CN1832120A - 制备半导体器件的方法 - Google Patents
制备半导体器件的方法 Download PDFInfo
- Publication number
- CN1832120A CN1832120A CNA2006100547790A CN200610054779A CN1832120A CN 1832120 A CN1832120 A CN 1832120A CN A2006100547790 A CNA2006100547790 A CN A2006100547790A CN 200610054779 A CN200610054779 A CN 200610054779A CN 1832120 A CN1832120 A CN 1832120A
- Authority
- CN
- China
- Prior art keywords
- univalence hydrocarbyl
- semiconductor device
- general formula
- carbon atom
- silane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 78
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 36
- 239000011347 resin Substances 0.000 claims abstract description 36
- 238000009832 plasma treatment Methods 0.000 claims abstract description 25
- 239000008393 encapsulating agent Substances 0.000 claims abstract description 11
- 125000004432 carbon atom Chemical group C* 0.000 claims description 55
- -1 silane compound Chemical class 0.000 claims description 45
- 239000000203 mixture Substances 0.000 claims description 44
- 229910000077 silane Inorganic materials 0.000 claims description 39
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 37
- 239000003054 catalyst Substances 0.000 claims description 29
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 26
- 229910052799 carbon Inorganic materials 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 19
- 239000001257 hydrogen Substances 0.000 claims description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims description 19
- 238000009833 condensation Methods 0.000 claims description 18
- 230000005494 condensation Effects 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 18
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical group CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 16
- 239000003085 diluting agent Substances 0.000 claims description 16
- 125000000962 organic group Chemical group 0.000 claims description 16
- 125000005375 organosiloxane group Chemical group 0.000 claims description 15
- 229910052786 argon Inorganic materials 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 229920002050 silicone resin Polymers 0.000 claims description 11
- 229920001296 polysiloxane Polymers 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 230000007062 hydrolysis Effects 0.000 claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- 230000003301 hydrolyzing effect Effects 0.000 claims description 8
- 239000007859 condensation product Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 239000004593 Epoxy Substances 0.000 claims description 6
- 239000003570 air Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229920001721 polyimide Polymers 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 239000004925 Acrylic resin Substances 0.000 claims description 3
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
- 239000009719 polyimide resin Substances 0.000 claims description 3
- 150000002118 epoxides Chemical class 0.000 claims 2
- 238000005538 encapsulation Methods 0.000 abstract description 6
- 238000011282 treatment Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 34
- 229920000647 polyepoxide Polymers 0.000 description 25
- 239000003822 epoxy resin Substances 0.000 description 22
- 238000004382 potting Methods 0.000 description 21
- 238000001723 curing Methods 0.000 description 15
- 238000012360 testing method Methods 0.000 description 15
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 15
- 150000002924 oxiranes Chemical class 0.000 description 11
- 239000011342 resin composition Substances 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 7
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical class OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 125000000217 alkyl group Chemical group 0.000 description 5
