Google Patents
可硬化性聚矽氧組合物、其硬化產品、及光半導體裝置 Download PDFInfo
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- TWI621665B TWI621665B TW102138282A TW102138282A TWI621665B TW I621665 B TWI621665 B TW I621665B TW 102138282 A TW102138282 A TW 102138282A TW 102138282 A TW102138282 A TW 102138282A TW I621665 B TWI621665 B TW I621665B
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 97
- 239000000203 mixture Substances 0.000 title claims abstract description 87
- 230000003287 optical effect Effects 0.000 title claims description 34
- 239000004065 semiconductor Substances 0.000 title claims description 33
- -1 polysiloxane Polymers 0.000 claims abstract description 148
- 125000003342 alkenyl group Chemical group 0.000 claims abstract description 29
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 27
- ZQTYRTSKQFQYPQ-UHFFFAOYSA-N trisiloxane Chemical compound [SiH3]O[SiH2]O[SiH3] ZQTYRTSKQFQYPQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006459 hydrosilylation reaction Methods 0.000 claims abstract description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 25
- 125000003118 aryl group Chemical group 0.000 claims description 16
- 125000003710 aryl alkyl group Chemical group 0.000 claims description 15
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 9
- 125000001624 naphthyl group Chemical group 0.000 claims description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims 1
- 230000035699 permeability Effects 0.000 abstract description 18
- 230000009257 reactivity Effects 0.000 abstract description 5
- 239000007809 chemical reaction catalyst Substances 0.000 abstract description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 34
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical group [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 28
- 239000000126 substance Substances 0.000 description 27
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 20
- 125000003545 alkoxy group Chemical group 0.000 description 14
- 229910000077 silane Inorganic materials 0.000 description 14
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 14
- 229920002554 vinyl polymer Polymers 0.000 description 13
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 229910052697 platinum Inorganic materials 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 8
- 230000020169 heat generation Effects 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 7
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
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- 238000006243 chemical reaction Methods 0.000 description 6
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- 125000005843 halogen group Chemical group 0.000 description 6
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- 229910052710 silicon Inorganic materials 0.000 description 6
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- 239000003795 chemical substances by application Substances 0.000 description 5
