TW201508083A - 有機無機複合薄膜及其製造方法 - Google Patents
有機無機複合薄膜及其製造方法 Download PDFInfo
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- TW201508083A TW201508083A TW102144000A TW102144000A TW201508083A TW 201508083 A TW201508083 A TW 201508083A TW 102144000 A TW102144000 A TW 102144000A TW 102144000 A TW102144000 A TW 102144000A TW 201508083 A TW201508083 A TW 201508083A
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- inorganic composite
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- 238000000034 method Methods 0.000 title abstract description 27
- 239000010409 thin film Substances 0.000 title abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 68
- 238000004519 manufacturing process Methods 0.000 claims abstract description 38
- 239000002052 molecular layer Substances 0.000 claims abstract description 27
- 239000002131 composite material Substances 0.000 claims description 117
- 150000001875 compounds Chemical class 0.000 claims description 47
- 239000000126 substance Substances 0.000 claims description 36
- 239000000758 substrate Substances 0.000 claims description 22
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 15
- 125000003396 thiol group Chemical group [H]S* 0.000 claims description 13
- 238000000231 atomic layer deposition Methods 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- 229910052710 silicon Inorganic materials 0.000 claims description 11
- 125000003118 aryl group Chemical group 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- 229910052793 cadmium Inorganic materials 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 9
- 229910052733 gallium Inorganic materials 0.000 claims description 9
- 229910052738 indium Inorganic materials 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 229910052748 manganese Inorganic materials 0.000 claims description 9
- 229910052758 niobium Inorganic materials 0.000 claims description 9
- 229910052718 tin Inorganic materials 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- 229910052721 tungsten Inorganic materials 0.000 claims description 9
- 229910052720 vanadium Inorganic materials 0.000 claims description 9
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- 229910052726 zirconium Inorganic materials 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 8
- 125000000753 cycloalkyl group Chemical group 0.000 claims description 8
- 125000001072 heteroaryl group Chemical group 0.000 claims description 8
