US20150213990A1 - Barrier film constructions and methods of making same - Google Patents

Barrier film constructions and methods of making same Download PDF

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US20150213990A1
US20150213990A1 US14/419,352 US201314419352A US2015213990A1 US 20150213990 A1 US20150213990 A1 US 20150213990A1 US 201314419352 A US201314419352 A US 201314419352A US 2015213990 A1 US2015213990 A1 US 2015213990A1
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layer
adhesion
polymer layer
base polymer
oxide
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Joseph C. Spagnola
Mark A. Roehrig
Thomas P. Klun
Alan K. Nachtigal
Christopher S. Lyons
Guy D. Joly
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3M Innovative Properties Co
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3M Innovative Properties Co
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Assigned to 3M INNOVATIVE PROPERTIES COMPANY reassignment 3M INNOVATIVE PROPERTIES COMPANY ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: SPAGNOLA, JOSEPH C., JOLY, GUY D., KLUN, THOMAS P., LYONS, CHISTOPHER S., NACHTIGAL, ALAN K., ROEHRIG, MARK A.
Publication of US20150213990A1 publication Critical patent/US20150213990A1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
    • C08J7/0423—Coating with two or more layers, where at least one layer of a composition contains a polymer binder with at least one layer of inorganic material and at least one layer of a composition containing a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/043—Improving the adhesiveness of the coatings per se, e.g. forming primers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/048—Forming gas barrier coatings
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
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    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
    • H01J1/54—Screens on or from which an image or pattern is formed, picked-up, converted, or stored; Luminescent coatings on vessels
    • H01J1/62—Luminescent screens; Selection of materials for luminescent coatings on vessels
    • H01J1/70—Luminescent screens; Selection of materials for luminescent coatings on vessels with protective, conductive, or reflective layers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
    • C08J2433/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C08J2433/08—Homopolymers or copolymers of acrylic acid esters
    • C—CHEMISTRY; METALLURGY
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    • C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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    • C—CHEMISTRY; METALLURGY
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    • C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
    • C08J2433/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
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    • C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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Definitions

  • the present disclosure relates generally to barrier films and methods of making barrier films.
  • Multilayer stacks of polymers and oxides are deposited in a single pass coating process on flexible polymeric films to make barrier films resistant to moisture permeation.
  • barrier films can be prepared by a variety of production methods, including liquid coating techniques such as solution coating, roll coating, dip coating, spray coating, spin coating; and dry coating techniques such as Chemical Vapor Deposition (CVD), Plasma Enhanced Chemical Vapor Deposition (PECVD), sputtering and vacuum processes for thermal evaporation of solid materials. Examples of such barrier films and processes can be found, for example, in U.S. Pat. No. 5,440,446 (Shaw et al.); U.S. Pat. No.
  • the inventors of the present application sought to develop barrier films with improved weatherability and resistance to inter-layer delamination.
  • a barrier film include a substrate, a base polymer layer adjacent to the substrate, an oxide layer adjacent to the base polymer layer, an adhesion-modifying layer adjacent to the oxide layer; and a top coat polymer layer adjacent to the adhesion-modifying layer.
  • the top coat polymer includes an acrylate.
  • an inorganic layer can be located on the top coat polymer layer.
  • the adhesion-modifying layer is an adhesion-promoting layer. In other embodiments, the adhesion-modifying layer is a release layer.
  • Some embodiments of a process for making barrier films includes the steps of providing a substrate, applying a base polymer layer to the substrate, applying an oxide layer to the base polymer layer, applying a adhesion-modifying layer to the oxide layer; and applying a top coat polymer layer on the adhesion-modifying layer.
  • a separate adhesion-promoting layer provides for enhanced resistance to moisture and improved peel strength adhesion of the top coat layer to the underlying barrier stack layers.
  • a separate release layer provides for application and subsequent removal of a temporary protective layer to one of the oxide layer and polymer layer, creating an improved barrier assembly.