- 229910052801 chlorine Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
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- 125000003944 tolyl group Chemical group 0.000 description 5
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 description 4
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 4
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 4
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- 229910004283 SiO 4 Inorganic materials 0.000 description 4
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- 230000000052 comparative effect Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 125000004122 cyclic group Chemical group 0.000 description 4
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
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- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
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- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 3
- 229910052794 bromium Inorganic materials 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 3
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 125000000962 organic group Chemical group 0.000 description 3
- 125000005561 phenanthryl group Chemical group 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 150000004756 silanes Chemical class 0.000 description 3
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- RWNUSVWFHDHRCJ-UHFFFAOYSA-N 1-butoxypropan-2-ol Chemical compound CCCCOCC(C)O RWNUSVWFHDHRCJ-UHFFFAOYSA-N 0.000 description 2
- RMZNKGBPQWTSFN-UHFFFAOYSA-N 2,2-diphenylethoxy(methyl)silane Chemical compound C[SiH2]OCC(C1=CC=CC=C1)C1=CC=CC=C1 RMZNKGBPQWTSFN-UHFFFAOYSA-N 0.000 description 2
- 125000000094 2-phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
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- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
- 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 2
- BYLOHCRAPOSXLY-UHFFFAOYSA-N dichloro(diethyl)silane Chemical compound CC[Si](Cl)(Cl)CC BYLOHCRAPOSXLY-UHFFFAOYSA-N 0.000 description 2
- ZZNQQQWFKKTOSD-UHFFFAOYSA-N diethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OCC)(OCC)C1=CC=CC=C1 ZZNQQQWFKKTOSD-UHFFFAOYSA-N 0.000 description 2
- MNFGEHQPOWJJBH-UHFFFAOYSA-N diethoxy-methyl-phenylsilane Chemical compound CCO[Si](C)(OCC)C1=CC=CC=C1 MNFGEHQPOWJJBH-UHFFFAOYSA-N 0.000 description 2
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- 125000003438 dodecyl 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])C([H])([H])C([H])([H])* 0.000 description 2
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- URZLRFGTFVPFDW-UHFFFAOYSA-N ethenyl-diethoxy-phenylsilane Chemical compound CCO[Si](OCC)(C=C)C1=CC=CC=C1 URZLRFGTFVPFDW-UHFFFAOYSA-N 0.000 description 2
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- 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
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- 150000004767 nitrides Chemical class 0.000 description 2
