WO1999065838A9 - Anti-solar and low emissivity functioning multi-layer coatings on transparent substrates - Google Patents
Anti-solar and low emissivity functioning multi-layer coatings on transparent substratesInfo
- Publication number
- WO1999065838A9 WO1999065838A9 PCT/US1999/013444 US9913444W WO9965838A9 WO 1999065838 A9 WO1999065838 A9 WO 1999065838A9 US 9913444 W US9913444 W US 9913444W WO 9965838 A9 WO9965838 A9 WO 9965838A9
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- layer
- coated article
- reflection layer
- reflection
- substrate
- Prior art date
Links
Classifications
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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
- C03C17/3618—Coatings of type glass/inorganic compound/other inorganic layers, at least one layer being metallic
-
- 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
- C03C17/3636—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 one layer at least containing silicon, hydrogenated silicon or a silicide
-
- 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
- C03C17/3639—Multilayers containing at least two functional metal layers
-
- 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
- C03C17/3644—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 the metal being silver
-
- 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
- C03C17/3652—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 the coating stack containing at least one sacrificial layer to protect the metal from oxidation
-
- 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
- C03C17/3657—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 the multilayer coating having optical properties
- C03C17/366—Low-emissivity or solar control 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
- C03C2217/70—Properties of coatings
- C03C2217/78—Coatings specially designed to be durable, e.g. scratch-resistant
Definitions
- the present invention is directed to transparent substrates having double functioning multi ⁇
- the invention relates, in particular, to anti-solar, low emissivity
- Low emissivity coatings for glazing products are disclosed, for example, in
- Hayward et al. The multi-layer coating of Hayward et al. is said to comprise a layer of sputtered zinc, tin,
- titanium, indium/tin or bismuth oxide next a layer of sputtered silver or silver alloy, then a layer
- Such multi-layer film is said to have excellent visible light transmission while controlling
- a temperable coated article is
- metal-containing film such as titanium nitride which ordinarily oxidizes at the high temperatures
- properties of the coating can be changed independent of its reflection properties, by varying the
- a buffer film typically is positioned between the metal and the second dielectric films.
- dielectric materials include, for example,
- oxides such as zinc oxide, tin oxide, zinc/tin oxide composites, indium/tin oxide, bismuth oxide,
- the metal layer frequently employs silver,
- protecting a silver or other metal film have typically been, for example, a sub-oxide of chrome or
- chrome/nickel or nitride of silicon or titanium film lOO ⁇ to 120A thick chrome/nickel or nitride of silicon or titanium film lOO ⁇ to 120A thick. The thickness of the metal
- film is selected to provide adequately low emissivity while maintaining sufficiently high
- the bottom and top dielectric films is selected typically to achieve adequate anti-reflectance for the metal film, whereby the entire multi-layer coating has improved transparency to visible light.
- large area deposition refers to deposition
- layer coating having long shelf life is intended to mean, especially, that the coated surface can be
- substrate having a double functioning multi-layer coating on at least one surface of the substrate.
- Such coating providing both low emissivity and anti-solar performance characteristics.
- a coated article of manufacture comprises
- the substantially transparent coating comprises a first anti-reflection layer
- anti-reflection layer is a layer of dielectric material overlying the surface of the substrate.
- anti-reflection layer is a layer of dielectric material overlying the surface of the substrate.
- any particular layer of the coating may be said to lie directly on another layer Qf the coating notwithstanding that there may be a slight transition zone between the two layers
- An infra-red reflective layer of silver metal is different from the primary composition of the layers.
- a buffer layer directly overlies the infra-red reflective layer of
- a second anti-reflection layer of tungsten oxide overlies the buffer layer.
- the first anti-reflection layer of dielectric material is tungsten oxide.
- the buffer layer preferably
- silicon buffer layer comprises silicon, silicon nitride or tungsten nitride and is referred to here as the silicon buffer layer.
