WO2010059507A1 - Sous-couches conférant une fonctionnalité supérieure de couche de finition - Google Patents

Sous-couches conférant une fonctionnalité supérieure de couche de finition Download PDF

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Publication number
WO2010059507A1
WO2010059507A1 PCT/US2009/064292 US2009064292W WO2010059507A1 WO 2010059507 A1 WO2010059507 A1 WO 2010059507A1 US 2009064292 W US2009064292 W US 2009064292W WO 2010059507 A1 WO2010059507 A1 WO 2010059507A1
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WO
WIPO (PCT)
Prior art keywords
coating
article
titania
oxides
silica
Prior art date
Application number
PCT/US2009/064292
Other languages
English (en)
Inventor
Songwei Lu
Caroline S. Harris
James Mccamy
Ilya Koltover
Mehran Arbab
Cheri M. Boykin
Original Assignee
Ppg Industries Ohio, Inc.
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from US12/273,623 external-priority patent/US20100124642A1/en
Priority claimed from US12/273,641 external-priority patent/US8133599B2/en
Priority claimed from US12/273,617 external-priority patent/US7998586B2/en
Application filed by Ppg Industries Ohio, Inc. filed Critical Ppg Industries Ohio, Inc.
Priority to RU2011124950/05A priority Critical patent/RU2481364C2/ru
Priority to CA2743845A priority patent/CA2743845A1/fr
Priority to CN200980148470.XA priority patent/CN102239221B/zh
Priority to DE112009003493T priority patent/DE112009003493T5/de
Priority to JP2011537513A priority patent/JP5343133B2/ja
Publication of WO2010059507A1 publication Critical patent/WO2010059507A1/fr

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Classifications

    • 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
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • 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
    • 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
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1693—Antifouling paints; Underwater paints as part of a multilayer system
    • 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
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/401—Oxides containing silicon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/405—Oxides of refractory metals or yttrium
    • 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
    • C03C2217/00—Coatings on glass
    • C03C2217/70—Properties of coatings
    • C03C2217/71—Photocatalytic 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
    • C03C2217/00—Coatings on glass
    • C03C2217/90—Other aspects of coatings
    • C03C2217/91—Coatings containing at least one layer having a composition gradient through its thickness
    • 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
    • C03C2217/00—Coatings on glass
    • C03C2217/90—Other aspects of coatings
    • C03C2217/94—Transparent conductive oxide layers [TCO] being part of a multilayer coating

Definitions

  • This invention relates generally to coated articles and, in particular, to multi-layer coated articles having a functional topcoat and at least one undercoating layer.
  • a typical solar cell comprises a substrate, such as a glass plate, having a transparent conductive film (first electrode).
  • a semiconductor film having a photoelectric conversion material is deposited on the transparent conductive film.
  • the cell includes another substrate having a transparent conductive film (second electrode).
  • An electrolyte could be enclosed between the two electrodes.
  • the electrons move as rapidly as possible through the first conductive film to the other electrode it is desirable if the surface resistivity of the transparent conductive film is low. If the electrons do not move rapidly, recombination of the electrons with the photoelectric conversion material (conventionally referred to as "reverse current” or "back current”) can occur. It is also desirable if the conductive film is highly transparent to permit the maximum amount of solar radiation to pass to the photoelectric conversion material. Therefore, it would be desirable to provide a coated article for a solar cell that enhances the electron flow through a transparent conductive film. That is, a transparent conductive film having a low surface resistivity.
  • FIG. 1 Another example of a field utilizing coated articles is the field of photocatalytic articles. It is known to apply a photocatalytic coating, such as titania, onto a substrate to provide a coated article having self-cleaning properties. Upon exposure to certain electromagnetic radiation, such as ultraviolet radiation, the photocatalytic coating interacts with organic contaminants on the coating surface to degrade or decompose the organic contaminants.
  • a photocatalytic coating such as titania
  • FIG. 1 Another example of a field utilizing coated articles.
  • photocatalytic articles have a relatively high visible light reflectance and, therefore, can be inappropriate for use in some architectural applications.
  • conventional photocatalytic coatings can be subject to degradation through what is conventionally termed "sodium ion poisoning" caused by sodium ions defusing from the underlying glass substrate into the photocatalytic coating. Further, conventional photocatalytic coatings tend to display iridescence effects that detract from the aesthetic appearance of the coated article.
  • a coated article having an undercoating layer positioned between a substrate and a functional top coat (such as but not limited to a conductive photovoltaic transparent conductive coating or a photocatalytic coating) that not only acts as a barrier to sodium ion diffusion but also enhances the performance of the coated article.
