CN110786078A - 柔性装置用基板 - Google Patents
柔性装置用基板 Download PDFInfo
- Publication number
- CN110786078A CN110786078A CN201880042096.4A CN201880042096A CN110786078A CN 110786078 A CN110786078 A CN 110786078A CN 201880042096 A CN201880042096 A CN 201880042096A CN 110786078 A CN110786078 A CN 110786078A
- Authority
- CN
- China
- Prior art keywords
- glass
- layer
- substrate
- nickel plating
- plating layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000758 substrate Substances 0.000 title claims abstract description 95
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 190
- 239000011521 glass Substances 0.000 claims abstract description 158
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 95
- 238000007747 plating Methods 0.000 claims abstract description 86
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 44
- 239000010935 stainless steel Substances 0.000 claims abstract description 40
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 28
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 abstract description 38
- 230000004888 barrier function Effects 0.000 abstract description 13
- 238000005452 bending Methods 0.000 abstract description 10
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 6
- 238000010292 electrical insulation Methods 0.000 abstract 1
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 160
- 239000010408 film Substances 0.000 description 48
- 239000000203 mixture Substances 0.000 description 18
- 238000010304 firing Methods 0.000 description 17
- 229910052751 metal Inorganic materials 0.000 description 14
- 239000002184 metal Substances 0.000 description 14
- 239000000843 powder Substances 0.000 description 11
- 238000000576 coating method Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 9
- 238000009792 diffusion process Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 239000002344 surface layer Substances 0.000 description 9