- silica that is silicon oxide
- the silicon At its exposed surface, the silicon would react with such oxygen, forming a transition zone of silicon
- Such methods comprise providing a substantially transparent
- the multi-layer, low emissivity, anti-solar coating is then formed on the surface of the
- the first anti-reflection layer of dielectric material is deposited, followed by the silver
- each of the layers of the substantially transparent coating is deposited by sputtering
- Suitable partitions such as curtains or the like, separate one sputter station from the next within the sputtering chamber, such that different
- a reactive atmosphere comprising
- nitrogen or oxygen or both can be used, for example, at a first station to deposit a tungsten oxide
- the substantially transparent dual-functions disclosed here coating is deposited by
- a multi-layer coating is deposited comprising the
- the coating in accordance with such preferred embodiments may be any one of the following preferred embodiments.
- multi-pass methods of the invention are found to have substantially improved coating properties
- the resulting coating has high durability, bulk or near bulk density and long shelf life. It is particularly advantageous that the tungsten oxide layer can be formed by reactive sputtering from
- the resulting tungsten oxide layer has a high
- refractive index (approximately 2.2 in the visible spectrum). This refractive index is comparable to
- Zinc oxide forms soft and weak films.
- coatings disclosed here can be accomplished in less time. As noted above, faster production speeds
- thicknesses of 400A or more to provide performance characteristics comparable to those achieved
- tungsten oxide anti-reflection films tin oxide deposits 3 - 4 times slower than tungsten oxide
- Zinc oxide although having relatively fast
- the tungsten oxide anti-reflection layer has advantageously low absorption
- the tungsten oxide anti-reflection layer of the dual-function coatings disclosed here has
- metal infra-red reflective layer specifically, a buffer layer formed of silicon, silicon oxide, silicon
- Silicon buffer layers having a thickness of only 2 ⁇ A to 25A are found to
- the silicon layer can be
- thickness to 5 ⁇ A is found to provide excellent protection for the underlying silver metal layer even
- a tungsten oxide layer for depositing the tungsten oxide layer.
- a tungsten oxide layer for depositing the tungsten oxide layer.
- thicker silicon buffer layer is employed when higher deposition power levels are to be used for
- Fig. 1 is a schematic cross-sectional view of a coated article of manufacture according to a
- Fig. 2 is a schematic cross-sectional view of a second preferred embodiment
- Fig. 3 is a schematic cross-sectional view of a third preferred embodiment
- Figs. 4-9 are graphical representations of the spectral properties of various preferred embodiments
- Figs. 10 and 11 are graphical representations discussed in Example 7, below.
- Fig. 12 is a schematic illustration of a multi-pane glazing system in accordance with a
- coated articles disclosed here comprising a substantially transparent
- substrate carrying a substantially transparent dual-function coating have numerous commercially
- Such panels have
- electrochromic devices such as display devices and glazing units
- a coated article 10 is seen to comprise a substantially transparent
- Coating 16 is dual-
- Coating 16 includes a first anti-reflection
- reflection layer 18 is formed of tungsten oxide. It should be understood that all references here and
- WO x unless otherwise clear from context.
- WO x where x is less than 3 is a blue oxide.
- Silver metal layer 20 lies directly on anti-reflection
- Silver metal layers of greater thickness will provide enhanced infra-red reflectivity, while
- thinner silver metal layers will provide increased transmittance of light in the visible wavelength
- the silver metal layer has a thickness
- preferably is formed of silicon for excellent protection of the underlying silver metal layer.
- the silicone layer will include native
- oxide of silicon to a certain depth, for example, about 10A to 15 A, at the interface with the overlying
- the buffer layer may be formed of silicon
- the silicon buffer layer preferably
- the overlying anti-reflection film 24 comprises tungsten oxide in accordance with the
- the tungsten oxide layer can be formed by sputter
- anti-reflection layer including low absorption coefficient in the visible and infra-red regions along
- the tungsten oxide anti-reflection layer 24 preferably has a thickness of about 30 ⁇ A to
- the first anti-reflection film 18, when formed of tungsten oxide, preferably has a thickness also within the range about 30 ⁇ A to 45 ⁇ A.