  • the protective layer is applied to the oxide layer to protect the oxide layer during processing. Inclusion of the protective layer during processing reduces defect formation in the oxide layer.
  • the protective layer is subsequently removed from the oxide layer during downstream processing.
  • the exposed oxide layer is immediately protected by application of an adhesive layer and/or a top sheet or protective liner.
  • FIG. 1 is a schematic cross-section showing a barrier film having an adhesion-modifying layer
  • FIG. 2 is a schematic diagram illustrating a process for making a barrier film.
  • adhesion between layers in a multilayer barrier film is insufficient for a desired application.
  • polymer layers e.g., a polyester layer, an acrylate or methacrylate layer
  • polymer layers may not have good adhesion to adjacent oxide layers.
  • Adhesion problems may occur, for example when a sputter process is used for forming oxide layers. In the sputter process, the deposition energy useful for forming a barrier oxide layer is generally high.
  • the energy involved in depositing polymer layers is generally low, and this difference in deposition energy may lead to adhesion problems.
  • a thin sputtered layer e.g., inorganic “tie” layer
  • silicon sub-oxide has been shown to be useful.
  • This inorganic tie layer element can then form chemical bonds to both the substrate layer, an oxide, and the polymeric capping layer.
  • the sputter process for making the inorganic tie layer must be carried out with precise power and gas flow settings to improve adhesion performance. This deposition process has historically been susceptible to noise, which results in varied and low adhesion of the polymer layer.
  • the adhesion between the sub oxide and polymer layer or between adjacent polymer layers has demonstrated weakness when exposed to accelerated aging conditions of 85° C. and 85% relative humidity.
  • defects in the oxide layer may occur during processing. Defects in the oxide layer may lower adhesion between polymer and oxide layers, resulting in an increased susceptibility of water ingress, degradation, and/or delamination of the barrier film from the devices it is intended to protect. A more robust solution for making a barrier film is desirable.
  • the inventors of the present application sought to develop a barrier film with improved weatherability and resistance to inter-layer delamination.
  • the inventors recognized the need to increase adhesion between the layers of the barrier film.
  • the inventors recognized the need to temporarily protect the oxide layer during processing in order to reduce defect formation.
  • FIG. 1 is a schematic cross-section of a barrier film 10 .
  • Film 10 includes layers arranged in the following order: a substrate 12 ; a base polymer layer 14 ; an inorganic layer (e.g., oxide layer) 16 ; a separate adhesion-modifying layer 18 ; a top coat polymer layer 20 ; and an optional inorganic layer 21 .
  • inorganic layer e.g., oxide layer
  • film 10 can include additional alternating layers of polymer and oxide between substrate 10 and top coat polymer layer 20 or inorganic layer 21 .
  • adhesion-modifying layer 18 being positioned between inorganic layer 16 and top coat polymer layer 20 in FIG.
  • the adhesion-modifying layer can be present at any polymer-polymer or polymer-oxide interface.
  • the adhesion-modifying layer may be disposed between the substrate and the base polymer layer, between the base polymer layer and the oxide layer, between the oxide layer and the top coat polymer layer, and/or above the top coat polymer layer.
  • the adhesion-modifying layer 18 is an adhesion-promoting layer, which improves the moisture resistance of film 10 and the peel strength adhesion of the barrier film 10 .
  • the adhesion-modifying layer is a release layer, which may provide for temporary protection of the oxide layer. Exemplary materials for the layers of barrier film 10 are identified below and in the Examples.
  • FIG. 2 is a diagram of a system 22 , illustrating an exemplary process for making barrier film 10 .
  • System 22 is under vacuum and includes a chilled drum 24 for receiving and moving substrate 12 , as represented by a film 26 , providing a moving web.
  • An evaporator 28 applies a base polymer, which is cured by curing unit 30 to form base polymer layer 14 as drum 24 advances the film in a direction shown by arrow 25 .