- ZZHNUBIHHLQNHX-UHFFFAOYSA-N butoxysilane Chemical class CCCCO[SiH3] ZZHNUBIHHLQNHX-UHFFFAOYSA-N 0.000 description 5
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 5
- 150000004756 silanes Chemical class 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 4
- 239000003963 antioxidant agent Substances 0.000 description 4
- 230000003078 antioxidant effect Effects 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 4
- 230000001678 irradiating effect Effects 0.000 description 4
- 238000006068 polycondensation reaction Methods 0.000 description 4
- 239000011241 protective layer Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- SJRJJKPEHAURKC-UHFFFAOYSA-N N-Methylmorpholine Chemical compound CN1CCOCC1 SJRJJKPEHAURKC-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 231100000989 no adverse effect Toxicity 0.000 description 3
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- LZMNXXQIQIHFGC-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propyl 2-methylprop-2-enoate Chemical compound CO[Si](C)(OC)CCCOC(=O)C(C)=C LZMNXXQIQIHFGC-UHFFFAOYSA-N 0.000 description 2
- URDOJQUSEUXVRP-UHFFFAOYSA-N 3-triethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CCO[Si](OCC)(OCC)CCCOC(=O)C(C)=C URDOJQUSEUXVRP-UHFFFAOYSA-N 0.000 description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 238000003848 UV Light-Curing Methods 0.000 description 2
- 238000007259 addition reaction Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 125000003710 aryl alkyl group Chemical group 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 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
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 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 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 2
- GAURFLBIDLSLQU-UHFFFAOYSA-N diethoxy(methyl)silicon Chemical compound CCO[Si](C)OCC GAURFLBIDLSLQU-UHFFFAOYSA-N 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 description 2
- 238000005227 gel permeation chromatography Methods 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
- 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
- 239000003112 inhibitor Substances 0.000 description 2
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
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- 125000005395 methacrylic acid group Chemical group 0.000 description 2
- 229940043265 methyl isobutyl ketone Drugs 0.000 description 2
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 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
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 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
- 239000003960 organic solvent Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 238000005382 thermal cycling Methods 0.000 description 2
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 2
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- GQEAMFCDHPUBGV-GRHBHMESSA-N (z)-but-2-enedioic acid;dibutyltin Chemical compound OC(=O)\C=C/C(O)=O.CCCC[Sn]CCCC GQEAMFCDHPUBGV-GRHBHMESSA-N 0.000 description 1
- OWRCNXZUPFZXOS-UHFFFAOYSA-N 1,3-diphenylguanidine Chemical compound C=1C=CC=CC=1NC(=N)NC1=CC=CC=C1 OWRCNXZUPFZXOS-UHFFFAOYSA-N 0.000 description 1
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
- GQHTUMJGOHRCHB-UHFFFAOYSA-N 2,3,4,6,7,8,9,10-octahydropyrimido[1,2-a]azepine Chemical compound C1CCCCN2CCCN=C21 GQHTUMJGOHRCHB-UHFFFAOYSA-N 0.000 description 1
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 description 1
- BMFMTNROJASFBW-UHFFFAOYSA-N 2-(furan-2-ylmethylsulfinyl)acetic acid Chemical compound OC(=O)CS(=O)CC1=CC=CO1 BMFMTNROJASFBW-UHFFFAOYSA-N 0.000 description 1
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 1