- 125000005187 nonenyl group Chemical group C(=CCCCCCCC)* 0.000 description 2
- 125000001400 nonyl 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])C([H])([H])[H] 0.000 description 2
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- 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 2
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- 125000005023 xylyl group Chemical group 0.000 description 2
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 description 1
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- 239000005055 methyl trichlorosilane Substances 0.000 description 1
- SKYCLDLCBIETAK-UHFFFAOYSA-N methyl(3-phenylprop-2-enoxy)silane Chemical compound C[SiH2]OCC=CC1=CC=CC=C1 SKYCLDLCBIETAK-UHFFFAOYSA-N 0.000 description 1
- GWHRHHNARBBJCU-UHFFFAOYSA-N methyl(4-phenylbut-3-enoxy)silane Chemical compound C[SiH2]OCCC=CC1=CC=CC=C1 GWHRHHNARBBJCU-UHFFFAOYSA-N 0.000 description 1
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000005054 phenyltrichlorosilane Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 239000003223 protective agent Substances 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
- 150000003839 salts Chemical class 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 125000005372 silanol group Chemical class 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- RSNQKPMXXVDJFG-UHFFFAOYSA-N tetrasiloxane Chemical compound [SiH3]O[SiH2]O[SiH2]O[SiH3] RSNQKPMXXVDJFG-UHFFFAOYSA-N 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical compound Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- FCVNATXRSJMIDT-UHFFFAOYSA-N trihydroxy(phenyl)silane Chemical compound O[Si](O)(O)C1=CC=CC=C1 FCVNATXRSJMIDT-UHFFFAOYSA-N 0.000 description 1
- JPMBLOQPQSYOMC-UHFFFAOYSA-N trimethoxy(3-methoxypropyl)silane Chemical compound COCCC[Si](OC)(OC)OC JPMBLOQPQSYOMC-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- AAPLIUHOKVUFCC-UHFFFAOYSA-N trimethylsilanol Chemical compound C[Si](C)(C)O AAPLIUHOKVUFCC-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
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- 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
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- C09D183/00—Coating compositions based on 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; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- 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
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- 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
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- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/31—Structure, shape, material or disposition of the layer connectors after the connecting process
- H01L2224/32—Structure, shape, material or disposition of the layer connectors after the connecting process of an individual layer connector
- H01L2224/321—Disposition
- H01L2224/32151—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