  • An oxide sputter unit 32 applies an oxide to form inorganic layer 16 as drum 24 advances film 26 .
  • drum 24 can rotate in a reverse direction opposite arrow 25 and then advance film 26 again to apply the additional alternating base polymer and oxide layers, and that sub-process can be repeated for as many alternating layers as desired or needed.
  • drum 24 further advances the film, and an evaporator 34 deposits an adhesion-modifying layer.
  • Drum 24 further advances the film, and an evaporator 36 deposits the top coat polymer layer 20 .
  • Adhesion-modifying layer 18 and top coat polymer layer 20 can be cured separately. Alternatively, adhesion-modifying layer 18 and top coat polymer layer 20 can be cured together by curing unit 38 .
  • Top coat polymer layer 20 can include, for example, a radiation cured monomer (e.g., a (meth)acrylate). The Examples describe in more detail exemplary processes using system 22 to make barrier film 10 .
  • adhesion-modifying layers may be present at any interface, as described above.
  • one or more layers may comprise an adhesion-promoting layer.
  • one or more layers may comprise a release layer.
  • a first layer may comprise an adhesion-promoting layer, while a second layer may comprise a release layer.
  • system 22 may comprise additional evaporators and/or curing units or the location of the existing evaporators/curing units may be altered.
  • drum 24 can rotate in a reverse direction opposite arrow 25 and then advance film 26 again to apply the additional alternating oxide, adhesion-modifying layer, and top polymer layers.
  • This sub-process can be repeated for as many alternating layers as desired or needed.
  • Adhesion-promoting materials often have at least one moiety that is reactive with or capable of non-reactive interaction with at least one adjacent layer.
  • the moieties are reactive and/or capable of non-reactive interaction with both adjacent layers.
  • Exemplary materials for use in the adhesion-promoting layer include, for example, silanes (e.g., silane coupling agents, alkoxy silanes, halo silanes, acetoxy silanes, cyclic aza-silanes, and amino functional silanes), hydroxamic acids, phosphoric acid esters, phosphonic acid esters, phosphonic acids, zirconates, titanates, and the like, all of which may have additional reactive groups such as, for example, (meth) acrylate and epoxy.
  • silanes e.g., silane coupling agents, alkoxy silanes, halo silanes, acetoxy silanes, cyclic aza-silanes, and amino functional silanes
  • hydroxamic acids
  • adhesion-promoting materials include those described in the following copending applications filed the same date as the present application: “Barrier Film, Method of Making the Barrier Film, and Articles Including the Barrier Film” (Attorney Docket No. 70169US002), “Composite Layers Including Urea Acrylate Silanes” (Attorney Docket No. 69821US002), “Composite Layers Including Diurethane Silanes” (Attorney Docket No. 69822US002), and “Composite Layers Including Urea Urethane Acrylate Silanes” (Attorney Docket No. 69823US002), all of which are incorporated herein by reference.
  • the adhesion-promoting layer is a silane coupling agent.
  • a characteristic of this type of material is its ability to react with metal-hydroxyl (metal-OH) groups on a freshly sputter deposited metal oxide layer, such as, for example, a freshly sputtered SiO 2 layer with surface hydroxyl-silanol (Si—OH) groups.
  • metal-OH metal-hydroxyl
  • Si—OH surface hydroxyl-silanol
  • adhesion between the release layer and at least one adjacent layer is low enough to enable the removal of said adjacent layer under appropriate conditions, but not so low that the layers prematurely separate by forces normally encountered in normal handling and processing operations.
  • exemplary materials used in the release layer include silicones, fluorinated materials (e.g., monomers, oligomers, or polymers containing fluoroalkyl or fluoroalkylene or perfluoropolyether moieties), soluble materials, alkyl chains (e.g., straight, branched, and/or cyclic hydrocarbon moieties containing 12-36 carbon atoms), and the like.