- 239000011230 binding agent Substances 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 8
- 238000005238 degreasing Methods 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 239000012298 atmosphere Substances 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000011888 foil Substances 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000010298 pulverizing process Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- -1 chromium oxyhydroxide Chemical compound 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000009713 electroplating Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229910000480 nickel oxide Inorganic materials 0.000 description 3
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 2
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 238000000879 optical micrograph Methods 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000002985 plastic film Substances 0.000 description 2
- 229920006255 plastic film Polymers 0.000 description 2
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- 239000009719 polyimide resin Substances 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 229940116411 terpineol Drugs 0.000 description 2
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 description 2
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 description 1
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000012461 cellulose resin Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000001087 glyceryl triacetate Substances 0.000 description 1
- 235000013773 glyceryl triacetate Nutrition 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical group [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 238000010902 jet-milling Methods 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 238000007645 offset printing Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920000379 polypropylene carbonate Polymers 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229960002622 triacetin Drugs 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
- H01B3/08—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances quartz; glass; glass wool; slag wool; vitreous enamels
- H01B3/088—Shaping of glass or deposition of glass
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
- C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/14—Silica-free oxide glass compositions containing boron
- C03C3/145—Silica-free oxide glass compositions containing boron containing aluminium or beryllium
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
- C03C8/16—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions with vehicle or suspending agents, e.g. slip
-
- 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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
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Abstract
本发明提供一种柔性装置用基板,其在展现优异的防锈性、水分阻隔性和玻璃层的密合性的同时,具有优异的耐弯曲性和玻璃层表面的优异的表面平滑性。该柔性装置用基板的特征在于,其包括:不锈钢基材;形成在不锈钢基材的表面上的镍镀层;以及在镍镀层的表面上以具有电绝缘性的铋系玻璃层的形式形成的玻璃层。
Description
技术领域
本发明涉及柔性装置用基板。更具体地,本发明涉及具有优异的防锈性、水分阻隔性、耐弯曲性和绝缘层的密合性且没有表面缺陷,因此,优选地适用于与有机EL相关的设备的柔性装置用基板。
背景技术
用于有机EL照明、有机EL显示器、有机太阳能电池等的柔性装置用基板需要具有例如水分阻隔性和气体阻隔性等阻隔性,以及平滑性和绝缘性。另外,基板需要具有优异的柔软性(耐弯曲性),使得其可以被应用在弯曲表面上或者可以以辊对辊工艺来制造。
下面的专利文献1公开了通过在塑料膜基材上依次层叠透明导电层、有机发光介质层和阴极层,并且进一步在其上经由粘接层层叠金属箔而制备的有机EL器件的结构。但是,从水分阻隔性和耐热性的观点出发,塑料膜基材并不令人满意。
下面的专利文献2公开了在不锈钢基材上设置有聚酰亚胺树脂的平坦化层的柔性装置用基板。然而,由于聚酰亚胺树脂的高吸水性,因此该柔性装置用基板不能提供令人满意的水分阻隔性。
下面的专利文献3公开了通过在不锈钢基材上形成二氧化硅系玻璃制的膜而制备的柔性太阳能电池基板。然而,一般地二氧化硅系玻璃的热膨胀系数小于不锈钢的热膨胀系数,因此,其缺乏与不锈钢基材的密合性。二氧化硅系玻璃的另一个问题在于,其容易弯曲且易受冲击。
为了解决这些问题,本发明人在专利文献4中提出了一种柔性装置用金属基板。该基板通过在金属基材的表面上形成镍镀层并且在镍镀层的表面上涂覆电绝缘性铋系玻璃来制备。
现有技术文献:
专利文献:
专利文献1:JP 2004-171806 A
专利文献2:JP 2011-97007 A
专利文献3:JP 2006-80370 A
专利文献4:JP 2014-107053 A
发明内容
发明要解决的问题
