# US 9,752,377 B2 · Nickel-aluminum blocker film controlled transmission coating

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- Number: US 9,752,377 B2
- Document ID: US9752377B2
- Status: Granted
- Kind: B2
- Application number: 14/663,616
- Filed: 2015-03-20
- Published: 2016-09-22
- Granted: 2017-09-05
- Earliest claimed: 2015-03-20
- Assignees: Cardinal CG Company
- Applicants: Cardinal CG Company
- Inventors: Kari B. Myli; Gary L. Pfaff; Daniel J. Plaggemeyer
- Web page: https://patentgrep.com/patent/US9752377B2

## CPC

- E06B 3/6612: {Evacuated glazing units}
- C01F 7/02: Aluminium oxide; Aluminium hydroxide; Aluminates
- C03C 3/087: containing calcium oxide, e.g. common sheet or container glass
- C03C 17/36: at least one coating being a metal
- C03C 17/3613: {Coatings of type glass/inorganic compound/metal/inorganic compound/metal/other}
- C03C 17/3639: {Multilayers containing at least two functional metal layers}
- C03C 17/3642: {the multilayer coating containing a metal layer}
- C03C 17/3644: {the metal being silver}
- C03C 17/366: {Low-emissivity or solar control coatings}
- C03C 17/3689: {one oxide layer being obtained by oxidation of a metallic layer}
- C03C 17/3694: {one layer having a composition gradient through its thickness}
- C23C 14/18: on other inorganic substrates
- C23C 14/35: by application of a magnetic field, e.g. magnetron sputtering {(C23C14/3457 takes precedence)}
- C23C 16/308: {Oxynitrides}
- E06B 3/66: Units comprising two or more parallel glass or like panes permanently secured together {(reforming and uniting glass sheets by fusing C03B23/00; joining glass to glass or to other materials C03C27/00; laminated glass B32B17/10)}
- E06B 3/6715: {specially adapted for increased thermal insulation or for controlled passage of light (E06B3/66323 takes precedence; coating of glass pains C03C17/00; devices or arrangements for controlling the intensity, colour, phase, polarisation or direction of light G02F1/00)}
- E06B 3/822: {with an internal foursided frame}
- C03C 2218/365: Coating different sides of a glass substrate
- E06B 3/66314: {of tubular shape (E06B3/66323 and E06B3/66333 take precedence)}
- E06B 3/7001: {Coverings therefor; Door leaves imitating traditional raised panel doors, e.g. engraved or embossed surfaces, with trim strips applied to the surfaces}
- Y02A 30/249: Glazing, e.g. vacuum glazing
- Y02B 80/22: Glazing, e.g. vaccum glazing
- E06B: FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES (shades or blinds for greenhouses A01G9/22; curtains A47H; lids for car boots or bonnets B62D25/10; skylights E04B7/18; sunshades, awnings E04F10/00)
- C01F: COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; sulfides or polysulfides of magnesium, calcium, strontium, or barium C01B17/42; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds other than ammonia or cyanogen containing nitrogen and non-metals and optionally metals C01B21/082; amides or imides of silicon C01B21/087}; metal {imides or} amides C01B21/092, {C01B21/0923}; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanic acid C01C3/14; salts of cyanamide C01C3/16; thiocyanates C01C3/20; {double sulfates of magnesium with sodium or potassium C01D5/12; with other alkali metals C01D15/00, C01D17/00})
- 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
- 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 (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)
- Y02A: TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02B: CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS

## Abstract

The invention provides a glazing sheet and a low-emissivity coating on the glazing sheet. The low-emissivity coating comprises, in sequence moving outwardly from the glazing sheet, a layer comprising oxide film, nitride film, or oxynitride film, an infrared-reflective layer, a nickel-aluminum blocker layer, and an oxide layer. Also provided are methods of depositing such a low-emissivity coating.

## Claims

### Claim 1

A multiple-pane insulating glazing unit having a between-pane space, the multiple-pane insulating glazing unit comprising a pane having a surface coated with a low-emissivity coating, said surface of said pane being exposed to said between-pane space, the low-emissivity coating comprising, in sequence moving outwardly from said surface of said pane, a dielectric base coat comprising oxide film, nitride film, or oxynitride film, a first infrared-reflective layer, a first nickel-aluminum blocker layer in contact with the first infrared-reflective layer, a dielectric middle coat comprising an oxide film in contact with the first nickel-aluminum blocker layer, a second infrared-reflective layer, a second nickel-aluminum blocker layer in contact with the second infrared-reflective layer, and a dielectric top coat comprising an oxide film in contact with the second nickel-aluminum blocker layer, the first and second infrared-reflective layers each comprising silver, the first and second nickel-aluminum blocker layers deposited in metallic form so as to consist of nickel, aluminum, and titanium as deposited, the first and second nickel-aluminum blocker layers having a combined thickness of from 90 Å to 165 Å, the first and second nickel-aluminum blocker layers each containing less than 30% aluminum by weight, wherein the low-emissivity coating has only two silver-containing infrared-reflective layers and the multiple-pane insulating glazing unit has a visible transmittance of between 0.3 and 0.5, a solar heat gain coefficient in the range of from 0.18 to 0.26, and an exterior reflected color characterized by a chroma magnitude number of less than 7.