- ZRXHQNQYIKVKNQ-UHFFFAOYSA-N 2-ethylhexanoic acid;zinc Chemical compound [Zn].CCCCC(CC)C(O)=O ZRXHQNQYIKVKNQ-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- WGRZHLPEQDVPET-UHFFFAOYSA-N 2-methoxyethoxysilane Chemical compound COCCO[SiH3] WGRZHLPEQDVPET-UHFFFAOYSA-N 0.000 description 1
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- NRRZGBVXJLJFJM-UHFFFAOYSA-N 3,3-diacetyl-2,4-dioxopentanoic acid Chemical compound CC(=O)C(C(C)=O)(C(C)=O)C(=O)C(O)=O NRRZGBVXJLJFJM-UHFFFAOYSA-N 0.000 description 1
- BQQGVSONEPNPAB-UHFFFAOYSA-N 3-(diethoxymethylsilyl)propyl 2-methylprop-2-enoate Chemical compound CCOC(OCC)[SiH2]CCCOC(=O)C(C)=C BQQGVSONEPNPAB-UHFFFAOYSA-N 0.000 description 1
- JIGUICYYOYEXFS-UHFFFAOYSA-N 3-tert-butylbenzene-1,2-diol Chemical compound CC(C)(C)C1=CC=CC(O)=C1O JIGUICYYOYEXFS-UHFFFAOYSA-N 0.000 description 1
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 1
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 1
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- 241000566113 Branta sandvicensis Species 0.000 description 1
- PXJZCBUXFVZSLL-UHFFFAOYSA-N CO[SiH2]OC.C=CC Chemical compound CO[SiH2]OC.C=CC PXJZCBUXFVZSLL-UHFFFAOYSA-N 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical class NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000004111 Potassium silicate Substances 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
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- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
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- AVBCBOQFOQZNFK-UHFFFAOYSA-N dipropoxy(dipropyl)silane Chemical compound CCCO[Si](CCC)(CCC)OCCC AVBCBOQFOQZNFK-UHFFFAOYSA-N 0.000 description 1
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- 239000000428 dust Substances 0.000 description 1
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- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 1
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- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- RJMRIDVWCWSWFR-UHFFFAOYSA-N methyl(tripropoxy)silane Chemical compound CCCO[Si](C)(OCCC)OCCC RJMRIDVWCWSWFR-UHFFFAOYSA-N 0.000 description 1
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- KBJFYLLAMSZSOG-UHFFFAOYSA-N n-(3-trimethoxysilylpropyl)aniline Chemical compound CO[Si](OC)(OC)CCCNC1=CC=CC=C1 KBJFYLLAMSZSOG-UHFFFAOYSA-N 0.000 description 1
- TWSLRROKQREASH-UHFFFAOYSA-N naphthalene-1-carboxylic acid;tin Chemical compound [Sn].C1=CC=C2C(C(=O)O)=CC=CC2=C1 TWSLRROKQREASH-UHFFFAOYSA-N 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 1
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- 125000004365 octenyl group Chemical group C(=CCCCCCC)* 0.000 description 1
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 description 1
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
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- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 description 1
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- 239000005011 phenolic resin Substances 0.000 description 1
- FABOKLHQXVRECE-UHFFFAOYSA-N phenyl(tripropoxy)silane Chemical compound CCCO[Si](OCCC)(OCCC)C1=CC=CC=C1 FABOKLHQXVRECE-UHFFFAOYSA-N 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
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- 235000011118 potassium hydroxide Nutrition 0.000 description 1
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 1
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- 230000037452 priming Effects 0.000 description 1
- UIDUKLCLJMXFEO-UHFFFAOYSA-N propylsilane Chemical compound CCC[SiH3] UIDUKLCLJMXFEO-UHFFFAOYSA-N 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 125000005504 styryl group Chemical group 0.000 description 1
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- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 description 1
