CN106133845B - 具有改善的玻璃强度性能的导电浆料 - Google Patents
具有改善的玻璃强度性能的导电浆料 Download PDFInfo
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- CN106133845B CN106133845B CN201580017987.0A CN201580017987A CN106133845B CN 106133845 B CN106133845 B CN 106133845B CN 201580017987 A CN201580017987 A CN 201580017987A CN 106133845 B CN106133845 B CN 106133845B
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- silver
- slurry
- glass
- electrocondution slurry
- pigment
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- 239000002002 slurry Substances 0.000 title claims description 56
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910052709 silver Inorganic materials 0.000 claims abstract description 45
- 239000004332 silver Substances 0.000 claims abstract description 45
- 239000000758 substrate Substances 0.000 claims abstract description 38
- 239000000049 pigment Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 20
- 230000008646 thermal stress Effects 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 5
- 238000010304 firing Methods 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 23
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 18
- 239000004615 ingredient Substances 0.000 claims description 18
- 229910052742 iron Inorganic materials 0.000 claims description 16
- 239000011248 coating agent Substances 0.000 claims description 15
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 14
- -1 ii.(Co Inorganic materials 0.000 claims description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 9
- 229910052744 lithium Inorganic materials 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- FULFYAFFAGNFJM-UHFFFAOYSA-N oxocopper;oxo(oxochromiooxy)chromium Chemical compound [Cu]=O.O=[Cr]O[Cr]=O FULFYAFFAGNFJM-UHFFFAOYSA-N 0.000 claims description 9
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052804 chromium Inorganic materials 0.000 claims description 8
- 229910002477 CuCr2O4 Inorganic materials 0.000 claims description 7
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- 239000000843 powder Substances 0.000 abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 20