- the thickness of the first anti-reflection layer formed of tungsten oxide is from about zero percent (0%) to ten percent (10%), more preferably
- first anti-reflection layer 38 overlying the
- the color control layer preferably
- the thickness less than 5 ⁇ A and is formed preferably of silicon or tungsten metal. It will be within
- the anti-reflection layer 38 in coating 36 of coated article 30 is comparable to anti-reflection
- Silver metal layer 40 in the embodiment of Fig. 2 is silver metal layer 40 in the embodiment of Fig. 2
- layer 42 corresponds generally to buffer layer 22 in the embodiment of Fig. 1. It will be within the
- the silver metal layer 40 within the constraints of meeting spectral performance requirements in the
- Tungsten oxide anti -reflection film 44 in the embodiment of Fig. 2 corresponds
- the outer anti-reflection layer that is, anti-reflection layer 24 in Fig.l and 44 in Fig. 2, is selected
- reflectance color preferably being neutral or between the bluish and pinkish reflectance
- a metal protection layer 46 directly overlies anti-reflection layer 44.
- the coated article 30 is subjected to a
- Metal protection layer 46 advantageously
- a glass substrate such as a soda-lime-silica glass substrate intended for architectural or
- metal protection layer 46 is formed of silicon or silicon nitride
- a second metal protection layer can be employed, being positioned preferably
- protection layer directly on the surface of the substrate is formed of silicon or silicon nitride or
- tungsten metal and has a thickness in the range 4 ⁇ A to lOOA, for example, 5 ⁇ A to 8 ⁇ A, more preferably about 5 ⁇ A to 7 ⁇ A.
- the thickness of metal protection layer 46 shown in Fig. 2 is a thickness in the range 4 ⁇ A to lOOA, for example, 5 ⁇ A to 8 ⁇ A, more preferably about 5 ⁇ A to 7 ⁇ A.
- the coating 36 (being the upper surface as viewed in Fig. 2) preferably is
- the coating comprises of first series
- coated article of manufacture 50 is seen to comprise a substrate 52 having a surface 54 carrying
- Coating 56 includes a first anti-reflection layer 58
- second anti-reflection layer 64 of tungsten oxide.
- reflection layer 66 of tungsten oxide directly overlies second anti-reflection layer 64.
- tungsten oxide layers 64 and 66 may alternatively be considered to be one
- fourth anti-reflection layer 72 of tungsten oxide directly overlies silicon buffer layer 70.
- color control layer(s) It will be recognized by those skilled in the art that in alternative embodiments color control layer(s)
- metal protection layer(s) may be employed in a double-layer structure, such as in Fig. 2, in
- the layer thicknesses in a double-layer structure are the same as for
- the substantially transparent dual-function coating is formed on the surface of the substantially transparent dual-function coating
- a coated article is manufactured by depositing each of the layers of the coating in
- each of the layers is deposited in turn as the substrate travels continuously
- the first anti-reflection layer of dielectric material is deposited by cathodic planar sputtering onto the
- one, two or more sputtering stations can be used to deposit the
- the infrared reflective layer of silver metal is
- the silicon buffer layer is deposited at a subsequent station within the
- the second anti-reflection layer is deposited on a subsequent station.
- the second anti-reflection layer is deposited on a subsequent station.
- the substrate moves continuously through the chamber, such that the individual layers are deposited
- the individual stations are sufficiently isolated by curtains or
- a station can
- Suitable multi-station sputter deposition chambers are
- pilot plant size coaters for example, Model Z600 from Balzers
- such preferred multi-station sputtering chambers employ sputtered targets
- the sputtering chamber is initially evacuated to about 5 x 10 "5 millibar and then
- Tungsten oxide layers are deposited by cathodic sputtering from a pure tungsten
- tungsten target to the substrate is typically about 5 to 15 cm.
