CN114040899A - 涂覆的玻璃基底的釉质涂层 - Google Patents
涂覆的玻璃基底的釉质涂层 Download PDFInfo
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- CN114040899A CN114040899A CN202080042056.7A CN202080042056A CN114040899A CN 114040899 A CN114040899 A CN 114040899A CN 202080042056 A CN202080042056 A CN 202080042056A CN 114040899 A CN114040899 A CN 114040899A
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- composition
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- enamel
- microns
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- 239000011521 glass Substances 0.000 title claims abstract description 126
- 239000000758 substrate Substances 0.000 title claims abstract description 84
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- 238000000034 method Methods 0.000 claims abstract description 61
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- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000007787 solid Substances 0.000 claims abstract description 29
- 238000010304 firing Methods 0.000 claims abstract description 26
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 20
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- 229910003069 TeO2 Inorganic materials 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 44
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- 238000004090 dissolution Methods 0.000 claims description 4
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- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 3
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims 1
- 239000011787 zinc oxide Substances 0.000 description 22
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 11
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- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 229910052709 silver Inorganic materials 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000007858 starting material Substances 0.000 description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- -1 K2A compound Chemical class 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 239000003989 dielectric material Substances 0.000 description 4
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- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
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- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
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- 229910052797 bismuth Inorganic materials 0.000 description 3
- 238000012669 compression test Methods 0.000 description 3
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- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 238000010902 jet-milling Methods 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
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- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 3
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
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- 229910052804 chromium Inorganic materials 0.000 description 2
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- 239000002131 composite material Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000000976 ink Substances 0.000 description 2
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- 238000007561 laser diffraction method Methods 0.000 description 2
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- 238000005240 physical vapour deposition Methods 0.000 description 2