- 229960001124 trientine Drugs 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-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
- UZIAQVMNAXPCJQ-UHFFFAOYSA-N triethoxysilylmethyl 2-methylprop-2-enoate Chemical compound CCO[Si](OCC)(OCC)COC(=O)C(C)=C UZIAQVMNAXPCJQ-UHFFFAOYSA-N 0.000 description 1
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- JRSJRHKJPOJTMS-MDZDMXLPSA-N trimethoxy-[(e)-2-phenylethenyl]silane Chemical compound CO[Si](OC)(OC)\C=C\C1=CC=CC=C1 JRSJRHKJPOJTMS-MDZDMXLPSA-N 0.000 description 1
- UOKUUKOEIMCYAI-UHFFFAOYSA-N trimethoxysilylmethyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)COC(=O)C(C)=C UOKUUKOEIMCYAI-UHFFFAOYSA-N 0.000 description 1
- OZWKZRFXJPGDFM-UHFFFAOYSA-N tripropoxysilane Chemical compound CCCO[SiH](OCCC)OCCC OZWKZRFXJPGDFM-UHFFFAOYSA-N 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- SRWMQSFFRFWREA-UHFFFAOYSA-M zinc formate Chemical compound [Zn+2].[O-]C=O SRWMQSFFRFWREA-UHFFFAOYSA-M 0.000 description 1
- WXKZSTUKHWTJCF-UHFFFAOYSA-N zinc;ethanolate Chemical compound [Zn+2].CC[O-].CC[O-] WXKZSTUKHWTJCF-UHFFFAOYSA-N 0.000 description 1
- JXNCWJJAQLTWKR-UHFFFAOYSA-N zinc;methanolate Chemical compound [Zn+2].[O-]C.[O-]C JXNCWJJAQLTWKR-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- 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
- C09D183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0208—Tissues; Wipes; Patches
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/00051—Accessories for dressings
- A61F13/00059—Accessories for dressings provided with visual effects, e.g. printed or colored
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/00051—Accessories for dressings
- A61F13/00063—Accessories for dressings comprising medicaments or additives, e.g. odor control, PH control, debriding, antimicrobic
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/70—Web, sheet or filament bases ; Films; Fibres of the matrix type containing drug
- A61K9/7023—Transdermal patches and similar drug-containing composite devices, e.g. cataplasms
- A61K9/703—Transdermal patches and similar drug-containing composite devices, e.g. cataplasms characterised by shape or structure; Details concerning release liner or backing; Refillable patches; User-activated patches
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/16—Fillings or auxiliary members in containers or encapsulations, e.g. centering rings
- H01L23/18—Fillings characterised by the material, its physical or chemical properties, or its arrangement within the complete device
- H01L23/24—Fillings characterised by the material, its physical or chemical properties, or its arrangement within the complete device solid or gel at the normal operating temperature of the device
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/31—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape
- H01L23/3107—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape the device being completely enclosed
- H01L23/3142—Sealing arrangements between parts, e.g. adhesion promotors
-
- H—ELECTRICITY
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Abstract
在制备包括半导体部件的半导体器件中,将半导体部件进行等离子体处理,并进行底层涂料处理,然后用封装剂封装该半导体部件。该半导体器件,特别是LED组件的高可靠之处在于在半导体部件与封装剂树脂之间建立牢固的粘结。
Description
技术领域
本发明涉及制备半导体器件、特别是LED组件的方法,更特别涉及制备其中在半导体部件与封装树脂之间建立牢固粘合的半导体器件的方法。这里使用的术语“半导体部件”用于同时表示半导体芯片和其上安装半导体芯片的衬底。
背景技术
通常,将半导体器件用各种树脂封装和保护,以保护衬底或者导线框架上的半导体芯片。为增强该半导体组件的可靠性,必须在半导体器件与封装树脂之间建立牢固的粘结或者紧密接触。然而,在苛刻的热循环试验和耐湿气试验中,目前的组件会带来一些问题如在半导体部件与封装树脂之间脱层。仍然存在对制备更可靠半导体器件的技术的需求。
现有技术中提出了各种用于增强半导体器件的可靠性的底层涂料。仍然需要制备承受苛刻条件的半导体器件的方法。
本发明的专利相关文献包括JP-B 03-054715、JP-A 05-179159(相应于USP5,213,617和USP5,238,708)、JP-B 07-091528、JP-A2004-079683和JP-A 2004-339450。
发明内容
本发明的一个目的是提供一种用于制备半导体器件,特别是LED组件的方法,该器件是高可靠性的,其在于在半导体器件与起到保护层的封装树脂之间建立牢固的粘结。
本发明人已发现,通过用等离子体处理半导体部件,用底层涂料组合物对其打底,然后用封装树脂封装,由此形成保护层,并在半导体部件与保护层之间建立更高度粘结。结果,改进半导体器件的可靠性。