通过将铋系玻璃涂覆在金属基材上来制备柔性装置用金属基板。由于铋系玻璃具有优异的水分阻隔性和对金属基材的优异的密合性,因此基板具有优异的绝缘性和平坦性。此外,基板重量轻且柔软。然而,烧制后的玻璃层表面会具有起颗粒(seeding)(微小的突起)和收缩(cissing)。这些微小的缺陷会损害玻璃层的平滑性。
当将钢材用于金属基材时,截面会生锈。即使当将耐生锈的不锈钢基材用于金属基材时,如果直接在不锈钢基材上形成玻璃层,则无法实现基材与玻璃层之间的充分的密合性。这会降低耐弯曲性并引起诸如玻璃层破损和剥离等问题。
作为对这些问题的研究结果,本发明人发现了问题的原因。即,金属基材与玻璃层之间的密合性一般由于金属从金属基材扩散至玻璃层中并且与玻璃组分反应以形成反应层而显示。在这种情况下,反应层会随着来自金属基材的金属的扩散量和扩散距离(在玻璃层的厚度方向上的距离)增大而进一步增长,并且这可以提高密合性。同时,在不锈钢的表面上形成水合羟基氧化铬作为钝化膜。由于来自该水合羟基氧化铬的铬的扩散量和扩散距离小,因此不能在玻璃层上形成能够充分改善密合性的反应层。结果,不能获得令人满意的密合性。
因此,本发明的目的是提供一种柔性装置用基板,该基板在防锈性、水分阻隔性和玻璃层的密合性方面优异。该基板在耐弯曲性和玻璃层表面的表面平滑性方面也优异。
用于解决问题的方案
本发明提供一种柔性装置用基板。该基板包括不锈钢基材、形成在不锈钢基材的表面上的镍镀层、以及在镍镀层的表面上以层状形成的电绝缘性铋系玻璃的玻璃层。
在本发明的柔性装置用基板中,优选的是:
1.在镍镀层的表面上形成具有凹凸表面的氧化物膜;
2.在玻璃层的厚度方向上与界面相距10nm的深度处的镍浓度为0.1原子%以上,所述界面在玻璃层与镍镀层之间,并且当在镍镀层的表面上形成有氧化物膜时,所述界面在玻璃层与氧化物膜之间;
3.在镍镀层或氧化物膜的厚度方向上与界面相距10nm的深度处的铋浓度为20原子%以下,所述界面在玻璃层与镍镀层之间,并且当在镍镀层的表面上形成有氧化物膜时,所述界面在玻璃层与氧化物膜之间;和
4.铋系玻璃包含Bi2O3、ZnO和B2O3。
发明的效果
在本发明的柔性装置用基板中,通过使用不锈钢基材有效地防止生锈。此外,通过在不锈钢基材上形成镍镀层,不锈钢基材与玻璃层之间的密合性得到显著改善。由于该基板具有优异的耐弯曲性,因此当其用作柔性装置用基板时,其具有足够的柔软性而不会剥离等。
此外,由于在镍镀层上形成了氧化物膜,并且在氧化物膜上形成了玻璃层,因此有效地减少了玻璃层中的气泡,从而可以提供在表面平滑性和绝缘性方面优异的具有玻璃层的基板。
此外,因为基板包括具有用于完美地防止水分渗透的致密结构的玻璃层,所以该基板在水分阻隔性方面也优异,因此,其可以有效地用作有机EL用基板。
附图说明
[图1]:示出本发明的柔性装置用基板的一个实例的结构的截面图。
[图2]:一组示出实施例2和比较例5中使用的基材表面的玻璃未涂覆的表面和端面的光学显微图片。
具体实施方式
(柔性装置用基板)
通过在不锈钢基材的表面上形成镍镀层,并且在该镍镀层的表面上形成玻璃层来制备本发明的柔性装置用基板。结果,镍镀层中足够量的镍充分深地扩散至玻璃层中,从而形成足以改善与玻璃层的密合性的反应层以显著改善镍镀层与玻璃层之间的密合性。这起到改善耐弯曲性的作用,并且基板可以适应辊对辊工艺而不会引起如上所述的玻璃层的剥离。
在本发明的柔性装置用基板中,镍从镍镀层充分扩散至玻璃层中,从而改善密合性。通过测量在玻璃层的厚度方向上距镍镀层与玻璃层之间的界面10nm深度处的镍浓度,可以明确该效果。在10nm深度处,以0.1原子%以上、特别是3原子%以上的量存在镍,以显著改善密合性。下述实施例中的结果进一步表明,耐弯曲性也得到显著改善。
下面描述的实施例中的结果表明,随着与镍镀层和玻璃层之间的界面的距离增加,玻璃层中的镍浓度降低。即使这样,如果在10nm深度处该浓度在上述范围内,则镍的扩散量和扩散距离足以获得上述效果。
如上所述,为了改善不锈钢基材与玻璃层之间的密合性,在不锈钢基材上形成镍镀层。这可以赋予密合性以抵抗弯曲,但是其可能在玻璃层中产生气泡。在玻璃层表面上形成的气泡会引起起颗粒和收缩,从而降低玻璃层的平滑性。为了防止这种气泡,在本发明中优选的是,在形成于不锈钢基材上的镍镀层的表面上形成氧化物膜。
即,根据本发明人的研究,当在镍镀层的表面上形成玻璃层时,在界面附近似乎发生由下式表示的反应。
2Bi2O3+4Ni→4NiO+O2+4Bi
