TW201807187A - 洗淨劑組成物及薄型基板之製造方法 - Google Patents
洗淨劑組成物及薄型基板之製造方法 Download PDFInfo
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- TW201807187A TW201807187A TW106113506A TW106113506A TW201807187A TW 201807187 A TW201807187 A TW 201807187A TW 106113506 A TW106113506 A TW 106113506A TW 106113506 A TW106113506 A TW 106113506A TW 201807187 A TW201807187 A TW 201807187A
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- Prior art keywords
- substrate
- mass
- detergent composition
- polysiloxane
- adhesive
- Prior art date
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- 239000000758 substrate Substances 0.000 title claims abstract description 210
- 239000000203 mixture Substances 0.000 title claims abstract description 94
- 239000004065 semiconductor Substances 0.000 claims abstract description 60
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 58
- 239000000853 adhesive Substances 0.000 claims abstract description 56
- 230000001070 adhesive effect Effects 0.000 claims abstract description 56
- 239000003960 organic solvent Substances 0.000 claims abstract description 16
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 15
- 239000003599 detergent Substances 0.000 claims description 68
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 46
- -1 polysiloxane Polymers 0.000 claims description 45
- 229920001296 polysiloxane Polymers 0.000 claims description 42
- 238000004140 cleaning Methods 0.000 claims description 28
- 239000012790 adhesive layer Substances 0.000 claims description 18
- 238000004519 manufacturing process Methods 0.000 claims description 17
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 238000012545 processing Methods 0.000 claims description 13
- 239000011347 resin Substances 0.000 claims description 11
- 229920005989 resin Polymers 0.000 claims description 11
- 150000001298 alcohols Chemical class 0.000 claims description 8
- 150000002430 hydrocarbons Chemical group 0.000 claims description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 7
- 150000001338 aliphatic hydrocarbons Chemical group 0.000 claims description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 239000010703 silicon Substances 0.000 abstract description 55
- 150000003242 quaternary ammonium salts Chemical class 0.000 abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 63
- 239000000243 solution Substances 0.000 description 38
- 238000003756 stirring Methods 0.000 description 36
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 24
- 238000001816 cooling Methods 0.000 description 22