根据本发明,提供一种制备包括半导体部件的半导体器件的方法,该方法包括如下步骤:将半导体部件进行等离子体处理,将该半导体部件用底层涂料组合物进行底涂层处理,然后用封装剂封装该半导体部件。
该半导体器件最通常为LED组件。
在优选的实施方案中,该底层涂料组合物包括硅烷偶联剂和/或其部分水解缩合物和非必要的稀释剂。该底层涂料组合物还可包括一种缩合催化剂。
在另一优选实施方案中,该底层涂料组合物包括具有如下平均组成式(1)的有机硅氧烷低聚物:
其中R1 aR2 bR3 cR4 d(OR5)eSiO(4-a-b-c-d-e)/2 (1)
其中R1为具有至少一个环氧化物的2至30个碳原子的单价有机基团,R2为具有至少一个非共轭双键基团的2至30个碳原子的单价烃基,R3为具有至少一个(甲基)丙烯酸系官能基团的3至30个碳原子的单价有机基团,R4为氢或1至20个碳原子的单价烃基,R5为氢或者1至10个碳原子的取代或未取代的单价烃基,下标a、b、c、d和e表示如下范围的数:0.1≤a≤1.0、0≤b≤0.6、0≤c≤0.6、0≤d≤0.8、1.0≤e≤2.0和2.0≤a+b+c+d+e≤3.0,和非必要的稀释剂。
具有式(1)的有机硅氧烷低聚物一般通过具有如下通式(2)的至少一种硅烷化合物、和非必要地具有如下通式(3)的至少一种硅烷化合物、和非必要地具有如下通式(4)的至少一种硅烷化合物、和非必要地具有如下通式(5)的至少一种硅烷化合物的(共)水解缩合获得,所述通式(2)为:
R1 xR4 ySi(OR5)4-x-y (2)
其中R1为具有至少一个环氧化物的2至30个碳原子的单价有机基团,R4为1至20个碳原子的单价烃基,R5为氢或者1至10个碳原子的取代或未取代的单价烃基,x为1或2,和y为0或1,x+y之和为1或2,所述通式(3)为:
R2 xR4 ySi(OR5)4-x-y (3)
其中R2为具有至少一个非共轭双键基团的2至30个碳原子的单价烃基,R4为1至20个碳原子的单价烃基,R5为氢或者1至10个碳原子的取代或未取代的单价烃基,x为1或2,和y为0或1,x+y之和为1或2,所述通式(4)为:
R3 xR4 ySi(OR5)4-x-y (4)
其中R3为具有至少一个(甲基)丙烯酸系官能基团的3至30个碳原子的单价有机基团,R4为1至20个碳原子的单价烃基,R5为氢或者1至10个碳原子的取代或未取代的单价烃基,x为1或2,和y为0或1,x+y之和为1或2,所述通式(5)为:
R4 zSi(OR5)4-z (5)
其中R4为氢或1至20个碳原子的单价烃基,R5为氢或者1至10个碳原子的取代或未取代的单价烃基,和z为1至3的整数。该底层涂料组合物可进一步包括缩合催化剂。
封装剂优选形成透明固化产品。优选的封装剂包括选自可固化硅氧烷树脂、可固化环氧-硅氧烷杂化树脂、可固化环氧树脂、可固化丙烯酸树脂和可固化聚酰亚胺树脂的一种可固化树脂。
在优选的实施方案中,等离子体处理包括使用选自氩、氮、氧、空气和其混合物的气体。
本发明的有益效果
由本发明制备的半导体器件(一般为LED组件)因在半导体部件与封装树脂之间建立牢固粘结而特别可靠。本发明当用于LED器件时特别有利。
附图说明
唯一的附图,图1为作为一个示例性表面安装半导体器件的发光二极管组件的横截面示意图,其中发光二极管与绝缘外壳冲模粘结。
具体实施方式
这里使用的术语“(甲基)丙烯酸系”拟包括丙烯酸系或甲基丙烯酸系。
本发明方法的特征在于在用封装树脂封装半导体部件之前预处理。该预处理包括等离子体处理和随后的底层涂料处理。这些预处理起到使所得半导体器件更可靠的作用。
制备本发明半导体器件的方法在下面详细描述。
半导体部件
如引言中注意的,将半导体芯片(或元件)和其上安装半导体芯片的衬底在整个说明书中累积称为“半导体部件”。
本发明所述的半导体芯片无特殊限制。合适的半导体芯片包括晶体管、二极管、电容器、变阻器、闸流体和光电转化元件,特别是发光半导体元件如发光二极管、光电晶体管、光电二极管、CCD、太阳能电池组、EPROM和光电耦合器。当使用发光二极管(LED)时可获得更多优点。还包括其上安装这种半导体晶片的衬底。
等离子体处理
根据本发明,等离子体处理通过如下进行:将半导体部件置于真空室中的电极上,将该室抽真空,将用于等离子体处理的气体加入真空室中,和在电极之间施加电压以在室中产生等离子体,如下通过蚀刻效应处理或者清洁半导体部件表面。用于等离子体处理的气体源可为氩气、氮气、氧气、氯气、溴气或者氟气或其混合物。为使等离子体处理对于改进粘结更有效,等离子体处理合适地在空气、氧气、氯气、溴气或氟气气氛中进行。对于某些组件,需要使用惰性气体如氩气和氮气。
有效的等离子体包括射频(RF)等离子体、微波等离子体、电子回旋加速器谐振源(ECR)等离子体等,其中任何一种都可用于本发明中。对于等离子体的频率和功率,优选功率高达约1,000W,特别是约10至500W,频率13.56MHz。等离子体处理系统(室)中的真空优选为约100至0.1Pa,特别是约50至1Pa。
等离子体照射到半导体部件表面的距离一般为约0.1至500mm,优选约0.5至30mm,尽管距离随等离子体照射系统的功率、喷嘴形状等而变化。对于等离子体照射时间,照射30分钟足够,优选的照射时间为约0.1至600秒,更优选约0.5至600秒。
此外,等离子体处理可通过用溶剂或其类似物使用超声清洁机、喷雾器或其类似物清洁半导体部件的步骤,或者用压缩空气吹掉灰尘和碎屑的步骤。
底层涂料处理
然后将等离子体处理过的半导体部件用底层涂料组合物进行涂底处理。
底层涂料组合物
这里使用的底层涂料组合物可为任一公知的底层涂料组合物。通常为包括硅烷偶联剂或其部分水解缩合物和非必要的稀释剂的底层涂料组合物。硅烷偶联剂和其部分水解缩合物的实例包括乙烯基三氯硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、2-(3,4-环氧环己基)乙基三甲氧基硅烷、3-环氧丙氧基丙基三甲氧基硅烷、3-环氧丙氧基丙基甲基二乙氧基硅烷、3-环氧丙氧基丙基三乙氧基硅烷、3-甲基丙烯酰氧基丙基甲基二甲氧基硅烷、3-甲基丙烯酰氧基丙基三甲氧基硅烷、3-甲基丙烯酰氧基甲基二乙氧基硅烷、3-甲基丙烯酰氧基丙基三乙氧基硅烷、N-2-(氨乙基)-3-氨丙基甲基二甲氧基硅烷、N-2-(氨乙基)-3-氨丙基三甲氧基硅烷、N-2-(氨乙基)-3-氨丙基三乙氧基硅烷、3-氨丙基三甲氧基硅烷、3-氨丙基三乙氧基硅烷、N-苯基-3-氨丙基三甲氧基硅烷、3-氯丙基三甲氧基硅烷、3-巯丙基三甲氧基硅烷以及三甲氧基硅烷、四甲氧基硅烷和其低聚物,和其混合物。
在一个优选的实施方案中,使用包括具有平均组成式(1)的含环氧化物有机硅氧烷低聚物和非必要的稀释剂的底层涂料组合物。
R1 aR2 bR3 cR4 d(OR5)eSiO(4-a-b-c-d-e)/2 (1)
其中R1为具有至少一个环氧化物的2至30个碳原子的单价有机基团,R2为具有至少一个非共轭双键基团的2至30个碳原子的单价烃基,R3为具有至少一个(甲基)丙烯酸系官能基团的3至30个碳原子的单价有机基团,R4为氢或者1至20个碳原子的单价烃基,和R5为氢或者1至10个碳原子的取代或未取代的单价烃基。下标a、b、c、d和e为满足如下范围的数:0.1≤a≤1、0≤b≤0.6、0≤c≤0.6、0≤d≤0.8、1.0≤e≤2.0和2.0≤a+b+c+d+e≤3.0,优选a、b、c、d和e为满足如下范围的数0.2≤a≤0.9、0.1≤b≤0.6、0≤c≤0.4、0≤d≤0.6、1.2≤e≤1.7和2.2≤a+b+c+d+e≤3.0。该有机硅氧烷低聚物一般具有重均分子量约300至30,000,优选约400至10,000,更优选约500至5,000,通过凝胶渗透色谱(GPC)借助聚苯乙烯标准物测定。
在更优选的实施方案中,具有式(1)的有机硅氧烷低聚物为下式(2)表示的含一个或多个环氧改性有机氧基硅烷、和下式(3)表示的非必要地带有一个或多个非共轭双键的有机氧基硅烷、和非必要地一种或多种下式(4)表示的具有可光聚合(甲基)丙烯酸系结构的(甲基)丙烯酸系改性有机氧基硅烷和非必要地下式(5)表示的一种或多种有机氧基硅烷的硅烷混合物的(共)水解缩合物。
R1 xR4 ySi(OR5)4-x-y (2)
R2 xR4 ySi(OR5)4-x-y (3)
R3 xR4 ySi(OR5)4-x-y (4)
R4 zSi(OR5)4-z (5)
其中R1为具有至少一个环氧化物的2至30个碳原子的单价有机基团,R2为具有至少一个非共轭双键基团的2至30个碳原子的单价烃基,R3为具有至少一个(甲基)丙烯酸系官能基团的3至30个碳原子的单价有机基团,R4为氢或者1至20个碳原子的单价烃基,和R5为氢或者1至10个碳原子的取代或未取代的单价烃基。下标x为1或2,y为0或1,x+y之和为1或2,和z为0至3的整数。