上式阐明了作为玻璃组分的Bi2O3被还原以生成O2作为气泡。同时,在镍镀层上形成氧化物膜的情况下,由氧化镍和铁氧化物(iron oxide)组成的氧化物膜形成与玻璃层之间的界面,从而防止或控制由该式表示的反应。这使得Bi2O3难以被还原,从而防止或减少气泡的产生。
因此,本发明能够通过在镍镀层的表面上形成氧化物膜来有效地防止气泡的产生。此外,氧化物膜与玻璃之间的反应可以进一步增强基材与玻璃层之间的密合性。
气泡的产生与扩散到基材表面层中的玻璃组分的量相关。在其中控制气泡(氧气)的产生的本发明的柔性装置用基板中,在基材表面层(镍镀层或氧化物膜)的厚度方向上距离基材表面层与玻璃层之间的界面10nm深度处的铋浓度20原子%以下、特别是15原子%以下。这表明防止或控制了玻璃组分从玻璃层向基材表面层的扩散。即,由于气泡(氧气)通过玻璃的还原而产生,因此,当玻璃组分进一步向基材表面层扩散时,产生更多的气泡(氧气)。结果,在10nm深度处存在大于20原子%的铋的情况下,大量的玻璃组分将扩散至基材表面层中,从而增加玻璃层中的气泡。
如下述实施例的结果所示,随着与镍镀层和玻璃层之间的界面的距离增大,基材表面层中的铋浓度降低。因此,当在距界面10nm的点处的铋浓度在上述范围内时,表明防止或控制了玻璃组分向基材表面层中的扩散,并且获得上述效果。
本发明的柔性装置用基板的第一特征在于,如图1的截面图所示,基板具有不锈钢基材10、形成在不锈钢基材10的表面上的镍镀层11、以及在镍镀层11的表面上以层状形成的电绝缘性铋系玻璃的玻璃层20。更具体地,在图1所示的具体实例中,具有凹凸12a的氧化物膜12形成在镍镀层11的表面上。
[不锈钢基材]
任何常规已知的不锈钢材料均可用于本发明的柔性装置用基板的不锈钢基材。在这些材料中,可以特别优选使用铁素体系不锈钢。优选使用热膨胀系数为9.9×10-6至21×10-6/℃、特别是10×10-6至14×10-6/℃的材料。
为了获得足够的柔软性,优选的是,不锈钢基材的厚度在10至200μm的范围内、特别是在25至100μm的范围内。
[镍镀层]
在本发明的柔性装置用基板中,形成在不锈钢基材表面上的镍镀层是通过镀覆镍而形成的层,并且该镀覆可以是如下所述的电解镀覆或化学镀覆。尽管在图1所示的实例中,镍镀层仅形成在不锈钢基材的一个表面上,但是其也可以形成在不锈钢基材的两个表面上。
优选地,镍镀层的厚度在0.1至10μm的范围内、特别优选在0.5至5μm的范围内。在镍镀层的厚度小于该范围的情况下,与该厚度在该范围内的情况相比,与玻璃层的密合性会较差。即使当镍镀层的厚度大于该范围时,也不能期望效果的进一步改善,并且从经济性的观点来看,该基材会较差。当形成氧化物膜时,镍镀层的厚度可以包括氧化物膜的厚度。
镍镀层可以在与不锈钢基材的界面上具有合金层。
如上所述,优选的是,在本发明的柔性装置用基板的镍镀层的表面上形成氧化物膜,从而防止或控制气泡的产生。
镍层以上述方式用于改善密合性。另外,通过氧化物膜与玻璃之间的反应形成密合层,这可以进一步改善不锈钢基材与玻璃层之间的密合性。
氧化物膜由氧化镍和铁氧化物组成。如下所述,通过在含氧气氛中烧制镍镀层的表面来形成氧化镍,并且铁氧化物从不锈钢基材中扩散出来。
在本发明中,推测为晶粒的凸部形成在氧化物膜的表面上以形成凹凸(粗糙化的表面),从而防止玻璃组合物在玻璃层形成期间散布,以有效地防止或控制收缩。此外,由于烧制了镍镀层,因此从镍镀层释放出解吸气体,从而有效地防止或控制会引起收缩的气泡。
优选的是,赋予氧化物膜表面上的凹凸(表面粗糙度),使得算术平均粗糙度(Ra)在30至100nm的范围内、特别是在50至90nm的范围内,并且最大高度粗糙度(Rz)在420至900nm的范围内、特别是在600至850nm的范围内。
氧化物膜的厚度优选在10至1200nm的范围内、特别优选在100至1000nm的范围内。当氧化物膜的厚度小于该范围时,与该厚度在该范围内的情况相比,镍镀层的表面改性会不足。当氧化物膜的厚度大于该范围时,与该厚度在该范围内的情况相比,镍镀层的表面层会进一步合金化,并且会削弱镍镀层且损害柔软性。
[玻璃层]
本发明的柔性装置用基板包括形成在上述镍镀层上或形成于镍镀层上的具有凹凸表面的氧化物膜上的绝缘层。绝缘层是具有优异的水分阻隔性和对金属基材的优异的密合性的铋系玻璃的玻璃层。