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- SGVYKUFIHHTIFL-UHFFFAOYSA-N 2-methylnonane Chemical compound CCCCCCCC(C)C SGVYKUFIHHTIFL-UHFFFAOYSA-N 0.000 description 13
- GTJOHISYCKPIMT-UHFFFAOYSA-N 2-methylundecane Chemical compound CCCCCCCCCC(C)C GTJOHISYCKPIMT-UHFFFAOYSA-N 0.000 description 11
- VKPSKYDESGTTFR-UHFFFAOYSA-N isododecane Natural products CC(C)(C)CC(C)CC(C)(C)C VKPSKYDESGTTFR-UHFFFAOYSA-N 0.000 description 11
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- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 8
- 239000004205 dimethyl polysiloxane Substances 0.000 description 8
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 8
- CFJYNSNXFXLKNS-UHFFFAOYSA-N p-menthane Chemical compound CC(C)C1CCC(C)CC1 CFJYNSNXFXLKNS-UHFFFAOYSA-N 0.000 description 8
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 8
- 239000010408 film Substances 0.000 description 7
- 239000010410 layer Substances 0.000 description 7
- VATRWWPJWVCZTA-UHFFFAOYSA-N 3-oxo-n-[2-(trifluoromethyl)phenyl]butanamide Chemical compound CC(=O)CC(=O)NC1=CC=CC=C1C(F)(F)F VATRWWPJWVCZTA-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 6
- 239000012778 molding material Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 229910004283 SiO 4 Inorganic materials 0.000 description 5
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 description 4
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 4
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 description 4
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 4
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 4
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 4
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- 229920000642 polymer Polymers 0.000 description 4
- 235000012431 wafers Nutrition 0.000 description 4
- QPRQEDXDYOZYLA-UHFFFAOYSA-N 2-methylbutan-1-ol Chemical compound CCC(C)CO QPRQEDXDYOZYLA-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 230000005856 abnormality Effects 0.000 description 3
- 239000012459 cleaning agent Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000006482 condensation reaction Methods 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 3
- 229920005591 polysilicon Polymers 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- PFNHSEQQEPMLNI-UHFFFAOYSA-N 2-methyl-1-pentanol Chemical compound CCCC(C)CO PFNHSEQQEPMLNI-UHFFFAOYSA-N 0.000 description 2
- MSXVEPNJUHWQHW-UHFFFAOYSA-N 2-methylbutan-2-ol Chemical compound CCC(C)(C)O MSXVEPNJUHWQHW-UHFFFAOYSA-N 0.000 description 2
