GB2081136A - Applying Powder Coating Reactants to Glass - Google Patents

Applying Powder Coating Reactants to Glass Download PDF

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Publication number
GB2081136A
GB2081136A GB8124345A GB8124345A GB2081136A GB 2081136 A GB2081136 A GB 2081136A GB 8124345 A GB8124345 A GB 8124345A GB 8124345 A GB8124345 A GB 8124345A GB 2081136 A GB2081136 A GB 2081136A
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United Kingdom
Prior art keywords
reactant
powder
coating
carrier gas
powder coating
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GB8124345A
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GB2081136B (en
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PPG Industries Inc
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PPG Industries Inc
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Filing date
Publication date
Priority claimed from US06/176,323 external-priority patent/US4325988A/en
Priority claimed from US06/176,322 external-priority patent/US4344986A/en
Application filed by PPG Industries Inc filed Critical PPG Industries Inc
Publication of GB2081136A publication Critical patent/GB2081136A/en
Application granted granted Critical
Publication of GB2081136B publication Critical patent/GB2081136B/en
Expired legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05BSPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/14Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas designed for spraying particulate materials
    • B05B7/1481Spray pistols or apparatus for discharging particulate material
    • B05B7/1486Spray pistols or apparatus for discharging particulate material for spraying particulate material in dry state
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/001General methods for coating; Devices therefor
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/001General methods for coating; Devices therefor
    • C03C17/002General methods for coating; Devices therefor for flat glass, e.g. float glass

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

Metal oxide films are coated onto glass by depositing the oxide as a reactant powder, the powder being applied as a turbulent stream in a carrier gas from nozzles (19). The turbulence in the stream is achieved by use of a baffle (17) upstream of the nozzles, the powder being supplied from a hopper (3) using carrier gas (13). <IMAGE>