- the silver infra-red reflective layer is deposited from a pure silver target in a non-
- the silicon buffer layer is deposited from a silicon target, preferably a doped
- silicon target such as silicon doped with boron, aluminum, etc., at a power level of about
- Another suitable dopant for the silica is nickel metal. Preferably a doping level of 5 parts per million is employed. The throw distance from the silicon
- target to the substrate is typically about 5 to 15 cm.
- tungsten oxide layer is deposited for enhanced performance characteristics.
- tungsten oxide layer is deposited for enhanced performance characteristics.
- the final tungsten oxide layer may
- the exposure time is determined primarily by the speed at which the substrate is
- glass test piece is also coated in the same system.
- the glass substrates were coated and
- the glass panel surface to be coated was washed with demineralized
- the sputtering conditions are provided for each layer of the dual-function
- Tvi s , Rvi s . R' v i s and other performance and color information shown in Tables 1-6 were determined by the "Window 4.0", and Uwinter and Usummer were calculated using the
- Window 4.1 calculation program both publicly available from the USA Department of
- the shading coefficient, sc was calculated as the performance ratio, T vis /T solar , was used to determine the quality of the coatings. The theoretical limit of the T vis /T total solar ratio is 2.15.
- Example 1 - A glass panel was prepared and passed through the multi-station sputtering chamber as described above.
- the multi-functional coating was WO 3 /Ag/Silicon Oxide/WQ , where the first Wp layer (directly on the glass substrate surface) is thicker than the top most WO 3 layer.
- the total thickness of the coating was around 500A.
- a 220 A thick layer of WO x was deposited by sputtering from a Tungsten (W) target at 4.65 Watts/cm 2 in an atmosphere of Argon and Oxygen gasses with the flow ratio of 40 to 53 seem (i.e., with Argon and Oxygen flow rates of 40 seem and 53 seem, respectively) at a vacuum level of 2.3 x 10 "3 mbar.
- a lOOA thick layer of Ag was deposited by sputtering from a Silver (Ag) target at 1.16 Watts/cm 2 in an atmosphere of Argon gas with a flow rate of 50 seem at a vacuum level of 2.2 x 10 "3 mbar.
- a 2 ⁇ A thick layer of Si was deposited by sputtering from a Silicon (Si) target at 0.46 Watts/cm 2 in an atmosphere of Argon gas with the flow rate of 40 seem at a vacuum level of 1.7 x 10 '3 mbar.
- WO x was deposited by sputtering from a Tungsten (W) target at 4.18 Watts/cm 2 in an atmosphere of Argon and Oxygen gasses with a flow rate of 40 to 53 seem at a vacuum level of 2.4 x 10 '3 mbar.
- coated glass panel had good color uniformity. Its spectral properties are shown in Table 1 below, and spectral transmittance properties of the coated panel of Example 1 are shown in the graph of Fig. 4, wherein the horizontal axis shows wavelength and the vertical axis shows level of transmittance. As noted above, coated articles of these examples were characterized by spectrophotometric measurements (Perkin Elmer Lambda 900 UV/VIS/NIR Spectrometer), resistance measurements (signatone four probes Model SYS 301 instrument combined with Keithly Model 224 current source and Model 2000 multimeter), and thickness measurements (Tencor Alpha Step Model 500).
- Spectrophotometric measurements were taken over 350 ran to 2100 nm spectral region, including transmittance T%, reflection R% measured from the coated side, and reflection R' % measured from the glass (uncoated) side.
- R, R' and T spectra and the thicknesses of each individual layer of the coating can be used for library preparation and modeling (Film 2000 modeling program of Kidger Optics). Modeling of the multi-functional layer system can help predict actual deposition, as well as any interface effects the total coating.
- the R, R' and T spectra are shown in the graphs of Figs. 4-7 as three corresponding lines.
- Each of the different lines is identified by legend which includes the three digit number of the "sample code name" (See Table 1 for the sample code name of the coating produced by Example 1 , and the tables associated with the other Examples for the sample code names of those other coatings.) and by the letter “T” for the transmittance spectrum line, the letter R for the reflectance spectrum line of the coated side, and the letters “RR” for the reflectance spectrum line of the opposite, i.e., uncoated side.