- MXLMTQWGSQIYOW-UHFFFAOYSA-N 3-methyl-2-butanol Chemical compound CC(C)C(C)O MXLMTQWGSQIYOW-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 125000000753 cycloalkyl group Chemical group 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
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000005227 gel permeation chromatography Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 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
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- KPSSIOMAKSHJJG-UHFFFAOYSA-N neopentyl alcohol Chemical compound CC(C)(C)CO KPSSIOMAKSHJJG-UHFFFAOYSA-N 0.000 description 2
- JYVLIDXNZAXMDK-UHFFFAOYSA-N pentan-2-ol Chemical compound CCCC(C)O JYVLIDXNZAXMDK-UHFFFAOYSA-N 0.000 description 2
- AQIXEPGDORPWBJ-UHFFFAOYSA-N pentan-3-ol Chemical compound CCC(O)CC AQIXEPGDORPWBJ-UHFFFAOYSA-N 0.000 description 2
- 229920002120 photoresistant polymer Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
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- 238000004544 sputter deposition Methods 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
- 238000012360 testing method Methods 0.000 description 2
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 2
- 125000003944 tolyl group Chemical group 0.000 description 2
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical class C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- RRQYJINTUHWNHW-UHFFFAOYSA-N 1-ethoxy-2-(2-ethoxyethoxy)ethane Chemical compound CCOCCOCCOCC RRQYJINTUHWNHW-UHFFFAOYSA-N 0.000 description 1
- TZYRSLHNPKPEFV-UHFFFAOYSA-N 2-ethyl-1-butanol Chemical compound CCC(CC)CO TZYRSLHNPKPEFV-UHFFFAOYSA-N 0.000 description 1
- CRWNQZTZTZWPOF-UHFFFAOYSA-N 2-methyl-4-phenylpyridine Chemical compound C1=NC(C)=CC(C=2C=CC=CC=2)=C1 CRWNQZTZTZWPOF-UHFFFAOYSA-N 0.000 description 1
- WVYWICLMDOOCFB-UHFFFAOYSA-N 4-methyl-2-pentanol Chemical compound CC(C)CC(C)O WVYWICLMDOOCFB-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 241001137862 IDIR agent Species 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
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- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229940019778 diethylene glycol diethyl ether Drugs 0.000 description 1
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 150000002367 halogens Chemical group 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229940035429 isobutyl alcohol Drugs 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 229940087305 limonene Drugs 0.000 description 1