在本发明中,可以优选使用包含Bi2O3、ZnO和B2O3的铋系玻璃。即,作为必要组分的ZnO和B2O3与Bi2O3一起作为主要组分而包含在其中,因此这些组分在共晶点的范围内。这可以形成非结晶玻璃网络结构。通过将玻璃与上述的镍镀层组合,可以提供一种能有效防止和控制玻璃表面上的收缩的柔性装置用基板。
对于铋系玻璃,优选软化点在300至500℃范围内的电绝缘性玻璃。对于玻璃组成,优选包含Bi2O3作为主要组分(特别是70重量%以上)的玻璃。特别优选的是,玻璃是包含70至84重量%的Bi2O3、10至12重量%的ZnO和6至12重量%的B2O3的铋系无铅玻璃,但是本发明不限于该实例。当包含在这些范围内的这些组分时,防止或控制了玻璃层的结晶化,并且可以有效地防止收缩。
除上述必要组分外,铋系玻璃还包含SiO2和/或Al2O3。优选的是,SiO2的含量为0至2重量%,Al2O3的含量为0至1重量%。由于共混这些组分中的至少一种,因而水分阻隔性和耐久性可以得到改善,从而使玻璃层稳定。
优选的是,除了上述必要组分以外,铋系玻璃还包含CuO和/或NiO。通过共混2重量%以下的CuO和2重量%以下的NiO,玻璃的熔融性可以得到改善。
另外,除了上述必要组分以外,铋系玻璃还可以包含1.5重量%以下的Y2O3、ZrO2、La2O3、CeO2、TiO2、CoO和Fe2O3中的任意者。这些组分可以改善玻璃的耐久性,但是这些组分的过量混合会降低玻璃的耐久性。这些组分可以以其至少两种的组合使用。在这种情况下,总量优选为1.5重量%以下。
在本发明中,玻璃层的厚度优选在2至45μm的范围内、特别是在5至20μm的范围内。当玻璃层的厚度小于该范围时,与该厚度在该范围内的情况相比,会无法确保充分的绝缘性。此外,在镍镀层上形成氧化物膜的情况下,会无法使氧化物膜的凹凸充分平滑化。当该厚度大于该范围时,与该厚度在该范围内的情况相比,柔软性会较差。
(柔性装置用基板的生产方法)
可以通过以下方法来生产本发明的柔性装置用基板:所述方法包括在不锈钢基材的至少一个表面上形成镍镀层的镀覆步骤;以及在镍镀层上形成铋系玻璃层的玻璃层形成步骤。在镍镀层上形成氧化物膜的情况下,在镀覆步骤和玻璃层形成步骤之间进一步进行氧化物膜形成步骤。在氧化物膜形成步骤中,在含氧气氛中烧制镍镀层,从而在镍镀层的表面上形成氧化物膜。
[镍镀层的形成步骤]
在本发明的柔性装置用基板上的镍镀层的形成可以通过任何常规方法来进行。
对于镍镀层的形成步骤,在镀覆之前,通过碱性电解等使基材脱脂,在水中洗涤,然后进行例如通过浸渍于硫酸等中的酸洗等常规已知的预处理。
如上所述,以任何常规已知的方法,例如电解镀覆和化学镀覆来镀覆预处理的不锈钢基材,从而可以形成镍镀层。从连续生产性的观点出发,电解镀覆是优选的。对于镀镍浴,可以根据已知配方在已知的电解条件下使用任何广泛使用的浴,例如瓦特浴和氨基磺酸浴。如上所述,镍镀层优选形成为厚度在0.1至10μm的范围内、特别是在0.5至5μm的范围内。
[氧化物膜的形成步骤]
在本发明的柔性装置用基板的生产方法中,在含氧气氛中烧制(以下也可称为“焙烧”)形成于不锈钢基材上的镍镀层,从而在镍镀层的表面上形成具有凹凸的氧化物膜。
焙烧的条件没有特别限制,只要能够形成上述氧化物膜即可,但是优选焙烧温度在550至1000℃、特别是在600至950℃的范围内。可以根据含氧气氛中的氧浓度和烧制温度来适当地改变焙烧时间。在大气中在上述温度范围内烧制的情况下,优选的是,在上述焙烧温度下烧制5至120秒。
如上所述,氧化物膜形成为厚度在10至1200nm的范围内、优选在100至1000nm的范围内。
根据焙烧条件,在该步骤期间通过烧制形成氧化物膜可以在镍镀层的表面上形成合金层。
[玻璃层的形成步骤]
接下来,在镍镀层上或在镍镀层上形成的氧化物膜上形成铋系玻璃层。
在玻璃层的形成步骤中,通常将玻璃粉末和介质混合并分散以制备玻璃糊剂,将其涂覆并干燥于镍镀层上或镍镀层表面的氧化物膜上,并且烧制,但是这些过程不限于该实例。
<玻璃糊剂的制备>
在玻璃糊剂的制备中,将上述玻璃组合物的玻璃料粉碎以形成玻璃组合物粉末,然后将其与介质混合并分散。
通过混合玻璃组合物,在800至1200℃的温度下加热以形成熔融玻璃,淬火以获得玻璃料,然后将玻璃料粉碎,来获得玻璃组合物粉末。可以通过任何常规已知方法进行粉碎,且实例包括JET粉碎、快速磨机粉碎和球磨机粉碎。
为了使玻璃表面平滑,玻璃组合物粉末的平均粒径为20μm以下、优选在1至10μm、更优选在1至5μm的范围内。为了获得细粉末,优选JET粉碎。