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 10
- 239000000377 silicon dioxide Substances 0.000 description 9
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- 239000011701 zinc Substances 0.000 description 3
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
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- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
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- DAFHKNAQFPVRKR-UHFFFAOYSA-N (3-hydroxy-2,2,4-trimethylpentyl) 2-methylpropanoate Chemical compound CC(C)C(O)C(C)(C)COC(=O)C(C)C DAFHKNAQFPVRKR-UHFFFAOYSA-N 0.000 description 1
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- WNJSKZBEWNVKGU-UHFFFAOYSA-N 2,2-dimethoxyethylbenzene Chemical compound COC(OC)CC1=CC=CC=C1 WNJSKZBEWNVKGU-UHFFFAOYSA-N 0.000 description 1
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 1
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- CRWNQZTZTZWPOF-UHFFFAOYSA-N 2-methyl-4-phenylpyridine Chemical compound C1=NC(C)=CC(C=2C=CC=CC=2)=C1 CRWNQZTZTZWPOF-UHFFFAOYSA-N 0.000 description 1
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- OVKDFILSBMEKLT-UHFFFAOYSA-N alpha-Terpineol Natural products CC(=C)C1(O)CCC(C)=CC1 OVKDFILSBMEKLT-UHFFFAOYSA-N 0.000 description 1
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- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
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- ZAUUZASCMSWKGX-UHFFFAOYSA-N manganese nickel Chemical compound [Mn].[Ni] ZAUUZASCMSWKGX-UHFFFAOYSA-N 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
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- 150000003672 ureas Chemical class 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
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- YEIGUXGHHKAURB-UHFFFAOYSA-N viridine Natural products O=C1C2=C3CCC(=O)C3=CC=C2C2(C)C(O)C(OC)C(=O)C3=COC1=C23 YEIGUXGHHKAURB-UHFFFAOYSA-N 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical group [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
-
- 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