- 235000001510 limonene Nutrition 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 125000005375 organosiloxane group Chemical group 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000007261 regionalization Effects 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3209—Amines or imines with one to four nitrogen atoms; Quaternized amines
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- 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
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/24—Hydrocarbons
- C11D7/242—Hydrocarbons branched
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/261—Alcohols; Phenols
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5022—Organic solvents containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5027—Hydrocarbons
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
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Abstract
本發明係提供一種洗淨劑組成物,其特徵為,為了去除殘留於基板上之聚矽氧系接著劑所使用之洗淨劑組成物中,含有(A)有機溶劑(但碳數3~6之醇除外)92.0質量%以上未達99.9質量%、(B)碳數3~6之醇,0.1質量%以上未達8.0質量%,及(C)四級銨鹽0.001質量%以上3.0質量%以下且上述(A)~(C)成分之總量為100質量%。
其效果為洗淨矽半導體基板等之基板時,可於短時間內得到良好之洗淨性,且不受接著劑污染、不會腐蝕基板可有效率洗淨基板。
Description
本發明係有關去除附著於半導體基板之聚矽氧系接著劑所使用之洗淨劑組成物及薄型基板之製造方法。
近年來隨著各種基板微細化及高積體化進展,例如於半導體實裝時,係藉由三次元實裝以實現進一步的高密度、大容量化。三次元半導體實裝技術係指,將單片半導體晶片薄型化後,藉由矽貫通電極(TSV;through silicon via)使該等連結的同時多層層合之半導體製作技術。為了實現該目的,需藉由對形成半導體電路之基板實施內面研削使其薄型化,再於內面形成含有TSV之電極等之電極形成步驟。薄型化時,曾有提案藉由介有接著劑接合形成半導體電路之基板到聚矽、玻璃等之支撐基板,而得可耐內面研削步驟及內面電極形成步驟等加工的系統。但上述步驟後需簡便剝離支撐基板,剝離支撐基板後需去除殘存於形成半導體電路之基板表面的接著劑,最後需洗淨薄膜半導體基板表面。又,加工步驟係使用
150℃以上之高溫,因此要求所使用之接著劑具有耐熱性。故多半係使用耐熱性良好之聚矽氧系接著劑。
但洗淨基板表面時,僅以溶解所使用之接著劑用之有機溶劑洗淨時係難充分去除接著劑,因基板表面之對水接觸角為100℃以上,故預測其後之製造步驟中會發生密封劑接合不良等之不宜情形。因此寄望於不會腐蝕基板表面可於短時間內充分去除殘存之接著劑之洗淨劑組成物。現階段尚未出現短時間內可充分洗淨被聚矽氧成分污染之基板表面的洗淨劑組成物。
又,與本發明相關連之先前技術如,下述專利公開公報所記載之半導體基板用洗淨劑組成物。特別是專利文獻2所記載之由有機溶劑及四級銨鹽所形成之洗淨劑組成物,但該洗淨劑組成物會有,因上述薄型半導體製造步驟複雜化,而藉由所使用之接著劑係無法解決基板上殘存接著劑之問題。
專利文獻1:日本特開2013-10888號公報
專利文獻2:日本特開平07-003294號公報
有鑑於上述事情,本發明之目的為,提供洗淨矽半導體基板等之基板時,相對於來自殘存於基板上之聚矽氧系接著劑的污染物可於短時間內得到良好洗淨性,且不會腐蝕基板可高效率洗淨基板之洗淨劑組成物,及薄型基板之製造方法。
本發明者們為了解決上述課題經專心檢討後發現,去除殘留於半導體基板等之基板上之聚矽氧系接著劑所使用的洗淨劑組成物中,含有(A)92.0質量%以上未達99.9質量%之碳數3~6之醇以外的有機溶劑、(B)0.1質量%以上未達8.0質量%之碳數3~6之醇,及(C)0.001質量%以上3.0質量%以下之四級銨鹽所形成的洗淨劑組成物,可於短時間內得到良好洗淨性,且相對於被聚矽氧系接著劑污染之基板可確實去除該聚矽氧系接著劑之污染物,不會腐蝕基板可高效率洗淨半導體基板,而完成本發明。
本發明之洗淨劑組成物係以一定比例含有上述(A)~(C)成分者,且為實質上不含水者。藉由使用該類洗淨劑組成物不會腐蝕基板可高效率洗淨基板。特別是洗淨洗淨對象之基板被聚矽氧系接著劑污染而具有100°以上之對水接觸角的矽半導體基板時,可有效發揮本發明之效果。即,可於短時間內充分洗淨基板進行薄型加工時被所使用之矽成分污染而使對水接觸角為100°以上之矽半
導體基板等之基板表面,結果可確實去除該污染物而使基板之對水接觸角未達100°。
因此本發明係提供下述洗淨劑組成物及薄型基板之製造方法。
〔1〕一種洗淨劑組成物,其特徵為去除殘留於基板上之聚矽氧系接著劑所使用之洗淨劑組成物中,含有(A)有機溶劑(但碳數3~6之醇除外)92.0質量%以上未達99.9質量%、(B)碳數3~6之醇0.1質量%以上未達8.0質量%,及,(C)四級銨鹽0.001質量%以上3.0質量%以下,且上述(A)~(C)成分之總量為100質量%。
〔2〕如〔1〕所記載之洗淨劑組成物,其中(C)成分為氫氧化四丁基銨。
〔3〕如〔1〕或〔2〕所記載之洗淨劑組成物,其中有機溶劑為碳數5~20之脂肪族烴。