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- 238000005245 sintering Methods 0.000 description 2
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Inorganic materials [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 2
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000003313 weakening effect Effects 0.000 description 2
- IJJWOSAXNHWBPR-HUBLWGQQSA-N 5-[(3as,4s,6ar)-2-oxo-1,3,3a,4,6,6a-hexahydrothieno[3,4-d]imidazol-4-yl]-n-(6-hydrazinyl-6-oxohexyl)pentanamide Chemical compound N1C(=O)N[C@@H]2[C@H](CCCCC(=O)NCCCCCC(=O)NN)SC[C@@H]21 IJJWOSAXNHWBPR-HUBLWGQQSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 239000004110 Zinc silicate Substances 0.000 description 1
- KKEYTLVFLSCKDE-UHFFFAOYSA-N [Sn+2]=O.[O-2].[Zn+2].[O-2] Chemical compound [Sn+2]=O.[O-2].[Zn+2].[O-2] KKEYTLVFLSCKDE-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000005328 architectural glass Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
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- 230000032798 delamination Effects 0.000 description 1
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- DQUIAMCJEJUUJC-UHFFFAOYSA-N dibismuth;dioxido(oxo)silane Chemical compound [Bi+3].[Bi+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O DQUIAMCJEJUUJC-UHFFFAOYSA-N 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
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- 238000001704 evaporation Methods 0.000 description 1
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- 239000000945 filler Substances 0.000 description 1
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- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
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- 239000007791 liquid phase Substances 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
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- 238000002360 preparation method Methods 0.000 description 1
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- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000006254 rheological additive Substances 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
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- 238000001429 visible spectrum Methods 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 description 1
- 235000019352 zinc silicate Nutrition 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/001—General methods for coating; Devices therefor
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/02—Surface treatment of glass, not in the form of fibres or filaments, by coating with glass
- C03C17/04—Surface treatment of glass, not in the form of fibres or filaments, by coating with glass by fritting glass powder
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3429—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
- C03C17/3435—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a nitride, oxynitride, boronitride or carbonitride
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- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3605—Coatings of the type glass/metal/inorganic compound
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- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/361—Coatings of the type glass/metal/inorganic compound/metal/inorganic compound/other
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3613—Coatings of type glass/inorganic compound/metal/inorganic compound/metal/other
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