### Claim 2 (depends on 1)

The multiple-pane insulating glazing unit of claim 1 wherein the first and second infrared-reflective layers each comprise metallic silver film, and wherein
(i) the first nickel-aluminum blocker layer has an outer interface and an inner interface, the outer interface of the first nickel-aluminum blocker layer adheres to said oxide film of the dielectric middle coat while the inner interface of the first nickel-aluminum blocker layer adheres to the metallic silver film of the first infrared-reflective layer, the outer interface of the first nickel-aluminum blocker layer comprising aluminum oxide, the inner interface of the first nickel-aluminum blocker layer comprising metallic nickel, and
(ii) the second nickel-aluminum blocker layer has an outer interface and an inner interface, the outer interface of the second nickel-aluminum blocker layer adheres to said oxide film of the dielectric top coat while the inner interface of the second nickel-aluminum blocker layer adheres to the metallic silver film of the second infrared-reflective layer, the outer interface of the second nickel-aluminum blocker layer comprising aluminum oxide, the inner interface of the second nickel-aluminum blocker layer comprising metallic nickel.

### Claim 3 (depends on 2)

The multiple-pane insulating glazing unit of claim 2 wherein one of the first and second nickel-aluminum blocker layers is at least 10% thicker than the other of the first and second nickel-aluminum blocker layers, in combination with each of the first and second nickel-aluminum blocker layers having a thickness of between 40 and 90 angstroms.

### Claim 4 (depends on 3)

The multiple-pane insulating glazing unit of claim 3 wherein the first nickel-aluminum blocker layer is more than 10% thicker than the second nickel-aluminum blocker layer.

### Claim 5 (depends on 4)

The multiple-pane insulating glazing unit of claim 4 wherein the first nickel-aluminum blocker layer is between 10% and 30% thicker than the second nickel-aluminum blocker layer.

### Claim 6 (depends on 3)

The multiple-pane insulating glazing unit of claim 3 wherein the second infrared-reflective layer is thicker than the first infrared-reflective layer, the first infrared-reflective layer has a thickness of between 60 and 110 angstroms, the second infrared-reflective layer has a thickness of between 90 and 130 angstroms, and the visible transmittance of the multiple-pane insulating glazing unit is between 0.35 and 0.45.

### Claim 7 (depends on 6)

The multiple-pane insulating glazing unit of claim 6 wherein the dielectric base coat has a total optical thickness of between 500 angstroms and 800 angstroms, the dielectric middle coat has a total optical thickness of between 1,250 angstroms and 1,650 angstroms, and the dielectric top coat has a total optical thickness of between 400 and 800.

### Claim 8 (depends on 7)

The multiple-pane insulating glazing unit of claim 7 wherein the thickness of the first nickel-aluminum blocker layer is between 50 angstroms and 85 angstroms, and the thickness of the second nickel-aluminum blocker layer is between 40 angstroms and 80 angstroms.

### Claim 9 (depends on 1)

The multiple-pane insulating glazing unit of claim 1 wherein the first and second nickel-aluminum blocker layers each contains more than 7.5% aluminum by weight.

### Claim 10 (depends on 1)

The multiple-pane insulating glazing unit of claim 1 wherein the first and second nickel-aluminum blocker layers each contains between 7.5% and 15% aluminum by weight.

### Claim 11 (depends on 1)

The multiple-pane insulating glazing unit of claim 1 wherein said pane is a glass sheet having a thickness in the range of 2 mm to 14 mm.

### Claim 12 (depends on 11)

The multiple-pane insulating glazing unit of claim 11 wherein the glass sheet is soda-lime glass.

### Claim 13 (depends on 1)

The multiple-pane insulating glazing unit of claim 1 wherein the first and second infrared-reflective layers each comprise at least 50% silver by weight.

### Claim 14 (depends on 1)

The multiple-pane insulating glazing unit of claim 1 wherein the multiple-pane insulating glazing unit has two opposed, external pane surfaces at least one of which is coated with a transparent conductive film.

### Claim 15 (depends on 14)

The multiple-pane insulating glazing unit of claim 14 wherein the transparent conductive film comprises both indium and tin.

### Claim 16 (depends on 14)

The multiple-pane insulating glazing unit of claim 14 wherein the two opposed, external pane surfaces are coated respectively with first and second transparent conductive films.

### Claim 17 (depends on 16)

The multiple-pane insulating glazing unit of claim 16 wherein the first transparent conductive film has a different thickness than the second transparent conductive film.

### Claim 18 (depends on 17)

The multiple-pane insulating glazing unit of claim 17 wherein the first transparent conductive film comprises both indium and tin, the second transparent conductive film comprises both indium and tin, wherein the first transparent conductive film has a thickness of from 600 to 900 angstroms, and the second transparent conductive film has a thickness of from 900 to 1,500 angstroms.