- 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
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
-
- 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
- C03C4/00—Compositions for glass with special properties
- C03C4/14—Compositions for glass with special properties for electro-conductive glass
-
- 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
- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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Abstract
银浆料包括具有不同物理特性的两种粉末、银薄片以及玻璃熔块和颜料,它们一起在烧制过程中改善基材的热应力特征。
Description
发明技术领域
本发明涉及银浆料,其相对于其所施用的玻璃基材具有类似的导热系数。
本发明涉及导电银浆料,当热熔合(烧制)的浆料施用到玻璃、硅、陶瓷或陶瓷玻璃珐琅基材时,提供导电性和类似于基材的导热系数,因此降低涂层和上述基材之间产生的瞬态热应力差,否则该瞬态热应力差将会发生。浆料包括具有不同熔融温度的较低密度的银粉末、高密度银粉末和中密度的银薄片,以及黑色颜料和较低膨胀玻璃熔块的组合物。因此玻璃熔块是不含锂的浆料。
特别是,本发明涉及导电银涂层,其包括具有在较宽范围内的熔融温度的较低膨胀玻璃熔块的组合,其使银在烧制基材上产生较少应力,并在扩展的温度范围增加联系,从而减少涂层和前述基材之间产生的热应力差,否则该压力差将会产生,特别是在烧制周期时间被缩短的情况下。
相关技术的描述
常规导电银浆料可以由包含铅、镉、锂、铋、锌、硼和/或二氧化硅的氧化物的低熔点熔块制成。导电浆料被印刷到玻璃或陶瓷基材上,并被烧制以烧结和结合所述导电浆料到基材。烧制涂层到玻璃基材的任何类型的施用都将弱化玻璃基材。
发明详述
因此,本技术需要导电浆料,当被施用和烧制到玻璃或陶瓷基材时,其不会弱化玻璃基材,或者与已知导电浆料相比,至少使玻璃基材弱化的程度更轻。本发明克服了现有技术的缺点,如下文所示。
本发明的一个实施方式是含银浆料,其施用和烧制在基材上,赋予基材以改善的强度。
本发明的一个实施方式是含银浆料,其施用和烧制在基材上,赋予基材改善的强度。
本发明的一个实施方式是含银浆料,其施用和烧制在基材上,在烧制到基材期间减少瞬时热应力。
本发明的一个实施方式是包括银组分的导电浆料,所述银组分包括第一银浆料和第二银浆料(具有不同振实密度)和银薄片。所述浆料包含玻璃组分,所述玻璃组分包括选自由Bi2O3、ZnO、SiO2、B2O3、Na2O、K2O和ZrO2组成的组中的至少一种熔块。浆料还可以包括含有氧的氧化物颜料以及铜、铬和铁中的至少一种。
本发明的一个实施方式是包括基材的设备,含银浆料被施用和烧制到该基材上,其中烧制到基材(浆料被施用和烧制在其上)期间所述浆料的存在将减少瞬时热应力。
本发明的一个实施方式是一种导电浆料,其包括以下组分:(a)50-90wt%的银组分,包括(i)10-55wt%的第一银粉末,其具有0.3-1.5g/cc的振实密度,(ii)10-35wt%的银薄片,其具有3.0-4.5g/cc的振实密度,和(iii)5-30wt%的第二银粉末,其具有2.0-4.5g/cc的振实密度,(b)2-10wt%的玻璃组分,其包含(i)25-50wt%的Bi2O3,(ii)2-15wt%的ZnO,(iii)15-45wt%的SiO2,(iv)5-20wt%的B2O3,(v)1-10wt%的Na2O+K2O以及(vi)0.1-10wt%的ZrO2,(c)0.1-2wt%的颜料,其选自(i)CuCr2O4、(ii)(Co,Fe)(Fe,Cr)2O4和(iii)(Fe,Co)Fe2O4组成的组。导电浆料的可替代实施方式包括上述成分加上(d)1-8wt%的至少一种有机粘合剂,和(e)8-40wt%的至少一种有机溶剂。可替代实施方式包括导电浆料,其包括以本文别处公开的量存在的本文别处公开的银粉末、银薄片、玻璃组分、颜料、有机粘合剂和有机溶剂中的任意一种。