  • a functional top coat such as but not limited to a conductive photovoltaic transparent conductive coating or a photocatalytic coating
  • the performance could be enhanced by decreasing the reflectance of the coated article and/or providing color suppression to the article and/or increasing the functionality of the top coat.
  • the undercoating layer could decrease the surface resistivity of the top coat (e.g., a transparent conductive layer) to increase electron flow.
  • the undercoating layer could increase the photocatalytic activity of the photocatalytic coating.
  • a coated article includes a substrate and a first coating formed over at least a portion of the substrate.
  • the first coating comprises oxides of at least two of P, Si, Ti, Al and Zr.
  • a functional coating is formed over at least a portion of the first coating.
  • the first coating comprises at least oxides of Ti and Si.
  • the first coating comprises at least oxides of Ti, Si and P.
  • the first coating comprises at least oxides of Ti, Si and Al.
  • Other embodiments can include any combination of two or more of these materials.
  • Examples of functional coatings include, but are not limited to, photoactive coatings (such as photocatalytic coatings and/or photohydrophilic coatings), and electrically conductive coatings.
  • the functional coating can be applied over a first coating having any combination of the above components.
  • Another coated article comprises a glass substrate and a first coating formed over at least a portion of the substrate.
  • the first coating comprises oxides of at least two of P, Si, Ti, Al and Zr.
  • a functional coating is formed over at least a portion of the first coating.
  • the functional coating is selected from titania and fluorine doped tin oxide.
  • a method of making a coated article comprises providing a glass substrate; forming a first coating over at least a portion of the glass substrate by CVD by directing a first coating composition toward the glass substrate, the first coating composition comprising a silica precursor, a titania precursor, and a silica accelerant comprising at least one accelerant material having at least one of P, Al, and Zr; and forming a functional coating over at least a portion of the first coating by CVD by directing a second coating composition toward the glass substrate, the second coating composition comprising a fluorine doped tin oxide precursor composition or a titania precursor composition.
  • a further coated article comprises a substrate and a first coating formed over at least a portion of the substrate.
  • the first coating comprises a mixture of oxides comprising oxides of at least two of P, Si, Ti, Al and Zr.
  • a conductive coating is formed over at least a portion of the first coating.
  • the the conductive coating comprises oxides of one or more of Zn, Fe, Mn, Al, Ce, Sn, Sb, Hf, Zr, Ni, Zn, Bi, Ti, Co, Cr, Si or In or an alloy of two or more of these materials.
  • a method of decreasing the surface resistivity of a conductive coating comprises providing a substrate; forming a first coating over at least a portion of the substrate, the first coating comprising oxides of at least two of P, Si, Ti, Al and Zr; and forming a conductive coating over at least a portion of the first coating.
  • a method of increasing the haze and/or increasing the visible light transmittance of a coated article comprises providing a substrate; forming a first coating over at least a portion of the substrate, the first coating comprising oxides of at least two of P, Si, Ti, Al and Zr; and forming a functional coating over at least a portion of the first coating.
  • a still further coated article comprises a substrate and a first coating formed over at least a portion of the substrate.
  • the first coating comprises a mixture of oxides comprising oxides of at least two of P, Si, Ti, Al and Zr.
  • a photoactive coating is formed over at least a portion of the first coating.
  • a photoactive article comprises a glass substrate and a first coating formed over at least a portion of the substrate.
  • the first coating comprises a mixture of silica, titania and alumina.
  • a photoactive functional coating comprising titania is formed over at least a portion of the first coating.
  • a method of increasing the photocatalytic activity of a photoactive coating comprises providing a substrate; forming a first coating over at least a portion of the substrate, the first coating comprising oxides of at least two of P, Si, Ti, Al and Zr; and forming a photoactive coating over at least a portion of the first coating.
  • a method of making a photoactive article comprises providing a glass substrate; forming a first coating on at least a portion of the glass substrate by CVD by directing a first coating composition toward the glass substrate, the first coating composition comprising tetraethylorthosilicate, titanium isopropoxide, and dimethylaluminumisopropoxide; and forming a photoactive coating over at least a portion of the first coating by CVD by directing a second coating composition toward the glass substrate, the photoactive coating comprising titania.
  • FIG. 1 is a side, sectional view (not to scale) of a coated article incorporating features of the invention
  • Fig. 2 is a graph of surface resistance versus [Sn] for fluorine doped tin oxide coatings formed directly on glass or on an undercoating of the invention
  • Fig. 3 is a graph of percent transmittance versus wavelength for fluorine doped tin oxide coatings formed directly on glass or on an undercoating of the invention
  • Fig. 4. is a graph of reflectance versus titania thickness for the coated articles of Example 5
  • Fig. 5 is a graph of color change for the coated articles of Example 6.