R1表示的单价有机基团具有2至30个碳原子、优选3至20个碳原子、更优选6至12个碳原子,并具有至少一个环氧化物,该有机基团一般为具有至少一个环氧化物并且可含有醚键氧原子和/或氮原子由此构成氨基的单价烃基,但不限于此。实例包括3-环氧丙氧基丙基、2-(3,4-环氧环己基)乙基、2-(2,3-环氧环己基)乙基、3-(N-烯丙基-N-缩水甘油基)氨丙基和3-(N,N-缩水甘油基)氨丙基。
R2表示的单价烃基具有2至30个碳原子、优选2至20个碳原子,更优选2至8个碳原子,并具有至少一个非共轭双键基团。合适的单价烃基的实例包括但不限于乙烯基、烯丙基、丁烯基、异丁烯基、丙烯基、异丙烯基、戊烯基、己烯基、环己烯基和辛烯基。
R3表示的单价有机基团具有3至30个碳原子、优选5至20个碳原子,更优选5至10个碳原子,并具有至少一个(甲基)丙烯酸系结构。实例为丙烯酸系和甲基丙烯酸系官能基团如CH2=CHCOO-、CH2=C(CH3)COO-、CH2=CHCO-和CH2=C(CH3)CO-。R3表示的具有这种(甲基)丙烯酰基的单价有机基团的实例包括但不限于具有一个或多个丙烯酰氧基或者甲基丙烯酰氧基取代的烷基如CH2=CHCOOCH2CH2-、CH2=C(CH3)COOCH2CH2-、[CH2=C(CH3)COOCH2]3C-CH2-、(CH2=CHCOOCH2)3C-CH2-和(CH2=CHCOOCH2)2CH(C2H5)CH2-。优选CH2=CHCOOCH2-、CH2=C(CH3)COOCH2-、CH2=CHCOOCH2CH2CH2-和CH2=C(CH3)COOCH2CH2CH2-。
R4表示的单价烃基优选选自不同于脂族不饱和类如链烯基的未取代单价烃基,和特别是选自1至10个碳原子的烷基、6至20个碳原子的芳基和7至20个碳原子的芳烷基。C1-C10烷基的实例是甲基、乙基、丙基、异丙基、丁基、异丁基、叔丁基、戊基、新戊基、己基、庚基、环己基、环庚基、辛基和α-乙基己基,最优选甲基和乙基。C6-C20芳基和C7-C20芳烷基的实例是苯基、苄基、甲苯基和苯乙烯基,其中最优选苯基。
R5表示的单价烃基优选选自1至10个碳原子的烷基和烷氧基取代的烷基。实例包括甲基、乙基、丙基、异丙基、丁基、异丁基、叔丁基、戊基、新戊基、己基、庚基、环己基、环庚基、辛基和α-乙基己基,最优选甲基和乙基。
具有式(2)的环氧改性有机氧基硅烷的说明性非限制性实例包括3-环氧丙氧基丙基三甲氧基硅烷、2-(3,4-环氧环己基乙基)三甲氧基硅烷、3-环氧丙氧基丙基三乙氧基硅烷、二甲基乙氧基-3-环氧丙氧基丙基硅烷和二乙氧基-3-环氧丙氧基丙基甲基硅烷。
具有通式(3)的带非共轭双键的有机氧基硅烷的说明性非限制性实例包括乙烯基三甲氧基硅烷、烯丙基三甲氧基硅烷、甲基乙烯基二甲氧基硅烷、二乙烯基二甲氧基硅烷、三甲氧基甲硅烷基降冰片烯和2-(4-环己烯基乙基)三甲氧基硅烷。
具有通式(4)的(甲基)丙烯酸改性有机氧基硅烷的说明性非限制性实例包括3-甲基丙烯酰氧基丙基三甲氧基硅烷、3-丙烯酰氧基丙基三甲氧基硅烷、3-甲基丙烯酰氧基丙基三乙氧基硅烷、3-丙烯酰氧基丙基三乙氧基硅烷、甲基丙烯酰氧基丙烯基三甲氧基硅烷、甲基丙烯酰氧基丙烯基三乙氧基硅烷、甲基丙烯酰氧基甲基三甲氧基硅烷、甲基丙烯酰氧基甲基三乙氧基硅烷、甲基丙烯酰氧基丙基三(甲氧基乙氧基)硅烷、3-甲基丙烯酰氧基丙基二甲氧基甲基硅烷和3-甲基丙烯酰氧基丙基二乙氧基甲基硅烷。
具有通式(5)的有机氧基硅烷的说明性非限制性实例包括甲基三甲氧基硅烷、甲基三乙氧基硅烷、甲基三丙氧基硅烷、甲基三丁氧基硅烷、乙基三甲氧基硅烷、乙基三乙氧基硅烷、乙基三丙氧基硅烷、乙基三丁氧基硅烷、丙基三甲氧基硅烷、丙基三乙氧基硅烷、丙基三丙氧基硅烷、丙基三丁氧基硅烷、苯基三甲氧基硅烷、苯基三乙氧基硅烷、苯基三丙氧基硅烷、苄基三甲氧基硅烷、苄基三乙氧基硅烷、对苯乙烯基三甲氧基硅烷、二甲基二甲氧基硅烷、二甲基二乙氧基硅烷、二甲基二丙氧基硅烷、二甲基二丁氧基硅烷、二乙基二甲氧基硅烷、二乙基二乙氧基硅烷、二乙基二丙氧基硅烷、二乙基二丁氧基硅烷、二丙基二甲氧基硅烷、二丙基二乙氧基硅烷、二丙基二丙氧基硅烷、二丙基二丁氧基硅烷、二苯基二羟基硅烷、
三甲基甲氧基硅烷、三甲基乙氧基硅烷、三甲基丙氧基硅烷、三甲基丁氧基硅烷、三乙基甲氧基硅烷、三乙基乙氧基硅烷、三乙基丙氧基硅烷、三乙基丁氧基硅烷、三丙基甲氧基硅烷、三丙基乙氧基硅烷、三丙基丙氧基硅烷、三丙基丁氧基硅烷、三苯基羟基硅烷、三甲氧基硅烷、三乙氧基硅烷、四甲氧基硅烷、四乙氧基硅烷和四丁氧基硅烷。
对于具有式(2)、(3)、(4)和(5)的硅烷的混合比,优选具有式(2)的环氧改性有机氧基硅烷的量为总硅烷的10至100mol%,特别是30至100mol%;非必要加入的具有式(3)的带非共轭双键的有机氧基硅烷的量为总硅烷的0至60mol%,特别是10至50mol%;非必要加入的具有式(4)表示的(甲基)丙烯酸改性有机氧基硅烷的量为总硅烷的0至60mol%,特别是10至50mol%;和在具有式(5)的硅烷中,单有机三有机氧基硅烷的量为总硅烷的0至80mol%,特别是0至50mol%;二有机二有机氧基硅烷的量为总硅烷的0至50mol%,特别是0至20mol%;三有机单有机氧基硅烷的量为0至30mol%,特别是0至20mol%,按具有式(1)的硅烷摩尔量计,和总硅烷的0至30mol%,特别是0至20mol%,当具有式(3)的硅烷为四有机氧基硅烷时。
优选的硅氧烷低聚物包括低聚物(i)、(ii)和(iii)。
(i)通过(共)水解缩合一种或多种具有如下通式(2)的硅烷化合物、一种或多种具有如下通式(3)的硅烷化合物和非必要的一种或多种具有如下通式(4)的硅烷化合物获得的硅氧烷低聚物,所述通式(2)为:
R1 xR4 ySi(OR5)4-x-y (2)
其中R1、R4、R5、x和y为上面定义的,所述通式(3)为:
R2 xR4 ySi(OR5)4-x-y (3)
其中R2、R4、R5、x和y为上面定义的,所述通式(4)为:
R3 xR4 ySi(OR5)4-x-y (4)
其中R3、R4、R5、x和y为上面定义的。
(ii)通过(共)水解缩合一种或多种具有如下通式(2)的硅烷化合物、一种或多种具有如下通式(4)的硅烷化合物和非必要的一种或多种具有如下通式(5)的硅烷化合物获得的硅氧烷低聚物,所述通式(2)为:
R1 xR4 ySi(OR5)4-x-y (2)
其中R1、R4、R5、x和y为上面定义的,所述通式(4)为:
R3 xR4 ySi(OR5)4-x-y (4)
其中R3、R4、R5、x和y为上面定义的,所述通式(5)为:
R4 zSi(OR5)4-z (5)
其中R4、R5和z为上面定义的。
(iii)通过(共)水解缩合一种或多种具有如下通式(2)的硅烷化合物、一种或多种具有如下通式(3)的硅烷化合物、一种或多种具有如下通式(4)的硅烷化合物和非必要的一种或多种具有如下通式(5)的硅烷化合物获得的硅氧烷低聚物,所述通式(2)为:
R1 xR4 ySi(OR5)4-x-y (2)
其中R1、R4、R5、x和y为上面定义的,所述通式(3)为:
R2 xR4 ySi(OR5)4-x-y (3)
其中R2、R4、R5、x和y为上面定义的,所述通式(4)为:
R3 xR4 ySi(OR5)4-x-y (4)
其中R3、R4、R5、x和y为上面定义的,所述通式(5)为:
R4 zSi(OR5)4-z (5)
其中R4、R5和z为上面定义的。
制备具有式(1)的有机硅氧烷低聚物的方法无特殊限制。在使用具有式(2)、(3)、(4)和(5)的硅烷的一个实施方案中,通过使用式(2)的环氧改性有机氧基硅烷或者非必要地将其与式(3)的带非共轭双键的有机氧基硅烷、式(4)的(甲基)丙烯酸改性有机氧基硅烷和/或式(5)的有机氧基硅烷结合、非必要地加入催化剂和溶剂,并在中性或者弱碱性条件下进行水解和缩聚,获得带硅烷醇的共水解缩合物。
如上所述,(共)水解在中性或者弱碱性条件下进行。当使用催化剂时,可使用公知的碱性催化剂,如NaOH、KOH、硅酸钠、硅酸钾、胺和铵盐。特别优选KOH。
(共)水解优选在5至40℃下进行120分钟或者更长的时间。若必要,将由此获得的(共)水解物进行缩聚。缩聚反应的条件对于控制硅氧烷树脂的分子量是重要的。缩聚反应优选在50至80℃下进行约60至120分钟。
当有机硅氧烷低聚物通过借助上述方法(共)水解缩合具有式(2)、(3)、(4)和(5)的硅烷获得时,其中形成的硅烷醇起到增强底层涂料效果的作用。
在式(2)的R1中的环氧化物、在式(3)的R2中的非共轭双键基团、在式(4)的R3中的(甲基)丙烯酰基作为底层涂料中的活性取代基存在并起到增强组件或者衬底与封装树脂之间的界面处的粘结强度的作用,由此改进底层涂料性能。
稀释剂