本发明的另一个实施方式是导电浆料,其包括以下组分:(a)55-85wt%的银组分,包括(i)15-30wt%的银粉末,其具有0.4-1.2g/cc的振实密度和2.5-6.5微米的D50粒径,(ii)15-30wt%的银薄片,其具有3.2-4.2g/cc的振实密度和1.3-3.3微米的D50粒径,和(iii)10-28wt%的银粉末,其具有2.6-4.3g/cc的振实密度和1-2微米的D50粒径,(b)3-8wt%的玻璃组分,其包括(i)25-50wt%的Bi2O3,(ii)2-15wt%的ZnO,(iii)15-45wt%的SiO2,(iv)5-20wt%的B2O3,(v)1-10wt%的Na2O+K2O以及(vi)0.1-10wt%的ZrO2,(c)1-2wt%的颜料,其选自(i)CuCr2O4、(ii)(Co,Fe)(Fe,Cr)2O4和(iii)(Fe,Co)Fe2O4组成的组。可替代的实施方式包括上述成分,另加(d)1-8wt%的至少一种有机粘合剂,和(e)8-40wt%的至少一种有机溶剂。
本发明的一个实施方式是基材,其至少部分地覆盖有烧制浆料,其中所述浆料是本文公开的任何导电浆料。
本发明的一个实施方式是减少瞬时热应力的方法,其包括将本文所公开的任何导电浆料施用到基材上,烧制浆料以烧结金属(即银),以及熔合玻璃成分或玻璃熔块,使得包括银金属和熔合玻璃的导电线迹被牢固的附加和集成到基材上。
本发明的一个实施方式是减少烧制过程中涂层和基材之间的瞬时热应力的方法,所述方法包括以重量计的以下组分:(a)施用于基材的不含锂的导电浆料,所述浆料包括(i)50-90wt%的银组分,其包括:(1)10-55wt%的第一银粉末,其具有0.3-1.5g/cc的振实密度,(2)10-35wt%的银薄片,其具有3.0-4.5g/cc的振实密度,和(3)5-30wt%的第二银粉末,其具有2.0-4.5g/cc的振实密度,(ii)2-10wt%的玻璃组分,其包括(1)25-50wt%的Bi2O3,(2)2-15wt%的ZnO,(3)15-45wt%的SiO2,(4)5-20wt%的B2O3,(5)1-10wt%的Na2O+K2O,(6)0.1-10wt%的ZrO2,(iii)0.1-5wt%的颜料,其选自(1)CuCr2O4、(2)(Co,Fe)(Fe,Cr)2O4和(3)(Fe,Co)Fe2O4组成的组,和(b)在烧制温度下,烧制所述浆料足够的时间以烧结银金属和熔合玻璃组分。减少瞬时热应力的方法的可替代实施方式包括施用浆料,所述浆料包括上述成分另加(d)1-8wt%的至少一种有机粘合剂,和(e)8-40wt%的至少一种有机溶剂。另一个可替代的实施方式包括涉及导电浆料的方法,所述导电浆料包括以本文别处所公开的含量存在的本文别处公开的银粉末、银薄片、玻璃组分、颜料、有机粘合剂和有机溶剂中的任意一种。另一个可替代的实施方式的方法包括在约950华氏度至约1400华氏度的烧制温度下烧制,优选约1200华氏度至约1300华氏度,更优选约1200华氏度至约1250华氏度。另一个可替代实施方式中的方法包括在约1至约6000秒的烧制时间烧制,优选约1至约600秒,更优选约1至约300秒,更优选约1至约180秒,更优选约1至约150秒,更优选约60至约150秒。
本发明还包括汽车玻璃、太阳能电池以及家电,其包括含有本文别处公开的任何浆料的涂层,或包括至少部分地由本文别处所公开的任何方法制成的被涂覆的基材的涂层。
本发明前述的内容和其它特征在下文更充分地描述并在权利要求中特别指出,下面的描述中详细阐述本发明的某些示例性的实施方式,这些实施方式是指示性的,但也是采用本发明原理的各种方式中的少数。
具体实施方式的描述
基于上述情况,现有技术没有这样的导电银涂层,其可以充分熔化同时在短烧制周期和需要提高烧制温度(即高于约1100华氏度)的烧制周期过程中使银涂层和相关基材(玻璃、硅、陶瓷或陶瓷珐琅)之间的热差异最小化。本发明允许用更广泛的玻璃熔块制成的导电涂层,该玻璃熔块包括基于锌、铋的硼硅酸盐及其组合,并且因此允许更广泛的烧制范围。本发明的银涂层允许在宽的温度范围内烧制,同时确保与基材的良好黏附,而不会因组装而增加热应力。玻璃熔块的熔合温度范围以及无机颜料和化合物的熔融温度设定烧制温度的上限,该烧制温度被需要为充分地将银金属和其他无机材料熔合在一起,并随后熔合到基材上,而引起进一步的热应力。
热应力在本文中定义为小区域内由温度差引起的每单位面积上的力。相关区域是浆料或其他涂层被施用和烧制到的基材区域。应力可被称为“瞬态”,因为它是短暂的,即它是仅在浆料加热(即烧制)以确保其附着到基材的过程中的因素。特别是,因为基材和导电银涂层被加热,基材承载常规银涂层的部分将比基材没有承载这种涂层的部分具有更低的温度。温度差产生热应力。本发明的组合物允许在扩展的烧制温度范围内相对一致的红外吸收,因此,涂层的热吸收率更紧密地与基材的热吸收率匹配,例如高红外吸收的黑色陶瓷珐琅,产生导电银涂层和基材之间更接近的热平衡。因此,在基材(例如玻璃、珐琅、陶瓷和陶瓷珐琅)上形成这种导电涂层过程中的热应力减小。