- H01L2224/32221—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
- H01L2224/32245—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic
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- H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
- H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
- H01L2224/481—Disposition
- H01L2224/48151—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
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Abstract
本發明係關於一種可硬化性聚矽氧組合物,其包含:(A)由特定平均單元式表示且一分子中具有至少兩個烯基的有機聚矽氧烷;(B)一分子中具有至少兩個烯基且不含任何矽鍵結氫原子之可選直鏈有機聚矽氧烷;(C)一分子中具有至少兩個矽鍵結氫原子之有機聚矽氧烷,其中至少80質量%的此組分包含由式H(CH3)2SiO(C6H5)2SiOSi(CH3)2H表示的有機三矽氧烷;及(D)氫矽化反應觸媒。該可硬化性聚矽氧組合物具有極佳可加工性及高反應性並形成具有低透氣性之硬化產品。
Description
本發明係關於一種可硬化性聚矽氧組合物、藉由使該組合物硬化所形成之硬化產品、及使用該組合物製得之光學半導體裝置。
本發明主張於2012年10月24日申請之日本專利申請案第2012-235184號之優先權,該案之內容以引用之方式併入本文中。
可硬化性聚矽氧組合物係用作光學半導體裝置(例如發光二極體(LED))中之光學半導體元件之密封材料或保護性塗料。然而,由於可硬化性聚矽氧組合物之硬化產品之透氣性較高,因此,當用於具有高光學強度及大量熱生成之高亮度LED中時,會出現例如因腐蝕性氣體所引起的密封材料褪色及因LED基板上的銀板腐蝕所引起的亮度降低問題。
因此,日本未審查專利申請公開案第2012-052045號提出一種包含具有甲基苯基乙烯基矽氧烷單元之分支鏈有機聚矽氧烷、有機氫聚矽氧烷及加成反應觸媒之可硬化性聚矽氧組合物,該可硬化性聚矽氧組合物可形成具有低透氣性之硬化產品。
然而,該可硬化性聚矽氧組合物具有高黏度、較差可加工性及低硬化反應速率(此導致完成該硬化反應需要大量時間及能量的問題)。
本發明之目標係提供一種具有極佳可加工性及高反應性並形成
具有低透氣性之硬化產品之可硬化性聚矽氧組合物。本發明之另一目標係提供一種具有低透氣性之硬化產品及另外關於提供一種具有極佳可靠性之光學半導體裝置。
本發明之可硬化性聚矽氧組合物包含:(A)一分子中具有至少兩個烯基且由以下平均單元式表示之有機聚矽氧烷:(R1R2R3SiO1/2)a(R4 2SiO2/2)b(R2SiO3/2)c
其中,R1係具有1至12個碳之烷基;R2係具有6至20個碳之相同或不同芳基或具有7至20個碳之芳烷基;R3係具有2至12個碳之烯基;R4係具有1至12個碳之相同或不同烷基、具有2至12個碳之烯基或苯基;且「a」、「b」及「c」分別係滿足0.01a0.5、0b0.7、0.1c<0.9且a+b+c=1的數值;(B)一分子中具有至少兩個烯基且不含任何矽鍵結氫原子的直鏈有機聚矽氧烷,其佔該組合物之0至70質量%;(C)一分子中具有至少兩個矽鍵結氫原子之有機聚矽氧烷,且至少80質量%的此組分包含由下式表示的有機三矽氧烷:H(CH3)2SiO(C6H5)2SiOSi(CH3)2H,其含量為此組分中矽鍵結氫原子的含量為0.1至5mol/組分(A)及(B)中之1mol總烯基;及(D)有效量的氫矽化反應觸媒。
本發明之硬化產品係藉由使前述可硬化性聚矽氧組合物硬化來形成。
本發明之光學半導體裝置係藉由使用上述可硬化性聚矽氧組合物之硬化產品密封光學半導體元件來製造。
本發明之效應
本發明之可硬化性聚矽氧組合物之特徵係具有極佳可加工性及高反應性並形成具有低透氣性之硬化產品。另外,本發明之硬化產品之特徵在於透氣性較低。本發明之光學半導體裝置之特徵在於具有極佳可靠性。
1‧‧‧光學半導體元件
2‧‧‧鉛框架
3‧‧‧鉛框架
4‧‧‧接線
5‧‧‧框架材料
6‧‧‧該可硬化性聚矽氧組合物之硬化產品
圖1係本發明之光學半導體裝置之實例LED之橫截面視圖。
首先,將詳細描述本發明之可硬化性聚矽氧組合物。
用於組分(A)(其係此組合物之主要組分)之有機聚矽氧烷係由以下平均單元式表示且一分子中具有至少兩個烯基:(R1R2R3SiO1/2)a(R4 2SiO2/2)b(R2SiO3/2)c。
在該式中,R1係具有1至12個碳之烷基,其實例包括甲基、乙基、丙基、丁基、戊基、己基、庚基、辛基、壬基、癸基、十一烷基及十二烷基,且在此等基團中,以甲基較佳。R2係具有6至20個碳之相同或不同芳基或具有7至20個碳之芳烷基。R2之芳基實例包括苯基、甲苯基、二甲苯基、萘基、蒽基、菲基、芘基及其中此等芳基中之氫原子經烷基(例如甲基及乙基)、烷氧基(例如甲氧基及乙氧基)或鹵原子(例如氯原子及溴原子)取代之基團。在此等基團中,以苯基及萘基較佳。R2之芳烷基實例包括苄基、苯乙基、萘乙基、萘丙基、蒽乙基、菲乙基、芘乙基及其中此等芳烷基中之氫原子經烷基(例如甲基及乙基)、烷氧基(例如甲氧基及乙氧基)或鹵原子(例如氯原子及溴原子)取代之基團。另外,R3係具有2至12個碳之烯基,其實例包括乙烯基、烯丙基、丁烯基、戊烯基、己烯基、庚烯基、辛烯基、壬烯基、癸烯基、十一烯基及十二烯基,且在此等基團中,以乙烯基較佳。R4係具有1至12個碳之相同或不同烷基、具有2至12個碳之烯基、或苯基。R4之烷基實例包括針對R1所述的相同基團。R4之烯基實例包
括針對R3所述的相同基團。
另外,在該式中,「a」、「b」及「c」分別係滿足0.01a0.5、0b0.7、0.1c<0.9且a+b+c=1的數值,較佳係滿足0.05a0.5、0b0.5、0.4c<0.85且a+b+c=1的數值,且甚至更佳係滿足0.05a0.4、0b0.4、0.45c<0.8且a+b+c=1的數值。原因在於:當「a」大於或等於上述範圍之下限時,該硬化產品之透氣性降低,且當「a」小於或等於上述範圍之上限時,該硬化產品具有足夠的強度。原因亦在於:當「b」小於或等於上述範圍之上限時,該硬化產品之硬度係有利且可靠性提高。原因亦在於:當「c」大於或等於上述範圍之下限時,該硬化產品之折射率係有利,且當「c」小於或等於上述範圍之上限時,該硬化產品之機械特徵改良。