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 5
- 101100134925 Gallus gallus COR6 gene Chemical group 0.000 claims description 4
- 150000004703 alkoxides Chemical class 0.000 claims description 4
- 125000003545 alkoxy group Chemical group 0.000 claims description 4
- 125000003277 amino group Chemical group 0.000 claims description 4
- 125000001033 ether group Chemical group 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 4
- 125000003837 (C1-C20) alkyl group Chemical group 0.000 claims description 3
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- 238000005538 encapsulation Methods 0.000 claims description 3
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- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 2
- 125000005586 carbonic acid group Chemical group 0.000 claims description 2
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
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- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 230000008021 deposition Effects 0.000 abstract description 11
- 125000000524 functional group Chemical group 0.000 abstract description 6
- 239000010408 film Substances 0.000 description 157
- IGFHQQFPSIBGKE-UHFFFAOYSA-N 4-nonylphenol Chemical compound CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 40
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 32
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical group CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 description 26
- 238000000151 deposition Methods 0.000 description 23
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 18
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- 230000000052 comparative effect Effects 0.000 description 14
- 239000010410 layer Substances 0.000 description 13
- 238000010586 diagram Methods 0.000 description 11
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 9
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 9
- 229910052786 argon Inorganic materials 0.000 description 9
- 238000002347 injection Methods 0.000 description 9
- 239000007924 injection Substances 0.000 description 9
- 238000010926 purge Methods 0.000 description 9
- 229910052707 ruthenium Inorganic materials 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 238000004566 IR spectroscopy Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- 230000006870 function Effects 0.000 description 5
- 230000035699 permeability Effects 0.000 description 5