Description

SPECIFICATION Method of and Apparatus for Applying Powder Coating Reactants This invention relates generally to the art of depositing a coating on a substrate, especially a glass substrate, and relates more particularly to the art of depositing a coating from a powder coating composition.
Various methods of coating glass with metal or metal oxide films are well-known in the art. A technique for depositing a variety of metal oxide films onto a hot glass surface in a continuous float glass ribbon environment is described in U.S. Patent No.3,660,061 to Donley et al. A mixture of organo metallic compounds in organic solution is sprayed onto a glass surface at a temperature high enough for thermal reaction of the organometals to form a metal oxide film. This technique produces durable metal oxide films having desirable aesthetic and solar energy control properties. Although the use of large volumes of solvent results in rapid cooling of the glass, more significant disadvantages are the health, safety and environmental effects.
These disadvantages may be abated by elimination of the organic solvent. A method of solventless chemical vapor deposition of coatings from vaporized powder coating reactants is described in U.S. Patent No. 3,852,098 to Bloss et al. A powder coating reactant is dispersed into a hot stream of gas, vaporized, and conveyed to the surface to be coated, which is maintained at or above the temperature at which the coating reactant pyrolyzes to deposit a film. Although the disadvantages of a solvent system are avoided, vaporization of the coating reactant requires high temperatures, with the possibility of premature reaction of some coating reactants.
Another method of vapor deposition is described in U.S. Patent No. 4,182,783 to Henery, wherein a solid particulate coating reactant is fluidized by introducing a volume of fluidizing gas through a mass of reactant. The fluidized mixture of coating reactant and gas is diluted with an additional volume of gas prior to delivery to the surface of the substrate to be coated. An apparatus for carrying out the technique of fluidizing a bed of solid particulate coating reactant is illustrated in U.S.
Patent No. 4,182,783.
A method which avoids the health, safety and environmental problems of a solvent-based coating method, the high-temperature vaporization risks of a vapor deposition method, and the complexity of a fluidized bed powder coating method is the subject matter of the present invention.
The present invention provides a method of and apparatus for dispersing powder coating reactants in a carrier gas stream and delivering the powder coating composition uniformly to the surface of a substrate to be coated. A powder coating reactant is obtained in very fine particle size and mixed with a carrier gas stream. Turbulence of the mixture is obtained, for example by means of at least one baffle, to maintain uniform distribution of the powder coating reactant in the carrier gas en route to the substrate to be coated. The powder coating reactant is delivered to the surface of the substrate, for example through a nozzle positioned a short distance from the surface to be coated.The length of the nozzle is typically greater than its width, preferably substantially equal to the parallel dimension of the substrate, and is generally disposed perpendicular to the direction of relative motion between the slot and the substrate.
The present invention will now be further described with reference to the accompanying drawings, in which Figs. 1 and 2 illustrate powder spray coating systems according to the present invention.
Referring to the drawings, in which like reference numerals denote like parts, powder coating reactant is fed into the system 1 from a powder store 3 by means of a screw-feed 5. Screw feed 5 is driven by a drive unit 7 mounted on a base 9. A vibrator 11 facilitates the flow of powder.
In the embodiment of the invention depicted in Fig. 1, the powder coating reactant is mixed with air from air supply 1 3 and is passed into a coating chamber 1 5. As the mixture enters coating chamber 15, baffles 1 7 create turbulence which keeps the powder uniformly distributed in the mixture until it is delivered through the slot-shaped nozzles 19 in the form of a spray 21 to the surface to be coated (not shown).
In the embodiment of the invention depicted in Fig. 2, the powder coating reactant is passed through a jet mill 23 and air from air supply 25 is mixed with the powder coating reactant. The jet mill 23 reduces the average particle size of the powder coating reactant to less than about 10 microns to produce a coating reactant with physical properties similar to the properties of dust. The powder coating reactant/air mixture passes from jet mill 23 into a coating chamber 1 5. As the mixture enters coating chamber 15, a cylindrical rod 27 creates turbulence which keeps the powder uniformly distributed in the mixture until it is delivered through the slot-shaped nozzles 19 in the form of a spray 21 to the surface of the substrate (not shown).
The following description is a description of preferred embodiments of the present invention.
A substrate to be coated, preferably a sheet of glass, is maintained in a preferably horizontal position in a coating environment. In a particularly preferred embodiment, the substrate is maintained in an oxidizing atmosphere at a temperature sufficient to pyrolyze a coating reactant to deposit a metal oxide film on the surface of the substrate.
A coating reactant is obtained in the form of a powder, preferably of fairly uniform size distribution of about 500 to 600 microns or less. Coating reactants useful in accordance with the present invention include metal beta diketonates and other organic metal salts, e.g. acetates, hexanoates and formates. Organometallic compounds e.g. alkyl and aryl tin halides. Particularly alkyltin fluorides, may also be used. Halogenated acetonates and acetylacetonates, preferably mixtures of metal acetylacetonates, are preferred.
Preferably acetylacetonate coating reactants are milled and/or sifted to obtain a relatively uniform size distribution. A powder comprising particles having an average diameter of about 500 to 600 microns or less is especially desirable. Such a powder coating reactant has physical properties similar to the properties of flour. The powder coating reactant is mixed with a carrier gas, preferably air, and preferably at ambient temperature. The powder coating reactant may be injected. blown or aspirated into the carrier gas stream. While any means for mixing the powder coating reactant and the carrier gas is suitable, the drawing illustrates a screw-feeder. a preferred means is an aspirator having a vacuum ejector mounted within it.Preferably, the powder/gas mixture passes through a jet mill which effectively reduces the average particle size of the powder coating reactant to a dust-like 1 to 2 microns by means of impingement of the particles and centrifugal air forces created within the jet mill.
The carrier gas may be maintained at any temperature below the decomposition temperature of the coating reactant, preferably below its vaporization temperature, and most preferably ambient temperature, thereby minimizing the risks of coating reactant decomposition which can decrease the efficiency of vapor deposition methods. The distribution of powder coating reactant in the carrier gas is kept substantially uniform en route to the substrate by the creation of turbulence by means of a baffle, such as a cylindrical rod at the entrance of the coating chamber, or a series of baffles, as shown in the drawings.