用於組分(A)之有機聚矽氧烷係由上述平均單元式表示,但其亦可具有位於不減損本發明之目標之範圍內的由式R1 3SiO1/2表示的矽氧烷單元、由式R1R2 2SiO1/2表示的矽氧烷單元、由式R1 2R2SiO1/2表示的矽氧烷單元、由式R1R3 2SiO1/2表示的矽氧烷單元、由式R1SiO3/2表示的矽氧烷單元或由式SiO4/2表示的矽氧烷單元。在該等式中,R1係具有1至12個碳之烷基,且其實例與上述基團相同。此外,在該等式中,R2係具有6至20個碳之芳基或具有7至20個碳之芳烷基,且其實例與上述基團相同。在該等式中,R3係具有2至12個碳之烯基,且其實例與上述基團相同。該有機聚矽氧烷亦可具有位於不減損本發明之目標之範圍內的矽鍵結烷氧基(例如甲氧基、乙氧基及丙氧基)或矽鍵結羥基。
一種製備該有機聚矽氧烷之方法之實例,係一種在酸或鹼之存在下使由以下通式(I):R2SiX3表示的矽烷化合物、由以下通式(II-1):R1R2R3SiOSiR1R2R3表示的二矽氧烷及/或由以下通式(II-2):R1R2R3SiX表示的矽烷化合物水解/縮合的方法。
由以下通式(I)R2SiX3表示的矽烷化合物係用於將式R2SiO3/2表示的矽氧烷單元引入該有機聚矽氧烷中之原料。在該等式中,R2係具有6至20個碳之芳基或具有7至20個碳之芳烷基,其實例與上述基團相同。在此等基團中,以苯基或萘基較佳。此外,在該等式中,X係烷氧基、醯氧基、鹵原子或羥基。X之烷氧基實例包括甲氧基、乙氧基及丙氧基。X之醯氧基實例包括乙醯氧基。X之鹵原子實例包括氯原子及溴原子。
該矽烷化合物之實例包括烷氧基矽烷(例如,苯基三甲氧基矽烷、萘基三甲氧基矽烷、蒽基三甲氧基矽烷、菲基三甲氧基矽烷、芘基三甲氧基矽烷、苯基三乙氧基矽烷、萘基三乙氧基矽烷、蒽基三乙氧基矽烷、菲基三乙氧基矽烷及芘基三乙氧基矽烷);醯氧基矽烷(例如,苯基三乙醯氧基矽烷、萘基三乙醯氧基矽烷、蒽基三乙醯氧基矽烷、菲基三乙醯氧基矽烷及芘基三乙醯氧基矽烷);鹵代矽烷(例如,苯基三氯矽烷、萘基三氯矽烷、蒽基三氯矽烷、菲基三氯矽烷及芘基三氯矽烷);及羥基矽烷(例如,苯基三羥基矽烷、萘基三羥基矽烷、蒽基三羥基矽烷、菲基三羥基矽烷及芘基三羥基矽烷)。
由以下通式(II-1)R1R2R3SiOSiR1R2R3表示的二矽氧烷係用於將式R1R2R3SiO1/2表示的矽氧烷單元引入該有機聚矽氧烷中之原料。在該等式中,R1係具有1至12個碳之烷基,其實例與上述基團相同,且在此等基團中,以甲基較佳。此外,在該等式中,R2係具有6至20個碳之芳基或具有7至20個碳之芳烷基,其實例與上述基團相同,且在此等基團中,以苯基或萘基較佳。在該等式中,R3係具有2至12個碳之烯基,其實例與上述基團相同,且在此等基團中,以乙烯基較佳。
該二矽氧烷之一實例係1,3-二乙烯基-1,3-二苯基-1,3-二甲基二矽氧烷。
由以下通式(II-2)R1R2R3SiX表示的矽烷化合物亦係用於將式
R1R2R3SiO1/2表示的矽氧烷單元引入該有機聚矽氧烷中之原料。在該等式中,R1係具有1至12個碳之烷基,其實例與上述基團相同,且在此等基團中,以甲基較佳。此外,在該等式中,R2係具有6至20個碳之芳基或具有7至20個碳之芳烷基,其實例與上述基團相同,且以苯基或萘基較佳。在該等式中,R3係具有2至12個碳之烯基,其實例與上述基團相同,且在此等基團中,以乙烯基較佳。此外,在該等式中,X係烷氧基、醯氧基、鹵原子或羥基;且其實例與上述基團相同。
該矽烷化合物之實例包括烷氧基矽烷(例如,甲基苯基乙烯基甲氧基矽烷及甲基苯基乙烯基乙氧基矽烷)、乙醯氧基矽烷(例如甲基苯基乙烯基乙醯氧基矽烷)、氯矽烷(例如甲基苯基乙烯基氯矽烷)及羥基矽烷(例如甲基苯基乙烯基羥基矽烷)。
在上述製法中,若必要,則可使用於引入式R4 2SiO2/2表示的矽氧烷單元之矽烷化合物或環狀聚矽氧化合物、用於引入式R1 3SiO1/2表示的矽氧烷單元、式R1R2 2SiO1/2表示的矽氧烷單元、式R1 2R2SiO1/2表示的矽氧烷單元、式R1R3 2SiO1/2表示的矽氧烷單元、式R1SiO3/2表示的矽氧烷單元或式SiO4/2表示的矽氧烷單元之矽烷化合物或矽烷寡聚物與該有機聚矽氧烷反應。在該等式中,R1係具有1至12個碳之烷基,且其實例與上述基團相同。此外,在該等式中,R2係具有6至20個碳之芳基或具有7至20個碳之芳烷基,且其實例與上述基團相同。在該等式中,R3係具有2至12個碳之烯基,且其實例與上述基團相同。在該等式中,R4係具有1至12個碳之相同或不同烷基、具有2至12個碳之烯基、或苯基,且其實例與上述基團相同。
該矽烷化合物之實例包括烷氧基矽烷(例如,二甲基二甲氧基矽烷、二甲基二乙氧基矽烷、二乙基二甲氧基矽烷、二乙基二乙氧基矽烷、甲基苯基二甲氧基矽烷、甲基苯基二乙氧基矽烷、二苯基二甲氧
基矽烷、二苯基二乙氧基矽烷、甲基乙烯基二甲氧基矽烷、甲基乙烯基二乙氧基矽烷、苯基乙烯基二甲氧基矽烷、苯基乙烯基二乙氧基矽烷、三甲基甲氧基矽烷、三甲基乙氧基矽烷、甲基二苯基甲氧基矽烷、甲基二苯基乙氧基矽烷、甲基三甲氧基矽烷、四甲氧基矽烷及四乙氧基矽烷);乙醯氧基矽烷(例如,二甲基二乙醯氧基矽烷、甲基苯基二乙醯氧基矽烷、二苯基二乙醯氧基矽烷、甲基乙烯基二乙醯氧基矽烷、苯基乙烯基二乙醯氧基矽烷、三甲基乙醯氧基矽烷、甲基二苯基乙醯氧基矽烷、甲基三乙醯氧基矽烷及四乙醯氧基矽烷);鹵代矽烷(例如,二甲基二氯矽烷、二乙基二氯矽烷、甲基苯基二氯矽烷、二苯基二氯矽烷、甲基乙烯基二氯矽烷、苯基乙烯基二氯矽烷、三甲基氯矽烷、甲基二苯基氯矽烷、甲基三氯矽烷及四氯矽烷);及羥基矽烷(例如,二甲基二羥基矽烷、二乙基二羥基矽烷、甲基苯基二羥基矽烷、二苯基二羥基矽烷、甲基乙烯基二羥基矽烷、三甲基羥基矽烷、甲基二苯基羥基矽烷及甲基三羥基矽烷)。該環狀聚矽氧化合物之實例包括環狀二甲基矽氧烷寡聚物、環狀苯基甲基矽氧烷寡聚物及環狀二苯基矽氧烷寡聚物。此外,矽烷寡聚物之實例包括四甲氧基矽烷之部分水解產物及四乙氧基矽烷之部分水解產物。
上述製法之特徵係在酸或鹼之存在下使矽烷化合物(I)、二矽氧烷(II-1)及/或矽烷化合物(II-2)及(若需要)其他矽烷化合物、環狀聚矽氧化合物或矽烷寡聚物水解/縮合。
可使用的酸之實例係鹽酸、乙酸、甲酸、硝酸、草酸、硫酸、磷酸、聚磷酸、聚羧酸、三氟甲磺酸及離子交換樹脂。此外,所使用的鹼之實例係無機鹼(例如,氫氧化鉀、氫氧化鈉及類似物)及有機鹼化合物(例如,三乙胺、二乙胺、單乙醇胺、二乙醇胺、三乙醇胺、氨水、氫氧化四甲基銨、具有胺基之烷氧基矽烷、胺丙基三甲氧基矽烷及類似物)。
此外,該製法中可使用有機溶劑。所使用的有機溶劑之實例係醚、酮、乙酸酯、芳族或脂族烴及γ-丁內酯及該等溶劑中之兩種或更多種之混合物。較佳的有機溶劑之實例係丙二醇單甲醚、丙二醇單甲醚乙酸酯、丙二醇單乙醚、丙二醇單丙醚、丙二醇單丁醚、丙二醇單第三丁醚、γ-丁內酯、甲苯及二甲苯。
為加速該製法中各組分之水解及縮合反應,較佳添加水或水與醇的混合溶液。甲醇及乙醇係較佳的醇實例。藉由加熱促進該反應,且若使用有機溶劑,則該反應較佳係在有機溶劑之回流溫度下進行。