〔4〕如〔1〕或〔2〕所記載之洗淨劑組成物,其中有機溶劑為碳數5~20之二烷二醇二烷基醚。
〔5〕如〔1〕~〔4〕中任一項所記載之洗淨劑組成物,其中基板為半導體基板。
〔6〕一種薄型基板之製造方法,其特徵為包含下述(a)~(d)步驟,(a)藉由接著劑組成物於基板或支撐基板上形成接著層後,介有該接著層接合上述基板與上述支撐基板之接合步驟、
(b)加工接合於上述支撐基板上之上述基板之加工步驟、(c)由上述支撐基板剝離上述加工後之上述基板之剝離步驟,及(d)藉由如〔1〕~〔4〕中任一項所記載之洗淨劑組成物而洗淨去除殘存於上述剝離後之基板上之接著層之洗淨去除步驟。
〔7〕如〔6〕所記載之薄型基板之製造方法,其中上述接著劑組成物為含有聚矽氧化合物之接著劑組成物。
〔8〕如〔7〕所記載之薄型基板之製造方法,其中上述聚矽氧化合物為,具有兩個以上鍵結於矽原子之羥基的直鏈狀或支鏈狀有機聚矽氧烷,與含有R3SiO2單位(R為單價烴基)及SiO2單位,且含有羥基之有機聚矽氧烷樹脂的(部分)脫水縮合物。
藉由本發明之洗淨劑組成物洗淨附著來自聚矽氧系接著劑之污染物的矽半導體基板等之基板時,可於短時間內良好洗淨,且不會腐蝕基板可高效率洗淨矽半導體基板等之基板。
下面將更詳細說明本發明。
本發明之洗淨劑組成物為,去除殘留於矽半導體基板
等之基板上之聚矽氧系接著劑所使用的洗淨劑組成物中,含有下述(A)~(C)成分(A)有機溶劑(但碳數3~6之醇除外)92.0質量%以上未達99.9質量%、(B)碳數3~6之醇0.1質量%以上未達8.0質量%,及(C)四級銨鹽0.001質量%以上3.0質量%以下,且上述(A)~(C)成分之總量為100質量%之組成物。
首先說明(A)成分,(A)有機溶劑如碳數5~20,較佳為碳數7~15,更佳為碳數8~12之脂肪族烴類。上述脂肪族烴類具體如,辛烷、壬烷、癸烷、十一烷、十二烷、十四烷、十六烷、異辛烷、異壬烷、異癸烷、異十二烷、烷基環己烷、p-薄荷烷等。該等可使用一種或二種以上組合使用。
又,(A)有機溶劑如碳數5~20,較佳為碳數6~15,更佳為碳數6~10之二烷二醇二烷基醚類。上述二烷二醇二烷基醚類具體如,二乙二醇二甲基醚、二乙二醇二乙基醚、二乙二醇二丁基醚、二丙二醇二甲基醚等。該等可使用一種或二種以上組合使用。
上述(A)成分之濃度為92.0質量%以上未達99.9質量%,上限值為減去(B)及(C)之合計量的殘部。上述(A)成分之濃度較佳為92.5質量%以上未達99.6質量%,更佳為93.8質量%以上未達99.6質量%。全體組成物中上述(A)成分之濃度未達92.0質量%時,將
無法溶解微量之接著劑成分會有洗淨性不足之可能性,僅使用有機溶劑並無洗淨效果。
又,本發明中藉由溶劑僅使用有機溶劑時,可減少以水為發生源之金屬污染而洗淨基板。因此本發明之組成物為實質上溶劑不含水者。
其次將說明(B)成分,(B)成分為碳數3~6之醇,係分子中含有至少1個羥基之物。(B)成分如碳數3~6,較佳為碳數3~5之飽和脂肪族醇類。上述飽和脂肪族單價醇類如,n-丙基醇、異丙基醇、1-丁醇、2-丁醇、異丁基醇、tert-丁基醇、1-戊醇、2-戊醇、3-戊醇、2-甲基-1-丁醇、異戊基醇、sec-丁基醇、tert-戊基醇、3-甲基-2-丁醇、新戊基醇、1-己醇、2-甲基-1-戊醇、4-甲基-2-戊醇、2-乙基-1-丁醇等。該等可使用一種或二種以上組合使用。
(B)成分之濃度為0.1質量%以上未達8.0質量%,較佳為0.4質量%以上未達7.5質量%,更佳為0.4質量%以上未達6.2質量%。全體組成物中(B)成分之濃度未達0.1質量%時會析出過剩之鹼成分,恐發生沈澱。相反地(B)成分之濃度為8.0質量%以上時會降低洗淨效果,或恐使液分離。
其次(C)成分為四級銨鹽,例如氫氧化四丁基銨等之四級銨鹽。上述(C)成分之添加量為0.001質量%以上3.0質量%以下,較佳為0.5~2.8質量%。上述(C)成分之濃度未達0.001質量%時將無法溶解微量之接
著劑成分,恐使洗淨性不足。相反地(C)成分之濃度超過3.0質量%時係無法改變洗淨效果,恐發生基板腐蝕等。
本發明之洗淨劑組成物為混合上述(A)~(C)成分及必要時所使用之其他成分所得者,各成分之混合順序於不會發生無法達成本發明之目的般發生沈澱或液分離等不宜之問題的範圍內,可以任意順序混合。即,洗淨劑組成物之各構成成分中,可預先添加二種成分或三種成分以上,其次再混合殘餘成分,或同時混合全部成分。
藉由本發明使用上述洗淨劑組成物洗淨、去除殘留於矽半導體基板等之基板上之聚矽氧系接著劑,可於短時間內洗淨上述基板,可以高效率良好洗淨矽半導體基板等之基板。
如上述般本發明之洗淨劑組成物為洗淨半導體基板等各種基板之表面用者,洗淨對象之基板非限定於矽半導體基板,例如可洗淨鍺基板、鎵-砷基板、鎵-磷基板、鎵-砷-鋁基板、鍍鋁矽基板、鍍銅矽基板、鍍銀矽基板、鍍金矽基板、鍍鈦矽基板、形成氮化矽膜之矽基板、形成氧化矽膜之矽基板、形成聚醯亞胺膜之矽基板、玻璃基板、石英基板、液晶基板、有機EL基板等之各種基板。
最近受人注目之TSV等之半導體封裝技術所使用的薄型基板之製造方法中使用本發明之洗淨劑組成物
係具有效果。具體為包含下述(a)~(d)步驟(a)藉由接著劑組成物於基板或支撐基板上形成接著層後,介有該接著層接合上述基板與上述支撐基板之接合步驟、(b)加工接合於上述支撐基板之上述基板之加工步驟、(c)由上述支撐基板剝離上述加工後之上述基板之剝離步驟,及(d)藉由洗淨劑組成物洗淨去除殘存於上述剝離後之基板上之接著層之洗淨去除步驟的製造方法中,上述(d)之洗淨去除步驟係使用本發明之洗淨劑組成物。
上述(a)步驟中接合基板與支撐基板之接著劑組成物可使用,由聚矽氧系、丙烯酸樹脂系、環氧樹脂系、聚醯胺系、聚苯乙烯系、聚醯亞胺系及苯酚樹脂系之至少一種中所選出之接著劑。特別是洗淨聚矽氧系之接著劑時,採用本發明之洗淨劑組成物係具有效果。
此時聚矽氧系接著劑較佳為,接著成分含有具有兩個以上鍵結與矽原子之羥基的直鏈狀或支鏈狀有機聚矽氧烷,與含有R3SiO2單位(R為單價烴基)與SiO2單位,且含有羥基之有機聚矽氧烷樹脂的(部分)脫水縮合物之物。