  • the films and processes described herein improve the overall adhesion and adhesion retention of vapor deposited multilayer barrier coatings after exposure to moisture by the addition of a separate adhesion-modifying layer.
  • the adhesion-modifying layer is applied in a vapor coating process where the adhesion-modifying layer adsorbs or condenses onto a moving web substrate that has just been sputter coated with an oxide of silicon and aluminum.
  • the adsorbed or condensed layer may then be exposed to subsequent processing steps, for example to curing (e.g., electron beam radiation), additional inorganic layer sputtering, and/or or additional polymer layer deposition.
  • the peel strength adhesion is greatly improved, especially after exposure to high heat and humidity conditions. Additionally, the addition of the adhesion-modifying layer removes the need for a tie layer, which greatly simplifies the coating process and barrier coating stack construction. The resulting barrier coatings retain high barrier properties and optical transmission performance
  • Exemplary polymers for use in the substrate, base polymer layer and/or top coat polymer layer include those listed in U.S. Patent Application Publication No. 2012/0003448 (Weigel et al), incorporated herein by reference in its entirety.
  • the barrier films of the present application may further comprise a top sheet.
  • the top sheet is adhered to the barrier film by means of a pressure sensitive adhesive.
  • Useful materials that can form the top sheet include polyesters, polycarbonates, polyethers, polyimides, polyolefins, fluoropolymers, and combinations thereof. Exemplary materials for use in the top sheet include those listed in U.S. Patent Application Publication No. 2012/0003448 (Weigel et al), incorporated herein by reference in its entirety.
  • the barrier films of the present application are used for encapsulating solar devices.
  • UV light e.g., in a range from 280 to 400 nm
  • the top sheets described herein can provide, for example, a durable, weatherable topcoat for a photovoltaic device.
  • the substrates are generally abrasion and impact resistant and can prevent degradation of, for example, photovoltaic devices when they are exposed to outdoor elements.
  • flexible electronic devices can be encapsulated directly with the methods described herein.
  • the devices can be attached to a flexible carrier substrate, and a mask can be deposited to protect electrical connections from the inorganic layer(s), (co)polymer layer(s), or other layer(s)s during their deposition.
  • the inorganic layer(s), (co)polymeric layer(s), and other layer(s) making up the multilayer barrier assembly can be deposited as described elsewhere in this disclosure, and the mask can then be removed, exposing the electrical connections.
  • the moisture sensitive device is a moisture sensitive electronic device.
  • the moisture sensitive electronic device can be, for example, an organic, inorganic, or hybrid organic/inorganic semiconductor device including, for example, a photovoltaic device such as a copper indium gallium (di)selenide (CIGS) solar cell; a display device such as an organic light emitting display (OLED), electrochromic display, electrophoretic display, or a liquid crystal display (LCD) such as a quantum dot LCD display; an OLED or other electroluminescent solid state lighting device, or combinations thereof and the like.
  • a photovoltaic device such as a copper indium gallium (di)selenide (CIGS) solar cell
  • a display device such as an organic light emitting display (OLED), electrochromic display, electrophoretic display, or a liquid crystal display (LCD) such as a quantum dot LCD display
  • OLED organic light emitting display
  • LCD liquid crystal display
  • the barrier assembly in an article or film can be fabricated by deposition of the various layers onto the substrate, in a roll-to-roll vacuum chamber similar to the system described in U.S. Pat. No. 5,440,446 (Shaw et al.) and U.S. Pat. No. 7,018,713 (Padiyath, et al.).
  • Comparative Laminate Construction A and Laminate Constructions 1-2 were prepared by using a 0.05 mm thick pressure sensitive adhesive (PSA) (obtained under the trade designation “3M OPTICALLY CLEAR ADHESIVE 8172P” from 3M Company, St. Paul, Minn.) to laminate 22.9 cm by 15.2 cm barrier films to an ethylene tetrafluoroethylene polymer sheet (ETFE) (0.05 mm thick, available under the trade designation “NORTON ETFE”, from St. Gobain Performance Plastics, Wayne, N.J.), with the top coat polymer layer of the barrier film adjacent the ETFE sheet.
