TWI514641B - 用於電子裝置或其他物件上之塗層中之混合層 - Google Patents
用於電子裝置或其他物件上之塗層中之混合層 Download PDFInfo
- Publication number
- TWI514641B TWI514641B TW096141151A TW96141151A TWI514641B TW I514641 B TWI514641 B TW I514641B TW 096141151 A TW096141151 A TW 096141151A TW 96141151 A TW96141151 A TW 96141151A TW I514641 B TWI514641 B TW I514641B
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- Prior art keywords
- mixed layer
- mixed
- layer
- precursor material
- vapor deposition
- Prior art date
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- 238000000576 coating method Methods 0.000 title claims description 37
- 239000000463 material Substances 0.000 claims description 174
- 239000002243 precursor Substances 0.000 claims description 78
- 238000000034 method Methods 0.000 claims description 72
- 238000000151 deposition Methods 0.000 claims description 53
- 238000006243 chemical reaction Methods 0.000 claims description 42
- 239000007789 gas Substances 0.000 claims description 38
- 239000000203 mixture Substances 0.000 claims description 34
- 230000008021 deposition Effects 0.000 claims description 33
- 239000011248 coating agent Substances 0.000 claims description 31
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 28
- 239000001301 oxygen Substances 0.000 claims description 27
- 229910052760 oxygen Inorganic materials 0.000 claims description 27
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 27
- 229920000642 polymer Polymers 0.000 claims description 20
- 238000005229 chemical vapour deposition Methods 0.000 claims description 17
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- -1 hydrazine compound Chemical class 0.000 claims description 15
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 14
- 239000012495 reaction gas Substances 0.000 claims description 14
- 229910052707 ruthenium Inorganic materials 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 12
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- 238000005137 deposition process Methods 0.000 claims description 10
- 238000011282 treatment Methods 0.000 claims description 10
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052804 chromium Inorganic materials 0.000 claims description 7
- 239000011651 chromium Substances 0.000 claims description 7
- YTPFRRRNIYVFFE-UHFFFAOYSA-N 2,2,3,3,5,5-hexamethyl-1,4-dioxane Chemical compound CC1(C)COC(C)(C)C(C)(C)O1 YTPFRRRNIYVFFE-UHFFFAOYSA-N 0.000 claims description 5
- GPBBNPPLBQIADY-UHFFFAOYSA-N 4,4-dimethyloxane Chemical compound CC1(C)CCOCC1 GPBBNPPLBQIADY-UHFFFAOYSA-N 0.000 claims description 5
- 229910052732 germanium Inorganic materials 0.000 claims description 5
- 238000009832 plasma treatment Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N hydrazine Substances NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 claims description 3
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- 238000002329 infrared spectrum Methods 0.000 claims description 2
- 238000002834 transmittance Methods 0.000 claims description 2
- 238000002211 ultraviolet spectrum Methods 0.000 claims description 2
- 238000007740 vapor deposition Methods 0.000 claims description 2
- 229910010272 inorganic material Inorganic materials 0.000 claims 2
- 239000011147 inorganic material Substances 0.000 claims 2
- 229910052747 lanthanoid Inorganic materials 0.000 claims 1
- 150000002602 lanthanoids Chemical class 0.000 claims 1
- 239000010410 layer Substances 0.000 description 215