- 230000003746 surface roughness Effects 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 4
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- 238000005516 engineering process Methods 0.000 description 4
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
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- 238000004627 transmission electron microscopy Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
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- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- AXAZMDOAUQTMOW-UHFFFAOYSA-N dimethylzinc Chemical compound C[Zn]C AXAZMDOAUQTMOW-UHFFFAOYSA-N 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 239000011147 inorganic material Substances 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- -1 oxyhydroxy Chemical group 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BXAVKNRWVKUTLY-UHFFFAOYSA-N 4-sulfanylphenol Chemical compound OC1=CC=C(S)C=C1 BXAVKNRWVKUTLY-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229910004541 SiN Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000313 electron-beam-induced deposition Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000007737 ion beam deposition Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- LFLZOWIFJOBEPN-UHFFFAOYSA-N nitrate, nitrate Chemical compound O[N+]([O-])=O.O[N+]([O-])=O LFLZOWIFJOBEPN-UHFFFAOYSA-N 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
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- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- 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
- H01L23/3157—Partial encapsulation or coating
- H01L23/3192—Multilayer coating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/02—Physical, chemical or physicochemical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/06—Zinc compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/06—Aluminium compounds
- C07F5/061—Aluminium compounds with C-aluminium linkage
- C07F5/062—Al linked exclusively to C
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- 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
-
- 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
- C23C16/42—Silicides
-
- 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
- C23C16/455—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 introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
- C23C16/45529—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations specially adapted for making a layer stack of alternating different compositions or gradient compositions