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Abstract
本发明提供了装饰具有涂层的玻璃基底的方法，所述方法包括：将糊剂以所需图案施加到所述涂层的至少一部分上；干燥所述糊剂以形成呈所述所需图案的干燥糊剂；以及焙烧所述干燥糊剂以形成呈所述所需图案的釉质，所述釉质通过溶解在焙烧步骤期间施加有糊剂的涂层的部分来直接粘结到所述玻璃基底上。该糊剂包含分散在分散介质中的固体部分，所述固体部分包含组合物，该组合物包含：10mol％至40mol％的ZnO；20mol％至40mol％的B2O3；25mol％至65mol％的Bi2O3、TeO2或PbO、或它们的混合物；和15mol％的Al2O3。
Description
技术领域
本发明涉及具有涂层的玻璃基底的釉质涂层，例如包括涂层诸如无机光学涂层的建筑或机动车玻璃。
背景技术
例如，建筑和汽车应用中使用的玻璃基底越来越多地涂覆有薄的多层叠堆。这些多层叠堆通常包括许多薄膜(每个通常<100nm)，这些薄膜是平面的、均匀的、在可见光谱内透明的，并且为玻璃基底提供所需的功能。该功能可以是例如近红外(NIR)反射或电导以加热透明基底。
这些多层涂层通常包括精确控制的材料序列，其被设计成提供总体期望的效果(参见H.Bach和D.Krause的玻璃上的薄膜(Thin Films on Glass)，Springer，1997)和H.Angus Macleod的薄膜和光学滤光器(Thin film and Optical filters)，CRC Press，2017)。这些材料可包括高折射率介电材料(例如TiO2、Nb2O5、ZrO2)、低折射率介电材料(例如Si3N4、SiO2、ZnO)和金属夹层(例如Ag、Au)。
在某些应用中，可能期望用釉质(例如施加在基底边缘上的不透明釉质)装饰或覆盖玻璃基底的一部分以保护下面的粘合剂免于UV降解。此类釉质通常来源于玻璃颜料组合物，一般来讲，使用印刷方法将其作为有机相中的分散体施加到玻璃基底。然后通常在热步骤中去除有机相。印刷组合物在合适的温度(通常介于400℃至700℃之间)下熔融，这导致釉质与玻璃基底具有永久且稳定的粘结。
常规的可商购获得的釉质不适用于装饰涂覆的玻璃基底，因为这些釉质不能够完全蚀刻多层涂层，从而导致不希望的缺陷，诸如变色、缺乏粘附性、分层和丧失涂层功能。如果首先将涂层以化学方式或机械方式从要施加釉质的区域去除使得釉质能够与裸露的玻璃基底直接熔合，则常规釉质仅可用于装饰涂覆的玻璃基底。该方法既昂贵又会导致质量缺陷。
WO2014/133929公开了一种替选方法，其中在焙烧步骤期间将印刷区下方的涂层溶解，使得釉质可与玻璃基底形成直接粘结。然而，WO2014/133929中未公开可用于此类方法中的组合物的类型。
因此，需要在各种涂覆的玻璃基底上提供良好的加工并且产生具有良好特性平衡的带装饰的涂覆玻璃制品的釉质形成组合物。具体地讲，需要釉质形成组合物，其中在所需焙烧范围内的釉质反应性足以完全溶解或与下面的涂层反应，并且该组合物形成良好的颜色、提供良好的化学耐久性和良好的玻璃强度。
发明内容
本说明书描述了用于装饰具有涂层的玻璃基底的组合物，所述组合物包含：
10mol％至40mol％的ZnO；
20mol％至40mol％的B2O3；
25mol％至65mol％的Bi2O3、TeO2或PbO、或它们的混合物；以及
0.1mol％至15mol％的Al2O3。
本说明书还描述了用于装饰具有涂层的玻璃基底的糊剂，所述糊剂包含分散在分散介质中的固体部分，所述固体部分包含如上文所述的组合物。
本说明书还描述了一种制备糊剂的方法，该方法包括以任何顺序混合：
(a)如上文所述的组合物；以及
(b)分散介质。
本说明书还描述了一种装饰具有涂层的玻璃基底的方法，所述方法包括：
(i)将如上文所述的糊剂以所需图案施加到所述涂层的至少一部分上；
(ii)干燥所述糊剂以形成呈所述所需图案的干燥糊剂；以及
(iii)焙烧所述干燥糊剂以形成呈所述所需图案的釉质，所述釉质直接粘结到所述玻璃基底。
本说明书提供了一种涂覆的玻璃基底，该涂覆的玻璃基底具有形成在其至少一部分上的釉质，该釉质可获得或通过如上文所述的方法获得。
具体实施方式
现在将阐述本发明的优选的和/或可选的特征。除非上下文另有需求，否则本发明的任何方面都可与本发明的任何其他方面组合。除非上下文另有需求，否则任何方面的任何优选的和/或可选的特征可单独地或组合地与本发明的任何方面组合。
在本文中指定范围的情况下，旨在范围的每个端点是独立的。因此，明确预期范围的每个列举的上端点可与每个列举的下端点独立地组合，反之亦然。
本文所述的组合物以摩尔百分比给出。这些摩尔百分比是基于氧化物，在制备组合物时用作原料的组分的摩尔百分比。如技术人员将理解的那样，除特定元素的氧化物之外的原料可用于制备本发明的组合物。在使用非氧化物原料向组合物提供特定元素的氧化物的情况下，使用适当量的原料提供等摩尔量的元素，使得该元素的氧化物以所列举的mol％提供。这种定义组合物特别是玻璃料组合物的方法在本领域中是典型的。如技术人员将易于理解的那样，挥发性物质(诸如氧气)在组合物的制造过程期间可能损失，因此最终组合物可能不完全对应于原料的摩尔百分比，该摩尔百分比在本文中基于氧化物给出。通过本领域技术人员已知的方法诸如感应耦合等离子体发射光谱法(ICP-ES)，对焙烧的组合物的分析可用于计算所讨论的组合物的起始组分。
如本文所用，术语“釉质”旨在表示由使已被施加到具有涂层的玻璃基底的至少一部分上的本发明糊剂经受焙烧步骤(例如，优选地在400℃至750℃的温度下)而产生的材料。
如本文所用，术语“糊剂”旨在涵盖糊剂(例如，如丝网印刷方法中所用的)和油墨(例如，如喷墨印刷方法中所用的)两者。
本说明书提供了适用于装饰具有涂层的玻璃基底例如建筑或机动车玻璃的组合物。该组合物适用于装饰任何种类的具有涂层的玻璃基底。待装饰的玻璃基底上的涂层可具有不同的厚度，但通常具有在50nm至300nm范围内的厚度。涂层通常包括一个或多个薄膜，薄膜已顺序地沉积(例如，通过物理气相沉积(PVD)等)在玻璃基底上。这些膜可包括高折射率介电材料(例如TiO2、Nb2O5、ZrO2)、低折射率介电材料(例如Si3N4、SiO2、ZnO)和金属夹层(例如Ag、Au)。带涂层的玻璃的代表性示例包括ClimaGuard(由Guardian制造)和Silverstar(由Glas 
制造)。使用如本文所述的组合物、糊剂和方法装饰的涂覆的玻璃基底可为平坦的(例如，玻璃片)或成型的(例如，弯曲的玻璃)。
本说明书的组合物包含：
10mol％至40mol％的ZnO；
20mol％至40mol％的B2O3；
25mol％至65mol％的Bi2O3、TeO2或PbO、或它们的混合物；以及
0.1mol％至15mol％的Al2O3。
已发现，本说明书的组合物在用于装饰具有涂层的玻璃基底时显示出良好的特性平衡，诸如上文所述的那些。这是因为组合物是低熔点的(例如，它们优选地在400℃至750℃的温度下，更优选地在620℃至720℃的温度下熔融)，这意味着它们可在施加到涂层(例如，以糊剂的形式)并焙烧之后溶解玻璃基底上的涂层。这导致所得釉质和玻璃基底之间的强且直接的粘结。此外，所得釉质具有良好外观(例如光滑并且不包含气泡)和良好颜色深度(例如它颜色深)。因此，所得釉质具有美学上令人愉悦的外观并具有良好的功能性能以用作遮光釉质并向例如可用于将玻璃基底附接到建筑物或机动车的下面的粘合剂提供紫外线防护。用于组合物的低焙烧温度也有益于防止对涂覆的玻璃基底的非印刷部分造成损坏或变形。
本说明书的组合物包含10mol％至40mol％的ZnO。优选地，该组合物包含15mol％至35mol％的ZnO，更优选地20mol％至30mol％的ZnO，并且甚至更优选地20mol％至25mol％的ZnO(例如23.3mol％的ZnO)。
本说明书的组合物包含20mol％至40mol％的B2O3。优选地，该组合物包含20mol％至35mol％的B2O3，更优选地20mol％至30mol％的B2O3，并且甚至更优选地24mol％至28mol％的B2O3(例如26mol％的B2O3)。