- 230000004888 barrier function Effects 0.000 description 21
- 239000010408 film Substances 0.000 description 20
- 239000000758 substrate Substances 0.000 description 16
- 230000007613 environmental effect Effects 0.000 description 15
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- 239000000356 contaminant Substances 0.000 description 11
- 229920001721 polyimide Polymers 0.000 description 11
- 229910004298 SiO 2 Inorganic materials 0.000 description 10
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 9
- 239000011541 reaction mixture Substances 0.000 description 9
- 230000035699 permeability Effects 0.000 description 8
- 230000003746 surface roughness Effects 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 6
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 6
- 230000001737 promoting effect Effects 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000004642 Polyimide Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 229910000420 cerium oxide Inorganic materials 0.000 description 4
- 229910052729 chemical element Inorganic materials 0.000 description 4
- 239000011888 foil Substances 0.000 description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 4
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000013047 polymeric layer Substances 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
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- 229920006254 polymer film Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 150000003304 ruthenium compounds Chemical class 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 2
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- 238000000255 optical extinction spectrum Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- KDTWXGUXWNBYGS-UHFFFAOYSA-N 1,2,3,3,4,4-hexamethyl-5H-diazepine Chemical compound CC1(C(N(N(C=CC1)C)C)(C)C)C KDTWXGUXWNBYGS-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- HSTCJLDQVIIDKF-UHFFFAOYSA-N 1-phenyldecylbenzene Chemical compound C=1C=CC=CC=1C(CCCCCCCCC)C1=CC=CC=C1 HSTCJLDQVIIDKF-UHFFFAOYSA-N 0.000 description 1
- UOWGDUWBNYEAQL-UHFFFAOYSA-N 10,13-dimethyldocosane Chemical compound CCCCCCCCCC(C)CCC(C)CCCCCCCCC UOWGDUWBNYEAQL-UHFFFAOYSA-N 0.000 description 1
- OFDDDOPWYXZDKQ-UHFFFAOYSA-N 11,11-dimethylhenicosane Chemical compound CCCCCCCCCCC(C)(C)CCCCCCCCCC OFDDDOPWYXZDKQ-UHFFFAOYSA-N 0.000 description 1
- IANXAXNUNBAWBA-UHFFFAOYSA-N 2,2,3-trimethylundecane Chemical compound CCCCCCCCC(C)C(C)(C)C IANXAXNUNBAWBA-UHFFFAOYSA-N 0.000 description 1
- GCZWJRLXIPVNLU-UHFFFAOYSA-N 2,2-dimethoxy-3-methylundecane Chemical compound CC(C(OC)(OC)C)CCCCCCCC GCZWJRLXIPVNLU-UHFFFAOYSA-N 0.000 description 1
- QDKSGHXRHXVMPF-UHFFFAOYSA-N 2,2-dimethylundecane Chemical compound CCCCCCCCCC(C)(C)C QDKSGHXRHXVMPF-UHFFFAOYSA-N 0.000 description 1
- FZUMQFUHECRZDF-UHFFFAOYSA-N 2-methylundecan-2-ylbenzene Chemical compound CCCCCCCCCC(C)(C)C1=CC=CC=C1 FZUMQFUHECRZDF-UHFFFAOYSA-N 0.000 description 1
- GTJOHISYCKPIMT-UHFFFAOYSA-N 2-methylundecane Chemical compound CCCCCCCCCC(C)C GTJOHISYCKPIMT-UHFFFAOYSA-N 0.000 description 1
- LDTSPHKYHWKPDN-UHFFFAOYSA-N 3-tert-butylundec-1-ene Chemical compound C(=C)C(C(C)(C)C)CCCCCCCC LDTSPHKYHWKPDN-UHFFFAOYSA-N 0.000 description 1
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- MALRERHOIDQYND-UHFFFAOYSA-N CC(C(N(C(C)=O)C)(N(C(C)=O)C)C=C)CCCCCCCC Chemical compound CC(C(N(C(C)=O)C)(N(C(C)=O)C)C=C)CCCCCCCC MALRERHOIDQYND-UHFFFAOYSA-N 0.000 description 1