### Claim 19 (depends on 16)

The multiple-pane insulating glazing unit of claim 16 further comprising a hydrophilic film over the first transparent conductive film, the hydrophilic film comprising titania.

### Claim 20 (depends on 19)

The multiple-pane insulating glazing unit of claim 19 wherein the hydrophilic film comprising titania has a thickness of from 20 angstroms to 175 angstroms.

### Claim 21

A multiple-pane insulating glazing unit having a between-pane space, the multiple-pane insulating glazing unit including a pane having a surface coated with a low-emissivity coating, said surface of said pane being exposed to said between-pane space, the low-emissivity coating comprising, in sequence moving outwardly from said surface of said pane, a dielectric base coat comprising oxide film, nitride film, or oxynitride film, a first infrared-reflective layer, a first nickel-aluminum blocker layer in contact with the first infrared-reflective layer, a dielectric middle coat comprising an oxide film in contact with the first nickel-aluminum blocker layer, a second infrared-reflective layer, a second nickel-aluminum blocker layer in contact with the second infrared-reflective layer, and a dielectric top coat comprising an oxide film in contact with the second nickel-aluminum blocker layer, the first and second infrared-reflective layers each comprising silver, the first and second nickel-aluminum blocker layers deposited in metallic form so as to consist of nickel, aluminum, and titanium as deposited, the first and second nickel-aluminum blocker layers having a combined thickness of from 90 angstroms to 165 angstroms, the first and second nickel-aluminum blocker layers each containing between 7.5% and 15% aluminum by weight, wherein the low-emissivity coating has only two silver-containing infrared-reflective layers and the multiple-pane insulating glazing unit has a visible transmittance of between 0.3 and 0.5, a solar heat gain coefficient in the range of from 0.18 to 0.26, and an exterior reflected color characterized by a chroma magnitude number of less than 7, and wherein
(i) the first nickel-aluminum blocker layer has an outer interface and an inner interface, the outer interface of the first nickel-aluminum blocker layer adheres to said oxide film of the dielectric middle coat while the inner interface of the first nickel-aluminum blocker layer adheres to the metallic silver film of the first infrared-reflective layer, the outer interface of the first nickel-aluminum blocker layer comprising aluminum oxide, the inner interface of the first nickel-aluminum blocker layer comprising metallic nickel, and
(ii) the second nickel-aluminum blocker layer has an outer interface and an inner interface, the outer interface of the second nickel-aluminum blocker layer adheres to said oxide film of the dielectric top coat while the inner interface of the second nickel-aluminum blocker layer adheres to the metallic silver film of the second infrared-reflective layer, the outer interface of the second nickel-aluminum blocker layer comprising aluminum oxide, the inner interface of the second nickel-aluminum blocker layer comprising metallic nickel.

### Claim 22 (depends on 21)

The multiple-pane insulating glazing unit of claim 21 wherein one of the first and second nickel-aluminum blocker layers is at least 10% thicker than the other of the first and second nickel-aluminum blocker layers, in combination with each of the first and second nickel-aluminum blocker layers having a thickness of between 40 and 90 angstroms.

### Claim 23 (depends on 22)

The multiple-pane insulating glazing unit of claim 22 wherein the first nickel-aluminum blocker layer is more than 10% thicker than the second nickel-aluminum blocker layer.

### Claim 24 (depends on 23)

The multiple-pane insulating glazing unit of claim 23 wherein the first nickel-aluminum blocker layer is between 10% and 30% thicker than the second nickel-aluminum blocker layer.

### Claim 25 (depends on 22)

The multiple-pane insulating glazing unit of claim 22 wherein the second infrared-reflective layer is thicker than the first infrared-reflective layer, the first infrared-reflective layer has a thickness of between 60 and 110 angstroms, the second infrared-reflective layer has a thickness of between 90 and 130 angstroms, and the visible transmittance of the multiple-pane insulating glazing unit is between 0.35 and 0.45.

### Claim 26 (depends on 25)

The multiple-pane insulating glazing unit of claim 25 wherein the dielectric base coat has a total optical thickness of between 500 angstroms and 800 angstroms, the dielectric middle coat has a total optical thickness of between 1,250 angstroms and 1,650 angstroms, and the dielectric top coat has a total optical thickness of between 400 and 800.

### Claim 27 (depends on 26)

The multiple-pane insulating glazing unit of claim 26 wherein the thickness of the first nickel-aluminum blocker layer is between 50 angstroms and 85 angstroms, and the thickness of the second nickel-aluminum blocker layer is between 40 angstroms and 90 angstroms.

### Claim 28 (depends on 1)

The multiple-pane insulating glazing unit of claim 1 wherein the solar heat gain coefficient is less than 0.24.

### Claim 29 (depends on 21)

The multiple-pane insulating glazing unit of claim 21 wherein the solar heat gain coefficient is less than 0.24.