The uniform mixture of powder coating reactant and carrier gas is delivered to the surface to be coated through a slot-type nozzle, defined for purposes of the present invention as having a length substantially greater than its width. The slot is preferably no more than 1/8 inch (0.32 centimeters) wide, and preferably is as long as the parallel dimension of the surface to be coated to enhance the uniformity of the coating. The slot is preferably disposed perpendicular to the direction of relative motion between the nozzle and the surface to be coated. A large stationary substrate may be coated by using one or more moving nozzles, or the substrate may travel past one or more stationary nozzles.The nozzle is preferably positioned less than 2 inches (about 5.1 centimeters) from the surface to be coated, preferably 1/2 to 3/4 inch (1.2 to 1.9 centimeters), thereby creating a back pressure that promotes uniform flow of the carrier gas/coating reactant mixture along the length of the slot to further enhance the uniformity of the coating.
The carrier gas/coating reactant mixture contacts the surface to be coated to deposit a film.
Preferably, the carrier gas/coating reactant mixture contacts a glass surface at a temperature sufficient to pyrolyze the coating reactant to form a metal oxide film, typically 950 to 1 0500F (about 510 to 5660C). In this environment, the coating reactant/carrier gas mixture may resemble a fog or smoke as it contacts the hot glass surface. Exhaust hoods draw unreacted dust away from the surface. The powder is easily recovered for reuse, thereby optimizing the efficiency of this method.
The thickness of the film may be controlled by varying the rate of relative motion between the nozzle and substrate, by adjusting the flow rate of the carrier gas/coating reactant mixture, by increasing or decreasing the concentration of coating reactant in the carrier gas or by raising or lowering the substrate temperature. The substrate may be coated in either a horizontal or vertical orientation.
The present invention will now be further illustrated by way of the following examples.
Examples 1-IX A freshly formed float glass ribbon travels at a line speed of about 360 inches per minute (about 9.1 meters per minute) past a stationary coating apparatus as shown in Fig. 1 of the drawings. Powder coating reactant having an average particle size of about 500 microns is fed at a rate of 1 50 to 200 grams per minute into a stream of air delivered at a rate of 30 cubic feet (0.85 meter3) per minute.
Turbulence is created in the powder/air mixture by a baffle at the entrance of the coating chamber. The powder/air mixture is delivered through a slot-shaped nozzle 1/1 6 inch (about 1.6 millimeters) wide and substantially as long as the width of the glass ribbon. The nozzles positioned 3/8 inch (about 9.5 millimeters) from the glass surface to provide a back pressure which helps to maintain uniform distribution of the powder coating reactant. The glass surface is at a temperature of about 1 0500F (about 5660C). A uniform metal oxide coating is deposited on the glass surface. The following metal acetylacetonates are successfully used as coating reactants.
Example Metal A cetylacetonate Cobalt II Chromium Ill Iron IV Nickel V Copper VI Copper/Chromium VII Cobalt/lron/Chromium VIII Manganese/Copper IX Iron/Copper/Chromium Example X A coating is prepared as in the previous examples with dibutyltin difluoride as the powder coating reactant. A uniform tin oxide film having a surface resistivity of 8 to 10 ohms per square is formed.
Example Xl A mixture of cobalt, iron and chrnmium acetylacetonates having an average particle size of 500 to 600 microns is prepared by ball mixing of the solid, particular coating reactants for about one hour. The coarse powder mixture is fed into a jet mill which reduces the powder mixture to a fine dust having an average particle size of about one micron or less. The fine dust is conveyed to a coating chamber using 40 pounds (18.14 Kg) of intake air (75 pounds per square inch at 50 cubic feet per minute) (5.27 Kg per square centimeter at 1.42 cubic meters per minute). A dowel-shaped rod at the entrance of the coating chamber causes immediate swirling of the dust/gas smoke. (If the bar is removed, air intake must be nearly doubled, resulting in poor texture of the film and requiring the use of high velocity exhaust hoods).The coating reactant dust is delivered through a slot-shaped nozzle 27 inches (68.7 centimeters) long and 1/8 inch (0.32 centimeters) wide at a rate of about 670 milligrams per second, and contacts a 26 inch (66 centimeter) wide sheet of glass at a rate of about 16.6 feet (5.1 meters) per second. The nozzle is stationary at about 3/4 inch (1.9 centimeters) above the glass surface while the glass ribbon is traveling by at a rate of 250 inches (6.35 meters) per minute at a temperature of about 10500F (about 5660C). A metal oxide coating is formed having durability and spectral properties nearly identical to the properties of a coating formed from a solution of the same coating reactants.
The spectral properties are compared below.
% Transmittance % Reflectance Total Total U-Value Coating Solar Solar Coated Glass Shading Winter Summer Reactant Luminous Energy Energy Surface Surface Coefficient Night Day Powder 23 28 13 35.6 0.47 1.09 1.11 Solution 22 27 31 36.0 14 0.46 1.10 1.11 Example XII The reactant composition, apparatus and operating parameters of the above example are used to deposit a film on a continuous float ribbon of 1/4 inch (6 millimeter) Solarbronze glass. The entire 27 inch (68.6 centimeter) wide area appears uniform in color and texture with a lumonous transmittance of 21 percent and reflectance from the coated side of 37 percent. Since the rod placed at the entrance of the coating chamber allows for low air flow rates, high velocity exhaust hoods are not required; only dust collectors are used to recover undeposited coating reacting.This material may be reused without further processing.
Example XIII The coating reactant composition and operating parameters of the above examples are used in conjunction with a similar powder coating apparatus enlarged to successfully coat a 66 inch (1.7 meter) span of glass. The spectral properties of the coated glass are comparable to the properties recited in Example XII.
Example XIV Dibutyltin difluoride powder coating reactant having an average particle size of about 500 to 600 microns is fed at a rate of 50 grams per minute into a jet mill wherein the particle size is reduced to about 1 to 2 microns. The dibutyltin difluoride dust is carried in air (50 cubic feet per minute at 75 pounds per square inch (1.42 cubic meters per minute at 5.27 Kg per square centimeter) and delivered to a glass surface through stationary double nozzles 12 inches (30.5 centimeters) long and 1/16 inch (1.6 millimeters) wide. The glass is at a temperature of 1100 to 11 600F (about'593 to 6270C) and travelling at a rate of 15 to 20 feet (4.6 to 6.1 meters) per minute. A clear, uniform tin oxide film having a resistivity of 20 ohms per square is formed.
The above examples are offered to illustrate the present inventions, the scope of whiCh is defined by the following claims.