- JWZSLFITTJTUNW-UHFFFAOYSA-N CC(CCCCCCCCCN=C=NCCCCCCCCCC(C)(C)C)(C)C Chemical compound CC(CCCCCCCCCN=C=NCCCCCCCCCC(C)(C)C)(C)C JWZSLFITTJTUNW-UHFFFAOYSA-N 0.000 description 1
- JIAQPKMRKIMXHV-UHFFFAOYSA-N CCCCCCCCC(C)C(ON(CC)CC)(ON(CC)CC)ON(CC)CC Chemical compound CCCCCCCCC(C)C(ON(CC)CC)(ON(CC)CC)ON(CC)CC JIAQPKMRKIMXHV-UHFFFAOYSA-N 0.000 description 1
- KMPSFPWSBZMKDS-UHFFFAOYSA-N COC1(OC(C(OC1)(OC)OC)(OC)OC)OC Chemical compound COC1(OC(C(OC1)(OC)OC)(OC)OC)OC KMPSFPWSBZMKDS-UHFFFAOYSA-N 0.000 description 1
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- 229920002675 Polyoxyl Polymers 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- DHXVGJBLRPWPCS-UHFFFAOYSA-N Tetrahydropyran Chemical compound C1CCOCC1 DHXVGJBLRPWPCS-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
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- 238000010521 absorption reaction Methods 0.000 description 1
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- 125000000217 alkyl group Chemical group 0.000 description 1
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- 125000004429 atom Chemical group 0.000 description 1
- 239000003124 biologic agent Substances 0.000 description 1
- 239000012472 biological sample Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
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- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- HOWGUJZVBDQJKV-UHFFFAOYSA-N docosane Chemical compound CCCCCCCCCCCCCCCCCCCCCC HOWGUJZVBDQJKV-UHFFFAOYSA-N 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
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- 239000003814 drug Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- HLXZNVUGXRDIFK-UHFFFAOYSA-N nickel titanium Chemical compound [Ti].[Ti].[Ti].[Ti].[Ti].[Ti].[Ti].[Ti].[Ti].[Ti].[Ti].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni] HLXZNVUGXRDIFK-UHFFFAOYSA-N 0.000 description 1
- 229910001000 nickel titanium Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 238000000399 optical microscopy Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 125000000082 organogermanium group Chemical group 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 150000002924 oxiranes Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 150000003839 salts Chemical class 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
- 239000002356 single layer Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/24—Deposition of silicon only
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/401—Oxides containing silicon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/505—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using radio frequency discharges
- C23C16/509—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using radio frequency discharges using internal electrodes
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Description
本發明係關於一種用於電子裝置之障壁塗層。
諸如有機發光裝置(OLED)之有機電子裝置當暴露至水蒸氣或氧氣時易遭受降級。OLED上用以減少其暴露至水蒸氣或氧氣之保護性障壁塗層可有助於改良裝置之壽命及效能。已成功用於食物包裝之氧化矽、氮化矽或氧化鋁之薄膜已被考慮為用作OLED之障壁塗層。然而，此等無機薄膜傾向於含有微觀缺陷，會使某些水蒸氣及氧氣通過薄膜擴散。在某些狀況下，該等缺陷會在脆性之薄膜中造成裂痕。雖然如此之水及氧氣擴散對於食品為可接受的，但是對於OLED則係不可接受的。為解決此等問題，已針對OLED嚐試使用交替之無機及聚合物層之多層障壁塗層且發現對水蒸氣及氧氣滲透具有改良之抵抗性。但是此等多層塗層具有複雜性及成本上的劣勢。因此，仍存在對形成適合用於保護OLED之障壁塗層之其他方法的需要。
在一態樣中，本發明提供一種用於在表面上形成塗層之方法，其包含：提供前驅物材料來源；將前驅物材料傳送至鄰近待塗佈之表面之反應位置；及使用前驅物材料來源藉由化學氣相沈積而在表面上沈積混合層，其中混合層包含聚合材料與非聚合材料之混合物，其中聚合材料與非聚合材料之重量比在95：5至5：95之範圍中，且其中聚合材料及非聚合材料由同一前驅物材料來源產生。