本说明书的组合物包含25mol％至65mol％的Bi2O3、TeO2、或PbO、或它们的混合物。优选地，该组合物包含35mol％至65mol％的Bi2O3、TeO2、或PbO、或它们的混合物，40mol％至60mol％的Bi2O3、TeO2、或PbO、或它们的混合物，更优选地40mol％至50mol％的Bi2O3、TeO2、或PbO、或它们的混合物，并且甚至更优选40mol％至45mol％的Bi2O3、TeO2、或PbO、或它们的混合物(例如43.7mol％的Bi2O3、TeO2、或PbO、或它们的混合物)。
优选地，本说明书的组合物包含25mol％至65mol％的Bi2O3，更优选地35mol％至65mol％的Bi2O3，甚至更优选地40mol％至60mol％的Bi2O3，甚至更优选地40mol％至50mol％的Bi2O3，并且甚至更优选地40mol％至45mol％的Bi2O3(例如43.7mol％的Bi2O3)。
优选地，本说明书的组合物包含25mol％至65mol％的TeO2，更优选地30mol％至55mol％的TeO2，甚至更优选地40mol％至50mol％的TeO2，并且甚至更优选地40mol％至45mol％的TeO2。
优选地，本说明书的组合物包含25mol％至65mol％的PbO，更优选地30mol％至55mol％的PbO，甚至更优选地40mol％至50mol％的PbO，并且甚至更优选地40mol％至45mol％的PbO。
任选地，本说明书的组合物包含Bi2O3、TeO2和/或PbO的混合物。
本说明书的组合物包含0.1mol％至15mol％的Al2O3。优选地，该组合物包含0.5mol％至14mol％，更优选地1.0mol％至13.5mol％，更优选地1.5mol％至12mol％，更优选地2.0mol％至10mol％，更优选地3.0mol％至9.5mol％，更优选地4.5mol％至8.5mol％的Al2O3，更优选地6.0mol％至8.0mol％的Al2O3，更优选地6.5mol％至7.5mol％的Al2O3，并且甚至更优选地6.8mol％至7.2mol％的Al2O3(例如7.0mol％的Al2O3)。
不能制备包含大于15mol％的Al2O3的组合物。这是因为超过该量的Al2O3，Al2O3变得与Bi2O3/TeO2/PbO-B2O3-ZnO基质不混溶，导致相分离(至少对于所研究的组合物而言)。
Al2O3在组合物中以上述量存在防止焙烧步骤期间的结晶，否则这会对釉质外观、颜色深度、光密度和玻璃强度产生负面影响。就具有复合涂层诸如多层涂层(例如，10个或更多个单独的溅射层)的涂覆的玻璃基底而言，已发现Al2O3的存在对于实现平滑的釉质表面是特别重要的。就玻璃强度而言，Al2O3的存在能够通过在釉质和玻璃基底之间提供较小的热膨胀失配来降低两者之间的张力(参见实施例)。
任选地，本说明书的组合物包含摩尔比在1.5:1至2.5:1范围内的Bi2O3/B2O3。该组合物可任选地包含摩尔比在1.4:1至3.7:1范围内的Bi2O3/ZnO。
优选地，本说明书的组合物还包含一种或多种碱金属氧化物，例如一种或多种选自Li2O、Na2O、K2O和Rb2O中的化合物，优选地一种或多种选自Li2O、Na2O和K2O中的化合物。该组合物还可包含0mol％至10mol％，优选地0mol％至5mol％，更优选地0mol％至2mol％的一种或多种碱金属氧化物。
优选地，本说明书的组合物还包含CeO2。该组合物还可包含0mol％至2.0mol％，优选地0mol％至1.0mol％，更优选地0mol至0.5mol％的CeO2。
本说明书的组合物还可包含一种或多种选自碱土金属氧化物和SnO2的化合物，例如一种或多种选自MgO、CaO、SrO和SnO2的化合物。该组合物还可包含0mol％至10mol％，优选地0mol％至5mol％，更优选地0mol％至2mol％的一种或多种选自碱土金属氧化物和SnO2的化合物。
本说明书的组合物还可包含SiO2。然而，已发现，本文所公开类型的组合物中大量SiO2的存在(即，>10mol％)导致焙烧步骤期间的复杂化，并且可导致粗糙的釉质表面。已发现对于具有复合涂层(例如，具有高Si3N4含量和/或多层涂层诸如10个或更多个单独层)的涂覆的玻璃基底而言尤其如此。不受理论的束缚，据认为SiO2在玻璃基底上的涂层溶解期间促进不可取的结晶，从而防止组合物在焙烧温度下的充分流动。因此，在一些示例中，本说明书的组合物还可包含0mol％至10mol％，优选地0mol％至7mol％，更优选地0mol％至5mol％，更优选地0mol％至2mol％的SiO2，并且任选地基本上不含SiO2。本说明书的组合物可基本上不含某些组分。如本文所用，与组合物相关的术语“基本上不含”是指该组合物具有小于或等于1mol％的所列举组分的总含量。如技术人员将易于理解的那样，在例如玻璃料颗粒的制造期间，玻璃组合物可能被低含量的杂质污染。例如，在熔融/淬火玻璃形成过程中，此类杂质可源自用于熔融步骤中的容器的耐火衬里。因此，尽管可期望完全不存在特定组分，但实际上这可能难以实现。如本文所用，术语“不含有意添加的X”(其中X是特定组分)意指在组合物的制造中不使用旨在将X输送至最终釉质组合物的原材料，并且该组合物中任何低含量的X的存在是由于制造过程中的污染所引起。
由于毒性问题，在本说明书的组合物中使用含铅化合物可能是不可取的。因此，在优选组合物中，该组合物基本上不含铅。如本文所用，术语“基本上不含铅”旨在包括不含有意添加的铅的组合物。例如，组合物可包含小于0.5mol％的PbO、小于0.1mol％的PbO、小于0.05mol％的PbO、小于0.01mol％的PbO或小于0.005mol％的PbO。
在本说明书的优选组合物中，该组合物基本上不含氟。如本文所用，术语“基本上不含氟”旨在包括不含有意添加的氟的组合物。例如，组合物可包含小于0.5mol％的氟、小于0.1mol％的氟、小于0.05mol％的氟、小于0.01mol％的氟或小于0.005mol％的氟。
在本说明书的优选组合物中，该组合物基本上不含钛。如本文所用，术语“基本上不含钛”旨在包括不含有意添加的钛的组合物。例如，组合物可包含小于1.0mol％的TiO2、小于0.5mol％的TiO2、小于0.1mol％的TiO2、小于0.05mol％的TiO2或小于0.01mol％的TiO2。
在本说明书的优选组合物中，该组合物基本上不含锰。如本文所用，术语“基本上不含锰”旨在包括不含有意添加的锰的组合物。例如，组合物可包含小于1.0mol％的MnO2，小于0.5mol％的MnO2，小于0.1mol％的MnO2，小于0.05mol％的MnO2或小于0.01mol％的MnO2。
在本说明书的优选组合物中，该组合物基本上不含钨。如本文所用，术语“基本上不含钨”旨在包括不含有意添加的钨的组合物。例如，组合物可包含小于1.0mol％的WO3、小于0.5mol％的WO3、小于0.1mol％的WO3、小于0.05mol％的WO3或小于0.01mol％的WO3。
本说明书的组合物优选地基本上由如本文所述的组合物和附带的杂质(诸如在组合物的制造期间拾取的杂质)组成。在这种情况下，如技术人员将易于理解的那样，所列举成分的总mol％将为100mol％，任何余量为附带的杂质。优选地，任何附带的杂质将以1mol％或更少，更优选地0.5mol％或更少，甚至更优选地0.2mol％或更少存在。
例如，本说明书的优选组合物基本上由以下组成：
(i)10mol％至40mol％的ZnO；
(ii)20mol％至40mol％的B2O3；
(iii)25mol％至65mol％的Bi2O3、TeO2或PbO、或它们的混合物；
(iv)0.1mol％至15mol％的Al2O3；
(v)0mol％至10mol％的一种或多种选自Li2O、Na2O和K2O的化合物；
(vi)0mol％至10mol％的一种或多种选自MgO、CaO、SrO和SnO2的化合物；
(vii)0mol％至2mol％的CeO2；
(viii)0mol％至10mol％的SiO2；以及