  • PSA pressure sensitive adhesive
  • ETF ethylene tetrafluoroethylene polymer sheet
  • NORTON ETFE ethylene tetrafluoroethylene polymer sheet
  • Comparative Laminate Construction A and Laminate Constructions 1-2 were prepared using barrier films of, respectively, Comparative Example A, and Examples 1-2.
  • PET polyethylene terephtalate
  • PTFE polytetrafluoroethylene
  • a 13 mm (0.5 in) wide desiccated edge tape (obtained under the trade designation “SOLARGAIN EDGE TAPE SET LP01” from Truseal Technologies Inc., Solon, Ohio) was placed around the perimeter of the PTFE-coated aluminum foil to secure the laminated barrier sheet to the PTFE layer.
  • a 0.38 cm (0.015 in) thick encapsulant film (obtained under the trade designation “JURASOL” from JuraFilms, Downer Grove, Ill.) was placed on the aluminum side of the PTFE-coated aluminum foil.
  • the PET layer of a second laminated barrier sheet identical in composition to the first laminated barrier sheet, was disposed over the encapsulant film, to form a laminate construction. The construction was vacuum laminated at 150° C. for 12 min.
  • Spectral transmission was measured using a spectrometer (model “LAMBDA 900”, commercially available from PerkinElmer, Waltham, Mass.). Spectral transmission is reported as average percent transmission (Tvis) between 400 nm and 700 nm at a 0° angle of incidence.
  • Water vapor transmission rate (WVTR) of the barrier films of Comparative Example A and Examples 1-2 was measured in accordance with the procedure outlined in ASTM F-1249-06, “Standard Test Method for Water Vapor Transmission Rate Through Plastic Film and Sheeting Using a Modulated Infrared Sensor”, using a MOCON PERMATRAN-W® Model 700 WVTR testing system (obtained from MOCON, Inc, Minneapolis, Minn.). Temperature of about 50° C. and relative humidity (RH) of about 100% were used and WVTR is expressed in grams per square meter per day (g/m2/day). The lowest detection limit of the testing system was 0.005 g/m2/day. In some instances, the measured WVTR was below the lowest detection limit and is reported as ⁇ 0.005 g/m2/day.
  • Barrier films were prepared by covering a polyetheylene teraphthalate (PET) substrate film (obtained from E. I. DuPont de Nemours, Wilmington, Del., under the trade name “XST 6642”) with a stack of an base polymer layer, an inorganic silicon aluminum oxide (SiAlOx) barrier layer, and an top coat polymer layer on a vacuum coater similar to the coater described in U.S. Pat. No. 5,440,446 (Shaw et al.) and U.S. Pat. No. 7,018,713 (Padiyath, et al), both of which are incorporated herein by reference.
  • the individual layers were formed as follows:
  • Layer 1 (base polymer layer): a 350 meter long roll of 0.127 mm thick ⁇ 366 mm wide PET film was loaded into a roll-to-roll vacuum processing chamber. The chamber was pumped down to a pressure of 1 ⁇ 10 ⁇ 5 Torn A web speed of 4.8 meter/min was held while maintaining the backside of the PET film in contact with a coating drum chilled to ⁇ 10° C. With the backside in contact with the drum, the film frontside surface was treated with a nitrogen plasma at 0.02 kW of plasma power. The film frontside surface was then coated with tricyclodecane dimethanol diacrylate monomer (obtained under the trade designation “SR-833S”, from Sartomer USA, Exton, Pa.).
  • SR-833S tricyclodecane dimethanol diacrylate monomer
  • the monomer was degassed under vacuum to a pressure of 20 mTorr prior to coating, loaded into a syringe pump, and pumped at a flow rate of 1.33 mL/min through an ultrasonic atomizer operating at a frequency of 60 kHz into a heated vaporization chamber maintained at 260° C.