本发明的导电银浆料允许烧制温度为约950华氏度至约1400华氏度,优选约1200华氏度至约1300华氏度,更优选约1200华氏度至约1250华氏度。另一种优选的烧制范围为约1300华氏度至约1400华氏度。可以认为,不同形态和粒径分布的银粉末以及银薄片与基于Bi2O3、ZnO、SiO2、B2O3、Na2O、K2O和ZrO2的玻璃熔块的组合提供适合于与各种金属、玻璃、陶瓷和珐琅基材一起使用的唯一匹配的热膨胀系数。
颜料(例如CuCr2O4、(Co,Fe)(Fe,Cr)2O4和(Fe,Co)Fe2O4)以及可选的氧化物改性剂(例如MnO、Fe2O3、Al2O4、CuO和NiO)被用于保持高水平的红外线吸收直至约1400华氏度。这允许增加烧制温度并且因此加速(即减小)烧制周期时间,而引起额外的热应力。在本文别处公开的温度下的本发明预期的烧制时间是约1至约6000秒,优选约1至约600秒,更优选约1至约300秒,更优选约1至约180秒,更优选约1至约150秒,更优选约60至约150秒。
本发明的导电浆料包括若干主要组分:银粉末、银薄片、玻璃熔块、颜料、颜料改性剂、有机粘合剂和溶剂。在下文依次对每个进行详细介绍。
银粉末及薄片。用于本发明的银粉末具有大致球形的形状。概括地说,粉末和薄片具有下表中列出的特性。可以理解的是,给定的粉末或薄片可以具有在给定的行中的任何或所有的特性。给定粉末或薄片的特性的组合构成单独的粉末或薄片,其可以在本发明中被使用并要求保护。从该表给定的粉末或者薄片的特性和本文其他特性的组合可以被认为是单独的粉末或薄片。概括地说,本发明的浆料包含任何形式的50-90wt%的银。在一个优选实施方式中,本发明的浆料包含任何形式的50-85wt%的银。在一个更优选的实施方式中,浆料包括任何形式的50-83wt%的银,以及在一个更优选的实施方式中,浆料包括任何形式的55-80wt%的银。不同的银成分(两种粉末和一种薄片)的子范围的总计被理解为总计达总的银范围,即使构成范围的总和可能会低于或超过该总的银范围。类似地,整个组合物被推测含有总组分的100wt%。
表1.用于本发明的银粉末和薄片
表2.优选的粉末和薄片特性
各种各样的银粉末和银薄片可从美国俄亥俄州克里夫兰市的费罗公司(FerroCorporation)购得,并以产品名称SPC、SFW和SFC20ED进行销售。粉末SPC20ED属于上表中的“粉末1”;粉末SPC属于上表中的“粉末2”,SFW属于上表中的“薄片”。缩写PSDxx表示粒径Dxx,其中xx可以是10、50、90或95。粒径D95意味着样品中所有颗粒中的95%比所列数值小(以微米为单位),D90类似。粒径D50是微米的数值,其中颗粒的50%是比该数值更大,50%是更小。粒径D10是微米的数值,其中颗粒的10%是比该数值更小。
Ferro公司还销售其他适当的银金属粉末和银金属薄片。振实密度是对给定重量的材料在经历一定量的如本领域公知的规定的压实作用之后的体积的测量;报告为g/cc。由下述两种技术中的至少一种来测定表面积:通过费氏粒度测量仪(FSSS)的渗透测量法;以及由康塔公司气体吸附仪(Quantachrome)的气体吸收(BET比表面测定法)。
玻璃组分。本发明的浆料包含以重量计的1-10wt%的玻璃成分,优选2-10wt%,更优选4-10wt%,更优选5-9wt%。玻璃成分可以包含一种或多种玻璃熔块。用于本发明的玻璃熔块没有特别的限制。然而,优选的玻璃熔块包括锌和铋中的至少一种的氧化物;上述的组合也是合适的。另一种玻璃熔块的组合物可以见于表3中。用于本发明的玻璃熔块具有的热膨胀系数(CTE)为50-90×10-7,优选55-85×10-7,更优选60-83×10-7,而被认为是较低膨胀的玻璃熔块。这是相对于现有技术的较高膨胀的玻璃熔块,其具有的热膨胀系数在100-150×10-7的范围内。
表3.玻璃熔块组合的范.围
玻璃组合物 | I | II | III |
成分(wt%) | |||
Bi2O3 | 22-51 | 27-48 | 30-45 |
ZnO | 2-20 | 3-18 | 5-15 |
SiO2 | 15-50 | 18-45 | 20-40 |
B2O3 | 5-25 | 8-22 | 10-15 |
Na2O+K2O | 3-20 | 4-15 | 5-9 |
F | 0.1-8 | 0.5-5 | 1-3 |
ZrO2 | 0.25-10 | 0.5-8 | 1-5 |
TiO2 | 0-7 | 0-5 | 0.1-2 |
任何形式的Li、Pb、Cd | 0 | 0 | 0 |
各种实施方式的玻璃熔块可以使用表3或其它表的不同列的范围来构造。另外,对于以零为边界的任何范围,所述表格将被作为可替换公开以0.01或0.1下端为边界的相同的范围。
黑色颜料。本发明的组合物还包括一种或多种无机黑色颜料(如上所述的与碳黑分开)。适用于本发明的颜料包括CuCr2O4和(Co,Fe)(Fe,Cr)2O4和类似物。实施例包括从华盛顿宾夕法尼亚的Ferro公司购得的颜料,诸如颜料2991(铜铬黑)、颜料2980(钴铬铁黑)、颜料2987(镍锰铁铬黑)和颜料O-1776(铜铬黑)。在本发明目前最优选的实施方式中,无机黑色颜料是铜铬尖晶石,作为V-7702或V-7709从Ferro公司购得。黑色颜料可以在浆料配方中使用0.1-5wt%的量,优选0.2-4wt%,更优选0.5-3wt%,更优选1-2wt%。