(ix)附带的杂质。
本说明书的特别优选的组合物基本上由以下组成：
(i)20mol％至25mol％的ZnO(例如23.3mol％的ZnO)；
(ii)24mol％至28mol％的B2O3(例如26.0mol％的B2O3)；
(iii)40mol％至45mol％的Bi2O3(例如43.7mol％的Bi2O3)；
(iv)6.0mol％至8.0mol％的Al2O3(例如，7.0mol％的Al2O3)；以及
(v)附带的杂质。
本文所述组合物的最佳D90粒度取决于用于将组合物施加于涂覆的玻璃基底的方法。
对于某些应用(例如丝网印刷)，本说明书的组合物优选地具有小于30微米的D90粒度。在一些示例中，该组合物的颗粒可具有5微米至20微米，优选地7微米至14微米，更优选地12微米至13微米的D90粒度。
对于某些应用(例如喷墨印刷)，本说明书的组合物优选地具有小于或等于1.5微米或者小于或等于1.0微米(任选地，不小于0.1微米)的D90粒度。在一些示例中，该组合物的颗粒可具有0.6微米至1.5微米，0.7微米至1.2微米，或0.8微米至1.0微米的D90粒度。
本文中的术语“D90粒度”是指粒度分布，并且D90粒度的值对应于特定样品中占总颗粒的90体积％以下的粒度值。D90粒度可使用激光衍射方法(例如使用MalvernMastersizer 2000)来确定。
本文所述的组合物的最佳D50粒度取决于用于将组合物施加于涂覆的玻璃基底的方法。
对于某些应用(例如丝网印刷)，本说明书的组合物优选地具有小于20微米的D50粒度。在一些示例中，组合物的颗粒可具有3微米至15微米，优选地5微米至10微米，更优选地6微米至7微米的D50粒度。
对于某些应用(例如喷墨印刷)，本说明书的组合物优选地具有小于或等于1.0微米的D50粒度。在一些示例中，组合物的颗粒可具有0.1微米至1.0微米，0.3微米至0.9微米，0.4微米至0.7微米，或0.45微米至0.6微米的D50粒度。
本文中的术语“D50粒度”是指粒度分布，并且D50粒度的值对应于特定样品中占总颗粒的50体积％以下的粒度值。D50粒度可使用激光衍射方法(例如使用MalvernMastersizer 2000)来确定。
对于某些应用(例如丝网印刷)，本说明书的组合物优选地具有小于50微米、30微米、25微米或20微米的最大粒度。在一些示例中，组合物的颗粒可具有10微米至50微米的最大粒度。
对于某些应用(例如喷墨印刷)，本说明书的组合物优选地具有小于2.0微米、1.5微米或1.0微米的最大粒度。在一些示例中，组合物的颗粒可具有0.5微米至2微米的最大粒度。
对于喷墨印刷应用，可将油墨制备成在100s-1的剪切速率下具有低粘度，例如15mPas至25mPas(毫帕斯卡秒)。在此类组合物中，固体粉末含量较低，例如介于30％和55％之间。
丝网印刷糊剂具有较高的粘度，例如在10s-1下12Pas至15Pas，并且在100s-1下8Pas至10Pas。固体粉末含量较高，例如75％至85％。并且对于本文所述的组合物，糊剂中甚至90％或更多的固体含量也是可能的。
优选地，本说明书的组合物的热膨胀系数(CTE)接近具有涂层的玻璃基底的CTE。因此，本说明书的组合物优选地具有小于或等于120×10-7/K，更优选地小于或等于115×10-7/K，甚至更优选地小于或等于110×10-7/K，甚至更优选地小于或等于108×10-7/K的CTE，如使用膨胀计所测量的。合适的膨胀仪是购自TA Instruments的DIL803双样品膨胀仪。在焙烧期间，涂层能够至少部分地溶解于釉质中，进一步将釉质的CTE降低至90×10-7/K，例如通过吸收ZnO和/或SiO2，这将釉质的CTE转移至较低的值。因此，可降低釉质和玻璃基底之间的应力。
在本说明书的优选组合物中，该组合物为粉末。优选地，该组合物为具有所列举组成的可熔材料，或共同提供所列举组成的一种或多种可熔材料的混合物。组合物可以是完全无定形的、部分结晶的或完全结晶的材料。优选地，组合物为结晶化合物。优选地，组合物为玻璃料。另选地，组合物为烧结材料。
在优选的组合物中，组合物为玻璃料。玻璃料组合物可通过将所需原材料混合在一起并将其熔融以形成熔融玻璃熔体，然后淬火以形成玻璃料来制备。该方法还可包括研磨所得的玻璃，以提供具有期望粒度的玻璃料颗粒。例如，可使用喷射研磨法、球磨法或珠磨法，诸如在基于醇、基于二醇或基于水的溶剂中进行湿珠磨，来研磨玻璃。技术人员知道用于制备玻璃料的替代的合适方法。合适的替代方法包括水淬火、溶胶-凝胶法和喷雾热解。
玻璃料组合物优选地具有在360℃至400℃范围内的膨胀软化点温度(Ts)。例如，玻璃料组合物可具有在360℃至380℃范围内的Ts。
如本文所用，术语“软化点”或“Ts”意指第一温度，在该第一温度下观察到玻璃软化或变形的迹象，如使用膨胀计所测量的。
玻璃料组合物优选地具有在330℃至400℃或350℃至400℃范围内的玻璃化转变温度(Tg)。例如，玻璃料组合物可具有在350℃至390℃范围内的Tg。
如本文所用，术语“玻璃化转变温度”或“Tg”意指如根据ASTM El356“通过差示扫描量热法指定玻璃化转变温度的标准测试方法”测得的玻璃化转变温度。
如本文所述的组合物可形成为釉质糊剂。
本说明书的糊剂适用于装饰具有涂层的玻璃基底。糊剂包含分散在分散介质中的固体部分，所述固体部分包含如上文所述的组合物。优选地，固体部分还包含颜料。
在本说明书的优选糊剂中，基于固体部分的总重量计，固体部分包含70重量％至90重量％，更优选地75重量％至85重量％(例如83重量％)的如上文所述的组合物，以及10重量％至30重量％的颜料，更优选地15重量％至25重量％的颜料(例如17重量％)。此类糊剂尤其适用于使用丝网印刷方法施加到涂覆的玻璃基底上，但对于喷墨印刷也可使用。
在优选的糊剂中，该糊剂包含75重量％至95重量％，更优选地80重量％至90重量％(例如85重量％)的固体部分和5重量％至25重量％，更优选地10重量％至20重量％(例如15重量％)的分散介质。此类糊剂尤其适用于使用丝网印刷方法施加到涂覆的玻璃基底。
在优选的糊剂中，该糊剂包含35重量％至55重量％，更优选地40重量％至50重量％(例如45重量％)的固体部分和45重量％至65重量％，更优选地50重量％至60重量％(例如55重量％)的分散介质。此类糊剂特别适用于使用喷墨印刷方法施加到涂覆的玻璃基底。
可将本说明书的糊剂施加到具有涂层的玻璃基底(例如，通过印刷)，以便将组合物沉积到玻璃基底的涂层的最上表面上。如本文所用，术语“最上表面”是指不与玻璃基底直接接触的涂层的表面。
如本文所用，术语“分散介质”是指在旨在将糊剂施加到玻璃基底的条件(即，印刷条件)下处于液相的物质。因此，在环境条件下，分散介质可以是固体或对于印刷而言过于粘稠的液体。如技术人员将易于理解的那样，如果需要，将本发明的组合物和颜料与分散介质组合以形成糊剂可以在升高的温度下进行。
待用于本说明书的糊剂中的分散介质可基于将糊剂施加到基底的预期方法来选择。通常，分散介质包括有机液体。
在示例中，分散介质在施加条件下充分地悬浮颗粒混合物，并且在干燥所施加的糊剂和/或焙烧所沉积的颗粒混合物期间被完全去除。影响介质选择的因素包括溶剂粘度、蒸发速率、表面张力、气味和毒性。合适介质优选地在印刷条件下表现出非牛顿行为。适当地，该介质包括水、醇、乙二醇醚、乳酸酯、乙二醇醚乙酸酯、醛、酮、芳族烃和油中的一种或多种。两种或更多种分散介质的混合物也是合适的。
糊剂还优选地包含一种或多种补充材料。这些可包括分散剂、粘结剂、树脂、粘度/流变改性剂、润湿剂、增稠剂、触变胶、稳定剂和表面活性剂。
在优选的糊剂中，固体部分还包含颜料。两种或更多种颜料的混合物也是合适的。优选的颜料包括黑色尖晶石型颜料。
糊剂优选地基本上不含铅，即任何含铅组分基本上不存在于糊剂中。例如，糊剂可包含少于0.1重量％的铅。
糊剂优选地基本上不含氟，即任何含氟组分基本上不存在于糊剂中。例如，糊剂可包含小于0.1重量％的氟。