-
- 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
- C23C16/455—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 introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/133305—Flexible substrates, e.g. plastics, organic film
-
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
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Abstract
本發明涉及一種有機無機複合薄膜及其製造方法,尤其涉及一種含穩定新官能基的有機無機複合薄膜,及交替使用無機物前驅物及有機物前驅物,通過分子層沉積法形成的有機無機複合薄膜的製造方法。
Description
本發明涉及有機無機複合薄膜及其製造方法,尤其涉及一種含穩定新官能基的有機無機複合薄膜,及交替使用無機物前驅物及有機物前驅物,通過分子層沉積法(Molecular Layer Deposition)形成的有機無機複合薄膜的製造方法。
有機無機複合材料(Organic-inorganic Hybrid Materials)是把有機材料和無機材料以物理或化學方法結合,從而能夠同時表現有機材料的性質和無機材料的性質的材料。
在製造有機無機複合薄膜時最常用的方法是溶膠-凝膠(Sol-gel)法,由於可在低溫條件下容易地製造有機無機複合材料,因此從很早以前開始,對這一方法展開了廣泛研究。但由於溶膠-凝膠法很難以單分子層為單位進行控制,存在熱處理後發生變形的問題,因此難以製造高品質的有機無機複合薄膜。
製造有機無機複合薄膜的其他方法有熔融插層法(Melt Intercalation),可以製造很難通過溶膠-凝膠法製造的有機無機複合材料。但這一方法也很難以單分子層為單位進行控制,且其沉積速度慢,因此很難製造高品質的有機無機奈米複合超晶格(superlattice)。
利用靜電力製造有機無機複合薄膜的自組裝法(self-assembly)是一種能夠層狀生長高分子、奈米粒子及奈米板等的極為有用的方法,目前在進行很多相關研究。但利用靜電力製造有機無機複合薄膜的自組裝法,在嚴格意義上說不是單分子層控制技術,且其熱穩定性低,因此難以製造高品質的有機無機複合薄膜。另外,在氣態下製造有機無機複合薄膜的熱沉積法(Evaporation)很難控制單分子層,原料分子方面受到很多局限,無法得到廣泛應用。
為了解決現有的這些有機無機複合薄膜製造方法的問題,開發了不僅可以沉積有機高分子,還可以沉積有機無機複合材料的分子層沉積技術。分子層沉積技術是通過自控制表面反應,可以以分子為單位控制無機或有機分子的氣態沉積法。典型的例子是S. M. George集團利用分子層沉積技術,利用三甲基鋁(trimethylaluminum,TMA)及乙二醇(ethylene glycol,EG)製造Alucone高分子膜。但這種現有的分子層沉積技術,在有機物前驅物所含官能基方面局限於羥基(hydroxyl group)、羧基(carboxyl group)及其衍生物(derivative),並且由此製造而成的有機無機複合薄膜放在空氣中時不穩定,發生分解的問題。
為了防止電子元件因氧氣或水分發生性能降低,現在正在開發理想的封裝膜。現在使用的封裝膜有利用SiO2, SiN, Al2O3 等無機物形成的單一膜,交替沉積無機物形成的多層膜,交替沉積無機物和有機物形成的多層膜等很多形態。現有技術中,利用離子束沉積法(Ion Beam Deposition)、電子束沉積法(Electron BeamDeposition)、等離子體沉積法(Plasma Beam Deposition)或化學氣相沉積法(Chemical Vapor Deposition)等,形成了無機鈍化(passivation)膜。而這種現有技術需要的沉積溫度高,薄膜覆蓋力差。
因此,可在低溫條件下形成封裝膜的原子層沉積法(Atomic Layer Deposition, ALD)受到青睞。ALD技術是最理想的無機及金屬薄膜製造技術,是以原子為單位,利用自控制反應沉積單原子層的技術,能夠利用基質表面上的化學吸附和釋放過程,控制單原子層的厚度,可稱之為全新概念的沉積方法。但採用原子層沉積法(Atomic Layer Deposition, ALD)時,由於形成封裝膜的過程中產生針孔,因此直至目前還很難獲得所需的性能。
技術問題本發明為了解決如上所述的現有技術問題,其目的在於提供一種交替使用用於形成無機層的前驅物化合物及包括新官能基的用於形成有機物層的前驅物化合物的一種新穎、穩定的有機無機複合薄膜的製造方法。
本發明的另一目的在於提供一種通過本發明的製造方法製造的有機無機複合薄膜。
技術方案本發明為了解決如上所述的問題,提供由如下化學式1表示的有機無機複合薄膜,[化學式1]-[M-X-R1-Y-]m- 其中,所述化學式1中m為1以上,R1為C1~20
烷基(alkyl)、C5~20
環烷基(cycloalkyl)、核原子數為5~60的芳基(aryl)或雜芳基(hetero aryl),M選自由Zn, Sn, In, Cd, Ga, Al,Ti, Si, V, Mn, Fe, Co, Cu, Zr,Ru, Mo, Nb及W構成的群組,X或Y分別選自由O, S, N, NH及CO構成的群組,X或Y中的一個是S。
本發明的有機無機複合薄膜,其特徵在於厚度是1Å至500 Å。