在另一態樣中，本發明提供一種用於在表面上形成多層塗層之方法，其包含：提供前驅物材料來源；將前驅物材料傳送至鄰近待塗佈之表面之反應位置；及使用前驅物材料來源藉由化學氣相沈積而在表面上沈積複數個混合層，其中每一混合層獨立地包含聚合材料與非聚合材料之混合物，其中聚合材料與非聚合材料之重量比在95：5至5：95之範圍中，且其中聚合材料及非聚合材料由同一前驅物來源產生。
在另一態樣中，本發明提供一種形成塗層之方法，該塗層具有與上面沈積塗層之表面的改良之界面內聚力，該方法包含：提供具有表面之基板；預處理待塗佈之表面；提供前驅物材料來源；將前驅物材料傳送至鄰近經預處理之表面之反應位置；及使用前驅物材料來源藉由化學氣相沈積而在表面上沈積混合層，其中混合層包含聚合材料與非聚合材料之混合物，其中聚合材料與非聚合材料之重量比在95：5至5：95之範圍中，且其中聚合材料及非聚合材料由同一前驅物材料來源產生。
在另一態樣中，本發明提供一種保護安置於充當電子裝置之基礎之表面上的電子裝置之方法，其包含：在電子裝置上形成塗層，包含以下步驟：(a)提供前驅物材料來源；(b)將前驅物材料傳送至鄰近待塗佈之電子裝置之反應位置；及(c)使用前驅物材料來源藉由化學氣相沈積而在電子裝置上沈積混合層，其中混合層包含聚合材料與非聚合材料之混合物，其中聚合材料與非聚合材料之重量比在95：5至5：95之範圍中，且其中聚合材料及非聚合材料由同一前驅物材料來源產生。
在另一態樣中，本發明提供一種用於控制形成於表面上之塗層之性質的方法，其包含：提供前驅物材料來源；將前驅物材料傳送至鄰近待塗佈之表面之反應位置；使用前驅物材料來源藉由化學氣相沈積而在表面上沈積混合層，其中混合層包含聚合材料與非聚合材料之混合物，其中聚合材料與非聚合材料之重量比在95：5至5：95之範圍中，且其中聚合材料及非聚合材料由同一前驅物材料來源產生；及控制沈積混合物層時之條件。
在一態樣中，本發明提供一種用於在表面上形成塗層之方法。該方法包含在表面上沈積包含聚合材料與非聚合材料之混合物之混合層。混合層可具有單一相或多個相。
如本文中所使用，術語"非聚合"指由具有含單一、良好界定之分子量的良好界定之化學式的分子構成之材料。"非聚合"分子可具有顯著較大之分子量。在一些情形下，非聚合分子可包括重複單元。如本文中所使用，術語"聚合"指由具有共價鏈接之重複子單元之分子構成且具有可因分子而改變之分子量(因為聚合反應可導致每一分子具有不同數目之重複單元)的材料。聚合物包括(但不限於)均聚物及諸如嵌段、接枝、無規或交替共聚物之共聚物，以及摻合物及其改質型式。聚合物包括(但不限於)碳或矽之聚合物。
如本文中所使用，"聚合材料與非聚合材料之混合物"指一般熟習此項技術者將理解為非純聚合亦非純非聚合之組合物。術語"混合物"意欲排除含有附帶量之非聚合材料(舉例而言，可自然存在於聚合材料之間隙中)但一般熟習此項技術者將仍認為係純聚合之任何聚合材料。同樣，此意欲排除含有附帶量之聚合材料但一般熟習此項技術者將仍認為係純非聚合之任何非聚合材料。在某些狀況下，混合層中之聚合材料與非聚合材料之重量比在95：5至5：95之範圍中，且較佳在90：10至10：90的範圍中，且更佳地，在25：75至10：90之範圍中。
可使用包括小水滴之濕潤接觸角、IR吸收、硬度及可撓性之各種技術來確定層之聚合/非聚合組合物。在某些情形下，混合層具有在30°至85°之範圍中，且較佳在30°至60°之範圍中，且更佳在36°至60°的範圍中的濕潤接觸角。注意，濕潤接觸角為剛沈積之薄膜之表面上之組合物(在進行確定時)之量測。因為濕潤接觸角可隨沈積後處理極大地改變，所以，在此等處理之後進行之量測可能未精確地反映層之組合物。咸信此等濕潤接觸角適用於由有機矽前驅物形成之廣泛範圍之層。在某些情形下，混合層具有在3 GPa至20 GPa之範圍中，且較佳在10 GPa至18 GPa之範圍中的奈米壓痕硬度。在某些情形下，混合層具有在0.1 nm至10 nm之範圍中，且較佳在0.2 nm至0.35 nm之範圍中的表面粗糙度(均方根)。在某些情形下，混合層當在50 μm厚之聚醯亞胺箔片基板上沈積為4 μm厚之層時充分可撓，使得以0.2%之拉伸應變(ε)在1英吋直徑滾筒上至少55,000個輥紮循環之後未觀測到微結構改變。在某些情形下，混合層充分可撓，使得在至少0.35%之拉伸應變(ε)(如一般熟習此項技術者認為，通常可使4 μm純氧化矽層裂開之拉伸應變位準)下未呈現裂痕。
術語"混合物"意欲包括具有單一相之組合物以及具有多個相之組合物。因此，"混合物"排除隨後沈積之交替聚合及非聚合層。換言之，為了被視為"混合物"，層應在相同反應條件下且/或在相同時間沈積。
混合層係使用前驅物材料之單一來源藉由化學氣相沈積而形成。如本文中所使用，"前驅物材料之單一來源"指當在存在或不存在反應氣體之情形下藉由CVD來沈積前驅物材料時提供形成聚合材料及非聚合材料所必需之所有前驅物材料的來源。此意欲排除聚合材料係使用一前驅物材料而形成且非聚合材料係使用不同前驅物材料而形成之方法。藉由使用前驅物材料之單一來源，沈積製程得以簡化。舉例而言，前驅物材料之單一來源將消除對前驅物材料之獨立流的需要及供應並控制獨立流之伴隨需要。
前驅物材料可為單一化合物或化合物之混合物。在前驅物材料為化合物之混合物之情形下，在某些狀況下，混合物中之不同化合物中之每一者自身能夠獨立地充當前驅物材料。舉例而言，前驅物材料可為六甲基二矽氧烷(HMDSO)與二甲基矽氧烷(DMSO)之混合物。
在某些狀況下，電漿增強型CVD(PE－CVD)可用於沈積混合層。出於各種原因(包括低溫沈積、均勻塗層形成及可控制之製程參數)PE－CVD可為所要的。適用於本發明之各種PE－CVD製程在此項技術中已知，包括使用RF能量以產生電漿之製程。
前驅物材料為能夠在藉由化學氣相沈積沈積時形成聚合材料及非聚合材料兩者之材料。各種此等前驅物材料適用於本發明且針對其各種特性加以選擇。舉例而言，前驅物材料可針對其化學元素之含量、其化學元素之化學計量比及/或在CVD下形成之聚合材料及非聚合材料來加以選擇。舉例而言，諸如矽氧烷類之有機矽化合物為適合用作前驅物材料之化合物類。矽氧烷化合物之代表性實例包括六甲基二矽氧烷(HMDSO)及二甲基矽氧烷(DMSO)。當藉由CVD沈積時，此等矽氧烷化合物能夠形成聚合材料(諸如，聚矽氧聚合物)及非聚合材料(諸如，氧化矽)。前驅物材料亦可針對各種其他特性來選擇，諸如，成本、無毒性、裝運特性、在室溫下維持液相之能力、揮發性、分子量等等。
適合用作前驅物材料之其他有機矽化合物包括甲基矽烷；二甲基矽烷；乙烯基三甲基矽烷；三甲基矽烷；四甲基矽烷；乙基矽烷；二矽烷基甲烷；雙(甲基矽烷基)甲烷；1,2－二矽烷基乙烷；1,2－雙(甲基矽烷基)乙烷；2,2－二矽烷基丙烷；1,3,5－三矽烷基－2,4,6－三亞甲基，及此等化合物之氟化衍生物。適合用作前驅物材料之含苯基有機矽化合物包括：二甲基苯基矽烷及二苯基甲基矽烷。適合用作前驅物材料之含氧之有機矽化合物包括：二甲基二甲氧基矽烷；1,3,5,7－四甲基環四矽氧烷；1,3－二甲基二矽氧烷；1,1,3,3－四甲基二矽氧烷；1,3－雙(矽烷基亞甲基)二矽氧烷；雙(1－甲基二矽氧烷基)甲烷；2,2－雙(1－甲基二矽氧烷基)丙烷；2,4,6,8－四甲基環四矽氧烷；八甲基環四矽氧烷；2,4,6,8,10－五甲基環五矽氧烷；1,3,5,7－四矽烷基－2,6－二氧基－4,8－二亞甲基；六甲基環三矽氧烷；1,3,5,7,9－五甲基環五矽氧烷；六甲基氧二矽氧烷，及此等化合物之氟化衍生物。適合用作前驅物材料之含氮有機矽化合物包括：六甲基二矽氮烷；二乙烯基四甲基二矽氮烷；六甲基環三矽氮烷；二甲基雙(N－甲基乙醯胺基)矽烷；二甲基雙(N－乙基乙醯胺基)矽烷；甲基乙烯基雙(N－甲基乙醯胺基)矽烷；甲基乙烯基雙(N－丁基乙醯胺基)矽烷；甲基三(N－苯基乙醯胺基)矽烷；乙烯基三(N－乙基乙醯胺基)矽烷；肆(N－甲基乙醯胺基)矽烷；二苯基雙(二乙基胺氧基)矽烷；甲基三(二乙基胺氧基)矽烷；及雙(三甲基矽烷基)碳化二醯亞胺。