然后,将由此获得的玻璃组合物粉末与介质混合并分散。混合-分散法的实例包括使用具有搅拌叶片的旋转混合机、珠磨机、油漆搅拌器、辊磨机、玛瑙研钵和超声波来分散。优选的是,通过使用珠磨机、油漆搅拌器或辊磨机进行混合和分散。
可以根据需要将已知的增稠剂或分散剂等根据已知配方添加至玻璃糊剂中。
与玻璃组合物粉末混合以组成糊剂的介质用于调节糊剂的粘度。通过将有机粘结剂溶解在溶剂中来制备介质。
优选的是,玻璃糊剂包含30至80重量%的玻璃组合物粉末、大于0且10重量%以下的有机粘结剂、以及10至70重量%的溶剂。当玻璃组合物粉末的量小于该范围时,糊剂粘度降低,从而难以形成具有期望厚度的玻璃层。当玻璃组合物粉末的量大于该范围时,糊剂粘度变得极高而使涂布性能下降。当有机粘结剂的量小于该范围时,涂布性能将下降。当有机粘结剂的量大于该范围时,在烧制步骤之后会残留未烧制的有机材料。此外,当溶剂的量小于该范围时,糊剂粘度变得极高而使涂布性能下降。并且,当溶剂的量大于该范围时,糊剂粘度变得极低,从而难以形成具有期望厚度的玻璃层。
对于介质,可以使用任何常规已知的溶剂系或水系介质,并且其实例包括以下有机粘结剂和溶剂,但是本发明不限于这些实例。
有机粘结剂的实例包括:例如甲基纤维素、乙基纤维素、羧甲基纤维素、羟乙基纤维素、苄基纤维素、丙基纤维素和硝化纤维素等纤维素系树脂;例如如甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丁酯、甲基丙烯酸-2-羟乙酯、丙烯酸丁酯和丙烯酸-2-羟乙酯等通过使至少一种丙烯酸系单体聚合而获得的丙烯酸系树脂等有机树脂;以及例如聚碳酸丙烯酯等脂肪族聚烯烃系碳酸酯树脂,但是本发明不限于这些实例。
可以根据使用的有机粘结剂适当地选择溶剂。实例包括:用于纤维素系树脂的水、松油醇、丁基卡必醇乙酸酯和乙基卡必醇乙酸酯等;用于丙烯酸系树脂的甲基乙基酮、松油醇、丁基卡必醇乙酸酯或乙基卡必醇乙酸酯等;以及用于脂肪族聚烯烃系碳酸酯的碳酸丙烯酯或三乙酸甘油酯等,但是本发明不限于这些实例。
<玻璃糊剂的涂覆、干燥和烧制>
通过根据玻璃糊剂的粘度选择的涂覆方法,将由此制备的玻璃糊剂涂覆在镍镀层或氧化物膜上。可以通过使用棒涂机、模头涂布机、辊涂机、凹版涂布机、丝网印刷、胶版印刷或涂抹器等进行涂覆,但是本发明不限于这些实例。
将涂覆的玻璃糊剂在80至180℃的温度下干燥。干燥后,根据需要进行脱脂处理。优选地,通过在180至450℃的温度下加热10分钟以上来进行脱脂处理。
干燥后,将根据需要预先进行脱脂处理的涂覆表面在550至900℃、优选650至900℃的温度下烧制10至300秒。当烧制温度低于该范围时,与该温度在该范围内的情况相比,熔融会不充分。当烧制温度高于该范围时,与该温度在该范围内的情况相比,镍镀层会受到影响。
实施例
1.不锈钢基材
使用厚度为0.05mm的五种不锈钢基材。
NK-430MA:铁素体系不锈钢箔(由Nippon Kinzoku Co.,Ltd.制造)
NCA-1:铁素体系不锈钢箔(由Nippon Steel Nisshin Co.,Ltd.制造)
SUS430:铁素体系不锈钢箔
SUS304:奥氏体系不锈钢箔
SUS316L:奥氏体系不锈钢箔
对于在比较例中使用的钢基材,准备通过使普通钢的冷轧板(厚度:0.05mm)退火脱脂而得到的钢板。
接下来,对上述基材(尺寸:长度为20cm、宽度为50cm)进行碱性电解脱脂并且通过浸渍于硫酸中而酸洗。
2.基材处理
对基材表面进行如表1中所示的焙烧-1、镀镍和焙烧-2中的任何一种处理或其组合处理。
(1)焙烧-1
如表1中所示,将不锈钢基材的表面在大气中在950℃的温度下加热20秒。
(2)镀镍
如表1中所示,在以下所述的条件下对未进行焙烧-1的不锈钢基材和钢板镀覆镍,由此在基材或板的两个表面上形成各自厚度为2μm的镍镀层。
浴液组成:300g/L硫酸镍;40g/L氯化镍;35g/L硼酸;和0.4mL/L防蚀剂(月桂基硫酸钠)。
pH:4至4.6
浴温:55℃至60℃
电流密度:25A/dm2
(3)焙烧-2
如表1中所示,与焙烧-1类似,仅将基材的镀覆有镍的表面在大气中在950℃的温度下加热20秒。
3.玻璃层的形成
在脱脂步骤中,为了脱脂的目的,用浸泡在醇中的纱布擦拭每个样品的表面。