  • the resulting monomer vapor stream condensed onto the film surface and was electron beam crosslinked using a multi-filament electron-beam cure gun operating at 7.0 kV and 4 mA to form a 720 nm thick base polymer layer.
  • Layer 2 (inorganic layer): immediately after the base polymer layer deposition and with the backside of the PET film still in contact with the drum, a SiAlOx layer was sputter-deposited atop a 23 m length of the base polymer layer.
  • Two alternating current (AC) power supplies were used to control two pairs of cathodes; with each cathode housing two 90% Si/10% Al sputtering targets (obtained from Materion Corporation, Mayfield Heights, Ohio).
  • the voltage signal from each power supply was used as an input for a proportional-integral-differential control loop to maintain a predetermined oxygen flow to each cathode.
  • the AC power supplies sputtered the 90% Si/10% Al targets using 5000 watts of power, with a gas mixture containing 450 standard cubic centimeter per minute (sccm) argon and 63 sccm oxygen at a sputter pressure of 3.5 millitorr. This provided a 30 nm thick SiAlOx layer deposited atop the base polymer layer of Layer 1 .
  • sccm standard cubic centimeter per minute
  • Layer 3 top coat polymer layer: immediately after the SiAlOx layer deposition and with the backside of the PET film still in contact with the drum, the acrylate monomer (same monomer of Layer 1 ) was condensed onto Layer 2 and crosslinked as described in Layer 1 , except that a multi-filament electron-beam cure gun operating at 7 kV and 5 mA was used. This provided a 720 nm thick top coat polymer layer atop Layer 2 .
  • a barrier film was prepared as described in Comparative Example A, with the exception that an adhesion-promoting material was deposited over (i.e., vaporized and condensed) Layer 2 and immediately prior to deposition and condensation of the top coat polymer layer (Layer 3 ). The barrier film was subsequently e-beam crosslinked as described in Comparative Example A.
  • a cyclic azasilane obtained under the trade designation “1932.4”, from Gelest, Morrisville, Pa. was used as adhesion-promoting material.
  • T-peel adhesion, spectral transmission (Tvis) and water vapor transmission rate (WVTR) of the barrier film of Example 1 were measured using the test methods described above.
  • the barrier film was then aged, following the procedure outlined above, for 250 and 500 hours. T-peel adhesion was measured for the aged sample. Results are reported in Table 1, below.
  • a barrier film was prepared as described in Example 1, with the exception that the adhesion-promoting material was (3-acryloxypropyl) trimethoxysilane (obtained under the trade designation “SIA0A200.0” from Gelest).
  • T-peel adhesion, spectral transmission (Tvis) and water vapor transmission rate (WVTR) of the barrier film of Example 2 were measured using the test methods described above.
  • the barrier film was then aged, following the procedure outlined above, for 250 and 500 hours. T-peel adhesion was measured for the aged sample. Results are reported in Table 1, below.
  • the words “on” and “adjacent” cover both a layer being directly on and indirectly on something, with other layers possibly being located therebetween.
  • major surface and “major surfaces” refer to the surface(s) with the largest surface area on a three-dimensional shape having three sets of opposing surfaces.

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US10947618B2 (en) 2021-03-16
US20190180968A1 (en) 2019-06-13
CN104684727A (zh) 2015-06-03
CN104684727B (zh) 2017-05-17
TWI598224B (zh) 2017-09-11
KR20150041062A (ko) 2015-04-15
KR102126719B1 (ko) 2020-06-25
EP2882587A4 (en) 2016-04-13
TW201410455A (zh) 2014-03-16
SG11201500934RA (en) 2015-03-30
EP2882587A1 (en) 2015-06-17
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JP2015530289A (ja) 2015-10-15
JP6316813B2 (ja) 2018-04-25

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