本發明的有機無機複合薄膜,其特徵在於:設所述有機無機複合薄膜的初始厚度為d0,所述有機無機複合薄膜在標準溫度和壓力(standard temperature and pressure, STP)條件下放置n小時後的厚度為dn時,滿足如下關係式:0 ≤ (dn/d0) ≤ 0.1(0 ≤n ≤ 240) 。
本發明提供一種功能性薄膜,其特徵在於包括本發明的有機無機複合薄膜;以及金屬氧化物層,其中金屬選自由Zn, Sn, In, Cd, Ga, Al, Ti, Si, V, Mn,Fe, Co, Cu, Zr, Ru, Mo, Nb及W構成的群組。所述功能性薄膜可以是超晶格薄膜。
含本發明的有機無機複合薄膜的功能性薄膜,其特徵在於所述金屬氧化物層的厚度為10Å至2000Å。
含本發明的有機無機複合薄膜的功能性薄膜,其特徵在於:設含所述有機無機複合薄膜的功能性薄膜的初始厚度為D0,含所述有機無機複合薄膜的功能性薄膜在STP條件下放置n小時後的厚度為Dn時,滿足如下關係式:0 ≤ (Dn/D0) ≤ 0.1(0 ≤n ≤ 240)。
本發明的功能性薄膜,其特徵在於用於封裝。
本發明提供一種有機無機複合分子膜的製造方法,其特徵在於,包括:(1)利用由如下化學式2表示的第一前驅物化合物在基板表面形成無機分子層的步驟,[化學式2]M(R21)(R22)…(R2n)其中,所述化學式2 中所述M 選自由Zn, Sn, Cd, Ti, Si, V, Mn,Fe, Co, Cu, Zr, Ru, Mo, Nb, W, In, Ga, Al 及Tl構成的群組,n由所述金屬M的氧化態決定,R21至R2n分別獨立為C1~20
烷基、C1~20
醇基(alkoxide)、氯基、羥基(hydroxyl group)、氧羥基(oxy hydroxy)、硝酸基、碳酸基、醋酸基或草酸基(oxalic acid);以及(2)使如下化學式3表示的第二前驅物化合物與所述無機分子層反應,在所述無機分子層上形成有機分子層的步驟,[化學式3]R3-S-R4-R5其中,所述化學式3中,R3為氫、COR6、C1~20
烷基、C5~20
環烷基、核原子數為5~60的芳基或雜芳基,R4為C1~20
烷基、C5~20
環烷基、核原子數為5~60的芳基或雜芳基,R5為選自由羥基、C1~20
烷氧基(alkoxy group)、醚基(ether group)、羧基(carboxylgroup)、COR6、硫醇基(thiol group)及氨基(aminegroup)構成的群組的任一種或以上的組合,R6為選自由氫、烷氧基、醚基、羧基、硫醇基及氨基構成的群組的任一種或以上的組合。
在本發明的有機無機複合分子膜的製造方法中,所述第一前驅物化合物與基板反應,在基板表面形成無機物層。
一切可形成無機薄膜的前驅物(precursor)均可作為所述第一前驅物化合物。為了在最短時間內把所需量的前驅物注入到腔體內,使用蒸汽壓高的金屬化合物。例如,所述第一前驅物化合物可以是含一種金屬的烷烴(alkyl)、 醇鹽(alkoxide)、氯化物(chloride)、氫氧化物(hydroxide)、羥基氧化物(oxyhydroxide)、硝酸鹽(nitrate)、碳酸鹽(carbonate)、醋酸鹽(acetate)、草酸鹽(oxalate)及其混合物構成的群組,所述金屬選自由Zn, Sn, In, Cd, Ga, Al, Ti, Si, V, Mn,Fe, Co, Cu, Zr, Ru, Mo, Nb及W構成的群組。
所述第一前驅物化合物包括由所述金屬M的氧化態決定的R21、R22…R2n等n個取代基,R21至R2n分別獨立為C1~20
烷基、C1~20
醇基、氯基、羥基、氧羥基、硝酸基、碳酸基、醋酸基或草酸基。
具體地,用於形成含金屬Zn的無機物層的原料氣體有二乙基鋅(Diethyl Zinc,DEZn)、二甲基鋅 (Dimethyl Zinc,DMZn)等,用於形成含金屬Al的無機物層的原料氣體可以是三甲基鋁(Trimethylaluminum,TMA)、三乙基鋁(Triethylaluminum,TEA)等。
在本發明的有機無機複合薄膜的製造方法中,由所述化學式3表示的所述第二前驅物化合物的SR3或R5與基板表面上由所述第一前驅物化合物形成的無機物層反應,形成有機無機複合薄膜。
在本發明的有機無機複合薄膜的製造方法中,所述第二前驅物化合物可使用由如下化學式4表示的化合物,[化學式 4] 其中,所述化學式4中,Z為硫醇基,Q為選自硫醇基及羥基中的一種,Z與Q的位置為鄰位(ortho)、間位(meta)或對位(para)。
本發明的有機無機複合薄膜的製造方法中,所述第二前驅物化合物具體可以使用由如下化學式5或6表示的化合物,[化學式 5] [化學式 6]
在本發明的有機無機複合薄膜的製造方法中,為了形成所需厚度的所述有機無機複合分子薄膜,可重複進行所述步驟(1)及步驟(2)。
本發明的有機無機複合薄膜的製造方法,所述基板選自由玻璃、矽(silicon)及塑膠構成的群組。
本發明的有機無機複合薄膜的製造方法,其特徵在於還包括:在所述步驟(1)之前,在基板表面形成氧化層的步驟。
並且,本發明的含有機無機複合薄膜的功能性薄膜的製造方法還包括:在通過所述步驟(1)及步驟(2)形成有機無機複合薄膜後,(3)通過原子層沉積法以選自Zn, Sn, In, Cd, Ga, Al, Ti, Si, V, Mn, Fe, Co, Cu, Zr, Ru, Mo, Nb及W的金屬,形成金屬氧化物層的步驟。
本發明的功能性薄膜的製造方法,其特徵在於:重複進行n1次(n1大於等於1)所述步驟(1)及步驟(2)後,重複進行n2次(n2大於等於1)步驟(3)。
本發明的功能性薄膜的製造方法,其特徵在於:重複進行所述步驟(1)至步驟(3)。