在一些应用中，例如机动车玻璃应用中，糊剂赋予所得釉质不粘特性是有利的。这是因为在这些应用中，通常需要在焙烧过程完成之后弯曲玻璃基底(例如以形成汽车挡风玻璃等)。如果釉质不具有不粘特性，则在弯曲过程中常常遇到加工问题。此类不粘特性可通过将添加剂材料掺入糊剂中来实现。因此，在优选的糊剂中，固体部分还包含添加剂材料。优选地，基于固体部分的总重量计，固体部分包含3重量％至10重量％、4重量％至10重量％、5重量％至10重量％或5重量％至8重量％(例如8重量％)的添加剂材料。优选地，添加剂材料为玻璃料组合物(例如硅酸铋玻璃料)。另选地，添加剂材料为结晶化合物或填充材料(例如，氧化铝、氧化镁、氧化锆、锆石、堇青石或熔融二氧化硅)。优选地，添加剂材料还包括晶种材料(seed material)(例如，晶种材料(crystal seed material))。更优选地，基于固体部分的总重量计，添加剂材料还包含0.2重量％至4重量％或1重量％至3重量％(例如，2重量％)的晶种材料。
本说明书的糊剂可通过以任何顺序混合以下物质来制备：
(a)如上文所述的组合物；以及
(b)分散介质。
在一些示例中，糊剂可通过以任何顺序混合以下物质来制备：
(a)如上文所述的组合物；
(b)颜料；以及
(c)分散介质。
在一些示例中，糊剂可通过以任何顺序混合以下物质来制备：
(a)如上文所述的组合物；
(b)颜料；
(c)分散介质；以及
(d)添加剂材料。
可例如使用溶解器、高剪切混合器或珠磨机来混合这些组分。在一些示例中，可在混合之前和/或期间加热分散介质和/或混合的组分。
在一些情况下，可期望将组合物在与分散介质混合后研磨成所需的粒度。合适的研磨技术包括珠磨、球磨、篮式研磨或其他适当的湿磨技术。
如本文所述的糊剂尤其可用于装饰具有涂层的玻璃基底的方法中，该方法包括：
(i)将如上文所述的糊剂以所需图案施加到所述涂层的至少一部分上；
(ii)干燥所述糊剂以形成呈所述所需图案的干燥糊剂；以及
(iii)焙烧所述干燥糊剂以形成呈所述所需图案的釉质，所述釉质直接粘结到所述玻璃基底上。
在步骤(i)中将糊剂沉积到涂层的至少一部分上可通过将一层上述糊剂施加到基底的涂层的该部分上来实现。该层糊剂可经由合适的印刷方法施加到涂覆玻璃基底。例如，该层糊剂可经由喷墨印刷、丝网印刷、辊涂或通过分配器施加而被施加到涂覆的玻璃基底。在优选的方法中，糊剂经由丝网印刷被施加到涂覆的玻璃基底。在替选方法中，糊剂经由喷墨印刷被施加到涂覆的玻璃基底。
所施加的该层糊剂优选地具有在20微米至45微米范围内，更优选地在25微米至40微米范围内，甚至更优选地在30微米至35微米范围内的湿层厚度。所施加的该层糊剂的湿层厚度可根据所用的印刷方法和最终装饰制品的预期最终用途而变化。例如，喷墨层可制得更薄，例如厚度为10μm至30μm、12μm至25μm或15μm至20μm。
在将糊剂层施加到涂覆的玻璃基底之后并且在焙烧之前，所施加的涂层经历干燥步骤(ii)以去除或部分去除存在于分散介质中的溶剂。干燥可在至多200℃的温度，更优选地至多150℃的温度下进行。干燥可例如通过在环境温度下空气干燥所施加的层、通过在合适的烘箱中加热经糊剂涂覆的玻璃基底或者通过将经糊剂涂覆的玻璃基底暴露于红外辐射下来进行。
在步骤(iii)中，焙烧干燥的糊剂以形成釉质，其中釉质直接粘结到玻璃基底。步骤(iii)导致最初施加糊剂的涂层部分溶解，优选地基本上完全溶解。这样，釉质在施加糊剂的部分的基本上整个表面区域上直接接触并粘附到下面的玻璃基底。例如，釉质可在施加糊剂的部分的表面积的至少50％、60％、70％、80％、90％、95％、99％、或100％上直接粘结到下面的玻璃基底。所谓“直接粘结”，意指没有可辨别的涂层设置在釉质和下面的玻璃基底之间，该涂层在焙烧步骤期间已溶解掉。
在步骤(iii)中，可通过将其上施加有干燥糊剂的玻璃基底加热至足够高的温度来焙烧干燥糊剂，从而使组合物的颗粒软化并流动，并且使得来源于分散介质的任何剩余组分被烧尽，并且还溶解下面的涂层而不会引起玻璃基底的不期望的变形。优选地通过将组件加热至400℃至750℃范围内，更优选地620℃至720℃范围内的温度来进行焙烧步骤。加热组件可经由对流加热，例如使用合适的窑或炉诸如两室辊道窑或连续式线炉来进行。
优选的方法还包括以下步骤：
(iv)使该玻璃基底弯曲。
本说明书还提供了涂覆的玻璃基底，该涂覆的玻璃基底具有形成在其至少一部分上的釉质，该釉质可获得或通过如上文所述的方法获得。
本说明书还提供了如上文所述的组合物形成糊剂的用途。
本说明书还提供了如上文所述的糊剂在具有涂层的玻璃基底的至少一部分上形成釉质的用途。
实施例
现在将参考以下实施例进一步描述本发明，这些实施例是例示性的，但不是对本发明的限制。
材料
使用可商购获得的原材料来制备玻璃料和烧结组合物。
实施例1：基于Bi-B-Zn的氧化物组合物和糊剂的制备
表1给出了玻璃料组合物的示例。在电窑中的陶瓷坩埚中混合并熔融用于玻璃料的原材料。以30℃/min的斜坡加热窑，并在850℃至950℃的峰值温度下保持15至20分钟。此后，发现玻璃熔体是均匀的，然后在水中淬火。然后将玻璃料在干燥箱中在120℃下干燥。干燥后，使用喷磨机(Alpine-Hosokawa pico喷磨机40AFG)将玻璃料研磨至粒度D(50)＝6μm至7μm，并且D(90)＝12μm至13μm。
表1：以mol％计的玻璃料组成及其以10-7K-1计的热膨胀系数(CTE)
不能制备包含大于15mol％的Al2O3的组合物。这是因为超过该量的Al2O3，Al2O3变得与Bi2O3-B2O3-ZnO基质不混溶，导致相分离。
另外，制备具有与玻璃料4相同的元素组成但通过烧结工艺制备的烧结组合物(在下表2中标记为“玻璃料4的SP”)。在该方法中，将原材料(此处为Bi2O3、H3BO3和ZnO)充分混合，然后在450℃的电窑中热处理3小时，随后在540℃下热处理9小时。烧结产物如上文对玻璃料所述的进行喷射研磨。
为了形成糊剂，将喷射研磨的玻璃料与背面颜料共混以形成固体部分(由83重量％的玻璃料和17重量％的黑色颜料组成)，然后通过三辊研磨将其分散在分散介质中。
实施例2：涂覆的玻璃基底的装饰
使用77T丝网将所得糊剂丝网印刷到6mm厚的湿层厚度为25μm至30μm的涂覆的玻璃板(300×150×6mm)上。在这些测试中采用的涂覆的玻璃板A、B、C和D各自为可商购获得的涂覆的玻璃(A＝ClimaGuard；B＝SilverStar；C＝SilverStar(2个银层)；D＝SunguardSN)。这些涂层中的每一个层的层结构(从玻璃基底开始的层顺序)如下：
A：氮化硅、氧化锌、银、镍/铬、氧化锡氧化锌、氮化硅。
B：氮化硅、氧化锡、氧化锌、银、镍/铬、氧化锌、氮化硅。
C：顺序类似于B，但具有由三层氧化锌、氧化锡、氧化锌隔开的两个银层。
D：2x A的序列。
首先将印刷品在150℃干燥15分钟。然后在双室辊窑(NBP燃烧系统，型号Fer 2C15 4Z-SDO)中进行焙烧，其中第一室中的设定温度为670℃，并且第二室中的设定温度为700℃。玻璃板在每个室中的停留时间分别为160s和150s。
实施例3：涂覆的玻璃基底的测试结果
对所得的釉质进行评价以确定以下特性：
(i)釉质是否完全溶解涂层
在涂覆的玻璃上焙烧釉质的特性是焙烧过程中印刷(热吸收)和非印刷(热反射)区域之间的强温差。因此，印刷品的边缘具有较低的温度，并且常规的釉质不能侵蚀印刷品边缘处的涂层或仅可以部分侵蚀印刷品边缘处的涂层，因此没有观察到涂层的完全溶解。
(ii)釉质是否形成光滑表面
常规的釉质通常导致表面缺陷，诸如粗糙表面或有气泡，或具有金属光泽的有色反射。气泡的形成表明涂层与釉质之间的反应在焙烧过程中未完成。粗糙表面表明在反应发生后，釉质变得过于粘稠而无法流动并形成光滑表面。
(iii)釉质从玻璃侧的颜色(L值)
用X-Rite色度计测量L值，排除反射。根据CIE L*a*b*系统从玻璃侧测量颜色(反向颜色)。对于本发明的应用而言优选的深黑色釉质表现出低L值。相反，对金属反射/干涉的观察表明涂层仍然完整并且没有被适当地破坏。
(iv)555nm下的光密度(OD)(可见光范围)