- the line indicated as "0412RR.SP” represents the reflectance spectrum measured for the uncoated side of the coated pane of Example 1.
- the line indicated as "0412R.SP” represents the reflectance spectrum measured for the coated side of the coated pane of Example 1.
- the line indicated as "0412T.SP" in Fig. 4 represents the transmittance spectrum.
- the coated panel prepared in accordance with this Example 1 has excellent transmittance of visible light together with low emissivity and good anti-solar properties. In addition, it has excellent mechanical properties, including long shelf life.
- the coating process can be seen from the description here to be fast and economical, so as to be commercially suitable for producing automotive and architectural glazing products. In that regard, the sputter deposition process required only approximately 2.5 minutes.
- DomWL Dominant wavelength
- a*, b*, L* Color coordinates in CIE uniform color space
- SCc Shedding coefficient
- SHGCc Solar heat gain coefficient
- RHG Relative heat gain
- Example 2 A glass panel was prepared and passed through the multi-station sputtering chamber as described above in Example 1 , except that in this example the coating was produced by passing the glass panel twice through the coater. That is, a coating was prepared as in Example 1 described above, and then the glass panel was passed through the sputtering chamber a second time to obtain a double-layer structure coating. The same deposition parameters were maintained during the second pass. Its spectral properties are shown in Table 2 below. Spectral transmittance properties of the coated panel of Example 2 are shown in the graph of Fig. 5. The total thickness of the resultant counting was around lOOOA. TABLE 2
- DomWL Dominant wavelength
- a*, b*, L* Color coordinates in CIE uniform color space
- SCc Shedding coefficient
- SHGCc Solar heat gain coefficient
- RHG Relative heat gain
- the coated panel prepared in accordance with this Example 2 has excellent transmittance of visible light together with low emissivity and good anti-solar properties. It is highly noteworthy that the ratio of visible transmittance to the total energy transmittance (.i.e, the T v /SHGCc value shown in Table 2 for the product of this Example 2 was 2.0. It will be recognized by those skilled in the art that the theoretical maximum for this value is approximately 2.15. That is, it is generally understood that the transmitted percentage of visible light cannot substantially exceed twice the transmitted percentage of total solar energy. Thus, the product of this Example 2, being a preferred embodiment of the present invention, is nearly the limit value. In addition, it has excellent mechanical properties, including long shelf life. Furthermore, the coating process can be seen from the description here to be fast and economical, so as to be commercially suitable for producing automotive and architectural glazing products. In that regard, the sputter deposition process required only approximately 5 minutes.
- Example 3 A glass panel was prepared and passed through the multi-station sputtering chamber as described above for Example 1.
- multi-functional coating was WO 3 /Ag/Silicon Oxide ⁇ VOj where the first WQ layer (i.e., the layer directly on the glass substrate surface) is thinner than the top most WO 3 layer.
- the total thickness of this system was around 40 ⁇ A.
- a 165 A thick layer of WO x was deposited by sputtering from a Tungsten (W) target at 3.83 Watts/cm 2 in an atmosphere of Argon and Oxygen gasses at the flow rate of 40 to 53 seem and a vacuum level of 2.7 x 10 "3 mbar.
- a 125A thick layer of Ag was deposited by sputtering from a Silver (Ag) target at 1.28 Watts/cm 2 in an atmosphere of Argon gas with a flow rate of 50 seem and a vacuum level of 2.2 x 10" 3 mbar.
- a 2 ⁇ A thick layer of Si was deposited by sputtering from a Silicon (Si) target at 0.58 Watts/cm 2 in an atmosphere of Argon gas with the flow rate of 40 seem and a vacuum level of 1.7 x 10 "3 mbar.
- WO x was deposited by sputtering from a Tungsten (W) target at 4.3 Watts/cm 2 in an atmosphere of Argon and Oxygen gasses with the flow rate of 40 to 53 seem, and at vacuum level of 2.4 x 10 "3 mbar.