當藉由CVD沈積時，取決於前驅物材料之類型、任何反應氣體之存在及其他反應條件，前驅物材料可形成各種量的各種類型之聚合材料。聚合材料可為無機或有機的。舉例而言，在有機矽化合物用作前驅物材料之情形下，所沈積之混合層可包括用以形成聚矽氧烷類、聚碳矽烷及聚矽烷以及有機聚合物之Si－O鍵、Si－C鍵或Si－O－C鍵的聚合物鏈。
當藉由CVD沈積時，取決於前驅物材料之類型、任何反應氣體之存在及其他反應條件，前驅物材料可形成各種量的各種類型之非聚合材料。非聚合材料可為無機或有機的。舉例而言，在有機矽化合物結合含氧反應氣體用作前驅物材料之情形下，非聚合材料可包括氧化矽，諸如SiO、SiO2
及混合價氧化物SiOx
。當以含氮反應氣體沈積時，非聚合材料可包括氮化矽(SiNx
)。可形成之其他非聚合材料包括碳氧化矽及氮氧化矽。
當使用PE－CVD時，前驅物材料可結合在PE－CVD製程中與前驅物材料反應之反應氣體來使用。反應氣體在PE－CVD中之使用在此項技術中係已知的且各種反應氣體適用於本發明，包括含氧氣體(例如O2
、臭氧、水)及含氮氣體(例如，氨)。反應氣體可用以改變反應混合物中存在之化學元素之化學計量比。舉例而言，當矽氧烷前驅物材料與含氧或含氮氣體使用時，反應氣體將改變反應混合物中之氧或氮關於矽及碳之化學計量比。反應混合物中之各種化學元素(例如，矽、碳、氧、氮)之間的化學計量關係可以若干方式改變。一個方式為改變反應中之前驅物材料或反應氣體之濃度。另一方式為改變進入反應之前驅物材料或反應氣體之流動速率。另一方式為改變反應中所使用之前驅物材料或反應氣體之類型。
改變反應混合物中之元素之化學計量比可影響所沈積之混合層中之聚合材料及非聚合材料之性質及相對量。舉例而言，矽氧烷氣體可與改變量之氧氣組合以調整混合層中之非聚合材料相對於聚合材料之量。藉由增加氧關於矽或碳之化學計量比，可增加非聚合材料(諸如，氧化矽)之量。相似地，藉由減少氧之化學計量比，可增加含矽及含碳聚合材料之量。混合層中之組合物亦可藉由調整其他反應條件來改變。舉例而言，在PE－CVD之狀況下，可改變諸如RF功率及頻率、沈積壓力、沈積時間及氣體流動速率之製程參數。
因此，藉由使用本發明之方法，有可能形成具有混合聚合/非聚合性質並具有適合用於各種應用之特性的混合層。此等特性包括光學透明性(例如，在某些狀況下，混合層為光學透明的)、不可滲透性、可撓性、厚度、黏著力及其他機械性質。舉例而言，此等特性中之一或多者可藉由改變混合層中之聚合材料之重量%來調整，其中剩餘部分為非聚合材料。舉例而言，為達成所要位準之可撓性及不可滲透性，聚合材料之wt%可較佳在5%至95%之範圍中，且更佳在10%至25%的範圍中。然而，取決於應用，其他範圍亦為可能的。
由純非聚合材料(諸如，氧化矽)構成之障壁層可具有關於光學透明性、良好黏著力及良好薄膜應力之各種優勢。然而，此等非聚合層傾向於含有微觀缺陷，其允許水蒸氣及氧氣通過層的些許擴散。給非聚合層提供某聚合性質可在未顯著改變純非聚合層之有利性質之情形下降低層之滲透性。在不意欲受理論束縛之情形下，發明者咸信，具有混合聚合/非聚合性質之層藉由減小缺陷(特定言之，微裂痕)之尺寸及/或數目來降低層之滲透性。
在某些狀況下，本發明之塗層可具有複數個混合層，其中每一混合層之組合物可獨立改變。在某些狀況下，一混合層之重量%比率與塗層中之另一混合層相差至少10重量%。每一混合層之厚度亦可獨立地改變。不同混合層可藉由依序調整在沈積混合層時所使用之反應條件來產生。舉例而言，在PE－CVD製程中，提供至反應混合物之反應氣體之量可被依序調整以產生多個混合層，其中每一混合層為離散的且具有不同組合物。
在塗層具有組合物自一高度至另一高度大體上連續改變之區之情形下，此區內之混合層可極薄，甚至如塗層內之最小分子單元一樣薄。舉例而言，塗層可具有聚合材料與非聚合材料之wt%比率連續改變之區。該連續改變可為線性的(例如，聚合材料與非聚合材料之wt%比率可隨更高之高度而穩定增加)或非線性的(例如，循環增加及減少)。
混合層可在各種類型之物件上沈積。在某些狀況下，物件可為有機電子裝置，諸如OLED。對於OLED，混合層可充當抵抗水蒸氣及氧氣之滲透之障壁塗層。舉例而言，具有小於每日10－6
g/m2
之水蒸氣穿透率及小於每日10－3
g/m2
之氧氣穿透率的混合層可適合用於保護OLED。在某些狀況下，混合層之厚度可在0.1 μm至10 μm之範圍內，但亦可取決於應用而使用其他厚度。又，具有賦予光學透明性之厚度及材料組合物之混合層可適合與OLED一起使用。為與可撓性OLED一起使用，混合層可經設計以具有所要量之可撓性。在某些狀況下，混合層可在對經由暴露至環境之降級敏感之其他物件上使用，諸如，醫藥、醫療裝置、生物劑、生物樣本、生物感應器或敏感性量測裝備。
在某些狀況下，混合層可結合亦可藉由使用前驅物材料之同一單一來源形成之未混合層(諸如，未混合聚合層或未混合非聚合層)而使用。未混合層可在沈積混合層之前或之後沈積。
各種類型之CVD反應器中之任一者可用以實施本發明之方法。作為一實例，圖1展示可用以實施本發明之某些實施例之PE－CVD設備10。PE－CVD設備10包含反應腔室20，其中電子裝置30裝載至固持器24上。反應腔室20經設計以含有真空且真空泵70連接至反應腔室20以產生且/或維持適當之壓力。N2
氣體貯槽50提供用於淨化設備10之N2
氣體。反應腔室20可進一步包括冷卻系統以減少由反應產生之熱。
為處置氣體之流動，設備10亦包括各種流量控制機構(諸如，質量流量控制器80、截流閥82及止回閥84)，其可被手動或自動控制。前驅物材料來源40提供經氣化且饋入反應腔室20中之前驅物材料(例如，呈液體形式之HMDSO)。在某些狀況下，前驅物材料可使用諸如氬氣之載氣而傳送至反應腔室20。反應氣體貯槽60提供反應氣體(例如，氧氣)，其亦饋入反應腔室20中。前驅物材料及反應氣體流入反應腔室20中以產生反應混合物42。反應腔室20內之壓力可經進一步調整以達成沈積壓力。反應腔室20包括安裝於可為導體或絕緣體之電極支架26上之一組電極22。裝置30及電極22之各種配置為可能的。可使用二極體或三極體電極或遠端電極。裝置30可如圖1中所示而遠端定位，或可安裝於二極體組態之一或兩個電極上。
電極22以RF功率供應以在反應混合物42中產生電漿條件。由電漿產生之反應產物沈積至電子裝置30上。允許反應進行足夠時段以在電子裝置30上沈積混合層。反應時間將取決於各種因素，諸如，裝置30關於電極22之位置、待沈積之混合層之類型、反應條件、混合層之所要厚度、前驅物材料及反應氣體。反應時間可為在5秒至5小時之間的持續時間，但亦可取決於應用而使用更長或更短時間。
下表1展示用以製造三個實例混合層之反應條件。實例1之混合層含有約7%之聚合材料及93%之非聚合材料，如由小水滴之濕潤接觸角所確定。實例2之混合層含有約94%之聚合材料及6%之非聚合材料，如由小水滴之濕潤接觸角所確定。實例3之混合層含有約25%之聚合材料及75%之非聚合材料，如由小水滴之濕潤接觸角所確定。
圖2展示實例3之混合層之光學透射光譜。此混合層具有自近UV光譜至近IR光譜之大於90%之透射率。圖3展示量測薄膜上之小水滴之接觸角的方式。圖4為在各種O2
/HMDSO氣體流量比下形成之若干混合層之接觸角與純SiO2
薄膜及純聚合物薄膜之接觸角比較之曲線圖。隨著沈積製程中之氧氣流動速率增加，混合層之接觸角接近純SiO2
薄膜之接觸角。
圖5為在PE－CVD製程期間施加之各種功率位準下形成之若干混合層的接觸角之曲線圖。隨著功率位準增加，混合層之接觸角接近純SiO2
薄膜之接觸角，此情形可歸因於較高功率位準使得O2
成為較強烈氧化劑之事實。圖6展示使用相對較高O2
流量及相對較低O2
流量而形成之混合層與純SiO2
(熱氧化物)或純聚合物之薄膜相比的紅外吸收光譜。較高O2
混合層在Si－O－Si頻帶中展示較強峰值。咸信熱氧化物(純SiO2
)薄膜在Si－CH3
頻帶中之標稱峰值與Si－O振動相關。圖7為在各種O2
/HMDSO氣體流量比下形成之各種混合層之奈米壓痕硬度與純SiO2