該直鏈狀或支鏈狀有機聚矽氧烷較佳為,下述一般式(1)所表示之有機聚矽氧烷。
(式中,R1、R2表示相同或相異之非取代或取代之碳數1~10之單價烴基,n為整數,特別是1,000~100,000之整數)。
R1、R2具體如,甲基、乙基、n-丙基、異丙基、n-丁基、tert-丁基、n-戊基、環戊基、n-己基等之烷基、環己基等之環烷基、苯基、甲苯基等之芳基等之單價烴基、該等基之部分或全部氫原子被鹵原子取代之基,較佳為甲基及苯基。
又,n較佳為1,000~100,000之整數,又以3,000~50,000為佳,更佳為5,000~10,000。
另外上述有機矽氧烷樹脂為R3SiO1/2單位(M單位)與SiO4/2單位(Q單位)之共聚物,R3SiO1/2單位與SiO4/2單位之莫耳比(R3SiO1/2/SiO4/2)較佳為0.6~1.7,特佳為0.8~1.5。又,RSiO3/2單位(T單位)、R2SiO2/2單位(D單位)可為全體共聚物之20莫耳%以下,特別是10莫耳%以下。
又,R為相同或相異之單價烴基,較佳為非取代或取代之碳數1~10之單價烴基或羥基。R具體如,甲基、乙基、n-丙基、異丙基、n-丁基、tert-丁基、n-戊基、環戊基、n-己基等之烷基、環己基等之環烷基、苯基、甲苯基等之單價烴基、該等基之部分或全部氫原子被
鹵原子取代之基、羥基等,較佳為甲基。
上述有機聚矽氧烷樹脂較佳為,一分子中鍵結於矽原子之羥基(矽烷醇基)之含有比例較佳為0.12~0.02莫耳%/100g,特佳為0.10~0.04莫耳%/100g。又,有機聚矽氧烷樹脂藉由凝膠滲透色譜(GPC)以聚苯乙烯換算之重量平均分子量較佳為500~20,000,特佳為1,000~10,000。
上述直鏈狀或支鏈狀有機聚矽氧烷與有機聚矽氧烷樹脂之(部分)脫水縮合物可由,使用質量比為99:1~50:50,較佳為98:2~85:15,更佳為97:3~90:10之前者與後者,藉由常法進行(部分)脫水縮合反應所得。
該類所得之(部分)脫水縮合物之重量平均分子量較佳為200,000~2,000,000,特佳為350,000~1,500,000。
上述聚矽氧系接著劑為,以相對於上述脫水縮合物100質量份含有約400~1,000,000質量份之壬烷、異十二烷、p-薄荷烷等之有機溶劑所得之溶液形態使用,藉由塗佈、乾燥該溶液而形成所希望之被膜之物。又,聚矽氧系接著劑可添加防氧化劑、顏料、染料、填充劑等之各種添加劑。
上述(a)步驟所使用之接著層厚度無特別限制,可因應目的適當調整,較佳為1~500μm,特佳為10~200μm。又,必要時支撐基板與接著層之間可適當形成硬化層等之其他層合物。此時之任意層合物較佳以剝離
支撐基板時可一起剝離般之方式形成。
上述(a)步驟中支撐基板如,矽基板、玻璃基板、石英基板等之基板。該等基板或支撐基板可藉由旋轉塗佈機等之已知塗佈技術塗佈一定厚度般之接著劑組成物而貼合。
另外介有接著層接合與支撐基板之基板為,表面形成電路等,且內面可加工之半導體基板等之基板。
上述(b)步驟為,加工接合於上述支撐基板之基板的加工步驟。該步驟具體為,藉由相對於接合支撐基板之半導體基板等的基板之內面實施切削、研磨等加工,而使基板薄板化。該步驟係包含晶圓水準下所使用之各種步驟。其具體例如,形成電極、形成金屬配線及形成保護膜等。更具體如,形成電極用之金屬濺鍍、蝕刻金屬濺鍍層之濕蝕、製作形成金屬配線之遮罩用之塗佈光阻膜、藉由曝光及顯像形成圖形、剝離光阻膜、乾蝕、形成金屬鍍層、形成TSV用之矽蝕刻、矽表面形成氧化膜等先前已知之半導體步驟。
又,使基板薄板化得薄型基板用之厚度無特別限制,典型上可加工為5~300μm,特別是10~100μm。
上述(c)步驟為,由上述支撐基板剝離加工後之上述基板的步驟,具體上係藉由機械剝離、溶劑剝離等之剝離方法,由支撐基板剝離基板。又,如上述(a)步驟所說明般,上述基板與上述支撐基板係介有接著層接合,但較佳為上述接著層係與支撐基板一體化後被剝離。
但上述(c)步驟未必能完全剝離附著於支撐基板側之接著劑,會使部分殘留於加工後之基板上。因此(d)步驟中係藉由上述本發明之洗淨劑組成物洗淨附著殘留之接著劑的基板表面,可充分分離去除基板上之接著劑。
即,上述(d)步驟為,藉由上述本發明之洗淨劑組成物洗淨去除殘存於之剝離後基板上之接著層的步驟,以去除殘留於基板之接著劑用的洗淨去除步驟,具體上係將殘留接著劑之薄型基板浸漬於成分適當調整後之洗淨劑溶液中,使用超音波洗淨等之方法,以洗淨去除上述接著劑。使用超音波洗淨時,其洗淨條件可依基板表面之狀態而適當選擇,例如藉由條件為20kHz~5MHz、10秒~30分鐘之洗淨處理,可充分去除殘存於基板上之接著劑。
又,上述(d)步驟較佳為,預先將基板預浸於各種溶劑中。預浸用溶劑無特別限制,可為能溶解所使用之接著劑之物,具體如,壬烷、戊烷、己烷、環己烷、癸烷、異十二烷及檸檬烯等。又,必要時上述浸漬步驟可適當加溫,具體上又以溫度10~80℃,較佳為15~65℃下30秒~30分鐘之條件浸漬,以去除殘餘之接著劑為佳。
如上述般本發明之薄型基板之製造方法的特徵為,包含上述(a)~(d)步驟,但也可包含上述(a)~(d)步驟以外之各種已知步驟,又,上述(a)~(d)步驟所記載之構成要素及方法要素於未脫離本發明要旨之範圍內可進行各種變更。
下面將舉實施例及比較例具體說明本發明,但本發明非限定於下述實施例。
四口燒瓶內將分子鏈兩末端被羥基封鏈之生橡膠狀二甲基聚矽氧烷(一般式(1)中,n為9,000)中,其30質量%甲苯溶液之25℃下黏度為98,000mPa.s之二甲基聚矽氧烷90質量份,與由(CH3)3SiO1/2單位0.75莫耳及SiO4/2單位1莫耳之比例所形成,且固體成分100g中含有1.0莫耳%之羥基的重量平均分子量5,000之甲基聚矽氧烷樹脂10質量份,溶解於甲苯900質量份中。將28質量%之氨水1質量份加入所得之溶液中,室溫下攪拌24小時進行縮合反應。其次於減壓狀態下加熱至180℃以去除甲苯、縮合水、氨等,得固體化之部分脫水縮合物。將甲苯900質量份加入該部分脫水縮合物100質量份中使其溶解。將六甲基二矽氮烷20質量份加入該溶液中,130℃下攪拌3小時將殘存之羥基封鏈。其次於減壓狀態下加熱至180℃以去除溶劑等,得固體化之非反應性部分脫水縮合物。又,將己烷900質量份加入上述非反應性部分脫水縮合物100質量份中,溶解後將其投入2,000質量份之丙酮中,回收所析出之樹脂後真空下去除己烷等,得分子量