上述硅烷偶联剂或者含环氧化物的有机硅氧烷低聚物可单独使用,尽管在使用前通常将其溶于稀释剂中作为底层涂料。稀释剂或溶剂无特殊限制,只要它可与硅烷偶联剂或者含环氧化物的有机硅氧烷低聚物相容即可。合适的稀释剂的实例包括醚如四氢呋喃、二甘醇二甲醚和三甘醇二甲醚,酮如甲基乙基酮和甲基异丁基酮,醇如甲醇、乙醇、丙醇、丁醇、2-丙醇、1-甲氧基-2-丙醇、2-乙氧基乙醇、2-乙基己基醇、1,4-丁二醇、乙二醇和丙二醇,芳烃如甲苯和二甲苯,脂族烃如己烷和庚烷,和低分子量硅氧烷如六甲基二硅氧烷。稀释剂的用量优选为至多约100,000重量份,更优选约100至100,000重量份,进一步更优选约400至10,000重量份,按每100重量份有机硅氧烷低聚物计。
缩合催化剂
硅烷偶联剂或者有机硅氧烷低聚物可与缩合催化剂一起使用。这里使用的缩合催化剂无特殊限制,只要它们通常用于缩合固化型硅氧烷组合物中即可。合适的催化剂为硅烷醇缩合催化剂,包括钛催化剂如钛酸四丁酯、钛酸四丙基酯和四乙酰基丙酮酸钛;锡催化剂如二月桂酸二丁基锡、马来酸二丁基锡、乙酸二丁基锡、辛酸锡、萘酸锡和乙酰丙酮酸二丁基锡;锌催化剂如二甲氧基锌、二乙氧基锌、2,4-戊烷二酸锌、2-乙基己酸锌、乙酸锌、甲酸锌、甲基丙烯酸锌、十一碳烯酸锌和辛酸锌;铝催化剂如三乙酰基丙酮酸铝、三乙基乙酰乙酸铝和乙基乙酰乙酸二异丙氧基铝;锆、铁、钴等的有机金属配合物催化剂;胺催化剂如丁基胺、辛基胺、二丁基胺、单乙醇胺、二乙醇胺、三乙醇胺、二亚乙基三胺、三亚乙基四胺、油酰胺、环己基胺、苄胺、二乙基氨基丙基胺、二甲苯二胺、三亚乙基二胺、胍、二苯基胍、2,4,6-三(二甲基氨甲基)苯酚、吗啉、N-甲基吗啉、2-乙基-4-甲基咪唑和DBU;带氨基的硅烷偶联剂如γ-氨基丙基三甲氧基硅烷和N-(β-氨乙基)氨丙基甲基二甲氧基硅烷;和其它公知的硅烷醇缩合催化剂,包括季铵盐如四烷基铵盐、其它酸性催化剂和碱性催化剂。这些催化剂可单独或者以混合物形式使用。
当使用时,加入的催化剂的量为0.01至2重量份,优选0.1至10重量份,更优选0.1至3重量份,按每100重量份不包括催化剂的总底层涂料组合物计(通常为硅烷偶联剂和/或其部分水解缩合物和稀释剂的总量,或有机硅氧烷低聚物和稀释剂的总量)。较低量的催化剂不能获得增加的效果,其中固化速率下降。大于催化剂的必须量不能起到进一步的效果。
其它组分
若必要,可将其它组分充分掺混入底层涂料组合物中,只要对底层涂料特征无不利影响即可。例如,若需要可加入聚合抑制剂如氢醌、氢醌单甲基醚、1,2,3-羟基苯、叔丁基儿茶酚和吩噻嗪,抗氧化剂如BHT和维生素B,消泡剂,和流平剂如硅氧烷表面活性剂和氟化学表面活性剂。
制备底层涂料组合物和底层涂料处理
底层涂料组合物可通过如下方法制备:将硅烷偶联剂或其部分水解的缩合物或有机硅氧烷低聚物溶于稀释剂中,非必要地加入缩合催化剂,非必要地进一步加入聚合抑制剂、抗氧化剂和其它组分,并将其混合至均匀。如此混合的组合物准备用作半导体器件的底层涂料。
当半导体部件进行等离子体处理后,例如可按照如下方式使用底层涂料组合物。使用合适的施涂器如旋涂器或者喷涂器,将底层涂料组合物涂于半导体部件上。接着加热或空气干燥以从底层涂料组合物中蒸出溶剂,由此形成具有干厚度至多约10μm,优选至多约1μm的底层涂料组合物涂层。涂层厚度的下限可根据需要合适地选取,尽管它通常为至少0.01μm。
封装
将半导体部件按照上述方式进行等离子体处理和随后的底层涂料处理后,进行封装处理以封装半导体部件。
用于封装半导体部件的封装剂可根据半导体芯片或者半导体器件等的类型从公知的封装剂中选取。
半导体封装剂通常为包括作为封装树脂的可固化树脂,固化剂和其量对可固化树脂的性能无不利影响的其它组分如抗氧化剂、抗脱色剂、光稳定剂、活性稀释剂、无机填料、阻燃剂和有机溶剂的组合物。这里使用的可固化树脂优选为透明的,一般选自可固化的硅氧烷树脂、可固化的环氧-硅氧烷杂化树脂、可固化的环氧树脂、可固化的丙烯酸类树脂和可固化的聚酰亚胺树脂。根据特定的可固化树脂,可从公知固化剂中选择固化剂,并以有效量用于固化可固化树脂。
下面详细描述封装树脂组合物中的可固化树脂。
封装树脂
优选的半导体封装树脂为形成透明固化产品的,特别是用于LED组件的透明树脂。透明树脂包括硅氧烷、环氧、丙烯酸类和聚酰亚胺基树脂,但不限于此。对于具有短波长和高能量特征的LED,优选硅氧烷树脂和无芳基的环氧树脂。将封装树脂用作包括该树脂组分作为基础、固化剂、和非必要的固化催化剂、填料等的封装树脂组合物。使用施涂器如分配器或旋涂器,将该封装树脂组合物直接涂于已进行等离子体处理和底层涂料处理的半导体部件上。可将如此施涂的封装树脂组合物在环境条件下或使用模塑机固化。
在透明树脂组合物中,可加入各种添加剂,加入量应对半导体器件无不利影响。合适的添加剂包括抗氧化剂(例如BHT和维生素B)、抗脱色剂(如有机磷化合物)、光稳定剂(如受阻胺)、活性稀释剂(如乙烯基醚、乙烯基酰胺、环氧树脂、氧杂环丁烷、邻苯二甲酸烯丙基酯、己二酸乙烯基酯)、增强填料(如锻制二氧化硅、沉淀二氧化硅)、阻燃改性剂、荧光剂和有机溶剂。该组合物可用着色组分染色。
硅氧烷树脂
这里使用的硅氧烷树脂包括那些高硬度型、橡胶型和凝胶型树脂。固化机理包括缩合固化型、加成反应固化型和UV固化型。可选取所有类型的硅氧烷树脂,取决于组件类型。
环氧树脂
这里使用的环氧树脂包括缩水甘油醚型环氧树脂如双酚A环氧树脂、双酚F环氧树脂、联苯型环氧树脂、酚醛线性酚醛清漆型环氧树脂和溴化环氧树脂;环脂族环氧树脂;缩水甘油基酯型环氧树脂;缩水甘油胺型环氧树脂;和杂环环氧树脂。对于具有短波长和高能量特征的LED,优选使用具有氢化芳香环的环氧树脂。
这些可固化环氧树脂通过包括热固化、UV固化和湿气固化的机理固化,其中最优选热固化。
环氧-硅氧烷杂化树脂
环氧-硅氧烷杂化树脂应优选含(A)分子中具有至少一个脂族不饱和单价烃基和至少一个硅键合羟基的有机硅化合物、(B)其中芳香环部分或完全氢化的芳香环氧树脂或者氢化环氧树脂和(C)有机氢聚硅氧烷作为必要组分。优选可进一步配混(D)铂族金属催化剂和(E)铝固化催化剂。优选的固化机理为热固化。
通过本发明方法,可制造可靠的半导体器件,通常为LED组件,原因在于在半导体部件与起保护层作用的封装剂树脂之间建立牢固粘结或者紧密接触。
实施例
下面给出用于说明本发明的制备例、实施例和比较例,但本发明不受此限制。
制备底层涂料A
通过将7g 3-环氧丙氧基丙基三甲氧基硅烷、3g四丁氧基钛酸酯和90g甲苯混合,并将该溶液经具有孔径0.8μm的过滤器过滤,制备底层涂料组合物。
制备底层涂料B
将0.5mol 2-(3,4-环氧环己基乙基)三甲氧基硅烷和0.5mol乙烯基三甲氧基硅烷投入已填充3.0mol去离子水的反应器中。在40℃下进行水解反应8小时。将如此获得的水解缩合物溶于甲醇中并将该溶液经具有孔径0.8μm的过滤器过滤。从滤液中在真空下在80℃和2mmHg下蒸出溶剂。通过将如此获得的7g硅氧烷低聚物、90g甲醇和3g辛酸锌混合,并将该溶液经具有孔径0.8μm的过滤器过滤,获得底层涂料组合物。
测试方法
发光半导体组件
使用的发光半导体器件为已装配具有InGaN发光层和主发射峰470nm的LED芯片的发光半导体组件。如图1所示,该组件包括玻璃纤维增强环氧树脂外壳1、发光器件2、导线电极3和4、模头粘结材料5、金导线6和封装树脂7。
等离子体清洁
在用封装树脂封装前,对发光半导体组件,用等离子体干燥清洁系统PDC210(Yamato Science Co.,Ltd.)在功率250W下在距离15cm下在氩气或者氧气气氛中进行等离子体照射20秒。
底层涂料处理
在等离子体清洁后,将发光半导体组件固定到硅晶片上。将按上述制备的底层涂料组合物浸入该组件内,在浸泡的同时,将该硅晶片在2,000rpm下旋转30秒。然后从硅晶片中取出该组件,当使用底层涂料A时将该组件在室温下空气干燥30分钟,或者当使用底层涂料B时将其在150℃下热处理10分钟。
热循环实验
在等离子体处理和底层涂料处理后,将该组件用实施例中给出的封装树脂组合物封装,最终获得图1所示的发光半导体组件。为进行比较,在不进行等离子体处理和底层涂料处理或者不进行其中之一处理下制备发光半导体组件。
制备50个发光半导体组件并在低温-45℃与高温125℃之间进行1,000次热循环试验。通过肉眼观察,数出具有因破裂和脱层导致的外观变化的样品数。
实施例1-8和比较例1-10
作为封装树脂组合物,使用加成反应固化硅氧烷树脂组合物LPS5510和LPS5520(购自Shin-Etsu Chemicaol Co.,Ltd.)。对应于相应组合物的结果在表1和2中给出。
表1:硅氧烷树脂LPS5510的测试结果。
等离子体处理 | 底层涂料处理 | 热循环测试(改变的样品/测试样品) | |||
氩气 | 氧气 | A | B | ||
实施例1 | ○ | - | ○ | - | 0/50 |
实施例2 | - | ○ | ○ | - | 0/50 |
实施例3 | ○ | - | - | ○ | 0/50 |
实施例4 | - | ○ | - | ○ | 0/50 |