組分(B)(其係賦予該硬化產品柔軟性、延展性及可撓性的可選組分)係一分子中具有至少兩個烯基且不含任何矽鍵結氫原子的直鏈有機聚矽氧烷。組分(B)中的烯基實例包括具有2至12個碳之烯基(例如,乙烯基、烯丙基、丁烯基、戊烯基、己烯基、庚烯基、辛烯基、壬烯基、癸烯基、十一烯基及十二烯基)。在此等基團中,以乙烯基較佳。組分(B)中鍵結至矽原子之除烯基以外之基團之實例包括具有1至12個碳之烷基(例如,甲基、乙基、丙基、丁基、戊基、己基、庚基、辛基、壬基、癸基、十一烷基及十二烷基)、具有6至20個碳之芳基(例如,苯基、甲苯基、二甲苯基、萘基、蒽基、菲基、芘基及此等芳基中之氫原子經烷基(例如甲基及乙基)、烷氧基(例如甲氧基及乙氧基)或鹵原子(例如氯原子及溴原子)取代之基團)、具有7至20個碳之芳烷基(例如,苄基、苯乙基、萘乙基、萘丙基、蒽乙基、菲乙基、芘乙基及此等芳烷基中之氫原子經烷基(例如甲基及乙基)、烷氧基(例如甲氧基及乙氧基)或鹵原子(例如氯原子及溴原子)取代之基團)及具有1至12個碳之鹵化烷基(例如氯甲基及3,3,3-三氟丙基)。在此等基團中,以甲基及苯基較佳。
該組分(B)之實例包括二甲基矽氧烷與甲基乙烯基矽氧烷之分子兩端經三甲基矽氧基封端之共聚物;分子兩端經三甲基矽氧基封端之
甲基乙烯基聚矽氧烷;二甲基矽氧烷、甲基乙烯基矽氧烷與甲基苯基矽氧烷之分子兩端經三甲基矽氧基封端之共聚物;分子兩端經二甲基乙烯基矽氧基封端之二甲基聚矽氧烷;分子兩端經二甲基乙烯基矽氧基封端之甲基乙烯基聚矽氧烷;二甲基矽氧烷與甲基乙烯基矽氧烷之分子兩端經二甲基乙烯基矽氧基封端之共聚物;二甲基矽氧烷、甲基乙烯基矽氧烷與甲基苯基矽氧烷之分子兩端經二甲基乙烯基矽氧基封端之共聚物;及此等有機聚矽氧烷中之兩種或更多種之混合物。
組分(B)於此組合物中之含量係在相對於此組合物為0至70質量%,較佳0至50質量%及特別佳0至40質量%之間。原因在於:當組分(B)的含量小於或等於上述範圍之上限時,可賦予該硬化產品柔軟性、延展性及可撓性且不增加該硬化產品之透氣性,因此可提高使用此組合物製得之光學半導體裝置之可靠性。
組分(C)係本發明組合物之交聯劑且係一分子中具有至少2個矽鍵結氫原子之有機聚矽氧烷,且至少80質量%的此組分包含由下式H(CH3)2SiO(C6H5)2SiOSi(CH3)2H表示的有機三矽氧烷。
原因在於:當使用上述有機三矽氧烷作為交聯劑時,該化合物對上述組分(A)具有良好反應性,此可使該組合物快速硬化。另外,諸如上述有機三矽氧烷可降低該組合物之黏度並增強該組合物之可加工性。
組分(C)具有至少80質量%的上述有機三矽氧烷,且其他有機聚矽氧烷不受特定限制,只要其一分子中具有至少兩個矽鍵結氫原子即可。該有機聚矽氧烷可具有直鏈、分支鏈、環狀、網狀或具部分分支鏈之直鏈分子結構。此有機聚矽氧烷中之其他矽原子鍵結基團之實例包括具有1至12個碳之烷基、具有6至20個碳之芳基、具有7至20個碳之芳烷基及具有1至12個碳之鹵化烷基。此等基團之實例包括與彼等上述者相同的基團,且以甲基及苯基較佳。
其他有機聚矽氧烷之實例係分子兩端經三甲基矽氧基封端之甲基氫聚矽氧烷;二甲基矽氧烷與甲基氫矽氧烷之分子兩端經三甲基矽氧基封端之共聚物;二甲基矽氧烷、甲基氫矽氧烷與甲基苯基矽氧烷之分子兩端經三甲基矽氧基封端之共聚物;分子兩端經二甲基氫矽氧基封端之二甲基聚矽氧烷;二甲基矽氧烷與甲基苯基矽氧烷之分子兩端經二甲基氫矽氧基封端之共聚物;分子兩端經二甲基氫矽氧基封端之甲基苯基聚矽氧烷;由通式R'3SiO1/2表示之矽氧烷單元及通式R'2HSiO1/2表示之矽氧烷單元及式SiO4/2表示的矽氧烷單元組成之有機聚矽氧烷共聚物;由通式R'2HSiO1/2表示之矽氧烷單元及式SiO4/2表示的矽氧烷單元組成之有機聚矽氧烷共聚物;由通式R'HSiO2/2表示之矽氧烷單元及通式R'SiO3/2表示之矽氧烷單元或由式HSiO3/2表示的矽氧烷單元組成之有機聚矽氧烷共聚物;兩種或更多種該等有機聚矽氧烷之混合物。在該等式中,R'係具有1至12個碳之烷基、具有6至20個碳之芳基、具有7至20個碳之芳烷基或具有1至12個碳之鹵化烷基,且其實例與上述基團相同。
相對於組分(A)及(B)中之每1莫耳總烯基,組分(C)於本發明組合物中之含量係在使得組分(C)中的矽鍵結氫原子在0.1至5mol之間且較佳在0.5至2mol之間的範圍內。原因在於:當組分(C)的含量大於或等於上述範圍之下限時,該組合物充分地硬化,且當該含量小於或等於上述範圍之上限時,該硬化產品之耐熱性提高,因此可提高使用此組合物製得之光學半導體裝置之可靠性。
組分(D)係用於加速本發明組合物硬化之矽氫化反應觸媒,且實例包括鉑基觸媒、銠基觸媒及鈀基觸媒。特定言之,組分(D)較佳係鉑基觸媒,因此可顯著加速本發明組合物之硬化。鉑基觸媒之實例包括鉑細粉、氯鉑酸、氯鉑酸之醇溶液、鉑-烯基矽氧烷錯合物、鉑-烯烴錯合物及鉑-羰基錯合物,以鉑-烯基矽氧烷錯合物為較佳。
組分(D)於此組合物中之含量係用於加速該組合物硬化之有效量。明確言之,為可充分地加速此組合物之硬化反應,組分(D)之含量較佳係使得組分(D)中的觸媒金屬在相對於此組合物為0.01至500ppm,更佳0.01至100ppm且特別佳0.01至50ppm(以質量為單位)之間的含量。
此組合物亦可包含黏著賦予劑,以改良該硬化產品在硬化期間對與該組合物接觸的基板之黏著性。較佳的黏著賦予劑係一分子中具有至少一個鍵結至矽原子之烷氧基之有機矽化合物。此烷氧基之實例係甲氧基、乙氧基、丙氧基、丁氧基及甲氧乙氧基;且以甲氧基特別佳。此外,此有機矽化合物中鍵結至矽原子之非烷氧基之實例係經取代或未經取代之單價烴基(例如,烷基、烯基、芳基、芳烷基及鹵化烷基);含環氧基之單價有機基團(例如,3-縮水甘油氧基丙基、4-縮水甘油氧基丁基或類似縮水甘油氧基烷基;2-(3,4-環氧基環己基)乙基、3-(3,4-環氧基環己基)丙基或類似環氧基環己基烷基;或4-環氧乙烷基丁基、8-環氧乙烷基辛基或類似環氧乙烷基烷基);含丙烯基之單價有機基團(例如3-甲基丙烯醯氧基丙基)及氫原子。此有機矽化合物較佳具有矽鍵結烯基或矽鍵結氫原子。此外,由於此有機矽化合物針對各種類型的基板賦有良好黏著能力,因此其一分子中較佳具有至少一個含環氧基之單價有機基團。此種有機矽化合物之實例係有機矽烷化合物、有機矽氧烷寡聚物及矽酸烷酯。該有機矽氧烷寡聚物或矽酸烷酯之分子結構之實例係直鏈結構、具部分分支鏈之直鏈結構、分支鏈結構、環狀結構及網狀結構。以直鏈結構、分支鏈結構及網狀結構特別佳。此種有機矽化合物之實例係矽烷化合物(例如,3-縮水甘油氧基丙基三甲氧基矽烷、2-(3,4-環氧基環己基)乙基三甲氧基矽烷、3-甲基丙烯醯氧基丙基三甲氧基矽烷及類似物);一分子中具有至少一個矽鍵結烯基或矽鍵結氫原子及至少一個矽鍵結烷氧基之矽氧
烷化合物;一分子中具有至少一個矽鍵結烷氧基之矽烷化合物或矽氧烷化合物與一分子中具有至少一個矽鍵結羥基或至少一個矽鍵結烯基之矽氧烷化合物之混合物;及聚矽酸甲酯、聚矽酸乙酯及含環氧基之聚矽酸乙酯。該黏著賦予劑於此組合物中之含量不受特定限制,但較佳在相對總共100質量份上述組分(A)至(D)為0.01至10質量份之間。