- the resultant coated glass panel had good color uniformity. Its spectral properties are shown in Table 3 below. Spectral transmittance properties of the coated panel of Example 3 are shown in the graph of Fig. 6.
- DomWL Dominant wavelength
- a*, b*, L* Color coordmates in CIE uniform color space
- SCc Shedding coefficient
- SHGCc Solar heat gam coefficient
- RHG Relative heat gam
- the coated panel prepared in accordance with this Example 3 has excellent transmittance of visible light together with low emissivity and good anti-solar properties. In addition, it has excellent mechanical properties, including long shelf life. Furthermore, the coating process can be seen from the description here to be fast and economical, so as to be commercially suitable for producing automotive and architectural glazing products. In that regard, the sputter deposition process required only approximately 2.5 minutes.
- Example 4 A glass panel was prepared and passed through the multi-station sputtering chamber as described above in Example 3, except that the glass panel was passed through the sputtering chamber a second time to obtain a double-layer structure coating. The same deposition parameters were maintained during the second pass. The resultant coated glass panel had good color uniformity. Its spectral properties are shown in Table 4 below. The total thickness of this the coating was about 80 ⁇ A. Spectral transmittance properties of the coated panel of Example 4 are shown in the graph of Fig. 7.
- DomWL Dominant wavelength
- a*, b*, L* Color coordinates in CIE uniform color space
- SCc Shedding coefficient
- SHGCc Solar heat gain coefficient
- RHG Relative heat gain
- the coated panel prepared in accordance with this Example 4 has excellent transmittance of visible light together with low emissivity and good anti-solar properties. In addition, it has excellent mechanical properties, including long shelf life.
- the coating process can be seen from the description here to be fast and economical, so as to be commercially suitable for producing automotive and architectural glazing products. In that regard, the sputter deposition process required only approximately 5 minutes. This cycle time depends on the number of targets used to deposit WO x anti-reflection films. Thus, using more targets can result in faster cycle times. Typically, the deposition process can be run so as to require only approximately 2.5 minutes cycle time.
- Example 5 A glass panel was prepared and passed through the multi-station sputtering chamber as described above, to deposit a multi-functional coating of WO 3 /AG/Silicon Oxide/WO 3 , where the first WO 3 layer directly on the glass is thicker than the top most WO 3 layer.
- the total thicknesses of the coating was about 93 ⁇ A.
- a 41 ⁇ A thick layer of WO x was deposited by sputtering from a Tungsten (W) target at 4.65 Watts/cm 2 in an atmosphere of Argon and Oxygen gases with a flow rate of 40 to 53 seem at a vacuum level of 2.5 x 10 "3 mbar.
- a 110 A thick layer of Ag was deposited by sputtering from a Silver (Ag) target at 1.16 Watts/cm 2 in an atmosphere of Argon gas with the flow rate of 50 seem at a vacuum level of 2.2 x 10 3 mbar.
- a 20A thick layer of Si was deposited by sputtering from a Silicon (Si) target at 0.46 Watts/cm 2 in an atmosphere of Argon gas with the flow rate of 40 seem at a vacuum level of 1.8 x 10' 3 mbar.
- a 390 A thick layer of WO x was deposited by sputtering from a Tungsten (W) target at 4.18 Watts/cm 2 in an atmosphere of Argon and Oxygen gases with a flow rate of 40 to 53 seem at a vacuum level of 2.5 x 10 "3 mbar.
- DomWL Dominant wavelength
- a*, b*, L* Color coordinates in CIE uniform color space
- SCc Shedding coefficient
- SHGCc Solar heat gain coefficient
- RHG Relative heat gain
- Example 6 A glass panel was prepared and passed through the multi-station sputtering chamber as described above in Example 5, except that the panel was then passed again through the multi-sputtering chamber to produce a double-layer structure coating.
- the total thickness of the resultant coating was about 186 ⁇ A.