  • each numerical value should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
  • all ranges disclosed herein are to be understood to encompass the beginning and ending range values and any and all subranges subsumed therein.
  • a stated range of "1 to 10" should be considered to include any and all subranges between (and inclusive of) the minimum value of 1 and the maximum value of 10; that is, all subranges beginning with a minimum value of 1 or more and ending with a maximum value of 10 or less, e.g., 1 to 3.3, 4.7 to 7.5, 5.5 to 10, and the like.
  • the terms “formed over”, “deposited over”, or “provided over” mean formed, deposited, or provided on but not necessarily in direct contact with the surface.
  • a coating layer “formed over” a substrate does not preclude the presence of one or more other coating layers or films of the same or different composition located between the formed coating layer and the substrate.
  • the terms “polymer” or “polymeric” include oligomers, homopolymers, copolymers, and terpolymers, e.g., polymers formed from two or more types of monomers or polymers.
  • the terms “visible region” or “visible light” refer to electromagnetic radiation having a wavelength in the range of 380 nm to 760 nm.
  • infrared region refers to electromagnetic radiation having a wavelength in the range of greater than 760 nm to 100,000 nm.
  • ultraviolet region or “ultraviolet radiation” mean electromagnetic energy having a wavelength in the range of 300 nm to less than 380 nm.
  • microwave region or “microwave radiation” refer to electromagnetic radiation having a frequency in the range of 300 megahertz to 300 gigahertz.
  • a coated article 10 incorporating features of the invention is illustrated in Fig. 1 .
  • the article 10 includes a substrate 12 having at least one major surface.
  • a first coating (undercoating layer) 14 of the invention is formed over at least a portion of the major surface.
  • a second coating (functional coating) 16 is formed over at least a portion of the first coating 14.
  • the substrate 12 can include any desired material having any desired characteristics.
  • the substrate 12 can be transparent, translucent, or opaque to visible light.
  • transparent is meant having a visible light transmittance of greater than 0% up to 100%.
  • the substrate 12 can be translucent or opaque.
  • translucent is meant allowing electromagnetic energy (e.g., visible light) to pass through but diffusing this energy such that objects on the side opposite the viewer are not clearly visible.
  • opaque having a visible light transmittance of 0%.
  • suitable materials include, but are not limited to, plastic substrates (such as acrylic polymers, such as polyacrylates; polyalkylmethacrylates, such as polymethylmethacrylates, polyethylmethacrylates, polypropylmethacrylates, and the like; polyurethanes; polycarbonates; polyalkylterephthalates, such as polyethyleneterephthalate (PET), polypropyleneterephthalates, polybutyleneterephthalates, and the like; polysiloxane- containing polymers; or copolymers of any monomers for preparing these, or any mixtures thereof); metal substrates, such as but not limited to galvanized steel, stainless steel, and aluminum; ceramic substrates; tile substrates; glass substrates; or mixtures or combinations of any of the above.
  • plastic substrates such as acrylic polymers, such as polyacrylates; polyalkylmethacrylates, such as polymethylmethacrylates, polyethy
  • the substrate can include conventional soda-lime-silicate glass, borosilicate glass, or leaded glass.
  • the glass can be clear glass.
  • clear glass is meant non-tinted or non-colored glass.
  • the glass can be tinted or otherwise colored glass.
  • the glass can be annealed or heat-treated glass.
  • heat treated means tempered or at least partially tempered.
  • the glass can be of any type, such as conventional float glass, and can be of any composition having any optical properties, e.g., any value of visible transmission, ultraviolet transmission, infrared transmission, and/or total solar energy transmission.
  • float glass glass formed by a conventional float process in which molten glass is deposited onto a molten metal bath and controllably cooled to form a float glass ribbon.
  • examples of glass suitable for the substrate are described in U.S. Patent Nos. 4,746,347; 4,792,536; 5,030,593; 5,030,594; 5,240,886; 5,385,872; and 5,393,593.
  • Non-limiting examples of glass that can be used for the practice of the invention include Solargreen®, Solextra®, GL-20®, GL-35TM, Solarbronze®, Starphire®, Solarphire®, Solarphire PV® and Solargray® glass, all commercially available from PPG Industries Inc. of Pittsburgh, Pennsylvania.
  • the glass can have a smooth surface or, alternatively, can have a rough or textured surface. In one non-limiting embodiment, the glass surface can have a surface roughness (RMS) in the range of 100 nm to 5 mm.
  • the substrate 12 can be of any desired dimensions, e.g., length, width, shape, or thickness.
  • the substrate 12 can be planar, curved, or have both planar and curved portions.
  • the substrate 12 can have a thickness in the range of 1 mm to 10 mm, such as 1 mm to 5 mm, such as 2 mm to 4 mm, such as 3 mm to 4 mm.