可將反應抑制劑(例如,炔醇(例如2-甲基-3-丁炔-2-醇、3,5-二甲基-1-己炔-3-醇及2-苯基-3-丁炔-2-醇)、烯炔化合物(例如,3-甲基-3-戊烯-1-炔及3,5-二甲基-3-己烯-1-炔)或1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷、1,3,5,7-四甲基-1,3,5,7-四己烯基環四矽氧烷或苯并三唑)作為可選組分併入本發明組合物中。該反應抑制劑於此組合物中之含量不受特定限制,但較佳在相對於總共100質量份上述組分(A)至(D)為0.0001至5質量份之間。
此組合物亦可包含作為可選組分的螢光物質。此螢光物質的實例係廣泛用於發光二極體(LED)中之物質,例如發黃光、紅光、綠光及藍光的螢光物質(例如氧化物螢光物質、氧氮化物螢光物質、氮化物螢光物質、硫化物螢光物質、氧硫化物螢光物質及類似物)。氧化物螢光物質之實例包括含有鈰離子之釔鋁石榴石型(YAG)發綠光至發黃光螢光物質;含有鈰離子之鋱鋁石榴石型(TAG)發黃光螢光物質;及含有鈰或銪離子之矽酸鹽發綠光至發黃光螢光物質。氧氮化物螢光物質之實例包括含有銪離子之矽鋁氧氮型(SiAlON)發紅光至發綠光螢光物質。氮化物螢光物質之實例包括含有銪離子之鈣鍶鋁矽氮型(CASN)發紅光螢光物質。硫化物螢光物質之實例包括含有銅離子或鋁離子之ZnS發綠光螢光物質。氧硫化物螢光物質之實例包括含有銪離子之Y2O2S發紅光螢光物質。可以一種或兩種或更多種之混合物之形式使用此等螢光物質。該螢光物質於此組合物中之含量不受特定限制,但較佳在佔此組合物之0.1至70質量%及更佳1至20質量%之間。
此外,亦可將無機填充劑(例如矽石、玻璃、礬土、氧化鋅及類似物)、聚甲基丙烯酸酯樹脂及類似物之有機樹脂細粉、耐熱劑、染料、顏料、阻燃劑、溶劑及類似物作為可選組分以不減損本發明目標之含量併入本發明組合物中。
本發明組合物係使得在室溫下或在加熱下可發生硬化者,但較佳加熱該組合物以達成快速硬化。該加熱溫度較佳係50至200℃。
現將詳細描述本發明之硬化產品。
本發明之硬化產品係藉由使前述可硬化性聚矽氧組合物硬化而形成。該硬化產品之形狀不受特定限制,且實例包括薄片形及薄膜形。可以簡單物質形式處理該硬化產品或亦可以其中該硬化產品覆蓋或密封光學半導體元件或類似物的狀態進行處理。
現將詳細解釋本發明之光學半導體裝置。
本發明之光學半導體裝置係藉由使用上述可硬化性聚矽氧組合物之硬化產品密封光學半導體元件來製造。本發明之該光學半導體裝置之實例包括發光二極體(LED)、光耦合器及CCD。光學半導體元件之實例包括發光二極體(LED)晶片及固態影像感測裝置。
圖1顯示單一表面安裝型LED(其係本發明光學半導體裝置之一實例)之橫截面視圖。在圖1中所示的LED中,LED晶片1係晶粒黏接至鉛框架2,且該LED晶片1與鉛框架3係經接線4線接合。框架材料5係提供於此LED晶片1周圍,且位於該框架材料5內側的LED晶片1係經本發明之可硬化性聚矽氧組合物之硬化產品6密封。
圖1中所示之表面安裝型LED之製造方法之一實例係將LED晶片1晶粒黏接至鉛框架2,使用金色接線4線接合LED晶片1與鉛框架3,使用本發明之可硬化性聚矽氧組合物填充提供於LED晶片1周圍的框架材料5之內側,且隨後藉由於50至200℃下加熱使該組合物硬化的方法。
實例
在下文中,將使用實際實例詳細描述本發明之可硬化性聚矽氧組合物、其硬化產品及本發明之光學半導體裝置。該黏度係在25℃下的值。可硬化性聚矽氧組合物、其硬化產品及光學半導體裝置之特徵係測量如下。
[硬化性評估]
根據使用差示掃描量熱儀(DSC7000;由SII Nanotechnology Inc.製造)以10℃/min的加熱速率測得的生熱峰值溫度(℃)及當使用硫化儀(RHEOMETER MDR2000;由Alpha Technologies Co.,Ltd.製造)在150℃測量溫度及1°晶粒偏轉角下測量時達到1dNm扭矩值所需的時間(秒)來評估該可硬化性聚矽氧組合物的硬化速率。
[硬化產品之水蒸氣滲透率]
藉由使用壓力機使該可硬化性聚矽氧組合物於150℃下硬化2小時來製備1mm厚度的硬化薄膜。根據JIS Z0208之杯法於40℃溫度及90%相對濕度的條件下測量該硬化薄膜之水蒸氣滲透率。
[光學半導體裝置之可靠性]
藉由於150℃下加熱該可硬化性聚矽氧組合物2小時來製造圖1中所示之光學半導體裝置。使此光學半導體裝置在50℃溫度、75%相對濕度及20ppm的硫化氫氣體濃度的條件下經歷24小時曝露測試。藉由測量該光學半導體裝置在曝露測試前後的發光效率的變化來評估該光學半導體裝置之可靠性。
[合成實例1]
首先,將預先混合的400g(2.02mol)苯基三甲氧基矽烷及93.5g(0.30mol)1,3-二乙烯基-1,3-二苯基二甲基二矽氧烷裝入反應器中。接著,添加1.74g(11.6mmol)三氟甲磺酸,並添加110g(6.1mol)水並攪拌加熱預回流2小時。隨後,藉由於大氣壓下加熱蒸餾該混合物,
直至該混合物達到85℃。接著,添加89g甲苯及1.18g(21.1mmol)氫氧化鉀,之後,藉由於大氣壓下加熱蒸餾該混合物,直至該反應溫度達到120℃,使該混合物於此溫度下反應6小時。使該混合物冷卻至室溫,並藉由添加0.68g(11.4mmol)乙酸進行中和反應。藉由過濾移除所生成的鹽。藉由於真空下加熱以自所得透明溶液移除低沸點物質,以獲得347g(98%產率)無色透明膠狀黏性液體。
通過核磁共振光譜,觀察到此液體係由以下平均單元式表示之有機聚矽氧烷:[(CH3)(C6H5)CH2=CHSiO1/2]0.23(C6H5SiO3/2)0.77。
此有機聚矽氧烷之質量平均分子量(Mw)係1,617,且分散度(Mw/Mn)係1.16。
[實際實例1]
藉由混合77.9質量份合成實例1中製得的有機聚矽氧烷、21.9質量份由下式H(CH3)2SiO(C6H5)2SiOSi(CH3)2H表示之有機三矽氧烷(含量為此組分中的矽鍵結氫原子含量係1mol/上述有機聚矽氧烷中的1mol乙烯基)及0.2質量份鉑-1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷錯合物(包含0.1質量%的鉑)之1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷溶液來製備黏度為8,300mPa.s的可硬化性聚矽氧組合物。
此可硬化性聚矽氧組合物達到1dNm扭矩值所需的時間係36秒,且該DSC生熱峰值溫度係122℃。該硬化產品之水蒸氣滲透率係6.7g/m2.24h。
[實際實例2]
藉由混合64.7質量份合成實例1中製得之有機聚矽氧烷、15.2質量份具有3,000mPa.s黏度的分子兩端經二甲基乙烯基矽氧基封端之甲基苯基聚矽氧烷、20.0質量份由下式H(CH3)2SiO(C6H5)2SiOSi(CH3)2H表示之有機三矽氧烷(含量為此組分中的矽鍵結氫原子含量係1mol/上