技術效果本發明的有機無機複合薄膜及封裝膜包括新官能基,在空氣中的性質穩定,因此可應用於顯示器元件的封裝、太陽能元件的封裝、半導體或電子元件製造所需的奈米圖案(nano patterning)、化學感測器及生物感測器、奈米摩擦學(nano tribology)、表面改性、奈米電子機械系統(NEMS)、微電子機械系統(MEMS)、非易失性記憶體等多種領域。
本發明的有機無機複合薄膜的製造方法交替使用無機物前驅物及有機物前驅物,利用分子層沉積法製造有機無機複合薄膜的過程中使用含現有技術所未曾使用過的新官能基的有機物前驅物,因此可提供在空氣環境下極為穩定的有機無機複合多層分子膜。
下面通過實施例進一步詳細說明本發明。但是本發明不限定於以下實施例。
實施例1用蒸餾水、丙酮(acetone)洗滌矽(Si)基板後,用氮氣(N2
)吹掃2-3次,去除基板表面的污染物質後,使用二乙基鋅(Diethylzinc, DEZn)作為第一前驅物化合物,通過分子層沉積法在矽基板上形成二乙基鋅(Diethylzinc, DEZn)薄膜。
使用4-巰基苯酚作為第二前驅物化合物,通過分子層沉積法在所述二乙基鋅(Diethylzinc,DEZn)薄膜上形成有機分子膜,從而製造有機無機複合薄膜。作為載氣(carrier gas)及吹掃氣體使用氬氣,並分別在20℃及70℃條件下蒸發DEZn及4-巰基苯酚。週期(cycle)由暴露於二乙基鋅(Diethylzinc, DEZn)2秒,用氬氣吹掃10秒,暴露於4-巰基苯酚2秒,用氬氣吹掃50秒的過程構成。所述薄膜在300m托(Torr)壓力下,在80℃至200℃的溫度下進行了生長。
實驗例檢測隨有機前驅物及無機前驅物注入時間變化的生長速度在所述實施例1中,檢測隨第一前驅物化合物二乙基鋅(Diethylzinc, DEZn)的注入時間變化的薄膜生長速度及隨所述第二前驅物化合物4-巰基苯酚注入時間變化的薄膜生長速度,分別用圖1、圖2顯示。
由圖1、圖2可知,薄膜生長速度隨著第一前驅物化合物二乙基鋅(Diethylzinc,DEZn)與第二前驅物化合物4-巰基苯酚的注入量增加到一定程度後不再增加,而是保持一定速度。
實驗例紅外線分光法檢測使用溴化鉀顆粒(KBr pellet)以代替所述矽基板,其他不變,通過與實施例1相同的方法製造有機無機複合薄膜。對該有機無機複合薄膜及4-巰基苯酚分別進行紅外線分光法檢測,結果如圖3所示。
由圖3可知,在只含4-巰基苯酚的比較例中,出現4-巰基苯酚的羥基及硫醇基,而在本發明的有機無機複合薄膜中,作為第二前驅物使用的巰基苯酚的羥基及硫醇基與由第一前驅物製造的無機分子層反應,形成複合薄膜,因此通過紅外線分光法檢測不到巰基苯酚的羥基及硫醇基。
實驗例UV-Vis分光法檢測對實施例1製造的有機無機複合薄膜進行UV-Vis吸光度檢測,結果如圖4所示。
由圖4可知,本發明的有機無機複合薄膜在可視光線領域沒有吸收。
比較例作為比較例,使用二乙基鋅(Diethylzinc,DEZn)作為第一前驅物化合物,通過分子層沉積法在矽基板表面形成二乙基鋅(Diethylzinc,DEZn)薄膜,之後使用對苯二酚(hydroquinone,HQ)作為第二前驅物化合物,除此之外與所述實施例1相同,從而製造有機無機複合薄膜。
實驗例空氣中的穩定性測試把所述實施例1的有機無機複合薄膜及所述比較例製造的有機無機複合薄膜放在空氣中並檢測其厚度變化,以此測試在空氣中的穩定性,結果如圖5所示。
由圖5可知,不同于本發明,不含S基的比較例中,厚度隨著放置於空氣中的時間急劇減小。而本發明的實施例,厚度不隨時間發生變化,由此可知本發明的含S基的有機無機複合多層膜在空氣中非常穩定。
實施例2與所述實施例1相同,使用二乙基鋅(Diethylzinc,DEZn)作為第一前驅物化合物,在矽基板表面上形成薄膜後,使用4-巰基苯酚作為第二前驅物化合物,通過分子層沉積法在所述二乙基鋅(Diethylzinc,DEZn)的薄膜上形成有機無機複合薄膜後,重複進行利用第一前驅物化合物形成二乙基鋅(Diethylzinc,DEZn)薄膜及利用第二前驅物化合物形成薄膜的過程,並檢測相應的厚度,結果如圖6所示。
由圖6可知,通過第一前驅物化合物形成薄膜及通過第二前驅物化合物形成薄膜的過程的重複次數,與所形成的薄膜厚度成比例。
實驗例表面粗糙度的檢測通過原子力顯微鏡(AFM)檢測所述實施例2製造的厚度為50nm的有機無機複合薄膜的表面粗糙度,結果如圖7所示。經檢測,平均粗糙度為2.2Å。
實施例3用蒸餾水、丙酮洗滌矽(Si)基板後,用氮氣(N2
)體吹掃2-3次,去除基板表面的污染物質後,使用三甲基鋁(Trimethyl aluminum,TMA)作為第一前驅物化合物,通過分子層沉積法在矽基板表面上形成三甲基鋁(Trimethyl aluminum,TMA)薄膜。
使用4-巰基苯酚作為第二前驅物化合物,通過分子層沉積法在所述三甲基鋁(Trimethyl aluminum,TMA)薄膜上形成有機分子膜,從而製造有機無機複合薄膜。
作為載氣(carrier gas)及吹掃氣體使用氬氣,並分別在20℃及70℃條件下蒸發三甲基鋁(Trimethylaluminum,TMA)及4-巰基苯酚。週期(cycle)由暴露於三甲基鋁(Trimethylaluminum,TMA)2秒,用氬氣吹掃10秒,暴露於4-巰基苯酚2秒,用氬氣吹掃50秒的過程構成。所述薄膜在300m托(Torr)壓力下,在80℃至200℃的溫度下進行了生長。
實驗例檢測隨有機前驅物及無機前驅物注入時間變化的生長速度在所述實施例3中,檢測隨第一前驅物化合物三甲基鋁(Trimethyl aluminum,TMA)的注入時間變化的薄膜生長速度及隨所述第二前驅物化合物4-巰基苯酚注入時間變化的薄膜生長速度,分別用圖8、圖9顯示。