  • the substrate 12 can have a high visible light transmission at a reference wavelength of 550 nanometers (nm).
  • high visible light transmission is meant visible light transmission at 550 nm of greater than or equal to 85%, such as greater than or equal to 87%, such as greater than or equal to 90%, such as greater than or equal to 91 %, such as greater than or equal to 92%.
  • the first coating (undercoating layer) 14 provides the coated article 10 with various performance advantages, as will be described in detail below.
  • the first coating 14 can be a homogeneous coating.
  • homogeneous coating is meant a coating in which the materials are randomly distributed throughout the coating.
  • the first coating 14 can comprise a plurality of coating layers or films, (such as, two or more separate coating films).
  • the first coating 14 can be a gradient layer.
  • gradient layer is meant a layer having two or more components with the concentration of the components continually changing (or stepped) as the distance from the substrate changes.
  • the first coating 14 comprises a mixture of two or more oxides selected from oxides of silicon, titanium, aluminum, zirconium and/or phosphorus.
  • the oxides can be present in any desired proportions.
  • the first coating 14 comprises a mixture of silica and titania, with the silica present in the range of 0.1 weight percent (wt.%) to 99.9 wt.% and the titania present in the range of 99.9 wt.% to 0.1 wt.%.
  • the first coating 14 can be a homogeneous coating.
  • the first coating 14 can be a gradient coating with the relative proportions of silica and titania varying through the coating.
  • the first coating 14 can be primarily silica in the region adjacent the substrate surface and primarily titania at the outer region of the first coating 14.
  • the first coating 14 can include mixtures of at least two oxides having elements selected from silicon, titanium, aluminum, zirconium and/or phosphorus.
  • Such mixtures include, but are not limited to, titania and phosphorous oxide; silica and alumina; titania and alumina; silica and phosphorous oxide; titania and phosphorous oxide; silica and zirconia; titania and zirconia; alumina and zirconia; alumina and phosphorous oxide; zirconia and phosphorous oxide; or any combination of the above materials.
  • the first coating 14 can include mixtures of at least three oxides, such as but not limited to three or more oxides having elements selected from silicon, titanium, aluminum, zirconium and/or phosphorus. Examples include, but are not limited to, mixtures comprising silica, titania and phosphorous oxide; silica, titania and alumina; and silica, titania and zirconia.
  • the first coating 14 comprises a mixture of silica and titania with at least one other oxide selected from alumina, zirconia, and phosphorous oxide.
  • the relative proportions of the oxides can be present in any desired amount, such as 0.1 wt.% to 99.9 wt.% of one material, 99.9 wt.% to 0.1 wt.% of a second material, and 0.1 wt.% to 99.9 wt.% of a third material.
  • One particular first coating 14 of the invention comprises a mixture of silica, titania and phosphorous oxide.
  • the silica can be present in the range of 30 volume percent (vol.%) to 80 vol.%.
  • the titania can be present in the range of 5 vol.% to 69 vol.%.
  • the phosphorous oxide can be present in the range of 1 vol.% to 15 vol.%.
  • the first coating 14 can have any desired thickness, such as but not limited to 10 nm to 120 nm, such as 30 nm to 80 nm, such as 40 nm to 80 nm, such as 30 nm to 70 nm.
  • the second coating (top coat) 16 comprises a functional coating.
  • the second coating 16 comprises at least one electrically conductive oxide layer, such as a doped oxide layer.
  • the second coating 16 can include one or more oxide materials, such as but not limited to one or more oxides of one or more of Zn, Fe, Mn, Al, Ce, Sn, Sb, Hf, Zr, Ni, Zn, Bi, Ti, Co, Cr, Si or In or an alloy of two or more of these materials, such as zinc stannate.
  • the second coating 16 can also include one or more dopant materials, such as but not limited to F, In, Al, and/or Sb.
  • the second coating 16 is a fluorine doped tin oxide coating, with the fluorine present in the coating precursor materials in an amount less than 20 wt.% based on the total weight of the precursor materials, such as less than 15 weight percent, such as less than 13 wt.%, such as less than 10 wt.%, such as less than 5 wt.%.
  • the second coating 16 can be amorphous, crystalline or at least partly crystalline.
  • the second coating 16 comprises fluorine doped tin oxide having a thickness greater than 200 nm, such as greater than 250 nm, such as greater than 350 nm, such as greater than 380 nm, such as greater than 400 nm, such as greater than 420 nm. In one non-limiting embodiment, the thickness is in the range of 350 nm to 420 nm.