颜料改性剂。各种氧化物已被认定为改变或扩展上文公开的颜料的特性是有用的。本发明的浆料或颜料还可包括MnO、Fe2O3、Al2O4、CuO和NiO中的任一种。
有机介质。所述有机介质包含粘合剂和溶剂,其基于预期应用而选择。所述介质充分悬浮微粒(即金属粉末、玻璃熔块、颜料等)并在烧制过程中完全燃烧是必要的。概括地说,该有机介质可包括石油/松木油基溶剂、酯醇基溶剂、十三醇基溶剂、热塑性蜡基粘合剂和/或水溶性乙二醇基溶剂。也可以使用简单的水溶剂。
特别是,也可以使用包括甲基纤维素、乙基纤维素、羟丙基纤维素、聚苯乙烯、改性聚苯乙烯和它们的组合的粘合剂。合适的溶剂包括二元醇,诸如乙二醇、丙二醇和己二醇;较高沸点的醇,诸如(二乙二醇单乙醚);丁基(二乙二醇单丁醚);二丁基(二甘醇二丁醚);丁基醋酸酯(二乙二醇丁醚醋酸酯);(2,2,4-三甲基-1,3-戊二醇单异丁酸酯),以及其他的醇酯、煤油和邻苯二甲酸二丁酯、二甘醇丁基醚;α-松油醇;β-松油醇:γ-松油醇;十三醇(例如商品名Exxal13);二乙二醇乙醚(CarbitolTM),二乙二醇丁醚(丁基CarbitolTM);松树油、植物油、矿物油、低分子量的石油馏分、十三醇和合成或天然树脂及其共混物。以商标销售的产品可从田纳西州金斯波特市的伊斯曼化学公司(Eastman Chemical Company)购得;这些以和商标销售的可以从密歇根州米德兰市的陶氏化学公司(DowChemical Co.)购得。表面活性剂和/或其它形成改性剂的膜也可包括在内。
介质也可以使用,其包括Ferro公司的编号为1331、1456、1562、1652和C92的产品。介质1331和1356包括不同量的乙基纤维素和十三醇。介质C92是甲基丙烯酸乙酯、13和二乙二醇丁醚醋酸酯的组合。
表4.用于本发明的介质的配方
分散表面活性剂。当使用不溶性颗粒状无机颜料时,分散表面活性剂有助于颜料润湿。分散表面活性剂通常包含带有颜料亲和基团的嵌段共聚物。例如,由德国韦瑟尔的毕克化学(Byk Chemie)以和商标销售的表面活性剂,如Disperbyk 110、140和163,它们是具有颜料亲和基团的高分子量嵌段共聚物的溶液和溶剂的共混物。Disperbyk 110是1∶1的丙二醇甲醚醋酸脂和烷基苯混合物。Disperbyk 140是在丙二醇甲醚醋酸脂溶剂中的酸性聚合物的烷基铵盐溶液。Disperbyk163具有4/2/5比例的二甲苯、醋酸丁酯和丙二醇甲醚醋酸脂溶剂。
流变改性剂。流变改性剂用于调节绿色颜料套组的组合物粘度。可以使用多种流变改性剂,包括那些以和商标销售、可从毕克化学公司购得的流变改性剂。它们包括例如BYK 400系列,诸如BYK 411和BYK 420(改性尿素溶液);BYK W-900系列(颜料润湿和分散添加剂);Disperplast系列(用于塑料溶胶和有机溶胶的颜料润湿和分散添加剂);和ViscObyk系列(用于塑料溶胶和有机溶胶的降粘剂)。
实施例。如表5中所示,使用Ferro公司的银粉末SPC20ED和SPC以及银薄片SFW,其分别对应于表1和2的粉末1、粉末2和薄片。浆料还包括玻璃熔块A、B、C和D,有机载体C-92和1356、P95-1W是含有少量锰的铜铬黑色颜料,可从日本东京的朝日产业株式会社公司(AsahiSangyo Kaisha Ltd.)购得,而且在某些情况下,浆料还包括TDA(十三醇)、和/或111。玻璃熔块A、B、C和D的特征在表7至10中,而玻璃料配方的建议和玻璃熔块的特性在表11中给出。
表5.示例性浆料组合物和粘性数据
SP-335是一种银粉末,其具有2.7至3.6的振实密度、23.2至32g/cc的表观密度和0.75至1.4m2/g的表面积。
是表面活性卵磷脂产品,从伊利诺伊州迪凯特的阿彻丹尼尔斯米德兰公司(Archer Daniels Midland Co)购得。此外,剪切速率可以从转子的转速由公式转速×转子因子=剪切速率来计算。#7转子的转子因子是0.209。“N.M.”表示未测量。
表6.基于CCL-268-B的连续试验
在上面的表格中,是硅酸锆,可从美国南卡罗来纳州安德鲁斯的特雷沃尔(Trebol)购得。
表7-9是示例性的熔块组合物。用于本发明的玻璃熔块不含锂,并具有以下的组成范围。表7-9各表示一种玻璃熔块(玻璃熔块A、B和C),其每一栏表示每种玻璃熔块的广泛的、优选的和更优选的范围。玻璃熔块A对应市售Ferro产品E-8008,而玻璃熔块B和C分别对应于Ferro公司的产品E-8018和E-8027。玻璃熔块D对应于Ferro公司的玻璃熔块E-8044。E-8018可被称为低膨胀玻璃熔块,而E-8027是一种超低膨胀玻璃熔块。