Claims (15)

Claims
1. A method of coating a substrate with a film by contacting a surface of the substrate with a coating reactant, the method comprising: a. obtaining the coating reactant in the form of a powder; b. dispersing said powder coating reactant in a carrier gas stream; c. creating turbulence in said stream; and d. delivering the powder coating reactant/carrier gas mixture to the surface to be coated.
2. A method as claimed in claim 1, wherein the powder coating reactant is created in the carrier gas at ambient temperatures.
3. A method as claimed in claim 1 or claim 2, wherein the carrier gas is air.
4. A method as claimed in any of claims 1 to 3, wherein turbulence is created in the carrier gas/coating reactant stream by means of at least one baffle.
5. A method as claimed in any of claims 1 to 4, wherein the powder coating reactant/carrier gas mixture is delivered to the surface to be coated through a slot-shaped nozzle.
6. A method as claimed in claim 5, wherein the slot-shaped nozzle is not more than 1/8 inch (1.6 millimeters) wide and is substantially as long as the parallel dimension of the surface to be coated.
7. A method as claimed in any of claims 1 to 6, wherein the substrate is contacted with the coating reactant/carrier gas mixture at a temperature sufficient to pyrolyze the coating reactant.
8. A method as claimed in claim 7, wherein a turbulent stream of powder metal acetylacetonate in air is delivered to the surface of a glass substrate to deposit a metal oxide film.
9. A method as claimed in any of claims 1 to 8, wherein the coating powder has an average particle size of about 500 microns.
10. A method as claimed in claim 9, wherein the average particle size of the reactant is reduced to less than about 10 microns.
11. A method as claimed in claim 10, wherein the particle size is reduced by jet milling.
12. A method as claimed in claim 1 and substantially as hereinbefore described with reference to the accompanying drawings.
13. An apparatus for delivering a powder coating reactant to a surface to be coated comprising: a. means for feeding a powder coating reactant into a stream of carrier gas; b. means for creating turbulence in said powder coating reactanticarrier gas stream; and c. means for delivering said turbulent mixture to said surface be coated.
14. An apparatus as claimed in claim 13, which further comprises means for reducing the average particle size of the powder coating reactant.
15. An apparatus as claimed in claim 14, wherein said means for reducing the particle size of the powder coating reactant is a jet mill.
1 6. An apparatus as claimed in claim 13 and substantially as hereinbefore described with reference to the accompanying drawings.
GB8124345A 1980-08-08 1981-08-10 Applying powder coating reactants to glass Expired GB2081136B (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US06/176,323 US4325988A (en) 1980-08-08 1980-08-08 Deposition of coatings from fine powder reactants
US06/176,322 US4344986A (en) 1980-08-08 1980-08-08 Method of delivering powder coating reactants

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GB2081136A true GB2081136A (en) 1982-02-17
GB2081136B GB2081136B (en) 1984-05-02