薄膜之硬度相比之曲線圖。混合層之硬度隨著沈積製程中之氧氣流動速率增加而增加，且此等混合層可接近較硬純SiO2
薄膜，且仍具韌性並極具可撓性。
圖8為藉由原子力顯微法量測之在各種O2
/HMDSO氣體流量比下形成之若干混合層的表面粗糙度(均方根)之曲線圖，且展示表面粗糙度隨著沈積製程中所使用之增加之O2
流動速率而增加。圖9為藉由原子力顯微法量測之在各種功率位準下形成之若干混合層的表面粗糙度(均方根)之曲線圖，且展示表面粗糙度隨著沈積製程中所使用之增加之功率位準而減少。
圖10A及圖10B展示50 μm厚之Kapton聚醯亞胺箔片上的4 μm混合層(在與以上實例3相同之來源溫度、氣體流動速率、壓力及RF功率下沈積)之表面之光學顯微圖。在圖10A中，影像係在經塗佈之箔片經受1英吋直徑滾筒上之循環輥紮(拉伸應變ε＝0.2%)之前及之後獲取。在58,600個輥紮循環之後未觀測到微結構改變。在圖10B中，經塗佈之箔片經受增加之拉伸應變，且影像係在第一次裂開(14 mm之滾筒直徑)出現之後且在擴展性裂開(2 mm之滾筒直徑)之後獲取。此等可撓性結果說明，本發明之方法可提供極具可撓性之塗層。
圖11展示經囊封之OLED 100之一部分的橫截面圖，其包含基板150上的OLED本身140及作為障壁塗層110的以上實例3之混合層。圖12展示具有障壁塗層之完整OLED之加速環境測試的結果。底部發射型OLED及透明OLED皆以實例3之6 μm厚之混合層塗佈。裝置接著在65℃及85%相對濕度之環境腔室中操作。影像展示起始時間點及所指示之時間間隔之後的OLED之條件。OLED在超過1000小時之後持續作用，進而說明本發明之方法可提供有效免於環境暴露之降級效應之塗層。
在混合層用作電子裝置之環境障壁之情形下，混合層可充當上面安置電子裝置之表面、電子裝置之覆蓋物或兩者。舉例而言，一混合層可安置於電子裝置上以覆蓋該電子裝置且另一混合層沈積於電子裝置下方之基板上以提供上面安置電子裝置之表面。以此方式，電子裝置密封於兩個混合層之間。
舉例而言，參考圖13中所示之實施例，經囊封之OLED 160包含基板150，其中混合層162沈積於該基板150上。OLED之主體140(包括電極)安置於混合層162之表面上。可能具有或可能不具有與混合層162相同之組合物之另一混合層164沈積於OLED主體140上方作為等形塗層。因而，除覆蓋OLED主體140之頂部之外，混合層164亦在OLED主體140之側面下延伸且接觸混合層162之表面。以此方式，OLED主體140夾於混合層162與混合層164之間。
在某些實施例中，上面沈積混合層之表面可在沈積混合層之前被預處理以便增加表面與混合層之間的界面內聚力。表面預處理可對各種表面性質進行改質，包括改進表面之黏著性、對表面化學性質進行改質(例如，活化表面)、改變表面粗糙度、增加表面能、平坦化表面及/或清潔表面。藉由增加表面與混合層之間的界面內聚力，此特徵可有助於減少來自混合層之邊緣之環境污染物(諸如，水分或氧氣)之橫向擴散。
可增加表面與混合層之間的界面內聚力之各種類型之表面處理適用於本發明，包括機械研磨、化學處理(例如，暴露至氧化劑、藉由引入官能基而活化)或物理化學處理(例如，暴露至電漿、電暈放電或UV照射)。在使用電漿處理之情形下，處理可在用以沈積混合層之同一腔室中執行，或電漿處理可在獨立設備中執行，在此狀況下，可使用此項技術中已知之各種類型之電漿處理設備中的任一者，包括筒型電漿系統及平行板型電漿系統。
電漿處理中習知使用之各種氣體中之任一者可適用於預處理表面，包括諸如氧氣、氫氣、氮氣、氬氣、氨氣或其混合物的氣體。尤其較佳之氣體包括氧氣及氬氣。不同之氣體可用以按照不同方式而對表面進行改質。舉例而言，利用氬氣氣體之電漿處理將以氬離子轟擊表面，其可清潔表面或使其在原子級上較粗糙，藉此改良其黏著至混合層之能力。利用氧氣之電漿處理可以含氧官能基來化學活化該表面，該等官能基可形成與混合層之接合。為達成所要表面性質，可調整電漿處理製程之各種其他參數，包括功率、頻率、持續時間、壓力或溫度。
在某些狀況下，表面可藉由在表面與混合層之間安置插入層來預處理。插入層包含可用以改良表面與混合層之間的界面內聚力之各種材料中之任一者。舉例而言，適用於插入層之材料包括氮化矽、鉻、鈦、鎳鈦合金或介電材料。此層可使用習知用於沈積薄膜之各種技術中之任一者來沈積，包括化學氣相沈積、電漿氣相沈積或濺鍍。插入層之厚度將根據特定應用而改變。在某些狀況下，插入層可為單原子或單分子層，或具有達到50 nm之厚度，但在其他狀況下其他厚度亦為可能的。插入層中之材料可進一步經歷與位於插入層上方或下方之層或結構中之材料之化學反應。
圖14展示沈積於經蝕刻之矽晶圓上之混合層的橫截面的掃描電子顯微圖(SEM)。矽晶圓之未蝕刻部分(在圖14之左側被展示為具有5 μm階躍高度之升高邊緣)以鉻之80 nm薄膜覆蓋，其亦充當矽晶圓之蝕刻期間的蝕刻遮罩。矽晶圓之蝕刻部分(展示於圖14之右側)未以鉻薄膜預處理。混合層係藉由PE－CVD在矽晶圓之兩個部分上在以下條件下沈積：
貫穿間歇沈積製程之加熱及冷卻循環，矽晶圓基板之平均溫度大於80℃(約22℃之起始溫度及約160℃之結束溫度)。在鉻處理之表面上，混合層具有緻密微結構。然而，在未處理之表面上，障壁層具有不規則、柱狀微結構。基於形態差異，可預期鉻處理之表面上之混合層(具有緻密微結構)相比沈積於未處理之表面上之混合層對水分及氧氣具有較少滲透。
在某些狀況下，插入層可為包含一或多個平坦化子層及一或多個黏著促進子層之多層結構。舉例而言，美國專利第6,597,111號(Silvernail等人)及第7,187,119號(Weaver)描述由交替系列之聚合平坦化子層及高密度子層形成之障壁層。聚合平坦化子層包含形成平滑表面之聚合平坦化材料。高密度子層包含高密度材料(例如，無機、陶瓷或介電材料)，其具有足夠接近之原子間隔使得環境污染物之擴散被阻止。在另一實例中，插入層可包含多個交替層之旋塗之聚合物層與混合層(按照以上所描述之方式而沈積)；或SiNx
層及混合層；或旋塗之聚合物層及SiNx
層。
舉例而言，參考圖15中所示之實施例，基板150以聚合材料之平坦化子層170塗佈。黏著促進子層172安置於平坦化子層170上。OLED之主體140(包括電極)安置於黏著促進子層172之表面上。混合層174接著沈積於OLED主體140上作為等形塗層。因而，除覆蓋OLED主體140之頂部之外，混合層174亦在OLED主體140之側面下延伸且接觸黏著促進子層172的表面。以此方式，混合層174與黏著促進子層172之間的黏著力可減少環境污染物經由界面區域之橫向擴散。
如以上所闡述，可改變沈積條件以給混合層提供不同結構、組合物及/或性質，包括其對環境污染物之滲透性及其黏著至上面沈積混合層之表面的能力。在某些狀況下，沈積溫度(例如，經由基板之加熱及冷卻)可經控制以降低混合層之滲透性。圖16A及16B展示沈積至經蝕刻之矽晶圓上之混合層的橫截面的掃描電子顯微圖(SEM)。矽晶圓之未蝕刻部分(在圖16A及圖16B之右側展示為升高邊緣)以鉻之薄膜覆蓋，其亦充當矽晶圓之蝕刻期間之蝕刻遮罩。矽晶圓之蝕刻部分(展示於圖16A及圖16B之左側)未以鉻薄膜預處理。混合層係藉由PE－CVD在矽晶圓之兩個部分上在以下條件下沈積：
貫穿間歇沈積製程之加熱及冷卻循環，矽晶圓之平均溫度為約35℃。在間歇沈積製程中，控制沈積溫度之一方式為調整加熱及/或循環之數目或持續時間。因而，因為此混合層以較短持續時間之加熱循環且以較大數目之冷卻循環來沈積，所以平均沈積溫度低於圖14中所示之沈積混合層時所使用之沈積溫度。結果，矽晶圓上之鉻處理表面及裸表面兩者上之混合層具有不規則、柱狀結構。又，階躍之橫向態樣上存在不良覆蓋。因此，可預期使用某範圍內之較高沈積溫度而形成之混合層相比使用較低沈積溫度而形成之混合層具有較低滲透性。在某些狀況下，混合層在40℃至90℃之範圍中之沈積溫度下沈積。
在某些狀況下，可控制沈積功率以降低混合層之滲透性。圖17A展示沈積於底部發射型OLED堆疊上之混合層之橫截面的掃描電子顯微圖(SEM)。混合層係藉由PE－CVD在以下條件下沈積： ＊