- DomWL Dominant wavelength
- a*, b*, L* Color coordinates in CIE uniform color space
- SCc Shedding coefficient
- SHGCc Solar heat gain coefficient
- RHG Relative heat gain
- Example 7 shows the design and optimization procedure of a multifunctional coating system in accordance with the present invention.
- a thin film multi-layer computer program was used, specifically, the Kidger Optics Film 2000 program, and a library was prepared for thin films of Tungsten Oxide, Silver and Silicon deposited by the planar magnetron sputtering process employed in Examples 1-6, above.
- the library of the sputtered materials comprised refractive index and extinction coefficient spectra determined in the spectral region extending from 350 nm to 2100 nm.
- the program calculates and plots the transmittance and reflective spectra of the designed multi-layer system.
- To identify buffer layer properties each individual layer thickness and the total thickness of the coating was measured. The T% and R% spectra of the actual and designed coatings were compared. This comparison predicts the buffer layer thickness comprising 3 A thick Si and 17A thick SiO 2 .
- the second aspect of this example is to show the color and performance control of the multi-functional coated article by changing the thickness of 1) the anti-reflecting oxide film, and 2) the IR reflecting silver film.
- a colorless multi-functional article in accordance with the present invention was prepared having the coating: WO 3 /Ag/Si+SiO 2 /WO 3 with the respective layer thicknesses (in angstroms) of 400/110/3+17/400. Visible T% and R% of the coated glazing system was about 86% and 4%, respectively.
- a 10% increase in Ag thickness (400/122/3+17/40 ⁇ As) improves the T vls /T totai solar ratio from 86/61 to 86/59 without any visible color effects.
- the same 10% thickness increase on WO 3 films does not effect the color appearance of the system. That is, the aforeseaid coating having film thicknesses of 440/110/3+17/360 and 360/110/3+17/440 are still colorless.
- coated articles of manufacture in accordance with the present invention can be prepared which are more or less colorless, depending on the thicknesses of the various films employed to form the coating.
- increasing the thickness of one or more of the anti-reflection oxide layers and/or decreasing the thickness of the silver infra-red reflective layer can be employed to provide a more colorless sample.
- a more color-forming article can be prepared by decreasing the thickness of the anti-reflection layers and increasing the silver layer thickness.
- Additional alternative embodiments of the present invention including those employing WO x and the like can be employed in accordance with the principles disclosed here to provide color-forming or colorless coated articles within the scope of the present invention.
Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP99930264A EP1089948A1 (en) | 1998-06-16 | 1999-06-16 | Anti-solar and low emissivity functioning multi-layer coatings on transparent substrates |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US09/098,316 | 1998-06-16 | ||
US09/098,316 US6040939A (en) | 1998-06-16 | 1998-06-16 | Anti-solar and low emissivity functioning multi-layer coatings on transparent substrates |
Publications (2)
Publication Number | Publication Date |
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WO1999065838A1 WO1999065838A1 (en) | 1999-12-23 |
WO1999065838A9 true WO1999065838A9 (en) | 2000-06-29 |
Family
ID=22268751
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/US1999/013444 WO1999065838A1 (en) | 1998-06-16 | 1999-06-16 | Anti-solar and low emissivity functioning multi-layer coatings on transparent substrates |
Country Status (4)
Country | Link |
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US (1) | US6040939A (en) |
EP (1) | EP1089948A1 (en) |
TR (1) | TR200003691T2 (en) |
WO (1) | WO1999065838A1 (en) |
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-
1999
- 1999-06-16 EP EP99930264A patent/EP1089948A1/en not_active Withdrawn
- 1999-06-16 TR TR2000/03691T patent/TR200003691T2/en unknown
- 1999-06-16 WO PCT/US1999/013444 patent/WO1999065838A1/en not_active Application Discontinuation
Also Published As
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US6040939A (en) | 2000-03-21 |
EP1089948A1 (en) | 2001-04-11 |
TR200003691T2 (en) | 2001-06-21 |
WO1999065838A1 (en) | 1999-12-23 |
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