由圖8、圖9可知,薄膜生長速度隨著第一前驅物化合物三甲基鋁(Trimethyl aluminum,TMA)與第二前驅物化合物4-巰基苯酚的注入量增加到一定程度後不再增加,而是保持一定速度。
實驗例紅外線分光法檢測使用溴化鉀顆粒(KBr pellet)以代替所述矽基板,其他不變,通過與實施例3相同的方法製造有機無機複合薄膜。對該有機無機複合薄膜及4-巰基苯酚分別進行紅外線分光法檢測,結果如圖10所示。
由圖10可知,本發明的有機無機複合薄膜中,作為第二前驅物使用的巰基苯酚的羥基及硫醇基與由第一前驅物製造的無機分子層反應,形成複合薄膜,因此通過紅外線分光法檢測不到巰基苯酚的羥基及硫醇基。
實驗例UV-Vis分光法檢測對所述實施例3製造的有機無機複合薄膜進行UV-Vis吸光度檢測,結果如圖11所示。
由圖11可知,本發明的有機無機複合薄膜在可視光線領域沒有吸收。
比較例作為比較例,使用三甲基鋁(Trimethyl aluminum,TMA)作為第一前驅物化合物,通過分子層沉積法在矽基板表面形成三甲基鋁(Trimethyl aluminum,TMA)薄膜,之後使用對苯二酚(hydroquinone,HQ)作為第二前驅物化合物,除此之外與所述實施例3相同,從而製造有機無機複合薄膜。
實驗例空氣中的穩定性測試把所述實施例3的有機無機複合薄膜及所述比較例製造的有機無機複合薄膜放在空氣中並檢測其厚度變化,以此測試在空氣中的穩定性,結果如圖12所示。
設初始厚度為d0,經過n小時後的厚度為dn時,由圖12可知,不同于本發明,不含S基的比較例,其厚度急劇減小,dn/d0上升到0.5以上,而本發明實施例,厚度不隨時間發生變化,dn/d0保持0.1以下。由此可知,本發明的有機無機複合薄膜在空氣中極為穩定。
實施例4與所述實施例3相同,使用三甲基鋁(Trimethyl aluminum,TMA)作為第一前驅物化合物,在矽基板表面上形成薄膜後,使用4-巰基苯酚作為第二前驅物化合物,通過分子層沉積法在所述三甲基鋁(Trimethyl aluminum,TMA)薄膜上形成有機無機複合薄膜後,重複進行利用第一前驅物化合物形成三甲基鋁(Trimethyl aluminum,TMA)薄膜及利用第二前驅物化合物形成薄膜的過程,並檢測相應的厚度,結果如圖13所示。
由圖13可知,通過第一前驅物化合物形成薄膜及通過第二前驅物化合物形成薄膜的過程的重複次數,與所形成的薄膜厚度成比例。
實驗例表面粗糙度的檢測通過原子力顯微鏡(AFM)檢測所述實施例4製造的厚度為50nm的有機無機複合薄膜的表面粗糙度,結果如圖14所示。經檢測,平均粗糙度為2.8Å。
實施例5通過與實施例1、3相同的方法製造有機無機複合薄膜後,通過原子層沉積法在所述有機無機複合薄膜的上部表面形成Al2
O3
薄膜,在調節利用原子層沉積法形成的Al2
O3
薄膜與通過本發明製造的有機無機複合薄膜之間比例的同時重複進行,從而製造有機無機複合功能性薄膜。
為了通過原子層沉積法形成Al2
O3
薄膜,作為載氣及吹掃氣體使用氬氣,在常溫條件下蒸發三甲基鋁(Trimethyl aluminum,TMA)及H2
O。週期(cycle)由暴露於三甲基鋁(Trimethyl aluminum,TMA)1秒,用氬氣吹掃5秒,暴露於H2
O1秒,用氬氣吹掃5秒的過程構成。所述薄膜在300m托(Torr)的壓力下,在80℃的溫度下生長。
實驗例透射電子顯微鏡(TEM)檢測檢測所述實施例5製造的有機無機複合薄膜: Al2
O3
薄膜之間的比例為1:2時的TEM照片,結果如圖15所示。由圖15可知,交替形成有通過原子層沉積法形成的Al2
O3
薄膜與本發明的有機無機複合薄膜。
實驗例針孔生成抑制效果的檢測
在所述實施例5中改變有機無機複合薄膜厚度的同時檢測針孔生成抑制率,結果如圖16、圖17所示。
如圖16所示,當本發明的有機無機複合薄膜的厚度大於80nm時,幾乎不生成針孔。
實驗例薄膜應力的檢測
對所述實施例5製造的有機無機複合功能性薄膜,使薄膜的總厚度相同的條件下,檢測Al2
O3
薄膜與本發明的有機無機複合薄膜之間的比例不同時所對應的薄膜應力,其結果如圖18所示。
實驗例抗透濕度及抗透氧度的檢測對所述實施例5製造的有機無機複合功能性薄膜及比較例的Al2
O3
薄膜,檢測抗透濕度及抗透氧度,結果如下表1及圖19所示。
由下表1及圖19可知,本發明的含有機無機複合薄膜及Al2
O3
的功能性薄膜與比較例相比,抗透濕度及抗透氧度特性優異。
無
圖1、圖2為本發明一實施例中,第一前驅物及第二前驅物注入量與薄膜生長速度的關係圖;圖3為本發明一實施例製造的有機無機複合薄膜及4-巰基苯酚 (4-mercaptophenol)的紅外線分光法檢測結果的示意圖;圖4為本發明一實施例製造的有機無機複合薄膜的UV-Vis吸光度檢測結果的示意圖;圖5為本發明一實施例製造的有機無機複合薄膜及比較例製造的薄膜在空氣環境中的穩定性測試結果的示意圖;圖6為本發明一實施例中重複進行有機無機複合薄膜形成過程時,隨重複進行而變化的薄膜厚度的檢測結果的示意圖;圖7為本發明一實施例製造的複合薄膜表面的粗糙度檢測結果的示意圖;圖8、圖9為本發明一實施例中,第一前驅物及第二前驅物注入量與薄膜生長速度的關係圖;圖10為本發明一實施例製造的有機無機複合薄膜的紅外線分光法檢測結果的示意圖;圖11為本發明一實施例製造的有機無機複合薄膜的UV-Vis吸光度檢測結果的示意圖;圖12為本發明一實施例製造的有機無機複合薄膜及比較例製造的薄膜在空氣環境中的穩定性測試結果的示意圖;圖13為本發明一實施例製造的有機無機複合薄膜的厚度檢測結果的示意圖;圖14為本發明一實施例製造的有機無機複合薄膜的表面粗糙度檢測結果的示意圖;圖15為本發明一實施例製造的有機無機複合功能性薄膜的透射電子顯微鏡(TEM)圖片檢測結果的示意圖;圖16、圖17為本發明一實施例製造的有機無機複合功能性薄膜中,在改變有機無機複合薄膜厚度的同時檢測的針孔生成抑制率的示意圖;圖18為本發明一實施例製造的有機無機複合功能性薄膜中,對應於通過原子層沉積法形成的 Al2