使用Gretag Macbeth D200-II透射密度计测量OD。优选地，当将玻璃片材组装在建筑物或汽车中时，需要99.9％的光吸收(OD＝3)来保护所用的底层粘合剂。然而，如果表面是粗糙且多孔的，则无法确定OD。
(v)釉质是否通过耐刮擦性测试(即Elcometer 3092Sclerometer笔划痕笔以16N的载荷进行)
使用Elcometer 3092Sclerometer笔划痕笔以16N的载荷进行的耐刮擦性测试是釉质粘附到玻璃基底上的强度的指示符。如果涂层未被破坏，则粘附性低。如果釉质和玻璃基底之间的张力过高或釉质表面粗糙，则刮擦性测试也失败。因此，如果表面是粗糙且多孔的，则无法确定耐刮擦性。
所测试的玻璃料组合物/烧结材料组合物的焙烧结果汇总于表2中。还测试了两种已知的釉质，釉质AF3601和釉质276000。釉质AF3601包含硅酸锌玻璃并用于装饰建筑玻璃。釉质27600是基于低熔点氧化铋的釉质。两种釉质均可从Johnson Matthey商购获得。
表2：焙烧结果
结果表明，可商购获得的釉质AF3601和27600在焙烧期间不能够破坏玻璃基底上的涂层。另一方面，来源于本说明书的组合物和糊剂的釉质具有良好的特性平衡，包括光滑表面和玻璃侧的黑色、低L值和高OD，使得它们理想地适用于建筑和机动车玻璃领域中的应用。此外，清楚地看出，在本发明的组合物中存在0.1mol％至15mol％的Al2O3是实现特性的良好平衡的关键：发现不含Al2O3的实施例展示出较高的CTE值、较高的L值和较低的OD值。发现使用烧结材料代替玻璃料产生可比较的结果(参见玻璃料4的结果相对于“玻璃料4的SP”的结果)。
一些釉质进一步经受环对环压缩测试，其涉及向玻璃片材施加增加的力直至断裂点。
首先用糊剂印刷100×110×4mm玻璃基底，该糊剂具有包含83重量％的玻璃料4或83重量％的玻璃料13、以及17重量％的黑色颜料的固体部分，该固体部分分散于分散介质中。然后将每种糊剂印刷成25μm的湿层厚度并干燥。然后将干燥的糊剂在辊窑中在680℃焙烧。
根据DIN 52 292的环对环压缩测试用Zwick/Roell Z010测试仪进行。Fmax为断裂前施加的最大压缩力。弯曲应力σ是与玻璃样品的厚度无关的物理参数，并且通过公式σ＝1.04Fmax/s2计算，其中s是玻璃板的厚度。结果在下表3中示出。
表3：环对环压缩测试的结果
当糊剂经受焙烧条件时，玻璃基底经历弱化。因此，希望尽可能地减少这种弱化。上述结果显示，当糊剂从包含玻璃料4的糊剂变为包含玻璃料13的糊剂时，使玻璃板断裂所需的力从727N上升至1174N。这两种玻璃料之间的区别在于玻璃料13包含7.0mol％的Al2O3，而玻璃料4不包含。如上所述，在本说明书的组合物和糊剂中存在少量Al2O3，因此导致具有改善的玻璃强度的装饰的涂覆玻璃制品。不受理论的束缚，Al2O3被认为可减小釉质和玻璃基底之间的张力。
如这些实施例所示，本说明书提供了可用于在涂覆的玻璃基底上形成釉质的组合物和糊剂。在焙烧期间，该组合物可溶解已施加有其的涂层的部分以形成与玻璃基底的直接粘结。所得釉质具有良好的特性平衡，包括良好的颜色、良好的化学耐久性和良好的玻璃强度。
Claims (19)
1.一种装饰具有涂层的玻璃基底的方法，所述方法包括：
(i)将糊剂以所需图案施加到所述涂层的至少一部分上；
(ii)干燥所述糊剂以形成呈所述所需图案的干燥糊剂；以及
(iii)焙烧所述干燥糊剂以形成呈所述所需图案的釉质，所述釉质直接粘结到所述玻璃基底上，
其中所述糊剂包含分散在分散介质中的固体部分，所述固体部分包含组合物，所述组合物包含：
10mol％至40mol％的ZnO；
20mol％至40mol％的B2O3；
25mol％至65mol％的Bi2O3、TeO2或PbO、或它们的混合物；以及
0.1mol％至15mol％的Al2O3，
并且其中步骤(iii)导致所述涂层的所述部分溶解。
2.根据权利要求1所述的方法，其中所述组合物包含0.5mol％至14mol％、更优选地1.0mol％至13.5mol％的Al2O3。
3.根据权利要求1或权利要求2所述的方法，其中所述组合物包含15mol％至35mol％的ZnO。
4.根据权利要求1至3中任一项所述的方法，其中所述组合物包含20mol％至30mol％的B2O3。
5.根据权利要求1至4中任一项所述的方法，其中所述组合物包含35mol％至65mol％的Bi2O3。
6.根据权利要求1至5中任一项所述的方法，其中所述组合物还包含0mol％至10mol％的SiO2。
7.根据权利要求1至6中任一项所述的方法，其中所述组合物基本上不含氟和/或基本上不含铅。
8.根据权利要求1至7中任一项所述的方法，其中所述组合物还包含0mol％至10mol％的一种或多种碱金属氧化物。
9.根据权利要求1至8中任一项所述的方法，其中所述组合物还包含0mol％至2mol％的CeO2。
10.根据权利要求1至9中任一项所述的方法，其中所述组合物还包含0mol％至10mol％的一种或多种选自碱土金属氧化物和SnO2的化合物。
11.根据权利要求1至10中任一项所述的方法，其中所述组合物为玻璃料。
12.根据权利要求1至10中任一项所述的方法，其中所述组合物为烧结材料。
13.根据权利要求1至12中任一项所述的方法，其中所述组合物的D90粒度为5微米至20微米，优选地7微米至14微米，更优选地12微米至13微米。
14.根据权利要求1至12中任一项所述的方法，其中所述组合物的D90粒度小于或等于1.0微米。
15.根据任一前述权利要求所述的方法，其中所述固体部分还包含颜料。
16.根据权利要求15所述的方法，其中基于所述固体部分的总重量计，所述固体部分包含70重量％至90重量％的所述组合物和10重量％至30重量％的颜料。
17.根据任一前述权利要求所述的方法，其中所述固体部分还包含添加剂材料。
18.根据任一前述权利要求所述的方法，所述方法还包括以下步骤：(iv)使所述玻璃基底弯曲。
19.一种涂覆的玻璃基底，所述涂覆的玻璃基底具有形成在其至少一部分上的釉质，能够通过或通过根据任一前述权利要求所述的方法获得。
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|---|---|---|---|
| GB1911367.9 | 2019-08-08 | ||
| GBGB1911367.9A GB201911367D0 (en) | 2019-08-08 | 2019-08-08 | Composition, paste and methods |
| PCT/GB2020/051697 WO2021023965A1 (en) | 2019-08-08 | 2020-07-15 | Enamel coating of a coated glass substrate |
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| CN114040899A true CN114040899A (zh) | 2022-02-11 |
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| EP (1) | EP4010290A1 (zh) |
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| CN (1) | CN114040899A (zh) |
| GB (2) | GB201911367D0 (zh) |
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| DE102021134016A1 (de) | 2021-12-21 | 2023-06-22 | Webasto SE | Verfahren zum Herstellen einer Verbundglasscheibe |