表7.玻璃熔块A的示例性配方范围
氧化物 | 广泛的 | 优选 | 更优选 |
Bi2O3 | 37-51 | 38.5-49.2 | 41.1-47.8 |
ZnO | 11-21 | 12.2-19.8 | 13.4-18.7 |
SiO2 | 12-25 | 14.3-23.2 | 16.9-21.7 |
B2O2 | 7.2+16.7 | 8.4-14.8 | 9.1-13.2 |
Na2O | 1.7-7.7 | 2.5-6.1 | 3.1-5.9 |
F | 0.9-3.4 | 1.3-3.1 | 1.7-2.8 |
ZrO2 | 0.7-2.1 | 0.9-1.8 | 1.1-1.7 |
TiO2 | 0.8-2.4 | 1.1-2.2 | 1.3-1.8 |
总计 | 100 | 100 | 100 |
表8.玻璃熔块B的示例性配方范围
氧化物 | 广泛的 | 优选 | 更优选 |
Bi2O3 | 37.2-51.1 | 39.3-47.8 | 41.4-46.6 |
ZnO | 1.7-5.1 | 2.2-4.8 | 2.5-4.3 |
SiO2 | 28.7-33.6 | 29.3-32.8 | 29.9-31.7 |
B2O2 | 11.9-17.2 | 12.7-16.8 | 13.2-15.7 |
Na2O | 4.7-9.1 | 5.2-8.2 | 5.9-7.5 |
F | 0 | 0 | 0 |
ZrO2 | 0.7-2.4 | 0.9-2.1 | 1.1-1.8 |
TiO2 | 0 | 0 | 0 |
总计 | 100 | 100 | 100 |
表9.玻璃熔块C的示例性配方范围
氧化物 | 广泛的 | 优选 | 更优选 |
Bi2O3 | 26.2-33.1 | 27.5-32.2 | 28.2-30.9 |
ZnO | 2.1-8.8 | 3.0-6.9 | 3.4-5.8 |
SiO2 | 38.5-43.2 | 39.2-42.2 | 39.7-41.8 |
B2O2 | 11.2-15.7 | 12.3-15.1 | 13.1-14.4 |
Na2O | 3.9-8.7 | 4.4-7.9 | 5.1-7.4 |
F | 0 | 0 | 0 |
ZrO2 | 2.7-8.1 | 3.2-7.1 | 3.9-6.4 |
TiO2 | 0 | 0 | 0 |
总计 | 100 | 100 | 100 |
表10.玻璃熔块D的示例性配方范围。
氧化物 | 广泛的 | 优选 | 更优选 |
Bi2O3 | 48.2-56.9 | 49.1-55.3 | 50.4-54.1 |
ZnO | 5.9-10.2 | 6.8-9.7 | 7.4-9.1 |
SiO2 | 21.6-30.3 | 23.2-28.5 | 24.4-27.2 |
B2O3 | 5.8-11.3 | 6.4-10.2 | 6.9-9.4 |
Li2O | 0.7-4.4 | 1.2-3.9 | 1.6-2.8 |
Na2O | 1.1-4.9 | 1.6-4.1 | 2.2-3.4 |
K2O | 0.4-2.8 | 0.6-2.2 | 0.8-1.7 |
F | 0.1-2.2 | 0.2-1.7 | 0.3-1.1 |
ZrO2 | 0.1-2.7 | 0.2-2.1 | 0.3-1.4 |
TiO2 | 0.3-3.1 | 0.5-2.4 | 0.6-1.7 |
总计 | 100 | 100 | 100 |
表11.来自表4中配方的玻璃熔块A-D的特性
玻璃熔块 | %范围 | 玻璃料的热膨胀系数 | 最低程度烧制 |
玻璃熔块A | 0.25-2.5% | 80×10-7 | 1110华氏度 |
玻璃熔块B | 1.5-3.5% | 83×10-7 | 1090 |
玻璃熔块C | 2.0-3.75% | 65×10-7 | 1170 |
玻璃熔块D | 未测定 | 87×10-7 | 未测定 |
在上表中,最低程度烧制是玻璃熔块将被熔合并形成多孔涂层的最低温度。
表12.当以发明的玻璃熔块印刷和烧制时,匹兹堡(PPG)和加迪安(Guardian)玻璃板的百分比强度减少的总结
表12中,对照是包含锂和不包含低膨胀玻璃熔块的现有技术领域的浆料。
表13中,本发明和现有技术的浆料的几个实施例被施用到市售的玻璃板(来自匹兹堡和加迪安)并在一定温度下烧制所指示的一定时间。
表13.在玻璃板上烧制的银浆料的特性
低膨胀玻璃料是E8018,额外的低膨胀玻璃料是E-8027。
在上面的表格中,对照是指玻璃印刷被烧制时没有银和黑色珐琅。JM2T1730是庄信万丰(Johnson Mattey)公司的黑色珐琅,相应样品是只有黑色珐琅和没有银印刷在玻璃上的测试。