740以下之低分子量成分為0.05質量%,重量平均分子量900,000之二甲基聚矽氧烷聚合物。得由上述二甲基聚矽氧烷聚合物10質量份與壬烷90質量份所形成「聚矽氧化合物壬烷溶液接著劑No.1」。
四口燒瓶內將分子鏈兩末端被羥基封鏈之生橡膠狀二甲基聚矽氧烷(一般式(1)中,n為9,000)中,其30質量%甲苯溶液之25℃下黏度為98,000mPa.s的二甲基聚矽氧烷95質量份,與由(CH3)3SiO1/2單位0.75莫耳及SiO4/2單位1莫耳之比例所形成,且固體成分100g中含有1.0莫耳%之羥基的重量平均分子量5,000之甲基聚矽氧烷樹脂5質量份,溶解於甲苯900質量份中。將28質量%之氨水1質量份加入所得溶液中,室溫下攪拌24小時進行縮合反應。其次於減壓狀態下加熱至180℃以去除甲苯、縮合水、氨等,得固體化之部分脫水縮合物。將甲苯900質量份加入該部分脫水縮合物100質量份中使其溶解。將六甲基二矽氮烷20質量份加入該溶液中,130℃下攪拌3小時將殘存之羥基封鏈。其次於減壓狀態下加熱至180℃以去除溶劑等,得固體化之非反應性部分脫水縮合物。另外將己烷900質量份加入上述非反應性部分脫水縮合物100質量份中,溶解後將其投入2,000質量份之丙酮中,再回收所析出之樹脂,其後於真空下去除己烷等,得分子量740以下之低分子量成分為0.05質量%的重量平均
分子量為800,000之二甲基聚矽氧烷聚合物。得由上述二甲基聚矽氧烷聚合物10質量份與壬烷90質量份所形成之「聚矽氧化合物壬烷溶液接著劑No.2」。
使用上述聚矽氧化合物壬烷溶液接著劑,將其旋轉塗佈於8英寸矽半導體基板(直徑200mm、厚725μm)上形成膜厚10μm之接著層。以8英寸玻璃基板(玻璃晶圓)做為支撐基板,於真空接合裝置內以200℃接合該支撐基板與具有接著層之矽半導體基板,製造由矽半導體基板、接著層及支撐基板所形成之層合體。其使用研磨機進行矽半導體基板內面研削,將其研磨(grind)至使最終基板厚度為50μm。接著將層合基板中矽半導體基板水平固定,剝離支撐基板後浸漬於壬烷中5分鐘再乾燥,得洗淨試驗用矽半導體基板。此時,將附著於支撐基板之約10質量%的接著層由基板去除,又藉由壬烷浸漬可去除基板上殘存之接著層約99質量%,但洗淨試驗用矽半導體基板會殘存約1質量%之接著層。其次下述實施例1~11及比較例1~4係以聚矽氧化合物壬烷溶液接著劑No.1、實施例12~15及比較例5~7係以聚矽氧化合物壬烷溶液接著劑No.2作為聚矽氧化合物壬烷溶液接著劑用。
將10質量%氫氧化四丁基銨/2-丙醇溶液2.00g、異
十二烷98.00g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物A。
將10質量%氫氧化四丁基銨/2-丙醇溶液5.00g、異十二烷95.00g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物B。
將10質量%氫氧化四丁基銨/2-丙醇溶液7.00g、異十二烷93.00g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物C。
將10質量%氫氧化四丁基銨/2-丙醇溶液2.50g、異十二烷97.50g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物D。
將10質量%氫氧化四丁基銨/2-丙醇2.50g、二丙二醇二甲基醚97.50g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物E。
將10質量%氫氧化四丁基銨/2-丙醇溶液2.50g、異辛烷97.50g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物F。
將10質量%氫氧化四丁基銨/2-丙醇溶液2.50g、異壬烷97.50g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物G。
將10質量%氫氧化四丁基銨/2-丙醇溶液2.50g、p-薄荷烷97.50g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物H。
將10質量%氫氧化四丁基銨/2-丙醇溶液8.00g、異辛烷92.00g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物I。
將10質量%氫氧化四丁基銨/2-丙醇溶液5.00g、異壬烷95.00g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物J。
將17質量%氫氧化四丁基銨/2-丙醇溶液7.94g、異十二烷92.06g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物K。
將17質量%氫氧化四丁基銨/2-丙醇溶液1.47g、1-丁醇1.00g及異辛烷97.53g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物L。
將17質量%氫氧化四丁基銨/2-丙醇溶液2.94g、1-戊醇1.00g及異壬烷96.06g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物M。
將17質量%氫氧化四丁基銨/2-丙醇溶液5.88g、1-己醇1.00g及p-薄荷烷93.12g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物N。