在涂膜形成步骤中,准备作为有机溶剂和粘结剂的混合物的介质。在将介质与表5中所述的铋系玻璃组合物粉末以25:75的重量比在研钵中混合。使用陶瓷辊磨机将混合物分散以生产涂覆用玻璃糊剂。通过使用棒涂机将玻璃糊剂涂覆在样品上,以使烧制后的膜厚度为10μm。之后,使用电炉通过干燥(温度:110℃,时间:20分钟)、脱脂(温度:330℃,时间:20分钟)和烧制(温度:850℃,时间:30秒)进行玻璃烧制步骤,以形成玻璃层。
4.评价
(1)盐雾试验(SST)
使实施例和比较例中生产的柔性装置用基板根据JIS Z 2371进行盐雾试验。结果示于表1中。图2包括实施例2和比较例5中使用的基材的玻璃未涂覆的表面和端面的光学显微图片。
(2)耐弯曲性
评价标准如下。
由卷绕试验引起的剥离和裂纹(目视观察)
○:玻璃/基材界面没有剥离并且没有裂纹。
△:玻璃/基材界面没有剥离,但有微小的裂纹。
×:玻璃/基材界面没有剥离,但有小的裂纹。
综合评价如下。
×:对或的评价包括△或×。
(3)玻璃层中的镍浓度
对于在实施例1、2和比较例1、2、12和13中生产的柔性装置用基板的玻璃层,通过使用能量分散X射线光谱(EDS)的分析来测量在与玻璃层和基材之间的界面相距10nm、20nm和50nm的深度处的镍浓度。结果示于表2中。
(4)氧化物膜的厚度和表面粗造度
使用场致发射俄歇微探针(AES:由JEOL制造,PN:JAMP-9500F)测量在实施例1、2以及比较例1至4、12和13中获得的柔性装置用基板的氧化物膜的厚度。此外,通过使用显微镜(PN:OLS3500,由Olympus Corporation制造的Nano Search Microscope)根据JIS B 0601以SPM测量模式来测量实施例1至4和比较例1至4、12和13中生产的柔性装置用基板的氧化物膜的算术平均粗糙度(Ra)和最大高度粗糙度(Rz)。结果示于表3中。
(5)基材中的铋浓度
对于在实施例1、2和比较例1、2、12和13中生产的柔性装置用基板的基材,通过使用能量分散X射线光谱(EDS)的分析来测量与玻璃层和基材之间的界面相距10nm、20nm和50nm的深度处的铋浓度。结果示于表4中。
(6)玻璃层中的气泡
对于在实施例1、2以及比较例1至4、12和13中生产的柔性装置用基板的玻璃层,通过使用显微镜(PN:OLS3500,由Olympus Corporation制造的Nano Search Microscope)的观察来检查玻璃层中的气泡。具体地,在聚焦在玻璃层的表面上之后,在玻璃层的深度方向上移动焦点的同时进行观察。结果示于表3中。
[表5]
组分 | 组成(wt%) |
Bi<sub>2</sub>O<sub>3</sub> | 81.00 |
ZnO | 10.87 |
B<sub>2</sub>O<sub>3</sub> | 6.21 |
SiO<sub>2</sub> | 1.31 |
Al<sub>2</sub>O<sub>3</sub> | 0.47 |
CuO | 0.14 |
NiO | 0.00 |
共计 | 100.00 |
产业上的可利用性
本发明的柔性装置用基板具有优异的防锈性、水分阻隔性、绝缘性、耐弯曲性、以及玻璃层的表面平滑性和密合性。其可适合用作有机EL照明、有机EL显示器和有机薄膜太阳能电池等的基板。
附图标记说明
1:柔性装置用基板
10:不锈钢基材
11:镍镀层
12:氧化物膜
20:玻璃层
Claims (5)
1.一种柔性装置用基板,其包括不锈钢基材、形成在所述不锈钢基材的表面上的镍镀层、以及在所述镍镀层的表面上以层状形成的电绝缘性铋系玻璃的玻璃层。
2.根据权利要求1所述的柔性装置用基板,其中在所述镍镀层的表面上形成具有凹凸表面的氧化物膜。
3.根据权利要求1或2所述的柔性装置用基板,其中在所述玻璃层的厚度方向上与界面相距10nm的深度处的镍浓度为0.1原子%以上,所述界面在所述玻璃层与所述镍镀层之间,并且当在所述镍镀层的表面上形成有所述氧化物膜时,所述界面在所述玻璃层与所述氧化物膜之间。
4.根据权利要求1至3中任一项所述的柔性装置用基板,其中在所述镍镀层或氧化物膜的厚度方向上与界面相距10nm的深度处的铋浓度为20原子%以下,所述界面在所述玻璃层与所述镍镀层之间,并且当在所述镍镀层的表面上形成有所述氧化物膜时,所述界面在所述玻璃层与所述氧化物膜之间。
5.根据权利要求1至4中任一项所述的柔性装置用基板,其中所述铋系玻璃包含Bi2O3、ZnO和B2O3。
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