CCL-268(68%银)从一个生产批次抽样,保持显示平均为72%的玻璃强度(类似于CCL-228)。CCL-268B(72%银)实验室样品平均为49%的玻璃强度的下降,其具有4010psi张力的平均基本强度,超出玻璃/银基本强度为1880至2820psi的张力的范围。Ferro的CCL-268B(不含镍)银浆料从生产批次抽样显示相同的60%玻璃强度的降低。对于这两个组的平均基本强度值为3032psi的张力,超出玻璃/银基本强度为1880至2820psi的张力的范围。
CCL-380(80%银)从一个生产批次取样保持平均为77%的玻璃强度的下降。2013年6月20日CCL-380B(80%银)实验室样品平均为68%的玻璃强度的下降,其具有2413psi张力的基本强度,在玻璃/银为1880至2820psi张力的基本强度的范围内。
Ferro的CCL-380B(不含镍)的实验室样品和CCL-380含镍的银浆料平均为76%的近似的强度降低。该实验室样品显示出的1793基本强度,低于玻璃/银的1880至2820psi张力的基本强度范围。
在上表中,“空气”是指该银印刷在熔融浮法玻璃的空气表面上,而“锡”是指银被印刷在玻璃的锡表面上。
其他优点和修改将容易被本领域的技术人员想到。因此,本发明在其更广泛的方面并不限于本文中示出和描述的特定的细节和示例性的实施例。因此,在不违反由附加权利要求和它们的等同物所限定的一般发明概念的精神或范围时,可以进行各种修改。
Claims (13)
1.不含锂的导电浆料,其包括以下组分:
a.55-85wt%的银组分,其包括:
i.15-30wt%但不为15wt%的第一银粉末,其具有0.4-1.2g/cc的振实密度和2.5-6.5微米的D50粒径,
ii.15-30wt%的银薄片,其具有3.2-4.2g/cc的振实密度和1.3-3.3微米的D50粒径,和
iii.10-28wt%的第二银粉末,其具有2.6-4.3g/cc的振实密度和1-2微米的D50粒径,
b.3-8wt%的玻璃组分,其包括:
i.25-50wt%的Bi2O3,
ii.2-15wt%的ZnO,
iii.15-45wt%的SiO2,
iv.5-20wt%的B2O3,
v.1-10wt%的Na2O+K2O,和
vi.0.1-10wt%的ZrO2,
所述玻璃组分为热膨胀系数为55-85×10-7的玻璃料,
c.1-2wt%的颜料,其选自以下组分组成的组:
i.CuCr2O4,
ii.(Co,Fe)(Fe,Cr)2O4,和
iii.(Fe,Co)Fe2O4,和
d.不含锂。
2.如权利要求1所述的导电浆料,其中所述第一银粉末具有0.5-1.5m2/g的比表面积。
3.如权利要求1所述的导电浆料,其中所述第二银粉末具有0.25-1.25m2/g的比表面积。
4.如权利要求1所述的导电浆料,其中所述银薄片具有0.75-1.5m2/g的比表面积。
5.如权利要求1所述的导电浆料,其中所述颜料还包含选自MnO、Fe2O3、Al2O4、CuO和NiO的组成的组中的至少一种。
6.如权利要求3所述的导电浆料,其中所述第一银粉末具有0.6-1.3m2/g的比表面积。
7.如权利要求3所述的导电浆料,其中所述第二银粉末具有0.5-1m2/g的比表面积。
8.如权利要求1所述的导电浆料,其中所述银薄片具有0.85-1.35m2/g的比表面积。
9.一种基材,其至少部分地覆盖有烧制浆料,其中所述浆料是根据权利要求1的导电浆料。
10.一种减少烧制过程中的涂层和基材之间的瞬时热应力的方法,所述方法包括:
a.施用不含锂的导电浆料到基材,所述浆料包括:
i.55-85wt%的银组分,其包含:
1.15-30wt%但不为15wt%的第一银粉末,其具有0.4-1.2g/cc的振实密度和2.5-6.5微米的D50粒径,
2.15-30wt%的银薄片,其具有3.2-4.2g/cc的振实密度和1.3-3.3微米的D50粒径,和
3.10-28wt%的第二银粉末,其具有2.6-4.3g/cc的振实密度和1-2微米的D50粒径,
ii.3-8wt%的玻璃组分,其含有:
1.25-50wt%的Bi2O3,
2.2-15wt%的ZnO,
3.15-45wt%的SiO2,
4.5-20wt%的B2O3,
5.1-10wt%的Na2O+K2O,和
6.0.1-10wt%的ZrO2,
所述玻璃组分为热膨胀系数为55-85×10-7的玻璃料,
iii.1-2wt%的颜料,其选自以下组成的组:
1.CuCr2O4,
2.(Co,Fe)(Fe,Cr)2O4,和
3.(Fe,Co)Fe2O4,和
iv.不含锂,和
b.在烧制温度下烧制浆料足够的时间以烧结所述银金属和熔合所述玻璃组分。
11.如权利要求10所述的方法,其中所述烧制温度为950华氏度至1400华氏度。
12.如权利要求10所述的方法,其中所述烧制温度为1200华氏度至1300华氏度。
13.如权利要求10所述的方法,其中所述烧制时间为1秒至300秒。
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