將10質量%氫氧化四丁基銨/2-丙醇溶液2.50g、異十二烷96.36g及二丙二醇二甲基醚1.14g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物O。
將2-丙醇溶液2.00g、異十二烷98.00g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌,得洗淨劑組成物R。
將2-丙醇溶液5.00g、異壬烷95.00g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌,得洗淨劑組成物S。
將10質量%氫氧化四丁基銨/2-丙醇溶液2.50g、水1.00g、二丙二醇二甲基醚96.50g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物T。
將10質量%氫氧化四丁基銨/2-丙醇溶液8.00g、1-
丁醇2.00g、異十二烷90.00g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物U。
將17質量%氫氧化四丁基銨/2-丙醇溶液11.76g、二丙二醇二甲基醚88.24g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物V。
將40質量%氫氧化四丁基銨/水溶液0.63g及二丙二醇二甲基醚99.37g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌至均勻,得洗淨劑組成物W。
將40質量%氫氧化四丁基銨/水溶液2.00g及異十二烷98.00g放入備有攪拌裝置、冷卻裝置及溫度計之500ml燒瓶內,室溫下攪拌,得洗淨劑組成物X。
其次使用上述所得之實施例之洗淨劑組成物A~O及比較例之洗淨劑組成物R~X,藉由超音波洗淨上述矽半導體基板。超音波洗淨係以周波數1MHz×5分鐘之條件進行。以下述基準評估各例之洗淨劑組成物。又,測
定實施例5、9、15及比較例1、4、7洗淨後之矽半導體基板與成型材料之接合力。結果如表1、2(實施例)及表3(比較例)所示。
以目視確定上述各例之洗淨劑組成物外觀。確認是否有沈澱物析出或水層分離等不宜情形,又,以「○」表示確認無異常者,以「×」表示確認異常者。
使用上述各例之洗淨劑組成物洗淨所製作之矽半導體基板。具體為,將矽半導體基板浸漬於洗淨劑組成物中5分鐘後,以流動純水清洗矽半導體基板表面1分鐘,再乾燥。觀察乾燥後之矽半導體基板表面,以「○」表示基板表面無異常,基板表面與聚矽氧化合物壬烷溶液接著劑塗佈前同等者,以「×」表示基板表面確認霧化或腐蝕等異常者。
使用上述各例之洗淨劑組成物洗淨所製作之矽半導體基板。具體為,將矽半導體基板浸漬於洗淨劑組成物中5分鐘後,以流動純水清洗矽半導體基板表面1分鐘,再乾燥。確認乾燥後矽半導體基板表面之對水接觸角。洗淨前之對水接觸角為108°,表1~3係表示浸漬5分鐘再洗淨後
之對水接觸角。
使用上述各例之洗淨劑組成物洗淨所製作之矽半導體基板。具體為,將矽半導體基板浸漬於洗淨劑組成物中5分鐘後,以流動純水清洗矽半導體基板表面1分鐘,再乾燥。藉由X線光電子分光分析裝置分析乾燥後之矽半導體基板表面。洗淨前基板表面之聚矽氧含有率為22質量%,洗淨後基板表面之聚矽氧含有率為5質量%以下時為容許範圍。表1~3係表示洗淨後基板表面殘存之聚矽氧含有率。
使用上述各例之洗淨劑組成物洗淨所製作之矽半導體基板。具體為,將矽半導體基板浸漬於洗淨劑組成物中5分鐘後,以流動純水清洗矽半導體基板表面1分鐘,再乾燥。相對於乾燥後矽半導體基板之表面,以剖面積為5mm方式使成型材料(信越化學工業公司製之製品名「SMC-375TGF-6」)成型,再藉由第一階段(120℃、30分鐘)及第二階段(165℃、3小時)二階段而使上述成型材料硬化。硬化後藉由DAGE公司製之萬能型黏著測試機「SERIE4000PXY」,測定矽半導體基板與成型材料之接合力。又,洗淨前矽半導體基板之接合力為0.2MPa。
由上述表1~3之結果得知,藉由本發明(各實施例)之洗淨劑組成物洗淨矽半導體基板時,可於短時間內得到良好洗淨性,且不會腐蝕基板可高效率洗淨矽半導體基板。
又,有關洗淨後矽半導體基板與成型材料之接合力,得知本發明(實施例5、9、15)方面相對於比較例1、4、7可具有格外高之接合力。
Claims (8)
- 一種洗淨劑組成物,其特徵為去除殘留於基板上之聚矽氧系接著劑所使用之洗淨劑組成物,其中含有(A)有機溶劑(但碳數3~6之醇除外)92.0質量%以上未達99.9質量%、(B)碳數3~6之醇,0.1質量%以上未達8.0質量%,及,(C)四級銨鹽0.001質量%以上3.0質量%以下,且上述(A)~(C)成分之總量為100質量%。
- 如請求項1之洗淨劑組成物,其中(C)成分為氫氧化四丁基銨。
- 如請求項1或2之洗淨劑組成物,其中(A)有機溶劑為碳數5~20之脂肪族烴。
- 如請求項1或2之洗淨劑組成物,其中(A)有機溶劑為碳數5~20之二烷二醇二烷基醚。
- 如請求項1~4中任一項之洗淨劑組成物,其中基板為半導體基板。
- 一種薄型基板之製造方法,其特徵為包含下述(a)~(d)步驟,(a)藉由接著劑組成物於基板或支撐基板上形成接著層後,介有該接著層接合上述基板與上述支撐基板之接合步驟、(b)加工接合於上述支撐基板之上述基板之加工步驟、(c)由上述支撐基板剝離上述加工後之上述基板之剝離 步驟,及(d)藉由如請求項1~4中任一項之洗淨劑組成物洗淨去除殘存於之上述剝離後基板上之接著層。
- 如請求項6之薄型基板之製造方法,其中上述接著劑組成物為含有聚矽氧化合物之接著劑組成物。
- 如請求項7之薄型基板之製造方法,其中聚矽氧化合物為,具有兩個以上鍵結於矽原子之羥基的直鏈狀或支鏈狀有機聚矽氧烷,與含有R3SiO2單位(R為單價烴基)及SiO2單位,且含有羥基之有機聚矽氧烷樹脂的(部分)脫水縮合物。
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