  • the undercoating layer 14 of the invention provides the top coat 16 (e.g., fluorine doped tin oxide) with a surface resistivity of less than 15 ohms per square ( ⁇ /D), such as less than 14 ⁇ /D, such as less than 13.5 ⁇ /D, such as less than 13 ⁇ /D, such as less than 12 ⁇ /D, such as less than 1 1 ⁇ /D, such as less than 10 ⁇ /D.
  • ⁇ /D ohms per square
  • the second coating 16 can be a photoactive coating.
  • photoactive or “photoactively” refer to the photogeneration of a hole- electron pair when illuminated by radiation of a particular frequency, e.g., ultraviolet ("UV") light.
  • the photoactive coating can be photocatalytic, photoactively hydrophilic, or both.
  • photocatalytic is meant a coating having self-cleaning properties, i.e., a coating which, upon exposure to certain electromagnetic radiation, such as UV, interacts with organic contaminants on the coating surface to degrade or decompose the organic contaminants.
  • photoactively hydrophilic is meant a coating for which the contact angle of a water droplet on the coating decreases with time as a result of exposure of the coating to electromagnetic radiation in the photoabsorption band of the material.
  • the contact angle can decrease to a value less than 15° such as less than 10° and can become superhydrophilic, e.g., decrease to less than 5°, after sixty minutes of exposure to radiation in the photoabsorption band of the material having an intensity of 24 W/m 2 at the coating surface.
  • the coating may not necessarily be photocatalytic to the extent that it is self-cleaning, i.e., may not be sufficiently photocatalytic to decompose organic material like grime on the coating surface in a reasonable or economically useful period of time.
  • the photocatalytic activity can be less than 4 x 10 3 per centimeter minute (crrT 1 min '1 ), such as less than 3 x 10 '3 cm "1 mirr 1 , such as less than 2 x 10 '3 cm "1 mirr 1 , such as less than 1 x 10 '3 crrT 1 min '1 .
  • the photoactive coating can include at least one photoactive coating material and, optionally, at least one additive or dopant configured to affect the photoactivity of the coating compared to that of the coating without the dopant material.
  • the photoactive coating material can include at least one oxide, such as but not limited to, one or more oxides or oxidesemiconductors, such as titanium oxides, silicon oxides, aluminum oxides, iron oxides, silver oxides, cobalt oxides, chromium oxides, copper oxides, tungsten oxides, zinc oxides, zinc/tin oxides, strontium titanate, and mixtures thereof.
  • the oxide can include oxides, super-oxides or sub-oxides of the element.
  • the oxide can be crystalline or at least partially crystalline.
  • the photoactive coating material is titanium dioxide (titania). Titanium dioxide exists in an amorphous form and three crystalline forms, i.e., the anatase, rutile and brookite crystalline forms.
  • the anatase phase titanium dioxide is particularly useful because it exhibits strong photoactivity while also possessing excellent resistance to chemical attack and excellent physical durability.
  • the rutile phase or combinations of the anatase and/or rutile phases with the brookite and/or amorphous phases are also acceptable for the present invention.
  • Examples of dopants for the photoactive coating useful for the invention include, but are not limited to, one or more of chromium (Cr), vanadium (V), manganese (Mn), copper (Cu), iron (Fe), magnesium (Mg), scandium (Sc), yttrium (Y), niobium (Nb), molybdenum (Mo), ruthenium (Ru), tungsten (W), silver (Ag), lead (Pb), nickel (Ni), rhenium (Re), tin (Sn), and/or any mixtures or combinations thereof in either the elemental or ionic state.
  • the second coating 16 comprises titania having a thickness greater than 10 nm, such as greater than 20 nm, such as greater than 30 nm, such as greater than 40 nm, such as greater than 50 nm, such as greater than 60 nm, such as greater than 70 nm, such as greater than 80 nm, such as greater than 90 nm, such as greater than 100 nm, such as in the range of 10 nm to 150 nm.
  • the first coating 14 of the invention can provide the article 10 having a titania second coating 16 with a reflectance in the visible region of less than 23%, such as less than 20%, such as less than 19%, such as less than 18%, such as less than 17%, such as less than 16%, such as less than 15%, such as less than 14%, such as less than 12%, such as less than 1 1 %, such as less than 10%.
  • the first coating 14 and/or second coating 16 can be formed over at least a portion of the substrate 12 by any conventional method, such as but not limited to spray pyrolysis, chemical vapor deposition (CVD), or magnetron sputtered vacuum deposition (MSVD).
  • an organic or metal-containing precursor composition having one or more oxide precursor materials e.g., precursor materials for titania and/or silica and/or alumina and/or phosphorous oxide and/or zirconia
  • a suspension e.g., an aqueous or non-aqueous solution
  • the composition can include one or more dopant materials.
  • a precursor composition is carried in a carrier gas, e.g., nitrogen gas, and is directed toward the heated substrate.