| FR3140624A1 (fr) * | 2022-10-11 | 2024-04-12 | Saint-Gobain Glass France | Feuille de verre comprenant une zone émaillée |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5306674A (en) * | 1992-09-04 | 1994-04-26 | Ferro Corporation | Lead-free glass coatings |
| JP2004284934A (ja) * | 2002-04-24 | 2004-10-14 | Central Glass Co Ltd | 無鉛低融点ガラス |
| US20080090034A1 (en) * | 2006-09-18 | 2008-04-17 | Harrison Daniel J | Colored glass frit |
| WO2014133929A2 (en) * | 2013-02-28 | 2014-09-04 | Guardian Industries Corp. | Window units made using ceramic frit that dissolves physical vapor deposition (pvd) deposited coatings, and/or associated methods |
| US20170016270A1 (en) * | 2015-07-13 | 2017-01-19 | Asahi Glass Company, Limited | Method of producing vacuum sealed component |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5252521A (en) * | 1992-10-19 | 1993-10-12 | Ferro Corporation | Bismuth-containing lead-free glass enamels and glazes of low silica content |
| TW379332B (en) * | 1994-06-27 | 2000-01-11 | Du Pont | Load-free glass composition and thick film paste composition comprising the same |
| DE60318517T2 (de) * | 2002-04-24 | 2009-07-23 | Central Glass Co., Ltd., Ube | Bleifreies niedrigschmelzendes Glas |
| JP5717043B2 (ja) * | 2008-09-04 | 2015-05-13 | 日本電気硝子株式会社 | 電極形成用ガラス組成物および電極形成材料 |
| TWI432392B (zh) * | 2009-02-06 | 2014-04-01 | Basf Se | 玻璃料 |
| US8772189B2 (en) * | 2011-05-04 | 2014-07-08 | Ferro Corporation | Glass frit compositions for enamels |
| JP6952950B2 (ja) * | 2016-04-21 | 2021-10-27 | 日本電気硝子株式会社 | 複合粉末材料 |
| CN107523117A (zh) * | 2017-08-14 | 2017-12-29 | 广东工业大学 | 一种汽车钢化玻璃油墨及其制备方法 |
-
2019
- 2019-08-08 GB GBGB1911367.9A patent/GB201911367D0/en not_active Ceased
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2020
- 2020-07-15 JP JP2021576217A patent/JP7486533B2/ja active Active
- 2020-07-15 US US17/615,448 patent/US20220227661A1/en active Pending
- 2020-07-15 WO PCT/GB2020/051697 patent/WO2021023965A1/en unknown
- 2020-07-15 CN CN202080042056.7A patent/CN114040899A/zh active Pending
- 2020-07-15 KR KR1020227001142A patent/KR20220032053A/ko not_active Application Discontinuation
- 2020-07-15 EP EP20747079.0A patent/EP4010290A1/en active Pending
- 2020-07-15 GB GB2010876.7A patent/GB2587484B/en active Active
- 2020-08-07 TW TW109126785A patent/TWI747424B/zh active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5306674A (en) * | 1992-09-04 | 1994-04-26 | Ferro Corporation | Lead-free glass coatings |
| JP2004284934A (ja) * | 2002-04-24 | 2004-10-14 | Central Glass Co Ltd | 無鉛低融点ガラス |
| US20080090034A1 (en) * | 2006-09-18 | 2008-04-17 | Harrison Daniel J | Colored glass frit |
| WO2014133929A2 (en) * | 2013-02-28 | 2014-09-04 | Guardian Industries Corp. | Window units made using ceramic frit that dissolves physical vapor deposition (pvd) deposited coatings, and/or associated methods |
| US20170016270A1 (en) * | 2015-07-13 | 2017-01-19 | Asahi Glass Company, Limited | Method of producing vacuum sealed component |
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| JP7486533B2 (ja) | 2024-05-17 |
| US20220227661A1 (en) | 2022-07-21 |
| TW202112701A (zh) | 2021-04-01 |
| GB201911367D0 (en) | 2019-09-25 |
| GB2587484A (en) | 2021-03-31 |
| EP4010290A1 (en) | 2022-06-15 |
| WO2021023965A1 (en) | 2021-02-11 |
| GB202010876D0 (en) | 2020-08-26 |
| JP2022538411A (ja) | 2022-09-02 |
| GB2587484B (en) | 2023-08-09 |
| TWI747424B (zh) | 2021-11-21 |
| KR20220032053A (ko) | 2022-03-15 |
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