O3
薄膜與有機無機複合薄膜之間的比例的薄膜應力(stress)檢測結果的示意圖;圖19為本發明一實施例製造的有機無機複合功能性薄膜及比較例製造的薄膜的Ca測試結果的示意圖。
Claims (17)
- 一種有機無機複合薄膜,其特徵在於:由如下化學式1表示:[化學式1]-[M-X-R1-Y-]m- 其中,所述化學式1中m為1以上,R1為經取代的或未經取代的C1~20 烷基(alkyl)、C5~20 環烷基(cycloalkyl)、核原子數為5~60的芳基(aryl)或雜芳基(hetero aryl),M選自由Zn, Sn,In, Cd, Ga, Al, Ti, Si, V, Mn, Fe, Co, Cu, Zr, Ru, Mo, Nb及W構成的群組,X, Y分別選自由O, S, N, NH及CO構成的群組,X或Y中的一個是S。
- 根據申請專利範圍第1項所述的有機無機複合薄膜,其中所述有機無機複合薄膜的厚度為1Å至500 Å。
- 根據申請專利範圍第1項所述的有機無機複合薄膜,其中:設所述有機無機複合薄膜的初始厚度為d0,所述有機無機複合薄膜在標準溫度和壓力條件下放置n小時後的厚度為dn時,滿足如下關係式:0 ≤ (dn/d0)≤ 0.1(0 ≤n ≤ 240) 。
- 一種含有機無機複合薄膜的功能性薄膜,其包括:申請專利範圍第1項所述的有機無機複合薄膜;以及金屬氧化物層,其中金屬選自由Zn, Sn,In, Cd, Ga, Al, Ti, Si, V, Mn, Fe, Co, Cu, Zr, Ru, Mo, Nb及W構成的群組。
- 根據申請專利範圍第4項所述的含有機無機複合薄膜的功能性薄膜,其中:所述含有機無機複合薄膜的功能性薄膜中,所述金屬氧化物層的厚度為10Å至2000Å。
- 根據申請專利範圍第4項所述的含有機無機複合薄膜的功能性薄膜,其中:設含所述有機無機複合薄膜的功能性薄膜的初始厚度為D0,含所述有機無機複合薄膜的功能性薄膜在標準溫度和壓力條件下放置n小時後的厚度為Dn時,滿足如下關係式:0 ≤ (Dn/D0)≤ 0.1(0 ≤n ≤ 240) 。
- 根據申請專利範圍第4項所述的含有機無機複合薄膜的功能性薄膜,其中所述功能性薄膜用於封裝。
- 一種申請專利範圍第1項的有機無機複合薄膜的製造方法,其包括:(1)利用由如下化學式2表示的第一前驅物化合物在基板表面形成無機分子層的步驟,[化學式2]M(R21)(R22)…(R2n)其中,所述化學式2 中所述M 選自由Zn, Sn,Cd, Ti, Si, V, Mn, Fe, Co, Cu, Zr,Ru, Mo, Nb, W, In, Ga, Al 及Tl構成的群組,n由所述金屬M的氧化態決定,R21至R2n分別獨立為C1~20 烷基、C1~20 醇基(alkoxide)、氯基、羥基(hydroxyl group)、氧羥基(oxy hydroxy)、硝酸基、碳酸基、醋酸基或草酸基(oxalic acid);以及(2)使如下化學式3表示的第二前驅物化合物與所述無機分子層反應,在所述無機分子層上形成有機分子層的步驟,[化學式3]R3-S-R4-R5其中,所述化學式3中,R3為氫、COR6、C1~20 烷基、C5~20 環烷基、核原子數為5~60的芳基或雜芳基,R4為C1~20 烷基、C5~20 環烷基、核原子數為5~60的芳基或雜芳基,R5為選自由羥基、C1~20 烷氧基(alkoxygroup)、醚基(ether group)、羧基(carboxyl group)、COR6、硫醇基(thiolgroup)及氨基(amine group)構成的群組的任一種或以上的組合,R6為選自由氫、烷氧基、醚基、羧基、硫醇基及氨基構成的群組的任一種或以上的組合。
- 根據申請專利範圍第8項所述的有機無機複合薄膜的製造方法,其中:所述第二前驅物化合物由如下化學式4表示:[化學式 4] 其中,所述化學式4中,Z為硫醇基,Q為選自硫醇基及羥基中的一種,Z與Q的位置為鄰位、間位或對位。
- 根據申請專利範圍第8項所述的有機無機複合薄膜的製造方法,其中所述第二前驅物化合物由如下化學式5表示:[化學式 5]
- 根據申請專利範圍第8項所述的有機無機複合薄膜的製造方法,其中所述第二前驅物化合物由如下化學式6表示:[化學式 6]
- 根據申請專利範圍第8項所述的有機無機複合薄膜的製造方法,其還包括:重複進行所述步驟(1)及步驟(2)的步驟。
- 根據申請專利範圍第8項所述的有機無機複合薄膜的製造方法,其中所述基板選自由玻璃、矽(silicon)及塑膠構成的群組。
- 根據申請專利範圍第8項所述的有機無機複合薄膜的製造方法,其還包括:在所述步驟(1)之前,在基板表面形成氧化層的步驟。
- 根據申請專利範圍第8項所述的含申請專利範圍第4項的有機無機複合薄膜的功能性薄膜的製造方法,其還包括:(3)通過原子層沉積法,以選自由Zn, Sn,In, Cd, Ga, Al, Ti, Si, V, Mn, Fe, Co, Cu, Zr, Ru, Mo, Nb及W構成的群組的金屬,形成金屬氧化物層的步驟。
- 根據申請專利範圍第15項所述的功能性薄膜的製造方法,其包括:重複進行n1次(n1大於等於1)所述步驟(1)及步驟(2)後,重複進行n2次(n2大於等於1)步驟(3)。
- 根據申請專利範圍第15項所述的功能性薄膜的製造方法,其包括:重複進行所述步驟(1)至步驟(3)。
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