  • one or more metal-containing cathode targets are sputtered under reduced pressure in an inert or oxygen-containing atmosphere to deposit a sputter coating over substrate.
  • the substrate can be heated during or after coating to cause crystallization of the sputtered coating to form the coating.
  • one or more CVD coating apparatus can be employed at one or more positions in a conventional float glass ribbon manufacturing process.
  • CVD coating apparatus may be employed as the float glass ribbon travels through the tin bath, after it exits the tin bath, before it enters the annealing lehr, as it travels through the annealing lehr, or after it exits the annealing lehr.
  • the CVD method can coat a moving float glass ribbon, yet withstand the harsh environments associated with manufacturing the float glass ribbon, the CVD method is particularly well suited to deposit coatings on the float glass ribbon in the molten tin bath.
  • one or more CVD coaters can be located in the tin bath above the molten tin pool. As the float glass ribbon moves through the tin bath, the vaporized precursor composition can be added to a carrier gas and directed onto the top surface of the ribbon. The precursor composition decomposes to form a coating (e.g., first coating 14 and/or second coating 16) on the ribbon.
  • a coating e.g., first coating 14 and/or second coating 16
  • the coating composition is deposited on the ribbon at a location in which the temperature of the ribbon is less than 1300 0 F (704 0 C), such as less than 125O 0 F (677 0 C), such as less than 1200 0 F (649 0 C), such as less than 1 190 0 F (643 0 C), such as less than 1 150 0 F (621 0 C), such as less than 1 130 0 F (610 0 C), such as in the range of 1 190 0 F to 1200 0 F (643 ⁇ € to 649 0 C).
  • a second coating 16 e.g., fluorine doped tin oxide
  • the composition comprises both a silica precursor and a titania precursor.
  • a silica precursor is tetraethylorthosilicate (TEOS).
  • titania precursors include, but are not limited to, oxides, sub-oxides, or super-oxides of titanium.
  • the titania precursor material can include one or more titanium alkoxides, such as but not limited to titanium methoxide, ethoxide, propoxide, butoxide, and the like; or isomers thereof, e.g., titanium isopropoxide, tetraethoxide, and the like.
  • Exemplary precursor materials suitable for the practice of the invention include, but are not limited to, tetraisopropyltitanate (TPT).
  • the titania precursor material can be titanium tetrachloride.
  • alumina precursors include, but are not limited to, dimethylaluminumisopropoxide (DMAP) and aluminum tri-sec-butoxide (ATSB).
  • DMAP dimethylaluminumisopropoxide
  • ATSB aluminum tri-sec-butoxide
  • the dimethylaluminumisopropoxide can be made by mixing trimethylaluminum and aluminumisopropoxide at a molar ratio of 2:1 in an inert atmosphere at room temperature.
  • phosphorous oxide precursors include, but are not limited to, triethyl phosphite.
  • zirconia precursors include, but are not limited to, zirconium alkoxides.
  • a first coating 14 having a combination of silica and titania provides advantages over previous oxide combinations.
  • the combination of a low refractive index material such as silica (refractive index of 1 .5 at 550 nm) with a high refractive index material such as titania (refractive index of 2.4 at 550 nm) allows the refractive index of the first coating 14 to be varied between these two extremes by varying the amount of silica and titania. This is particularly useful in providing the first coating 14 with color or iridescence suppression properties.
  • the deposition rate of titania is typically much faster than that of silica. Under typical deposition conditions, this limits the amount of silica to no more than about 50 wt. %, which in turn limits the lower range of the refractive index of the resultant silica/titania coating. Therefore, a dopant material can be added to the silica and titania precursor composition to accelerate the deposition rate of silica. The dopant forms part of the resultant oxide mixture and, therefore, can be selected to provide enhanced performance properties to the resultant coating. Examples of dopants useful for the practice of the invention include, but are not limited to, materials containing one or more of phosphorous, aluminum and zirconium to form oxides of these materials in the resultant coating.
  • Examples of phosphorous oxide precursor materials include triethylphosphite.
  • Examples of alumina precursor materials include aluminumtrisecbutoxide (ATSB) and dimethylaluminumisopropoxide (DMAP).
  • Examples of zirconia precursors include zirconium alkoxide.
  • This Example illustrates the use of an undercoating layer of the invention as a color suppression layer for a titania top coat.
  • the undercoating layer was a combination of silica, titania and phosphorous oxide.
  • the undercoating layer was deposited on a glass substrate by a chemical vapor deposition process using a laboratory coater. A titania coating was then deposited on the undercoating.
  • Table 1 shows the coating configurations (composition and thickness) for Samples 1 -4.
  • the undercoating was deposited as a multi-film layer having three undercoating films; a first undercoating film over the glass substrate, a second undercoating film over the first undercoating film, and a third undercoating film over the second undercoating film.