比较例1 | ○ | - | - | - | 38/50 |
比较例2 | - | ○ | - | - | 36/50 |
比较例3 | - | - | ○ | - | 28/50 |
比较例4 | - | - | - | ○ | 25/50 |
比较例5 | - | - | - | - | 50/50 |
表2:硅氧烷树脂LPS5520的测试结果。
等离子体处理 | 底层涂料处理 | 热循环测试(改变的样品/测试样品) | |||
氩气 | 氧气 | A | B | ||
实施例5 | ○ | - | ○ | - | 0/50 |
实施例6 | - | ○ | ○ | - | 0/50 |
实施例7 | ○ | - | - | ○ | 0/50 |
实施例8 | - | ○ | - | ○ | 0/50 |
比较例6 | ○ | - | - | - | 39/50 |
比较例7 | - | ○ | - | - | 36/50 |
比较例8 | - | - | ○ | - | 27/50 |
比较例9 | - | - | - | ○ | 28/50 |
比较例10 | - | - | - | - | 50/50 |
实施例9-16和比较例11-20
使用的封装树脂组合物为包括可热固化氢化环氧树脂YX8000(Japan Epoxy Resin Co.,Ltd.)、酸酐YH1120(Japan Epoxy ResinCo.,Ltd.)作为固化剂和固化促进剂U-CAT5003(San-Apro Ltd.)的可固化环氧树脂组合物,和使用可热固化氢化环氧树脂YL7170(Japan Epoxy Resin Co.,Ltd.)代替YX8000的类似可固化环氧树脂组合物。对应于相应组合物的结果在表3和4中给出。
表3:环氧树脂YX8000的测试结果。
等离子体处理 | 底层涂料处理 | 热循环测试(改变的样品/测试样品) | |||
氩气 | 氧气 | A | B | ||
实施例9 | ○ | - | ○ | - | 0/50 |
实施例10 | - | ○ | ○ | - | 0/50 |
实施例11 | ○ | - | - | ○ | 0/50 |
实施例12 | - | ○ | - | ○ | 0/50 |
比较例11 | ○ | - | - | - | 35/50 |
比较例12 | - | ○ | - | - | 32/50 |
比较例13 | - | - | ○ | - | 25/50 |
比较例14 | - | - | - | ○ | 25/50 |
比较例15 | - | - | - | - | 50/50 |
表4:环氧树脂YL7170的测试结果。
等离子体处理 | 底层涂料处理 | 热循环测试(改变的样品/测试样品) | |||
氩气 | 氧气 | A | B | ||
实施例13 | ○ | - | ○ | - | 0/50 |
实施例14 | - | ○ | ○ | - | 0/50 |
实施例15 | ○ | - | - | ○ | 0/50 |
实施例16 | - | ○ | - | ○ | 0/50 |
比较例16 | ○ | - | - | - | 35/50 |
比较例17 | - | ○ | - | - | 31/50 |
比较例18 | - | - | ○ | - | 20/50 |
比较例19 | - | - | - | ○ | 22/50 |
比较例20 | - | - | - | - | 50/50 |
实施例17-24和比较例21-30
作为封装树脂组合物,使用可热固化环氧-硅氧烷杂化树脂组合物X-45-720和X-45-722(Shin-Etsu Chemical Co.,Ltd.)。对应于相应组合物的结果在表5和6中给出。
表5:环氧-硅氧烷杂化树脂X-45-720的测试结果。
等离子体处理 | 底层涂料处理 | 热循环测试(改变的样品/测试样品) | |||
氩气 | 氧气 | A | B | ||
实施例17 | ○ | - | ○ | - | 0/50 |
实施例18 | - | ○ | ○ | - | 0/50 |
实施例19 | ○ | - | - | ○ | 0/50 |
实施例20 | - | ○ | - | ○ | 0/50 |
比较例21 | ○ | - | - | - | 35/50 |
比较例22 | - | ○ | - | - | 32/50 |
比较例23 | - | - | ○ | - | 23/50 |
比较例24 | - | - | - | ○ | 22/50 |
比较例25 | - | - | - | - | 50/50 |
表6:环氧-硅氧烷混杂树脂X-45-722的测试结果。
等离子体处理 | 底层涂料处理 | 热循环测试(改变的样品/测试样品) | |||
氩气 | 氧气 | A | B | ||
实施例21 | ○ | - | ○ | - | 0/50 |
实施例22 | - | ○ | ○ | - | 0/50 |
实施例23 | ○ | - | - | ○ | 0/50 |
实施例24 | - | ○ | - | ○ | 0/50 |
比较例26 | ○ | - | - | - | 34/50 |
比较例27 | - | ○ | - | - | 31/50 |
比较例28 | - | - | ○ | - | 22/50 |
比较例29 | - | - | - | ○ | 24/50 |
比较例30 | - | - | - | - | 50/50 |
Claims (10)
1.一种制备包括半导体部件的半导体器件的方法,该方法包括如下步骤:将半导体部件进行等离子体处理,将该半导体部件用底层涂料组合物进行底层涂料处理,然后用封装剂封装该半导体部件。
2.权利要求1的方法,其中半导体器件为LED组件。
3.权利要求1的方法,其中所述底层涂料组合物包括硅烷偶联剂和/或其部分水解缩合物和非必要的稀释剂。
4.权利要求3的方法,其中所述底层涂料组合物进一步包括缩合催化剂。
5.权利要求1的方法,其中所述底层涂料组合物包括具有如下平均组成式(1)的有机硅氧烷低聚物
R1 aR2 bR3 cR4 d(OR5)eSiO(4-a-b-c-d-e)/2 (1)
其中R1为具有至少一个环氧化物的2至30个碳原子的单价有机基团,R2为具有至少一个非共轭双键基团的2至30个碳原子的单价烃基,R3为具有至少一个(甲基)丙烯酸系官能基团的3至30个碳原子的单价有机基团,R4为氢或1至20个碳原子的单价烃基,R5为氢或者1至10个碳原子的取代或未取代的单价烃基,下标a、b、c、d和e表示如下范围的数:0.1≤a≤1.0、0≤b≤0.6、0≤c≤0.6、0≤d≤0.8、1.0≤e≤2.0和2.0≤a+b+c+d+e≤3.0,和非必要的稀释剂。
6.权利要求5的方法,其中具有式(1)的有机硅氧烷低聚物通过具有如下通式(2)的至少一种硅烷化合物、和非必要地具有如下通式(3)的至少一种硅烷化合物、和非必要地具有如下通式(4)的至少一种硅烷化合物、和非必要地具有如下通式(5)的至少一种硅烷化合物的(共)水解缩合获得,所述通式(2)为:
R1 xR4 ySi(OR5)4-x-y (2)
其中R1为具有至少一个环氧化物的2至30个碳原子的单价有机基团,R4为1至20个碳原子的单价烃基,R5为氢或者1至10个碳原子的取代或未取代的单价烃基,x为1或2,和y为0或1,x+y之和为1或2,所述通式(3)为:
R2 xR4 ySi(OR5)4-x-y (3)
其中R2为具有至少一个非共轭双键基团的2至30个碳原子的单价烃基,R4为1至20个碳原子的单价烃基,R5为氢或者1至10个碳原子的取代或未取代的单价烃基,x为1或2,和y为0或1,x+y之和为1或2,所述通式(4)为:
R3 xR4 ySi(OR5)4-x-y (4)
其中R3为具有至少一个(甲基)丙烯酸系官能基团的3至30个碳原子的单价有机基团,R4为1至20个碳原子的单价烃基,R5为氢或者1至10个碳原子的取代或未取代的单价烃基,x为1或2,和y为0或1,x+y之和为1或2,所述通式(5)为:
R4 zSi(OR5)4-z (5)
其中R4为氢或1至20个碳原子的单价烃基,R5为氢或者1至10个碳原子的取代或未取代的单价烃基,和z为1至3的整数。
7.权利要求5的方法,其中所述底层涂料组合物进一步包括缩合催化剂。
8.权利要求1的方法,其中所述封装剂形成透明固化产品。
9.权利要求1的方法,其中所述封装剂包括选自可固化硅氧烷树脂、可固化环氧-硅氧烷杂化树脂、可固化环氧树脂、可固化丙烯酸系树脂和可固化聚酰亚胺树脂的一种可固化树脂,并形成透明固化产品。
10.权利要求1的方法,其中所述等离子体处理使用选自氩、氮、氧、空气和其混合物的气体。
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