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DE (1) DE3130098A1 (en)
FR (1) FR2488154B1 (en)
GB (1) GB2081136B (en)
IT (1) IT1138128B (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0095765A2 (en) * 1982-06-01 1983-12-07 Ppg Industries, Inc. Method of and apparatus for applying powder coating reactants
EP0100740A2 (en) * 1982-08-02 1984-02-15 Saint Gobain Vitrage International Powder distribution in view of producing coated glass
FR2542636A1 (en) * 1983-03-14 1984-09-21 Saint Gobain Vitrage METHOD AND DEVICE FOR REGULARLY DISPENSING A PULVERULENT SOLID ON A SUBSTRATE FOR COATING IT AND SUBSTRATE THUS COATED
FR2542637A1 (en) * 1983-03-14 1984-09-21 Saint Gobain Vitrage REGULAR DISTRIBUTION OF A SOLID PULVERULENT ON A SUPPORT FOR COATING IT
EP0125153A2 (en) * 1983-03-14 1984-11-14 Saint Gobain Vitrage International Method and apparatus for evenly applying a powder coating to a substrate, and substrate thus coated
GB2156339A (en) * 1984-03-29 1985-10-09 Pilkington Brothers Plc Apparatus for and method of coating glass
US4808043A (en) * 1983-07-04 1989-02-28 Saint-Gobain Vitrage Apparatus for distribution of gas-entrained powders

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2759772A (en) * 1954-12-15 1956-08-21 Arthur C Hopkins Spray gun
US3478926A (en) * 1968-03-26 1969-11-18 Us Army Apparatus and method for blowing powder
JPS5818333B2 (en) * 1974-07-02 1983-04-12 日本板硝子株式会社 Glass larvae
FR2391966A1 (en) * 1977-05-23 1978-12-22 Saint Gobain Coating glass with metal oxide - to impart antistatic properties, for use in cockpits

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0095765A2 (en) * 1982-06-01 1983-12-07 Ppg Industries, Inc. Method of and apparatus for applying powder coating reactants
EP0095765A3 (en) * 1982-06-01 1984-07-04 Ppg Industries, Inc. Method of and apparatus for applying powder coating reactants
EP0100740A2 (en) * 1982-08-02 1984-02-15 Saint Gobain Vitrage International Powder distribution in view of producing coated glass
EP0100740A3 (en) * 1982-08-02 1984-07-25 Saint-Gobain Vitrage Powder distribution in view of producing coated glass
US5124211A (en) * 1982-08-02 1992-06-23 Saint-Gobain Vitrage Distribution of powder for making coated glass
EP0125153A2 (en) * 1983-03-14 1984-11-14 Saint Gobain Vitrage International Method and apparatus for evenly applying a powder coating to a substrate, and substrate thus coated
FR2542637A1 (en) * 1983-03-14 1984-09-21 Saint Gobain Vitrage REGULAR DISTRIBUTION OF A SOLID PULVERULENT ON A SUPPORT FOR COATING IT
US4533571A (en) * 1983-03-14 1985-08-06 Saint Gobain Vitrage Method and apparatus for uniformly coating a substrate with a powder
EP0125153A3 (en) * 1983-03-14 1985-08-28 Saint-Gobain Vitrage Method and apparatus for evenly applying a powder coating to a substrate, and substrate thus coated
US4562095A (en) * 1983-03-14 1985-12-31 Saint Gobain Vitrage Method and apparatus for manufacturing a uniformly coated substrate
FR2542636A1 (en) * 1983-03-14 1984-09-21 Saint Gobain Vitrage METHOD AND DEVICE FOR REGULARLY DISPENSING A PULVERULENT SOLID ON A SUBSTRATE FOR COATING IT AND SUBSTRATE THUS COATED
US4808043A (en) * 1983-07-04 1989-02-28 Saint-Gobain Vitrage Apparatus for distribution of gas-entrained powders
GB2156339A (en) * 1984-03-29 1985-10-09 Pilkington Brothers Plc Apparatus for and method of coating glass

Also Published As

Publication number Publication date
FR2488154A1 (en) 1982-02-12
DE3130098A1 (en) 1982-05-27
FR2488154B1 (en) 1985-07-26
IT8123311A0 (en) 1981-07-31
GB2081136B (en) 1984-05-02
IT1138128B (en) 1986-09-17

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