  • the multi-layer configuration simulates a graded undercoating layer.
  • Table 2 shows the reflected color performance data for Samples 1 -4 and Comparative Samples (titania coated glass sheets without the undercoating layer). The color data was modeled using conventional TFCalc® software for the coated side of the substrate at D65, 10 Q Observer.
  • the presence of the undercoating layer provides a generally lower (more negative) a * and a higher (more positive) b * compared to the article without the undercoating layer.
  • This Example illustrates the use of an undercoating layer of the invention as to provide enhanced photoactivity to a titania topcoat.
  • the undercoating layer comprised silica, titania and phosphorous oxide.
  • Both the undercoating layer and the top coat (titania) were formed by a chemical vapor deposition process.
  • the precursor for phosphorus oxide was triethyl phosphite (TEP).
  • the precursor for silica was tetraethyl orthosilicate (TEOS).
  • the precursor for titania in both the undercoating layer and the top coat was tetra isopropyl titanate (TPT).
  • Table 3 shows the deposition parameters for Samples 5-9.
  • Table 4 shows the layer thicknesses for Samples 5-9.
  • Table 5 shows the results of a conventional stearic acid test for Samples 5-9.
  • the stearic acid test is described in U.S. Patent No. 6,027,766, herein incorporated by reference.
  • the articles having the undercoating layer of the invention had higher photocatalytic activity than the articles without the undercoating layer (Sample 9).
  • This Example illustrates the use of an undercoating layer of the invention to reduce the surface resistance of a fluorine doped tin oxide top coat.
  • the undercoating layer was a silica, titania, phosphorous oxide undercoat deposited by CVD.
  • the precursors used were TEOS (silica), TPT (titania), and TEP
  • Fluorine doped tin oxide topcoats of various thickness were deposited on the undercoating layer and also on non-coated glass (as comparative samples). Both coatings were compared by surface resistance as measured by R-Chek+ 4 point meter commercially available from Electronic Design To Market, Inc. The amount of [Sn] was determined by X-ray florescence, which corresponds to the thickness of the fluorine doped tin oxide coatings.
  • Fig. 2 shows that the surface resistance of fluorine doped tin oxide coatings on an undercoating layer of the invention averaged 1 to 3 ohms/square lower than the same thickness fluorine doped tin oxide coatings on glass.
  • Fig. 1 shows that the surface resistance of fluorine doped tin oxide coatings on an undercoating layer of the invention averaged 1 to 3 ohms/square lower than the same thickness fluorine doped tin oxide coatings on glass.
  • the open squares and dotted line are for fluorine doped tin oxide on glass.
  • the closed circles and solid line are for the fluorine doped tin oxide coatings on the undercoating layer of the invention.
  • the undercoating layer (composition and thickness) was the same for each sample.
  • a piece of clear glass (12 inches by 24 inches; 30 cm by 61 cm) was coated using a CVD process with the precursors described above.
  • Half of the glass was coated with a fluorine doped tin oxide coating directly on the glass and the other half of the glass was coated with a silica, titania, phosphorous undercoating layer and a fluorine doped tin oxide top coat.
  • Samples were cut from each portion of the glass sheet and analyzed as described below.
  • the Samples were also tested for haze and transmittance. The results are shown in Table 7.
  • the transmittance spectra are shown in Fig. 4.
  • the haze was higher and the transmittance was also higher for the fluorine doped tin oxide (FTO)/undercoating layer (UL) coating stack as compared to the fluorine doped tin oxide (FTO) coating directly on glass.
  • the undercoating layer of the invention also provides a way to increase the haze and transmittance of a coated article. This could be useful in the field of solar cells where increased haze increases the absorption path of the electromagnetic energy which, in turn, provides increased opportunity for the electromagnetic energy to be absorbed.
  • the FTO coating thickness was slightly higher in the case of the FTO coating on glass (356 nm) versus the FTO on the UL (FTO top coating 334 nm) as determined by the etching method.
  • the coatings were viewed using scanning electron microscopy (SEM). Numerous small holes were seen in the FTO coating directly on glass. No holes were observed in the FTO/UL coating stack.
  • This Example illustrates the effect of an undercoating layer of the invention on the reflectance of a coated article.
  • Fig. 4 shows the change of reflectance for a 10 nm to 120 nm TiO 2 coating on clear glass (open diamond with dotted line) and for the same TiO 2 layer on an undercoating layer of the invention on clear glass.
  • the undercoating layer was 13 nm 75%SiO 2 -20%TiO 2 -
  • the change of TiO 2 thickness is from 10 nm to 120 nm with 5 nm intervals.