在以下間歇週期中：在100毫托下歷時9分鐘，接著8次在100毫托下歷時6分鐘，接著在130毫托下歷時8分鐘，接著在150毫托下歷時10分鐘，接著在125毫托下歷時9分鐘，接著在150毫托下歷時7分鐘，接著在125毫托下歷時8分鐘，接著在150毫托下歷時10分鐘，接著在125毫托下歷時8分鐘，且接著在125毫托下歷時9分鐘。
咸信較高沈積功率促進單體斷裂。因此，藉由將功率自24 W逐漸增加至50 W，觀測到混合層中之每一後續層呈現較類氧化物之性質及較少類聚合物之性質。在圖17A中，混合層中最接近表面之層(在較低功率下沈積)具有多孔、類聚合物微結構，而距表面較遠之層(在較高功率下沈積)具有較緻密、類氧化物之微結構。
圖17B展示另一混合層之橫截面之掃描電子顯微圖(SEM)，其係藉由PE－CVD在頂部發射型OLED堆疊上在以下條件下沈積：
與圖17A中之混合層相比，較高沈積功率用於沈積圖17B中所示之混合層。結果，此混合層具有比圖17A中所示之混合層之微結構更緻密之微結構。因此，可預期使用較高沈積功率而形成之混合層相比使用較低沈積功率而形成之混合層具有較低滲透性。
當安置兩種不同材料使其緊密接觸時，此接觸可引起應力，尤其在兩種材料之界面處。因此，在某些實施例中，可控制混合層之殘留內應力以減少混合層中應力誘發之缺陷的影響，諸如，裂痕、空隙、壓曲或分層。控制混合層中之內應力之一個方式為調整沈積條件。
圖18A至18C展示25 μm厚之Kapton－E聚醯亞胺基板與在不用條件下沈積於其上之各種混合層(具有320 nm至600 nm之厚度)之間的應變失配。正失配對應於混合層中之拉伸應力且負失配對應於混合層中之壓縮應力。參看圖18A，將沈積壓力自100毫托增加至150毫托(沈積功率及氣體流動速率保持恆定)導致在混合層中產生較大拉伸應力。參看圖18B，將沈積功率自50 W增加至80 W(沈積壓力及氣體流動速率保持恆定)導致在混合層中產生較大壓縮應力。參看圖18C，將HMDSO/O2
氣體流動速率自1.0/34增加至2.0/67(沈積壓力及功率保持恆定)導致在混合層中產生較大拉伸應力。
此等結果指示混合層中之內應力可藉由改變沈積參數來調節。此等結果亦指示，存在一組最佳沈積參數，其中可最小化混合層中之應力。舉例而言，一沈積參數可經調節以在混合層中產生壓縮應力，而另一沈積參數可經調節以在混合層中產生匹配拉伸應力，進而導致為零或接近零之殘留淨應力。在多層塗層包含複數個混合層之情形下，亦有可能獨立地調節每一混合層中之應力以控制塗層中之總應力。舉例而言，每一混合層可經調節以平衡塗層中之總應力，或隨著距表面之增加之距離而逐漸增加混合層中之應力的量。
在電子裝置安置於充當基礎之表面(亦即，基礎表面)上之某些實施例中，混合層及/或表面可進一步包含邊緣障壁以減少環境污染物(例如，水分或氧氣)因橫向擴散而通過基礎材料自身或通過基礎表面與混合層之間的界面之滲透。基礎可由本文中所描述之材料中之任一者或已知用於在上面安置電子裝置的任何其他材料(例如，用於平坦化及/或金屬箔片基板或障壁塗佈之塑膠基板上之絕緣層的材料)形成。此項技術中已知之各種類型之邊緣障壁中的任一者適用於本發明。在某些狀況下，邊緣障壁係藉由在周邊鄰近電子裝置之區域處將混合層接合至基礎表面來建構。接合可藉由對此等區域施加熱密封或黏著劑(例如，基於環氧樹脂之黏著劑)來達成。
在某些狀況下，邊緣障壁可為自電子裝置之頂表面沿電子裝置之橫向側面向下延伸且與基礎表面接觸之端蓋。可適用於本發明之一類型之端蓋在美國專利第7,002,294號(Forrest等人)中有所描述。端蓋可由可保護電子裝置免於環境污染物之橫向進入之任何材料製得，包括高密度陶瓷材料(例如，二氧化矽)或金屬材料。
舉例而言，參考圖19中所示之實施例，經囊封之OLED 180包含基板150，OLED之主體140(包括電極)安置於基板150上。混合層182沈積於OLED主體140上。端蓋184圍繞混合層182及OLED主體140安置以自混合層182之頂表面，沿OLED主體140之橫向態樣向下延伸且與基板150之表面接觸。端蓋184用以減少環境污染物通過OLED 180之橫向表面或邊緣之橫向進入。
在某些狀況下，邊緣障壁可藉由在周邊鄰近電子裝置之區域中之基礎表面中產生一或多個不連續性來形成。此等不連續性可藉由各種機制中之任一者而充當抵抗環境污染物之滲透的障壁，該等機制包括增加環境污染物之橫向進入之路徑長度，或在基礎材料充當環境污染物之進入之管道之情形下，在管道中形成斷裂。如本文中所使用，術語"不連續性"指藉由使用控制空隙之尺寸、形狀及位置之技術來移除或沈積材料而在基礎表面中產生的離散空隙(例如，溝槽、凹槽、槽、裂痕、斷裂、間隙、孔、穿孔)。舉例而言，此等技術包括使用高能波束(例如，雷射、離子或電子)之直接寫入蝕刻、微切削、微鑽、微影製程或基礎材料於待產生空隙之區域上利用選擇性遮罩的遮罩沈積。
舉例而言，參考圖20中所示之實施例，基板150以聚醯亞胺薄膜194塗佈。聚醯亞胺薄膜194充當上面安置OLED之主體140(包括電極)之基礎表面。蝕刻入聚醯亞胺薄膜194中的是圍繞OLED主體140之周邊之溝槽196。或者，溝槽196可藉由在聚醯亞胺薄膜194之沈積期間選擇性遮罩區域來形成。溝槽196延伸通過聚醯亞胺薄膜194之整個厚度。OLED主體140以混合層192覆蓋，混合層192覆蓋OLED主體140之頂部並沿OLED主體140之側面向下延伸至基礎表面。在基礎表面上，混合層192亦填充溝槽196以防止聚醯亞胺充當環境污染物之橫向進入之管道。
前述描述及實例僅經陳述以說明本發明且並非意欲限制。本發明之所揭示之態樣及實施例中之每一者可獨立或結合本發明之其他態樣、實施例及改變來考慮。熟習此項技術者可清楚併有本發明之精神及實質的所揭示之實施例之修改且此等修改在本發明之範疇內。
10．．．PE－CVD設備
20．．．反應腔室
22．．．電極
24．．．固持器
26．．．電極支架
30．．．電子裝置
40．．．前驅物材料來源
42．．．反應混合物
50．．．N2
氣體貯槽
60．．．反應氣體貯槽
70．．．真空泵
80．．．質量流量控制器
82．．．截流閥
84．．．止回閥
100．．．經囊封之OLED
110．．．障壁塗層
140．．．OLED主體
150．．．基板
160．．．經囊封之OLED
162．．．混合層
164．．．混合層
170．．．平坦化子層
172．．．黏著促進子層
174．．．混合層
180．．．經囊封之OLED
182．．．混合層
184．．．端蓋
192．．．混合層
194．．．聚醯亞胺薄膜
196．．．溝槽
圖1展示可用於實施本發明之某些實施例之PE－CVD設備的示意圖。
圖2展示根據一實施例之混合層之光學透射光譜。
圖3展示量測薄膜上之小水滴之接觸角之方式。
圖4展示在各種O2
/HMDSO氣體流量比下形成之若干混合層之接觸角的曲線圖。
圖5展示在PE－CVD製程期間施加之各種功率位準下形成之若干混合層的接觸角之曲線圖。
圖6展示使用相對較高O2
流量及相對較低O2
流量而形成之混合層與純SiO2
(熱氧化物)或純聚合物之薄膜相比的紅外吸收光譜。
圖7展示在各種O2
/HMDSO氣體流量比下形成之各種混合層之奈米壓痕硬度與純SiO2
薄膜之硬度相比之曲線圖。
圖8展示在各種O2
/HMDSO氣體流量比下形成之若干混合層之表面粗糙度的曲線圖。
圖9展示在各種功率位準下形成之若干混合層之表面粗糙度的曲線圖。
圖10A及圖10B展示沈積於50 μm厚之Kapton聚醯亞胺箔片上的4 μm混合層之表面的光學顯微圖。
圖11展示根據一實施例之經囊封之OLED的一部分的橫截面圖。
圖12展示具有障壁塗層之完整OLED之加速環境測試的結果。
圖13展示根據另一實施例之經囊封之OLED。
圖14展示根據另一實施例之混合層之橫截面的掃描電子顯微圖。
圖15展示根據另一實施例之經囊封之OLED。
圖16A及圖16B展示根據另一實施例之混合層之橫截面的掃描電子顯微圖。
圖17A展示在一組條件下沈積之混合層之橫截面的掃描電子顯微圖。圖17B展示在另一組條件下沈積之混合層之橫截面的掃描電子顯微圖。