述有機聚矽氧烷及甲基苯基聚矽氧烷中之1mol乙烯基)及0.2質量份鉑-1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷錯合物(包含0.1質量%鉑)之1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷溶液來製備黏度為4,300mPa.s的可硬化性聚矽氧組合物。
此可硬化性聚矽氧組合物達到1dNm扭矩值所需的時間係44秒,且該DSC生熱峰值溫度係120℃。該硬化產品之水蒸氣滲透率係7.8g/m2.24h。
[實際實例3]
藉由混合76.3質量份合成實例1中製得之有機聚矽氧烷、20.0質量份由下式H(CH3)2SiO(C6H5)2SiOSi(CH3)2H表示之有機三矽氧烷(含量為此組分中的矽鍵結氫原子含量係0.9mol/上述有機聚矽氧烷中之1mol乙烯基)、3.5質量份由以下平均式H(CH3)2SiO[(C6H5)2SiO]2.5Si(CH3)2H表示之有機聚矽氧烷(含量為此組分中的矽鍵結氫原子含量係0.1mol/上述有機聚矽氧烷中之1mol乙烯基)及0.2質量份鉑-1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷錯合物(包含0.1質量%鉑)之1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷溶液來製備黏度為11,500mPa.s的可硬化性聚矽氧組合物。
此可硬化性聚矽氧組合物達到1dNm扭矩值所需的時間係56秒,且該DSC生熱峰值溫度係122℃。該硬化產品之水蒸氣滲透率係6.5g/m2.24h。
[實際實例4]
藉由混合77.8質量份合成實例1中製得之有機聚矽氧烷、18.7質量份由下式H(CH3)2SiO(C6H5)2SiOSi(CH3)2H表示之有機聚矽氧烷(含量為此組分中的矽鍵結氫原子含量係0.72mol/上述有機聚矽氧烷中之1mol乙烯基)、3.3質量份由以下平均式(C6H5SiO3/2)0.4[(CH3)2HSiO1/2]0.6表示之有機三矽氧烷(含量為此組分中的矽鍵結氫原
子含量係0.28mol/上述有機聚矽氧烷中之1mol乙烯基)及0.2質量份鉑-1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷錯合物(包含0.1質量%鉑)之1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷溶液來製備黏度為10,600mPa.s的可硬化性聚矽氧組合物。
此可硬化性聚矽氧組合物達到1dNm扭矩值所需的時間係16秒,且該DSC生熱峰值溫度係110℃。該硬化產品之水蒸氣滲透率係6.6g/m2.24h。
[比較例1]
藉由混合65.2質量份合成實例1中製得之有機聚矽氧烷、34.8質量份由以下平均式H(CH3)2SiO[(C6H5)2SiO]2.5Si(CH3)2H表示之有機聚矽氧烷(含量為此組分中的矽鍵結氫原子含量係1mol/上述有機聚矽氧烷中之1mol乙烯基)及0.2質量份鉑-1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷錯合物(包含0.1質量%鉑)之1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷溶液來製備黏度為28,500mPa.s的可硬化性聚矽氧組合物。
此可硬化性聚矽氧組合物達到1dNm扭矩值所需的時間係166秒,且該DSC生熱峰值溫度係133℃。該硬化產品之水蒸氣滲透率係6.3g/m2.24h。
[比較例2]
藉由混合53.6質量份合成實例1中製得之有機聚矽氧烷、15.2質量份具有3,000mPa.s黏度的分子兩端經二甲基乙烯基矽氧基封端之甲基苯基聚矽氧烷、31.2質量份由以下平均式H(CH3)2SiO[(C6H5)2SiO]2.5Si(CH3)2H表示之有機聚矽氧烷(含量為此組分中的矽鍵結氫原子含量係1mol/上述有機聚矽氧烷及甲基苯基聚矽氧烷中之1mol乙烯基)及0.2質量份鉑-1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷錯合物(包含0.1質量%鉑)之1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷溶液來製備黏度為12,300mPa.s的可硬化性聚矽氧組合物。
此可硬化性聚矽氧組合物達到1dNm扭矩值所需的時間係211秒,且該DSC生熱峰值溫度係130℃。該硬化產品之水蒸氣滲透率係7.4g/m2.24h。
通過實際實例1與比較例1之比較及實際實例2與比較例2之比較,觀察到當使用由下式H(CH3)2SiO(C6H5)2SiOSi(CH3)2H表示之有機三矽氧烷作為交聯劑時,該可硬化性聚矽氧組合物之黏度下降且硬化速率上升。
[實際實例5]
使用實際實例1中製得之可硬化性聚矽氧組合物創造光學半導體裝置。當評估此光學半導體裝置之可靠性時,觀察到該光學半導體裝置於曝露測試前後之發光效率無變化。
工業適用性
本發明之可硬化性聚矽氧組合物可用作電氣/電子用途之黏著劑、灌封劑、保護劑、塗層劑或底部填充劑。特定言之,該可硬化性聚矽氧組合物具有極佳可加工性及高反應性且可形成具有低透氣性之硬化產品,因此該組合物適用作光學半導體裝置(例如發光二極體(LED))中之光學半導體元件之密封劑或保護性塗料。
Claims (4)
- 一種可硬化性聚矽氧組合物,其包含:(A)一分子中具有至少兩個烯基且由以下平均單元式表示之有機聚矽氧烷:(R1R2R3SiO1/2)a(R4 2SiO2/2)b(R2SiO3/2)c其中,R1係具有1至12個碳之烷基;R2係具有6至20個碳之相同或不同芳基或具有7至20個碳之芳烷基;R3係具有2至12個碳之烯基;R4係具有1至12個碳之相同或不同烷基、具有2至12個碳之烯基或苯基;且a、b及c分別係滿足0.01a0.5、0b0.7、0.1c<0.9且a+b+c=1的數值;(B)一分子中具有至少兩個烯基且不含任何矽鍵結氫原子的直鏈有機聚矽氧烷,其佔該組合物之0至70質量%;(C)一分子中具有至少兩個矽鍵結氫原子之有機聚矽氧烷,且至少80質量%的此組分包含由下式表示的有機三矽氧烷:H(CH3)2SiO(C6H5)2SiOSi(CH3)2H,其含量為此組分中矽鍵結氫原子的含量為0.1至5mol/組分(A)及(B)中之1mol總烯基;及(D)有效量的氫矽化反應觸媒。
- 如請求項1之可硬化性聚矽氧組合物,其中組分(A)中之R2係苯基或萘基。
- 一種硬化產品,其係藉由使請求項1或2中之可硬化性聚矽氧組合物硬化來製造。
- 一種光學半導體裝置,其中藉由如請求項1或2之可硬化性聚矽氧組合物之硬化產品來密封光學半導體元件。
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