  • Fig. 4 shows that when the TiO 2 functional coating thickness on glass increases, the reflectance swings widely (i.e., anywhere from 1 1.7% ⁇ R ⁇ 38.8%). However, when the
  • TiO 2 functional coating is deposited on the undercoating layer, the reflectance changes are much lower (i.e., ranging from 17.2% to 27.4%). This shows that with the variation of top coating thickness, the reflectance of the entire coating stack with an underlayer coating is not as sensitive as that without an underlayer coating.
  • the reflectance could be significantly reduced with an undercoating layer of the invention.
  • Table 10 shows the difference in reflectance at titania levels of 55 nm and 165 nm.
  • This Example illustrates the effect of an undercoating layer of the invention on the color (e.g., a * and b * ) of an article.
  • Fig. 5 shows the change of a * and b * for a 10 nm to 120 nm TiO 2 on clear glass
  • Fig. 5 shows that when the TiO 2 functional coating thickness increases, the color
  • This Example illustrates the effect of a gradient undercoating layer of silica and titania on the photocatalytic activity of a titania topcoat (120 nm thick).
  • Table 1 1 shows the compositions of two gradient undercoating layers.
  • Table 12 shows the effect of the two undercoating layers of Table 1 1 on the photocatalytic activity of a 120 nm thick topcoat of titania as compared to the activity of the titania without the undercoating layers.
  • [Ti] units are micrograms/cm 2 .

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  • General Chemical & Material Sciences (AREA)
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Abstract

L'invention porte sur un article revêtu qui comprend un substrat et un premier revêtement formé au moins sur une partie du substrat. Le premier revêtement comprend un mélange d'oxydes contenant des oxydes d'au moins deux éléments parmi P, Si, Ti, Al et Zr. Un revêtement fonctionnel est formé sur au moins une partie de premier revêtement. Le revêtement fonctionnel est choisi parmi un revêtement conducteur de l'électricité et un revêtement photoactif. Dans un mode de réalisation, le revêtement fonctionnel contient de l'oxyde d'étain dopé au fluor. Dans un autre mode de réalisation, le revêtement fonctionnel contient de l'oxyde de titane.
PCT/US2009/064292 2008-11-19 2009-11-13 Sous-couches conférant une fonctionnalité supérieure de couche de finition WO2010059507A1 (fr)

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RU2011124950/05A RU2481364C2 (ru) 2008-11-19 2009-11-13 Промежуточные слои, обеспечивающие улучшенную функциональность верхнего слоя
CA2743845A CA2743845A1 (fr) 2008-11-19 2009-11-13 Sous-couches conferant une fonctionnalite superieure de couche de finition
CN200980148470.XA CN102239221B (zh) 2008-11-19 2009-11-13 提供改善的外涂层功能性的底涂层
DE112009003493T DE112009003493T5 (de) 2008-11-19 2009-11-13 Grundierungsschichten, die eine verbesserte Deckschichtfunktionalität verleihen
JP2011537513A JP5343133B2 (ja) 2008-11-19 2009-11-13 トップコートの機能を向上させるアンダーコーティング層

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US12/273,623 US20100124642A1 (en) 2008-11-19 2008-11-19 Undercoating layers providing improved conductive topcoat functionality
US12/273,641 US8133599B2 (en) 2008-11-19 2008-11-19 Undercoating layers providing improved photoactive topcoat functionality
US12/273,617 2008-11-19
US12/273,641 2008-11-19
US12/273,617 US7998586B2 (en) 2008-11-19 2008-11-19 Undercoating layers providing improved topcoat functionality
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WO2013106312A3 (fr) * 2012-01-10 2013-11-07 Ppg Industries Ohio, Inc. Verres revêtus à faible résistance de couche, à surface lisse et/ou à faible émissivité thermique
WO2019043398A1 (fr) * 2017-08-31 2019-03-07 Pilkington Group Limited Article en verre revêtu, son procédé de fabrication, et cellule photovoltaïque fabriquée avec celui-ci
US11031514B2 (en) 2013-03-12 2021-06-08 Vitro, S.A.B. De C.V. Solar cell with selectively doped conductive oxide layer and method of making the same
US11485678B2 (en) 2017-08-31 2022-11-01 Pilkington Group Limited Chemical vapor deposition process for forming a silicon oxide coating

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CN106655995B (zh) * 2017-02-09 2019-03-12 河南弘大新材科技有限公司 自洁式光电转换太阳能瓦
CN107458052B (zh) * 2017-07-18 2019-07-02 南京工业职业技术学院 一种自清洁聚乙烯薄膜及其制备方法
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CN102239221A (zh) 2011-11-09
DE112009003493T5 (de) 2012-09-06
JP2012509214A (ja) 2012-04-19
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