圖18A至18C展示聚醯亞胺基板與沈積於其間的各種混合層之間的應變失配之曲線圖。
圖19展示根據另一實施例之經囊封之OLED。
圖20展示根據另一實施例之經囊封之OLED。
10．．．PE－CVD設備
20．．．反應腔室
22．．．電極
24．．．固持器
26．．．電極支架
30．．．電子裝置
40．．．前驅物材料來源
42．．．反應混合物
50．．．N2
氣體貯槽
60．．．反應氣體貯槽
70．．．真空泵
80．．．質量流量控制器
82．．．截流閥
84．．．止回閥
Claims (43)
- 一種用於在一表面上形成塗層之方法，其包含：使用一前驅物材料來源；將該前驅物材料傳送至一鄰近待塗佈表面之反應位置；及使用該前驅物材料來源藉由化學氣相沈積而在該表面上沈積混合層，其中該混合層實質上由聚合物矽與無機矽之混合物所組成，其中聚合物矽與無機矽之重量比在95：5至5：95之範圍中，且其中該聚合物矽及該無機矽係由同一該前驅物來源產生；其中厚度至少為0.1μm的混合層係在用於沈積方法中所有反應條件之相同反應條件下沈積；其中穿透厚度至少為0.1μm的混合層之水蒸氣穿透率係小於每日10-6 g/m2 。
- 如請求項1之方法，其中該前驅物材料為六甲基二矽氧烷或二甲基矽氧烷。
- 如請求項1之方法，其中該前驅物材料包含一單一有機矽化合物。
- 如請求項1之方法，其中該前驅物材料包含有機矽化合物之一混合物。
- 如請求項1之方法，其中該化學氣相沈積係電漿增強型化學氣相沈積。
- 如請求項5之方法，其進一步包含提供一反應氣體，且其中該化學氣相沈積在存在該反應氣體之情形下發生。
- 如請求項6之方法，其中該反應氣體為氧氣。
- 如請求項1之方法，其中聚合物矽與無機矽之該重量比在90：10至10：90之範圍中。
- 如請求項1之方法，其中聚合物矽與無機矽之該重量比在25：75至10：90之範圍中。
- 如請求項1之方法，其中厚度至少為1,600Å的混合層係在用於沈積方法中所有反應條件之相同反應條件下沈積。
- 如請求項1之方法，其中厚度為1,600Å至6,000Å的混合層係在用於沈積方法中所有反應條件之相同反應條件下沈積。
- 如請求項1之方法，其中該前驅物材料為六甲基二矽氧烷或二甲基矽氧烷，且其中該化學氣相沈積係電漿增強型化學氣相沈積。
- 如請求項1之方法，其進一步包含在沈積該混合層之前使用該前驅物材料來源而在該表面上沈積一未混合之聚合物矽層。
- 如請求項1之方法，其進一步包含在沈積該混合層之前使用該前驅物材料來源而在該表面上沈積一未混合之無機矽層。
- 如請求項1之方法，其進一步包含在沈積該混合層之後使用該前驅物材料來源而在該表面上沈積一未混合之聚合物矽層。
- 如請求項1之方法，其進一步包含在沈積該混合層之後 使用該前驅物材料來源而在該表面上沈積一未混合之無機矽層。
- 如請求項1之方法，其中剛沈積之該混合層具有在36°至60°之範圍中之一小水滴之一濕潤接觸角。
- 如請求項1之方法，其中該混合層為光學透明的。
- 如請求項18之方法，其中該混合層自近UV光譜至近IR光譜具有大於90%之透射率。
- 如請求項1之方法，其中該表面在沈積該混合層之前被預處理以改良該表面與該混合層之間的界面內聚力。
- 如請求項20之方法，其中該預處理該表面之步驟包含一化學處理。
- 如請求項20之方法，其中該預處理該表面之步驟包含一物理化學處理。
- 如請求項22之方法，其中該物理化學處理為一電漿處理。
- 如請求項20之方法，其中該預處理之步驟包含在沈積該混合層之前在該表面上沈積一插入層。
- 如請求項24之方法，其中該插入層包含一用以增加該表面與該混合層之間的該界面內聚力之材料。
- 如請求項1之方法，其中以相同反應條件沈積的該混合層之厚度在0.1μm至10μm之範圍內。
- 如請求項1之方法，其進一步包含：使用該前驅物材料來源藉由化學氣相沈積而在該表面上沈積複數個混合層，其中每一混合層獨立地實質上由 聚合物矽與無機矽之混合物組成，其中該聚合物矽與該無機矽之重量比在95：5至5：95之範圍中，且其中該聚合物矽及該無機矽係由同一該前驅物材料來源產生；其中複數個混合層之每一者，厚度至少為0.1μm的混合層係在用於沈積方法中所有反應條件之相同反應條件下沈積。
- 如請求項27之方法，其中該複數個混合層係藉由在該化學氣相沈積製程中依序改變反應條件中之一或多者來產生。
- 如請求項28之方法，其進一步包含提供一反應氣體，其中該化學氣相沈積在存在該反應氣體之情形下發生，且其中該複數個混合層係藉由在該化學氣相沈積製程中依序改變反應氣體之量來產生。
- 如請求項27之方法，其中一混合層中之聚合物矽之量與另一混合層中之該聚合物矽之量相差至少10重量%。
- 如請求項28之方法，其中該化學氣相沈積係電漿增強型化學氣相沈積，且其中該複數個混合層係藉由在該電漿增強型化學氣相沈積製程中依序改變電漿功率位準來產生。
- 如請求項27之方法，其中該多層塗層中之總內應力係藉由調節每一混合層中之內應力來控制。
- 如請求項32之方法，其中每一混合層中之該內應力係藉由控制用以沈積每一混合層之沈積條件來調節。
- 如請求項33之方法，其中該等混合層中之每一者中之該 內應力係藉由控制對該內應力具有一相反效應之至少兩個沈積條件來調節。
- 如請求項33之方法，其中每一混合層係藉由電漿增強型化學氣相沈積(PE-CVD)來沈積，且其中加以控制之該等沈積條件係選自由以下條件組成之群：沈積壓力、沈積功率、氣體流動速率及電極距離。
- 如請求項32之方法，其中每一混合層中之該內應力經調節以使得該多層塗層中之該總內應力得以平衡。
- 如請求項36之方法，其中該多層塗層中之該總內應力為零或接近零。
- 如請求項32之方法，其中較接近該表面之至少一混合層具有一低於較遠離該表面之至少一混合層之內應力的內應力。
- 如請求項24之方法，其中該插入層為光學透明的。
- 如請求項24之方法，其中該插入層包含一無機材料。
- 如請求項40之方法，其中該無機材料為鉻或氮化矽。
- 如請求項27之方法，其中該前驅物材料為六甲基二矽氧烷或二甲基矽氧烷，且其中該化學氣相沈積係電漿增強型化學氣相沈積。
- 如請求項27之方法，其中複數個混合層之每一者，以相同反應條件沈積的該混合層之厚度在0.1μm至10μm之範圍內。
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Also Published As
| Publication number | Publication date |
|---|---|
| WO2008057394A1 (en) | 2008-05-15 |
| JP2016207660A (ja) | 2016-12-08 |
| KR20090087457A (ko) | 2009-08-17 |
| EP2097555A1 (en) | 2009-09-09 |
| CN103187455B (zh) | 2017-07-04 |
| CN103187455A (zh) | 2013-07-03 |
| US20080102223A1 (en) | 2008-05-01 |
| JP2014150063A (ja) | 2014-08-21 |
| JP5968931B2 (ja) | 2016-08-10 |
| JP2018018830A (ja) | 2018-02-01 |
| JP2010508640A (ja) | 2010-03-18 |
| JP6716521B2 (ja) | 2020-07-01 |
| TW200832776A (en) | 2008-08-01 |
| JP5491186B2 (ja) | 2014-05-14 |
| EP2466665A1 (en) | 2012-06-20 |
| KR20150084893A (ko) | 2015-07-22 |
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