USRE40531E1 - Ultrabarrier substrates - Google Patents
Ultrabarrier substrates Download PDFInfo
- Publication number
- USRE40531E1 USRE40531E1 US10/890,437 US89043704A USRE40531E US RE40531 E1 USRE40531 E1 US RE40531E1 US 89043704 A US89043704 A US 89043704A US RE40531 E USRE40531 E US RE40531E
- Authority
- US
- United States
- Prior art keywords
- barrier
- barrier assembly
- layers
- assembly
- substrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- 239000000758 substrate Substances 0.000 title claims description 52
- 230000004888 barrier function Effects 0.000 claims abstract description 195
- 229920000642 polymer Polymers 0.000 claims abstract description 53
- 230000005540 biological transmission Effects 0.000 claims abstract description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000001301 oxygen Substances 0.000 claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims description 31
- 229910052751 metal Inorganic materials 0.000 claims description 26
- 239000002184 metal Substances 0.000 claims description 26
- 238000000576 coating method Methods 0.000 claims description 20
- -1 hafnium nitride Chemical class 0.000 claims description 15
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 10
- 230000003678 scratch resistant effect Effects 0.000 claims description 8
- 238000009499 grossing Methods 0.000 claims description 7
- 150000002739 metals Chemical class 0.000 claims description 6
- 150000004767 nitrides Chemical class 0.000 claims description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 5
- 229910044991 metal oxide Inorganic materials 0.000 claims description 5
- 150000004706 metal oxides Chemical class 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000006117 anti-reflective coating Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 3
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 3
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
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- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052582 BN Inorganic materials 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- 229910033181 TiB2 Inorganic materials 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 2
- 229910007948 ZrB2 Inorganic materials 0.000 claims description 2
- CFJRGWXELQQLSA-UHFFFAOYSA-N azanylidyneniobium Chemical compound [Nb]#N CFJRGWXELQQLSA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 claims description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- 229910003437 indium oxide Inorganic materials 0.000 claims description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 2
- 229920005787 opaque polymer Polymers 0.000 claims description 2
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 claims description 2
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 2
- 229910001887 tin oxide Inorganic materials 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- WQJQOUPTWCFRMM-UHFFFAOYSA-N tungsten disilicide Chemical compound [Si]#[W]#[Si] WQJQOUPTWCFRMM-UHFFFAOYSA-N 0.000 claims description 2
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 239000006116 anti-fingerprint coating Substances 0.000 claims 1
- 239000011195 cermet Substances 0.000 claims 1
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- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
- H10K50/8445—Encapsulations multilayered coatings having a repetitive structure, e.g. having multiple organic-inorganic bilayers
-
- 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
- B32B27/00—Layered products comprising a layer of synthetic resin
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/80—Constructional details
- H10K59/87—Passivation; Containers; Encapsulations
- H10K59/873—Encapsulations
- H10K59/8731—Encapsulations multilayered coatings having a repetitive structure, e.g. having multiple organic-inorganic bilayers
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F2201/00—Constructional arrangements not provided for in groups G02F1/00 - G02F7/00
- G02F2201/50—Protective arrangements
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31678—Of metal
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31855—Of addition polymer from unsaturated monomers
Definitions
- the present invention relates generally to barrier coatings, and more particularly to barrier coatings having improved barrier properties.
- environmentally sensitive means products which are subject to degradation caused by permeation of environmental gases or liquids, such as oxygen and water vapor in the atmosphere or chemicals used in the processing, handling, storage, and use of the product.
- Plastics are often used in product packaging.
- the gas and liquid permeation resistance of plastics is poor, often several orders of magnitude below what is required for product performance.
- the oxygen transmission rates for materials such polyethylene terephthalate (PET) are as high as 1550 cc/m 2 /day/micron of thickness (or 8.7 cc/m 2 /day for 7 mil thickness PET), and the water vapor transmission rates are also in this range.
- Certain display applications using environmentally sensitive display devices, such as organic light emitting devices require encapsulation that has a maximum oxygen transmission rate of 10 ⁇ 4 to 10 ⁇ 2 cc/m 2 /day, and a maximum water vapor transmission rate of 10 ⁇ 5 to 10 ⁇ 6 g/m 2 /day.
- Barrier coatings have been applied to plastic substrates to decrease their gas and liquid permeability.
- Barrier coatings typically consist of single layer thin film inorganic materials, such as Al, SiO x , AlO x , an Si 3 N 4 vacuum deposited on polymeric substrates.
- a single layer coating on PET reduces oxygen permeability to levels of about 0.1 to 1.0 cc/m 2 /day, and water vapor permeability to about 0.1 to 1.0 g/m 2 /day, which is insufficient for many display devices.
- U.S. Pat. Nos. 5,607,789 and 5,681,666 disclose a moisture barrier for an electrochemical cell tester. However, the claimed moisture barrier ranges from 2 to 15 micrograms/in 2 /day which corresponds to a rate of 0.003 to 0.023 g/m 2 /day.
- U.S. Pat. No. 5,725,909 to Shaw et al. discloses a coating for packaging materials which has an acrylate layer and an oxygen barrier layer. The oxygen transmission rate for the coating was reported to be 0.1 cc/m 2 /day at 23° C. and the water vapor transmission rate was reported to be 0.01 g/m 2 /day in D. G. Shaw and M. G. Langlois, Society of Vacuum Coaters, 37 th Annual Technical Conference Proceedings, p. 240-244, 1994. The oxygen transmission rates for these coatings are inadequate for many display devices.
- the present invention meets these needs by providing a barrier assembly and a method for making such an assembly.
- the barrier assembly includes at least one barrier stack having at least one barrier layer and at least one polymer layer.
- the barrier stack has an oxygen transmission rate of less than 0.005 cc/m 2 /day at 23° C. and 0% relative humidity, and an oxygen transmission rate of less than 0.005 cc/m 2 /day at 38° C. and 90% relative humidity. It also preferably has a water vapor transmission rate of less than 0.005 g/m 2/ day at 38° C. and 100% relative humidity.
- the barrier layers of the barrier stacks are substantially transparent.
- At least one of the barrier layers preferably comprises a material selected from metal oxides, metal nitrides, metal carbides, metal oxynitrides, metal oxyborides, and combinations thereof.
- the barrier layers can be substantially opaque, if desired.
- the opaque barrier layers are preferably selected from opaque metals, opaque polymers, and opaque ceramics.
- the barrier assembly can include a substrate adjacent to the at least one barrier stack.
- adjacent we mean next to, but not necessarily directly next to. There can be additional layers intervening between the adjacent layers.
- the substrate can either be flexible or rigid. It is preferably made of a flexible substrate material, such as polymers, metals, paper, fabric, and combinations thereof. If a rigid substrate is used, it is preferably a ceramic (including glasses), a metal, or a semiconductor.
- the polymer layers of the barrier stacks are preferably acrylate-containing polymers.
- acrylate-containing polymers includes acrylate-containing polymers, methacrylate-containing polymers, and combinations thereof
- the polymer layers can be the same or different.
- the barrier assembly can include additional layers if desired, such as polymer smoothing layers, scratch resistant layers, antireflective coatings, or other functional layers.
- the present invention also involves a method of making the barrier assembly.
- the method includes providing a substrate, and placing at least one barrier stack on the substrate.
- the barrier stack includes at least one barrier layer and at least one polymer layer.
- the at least one barrier stack can be placed on the substrate by deposition, preferably vacuum deposition, or by laminating the barrier stack over the environmentally sensitive device.
- the lamination can be performed using an adhesive, solder, ultrasonic welding, pressure, or heat.
- FIG. 1 is a cross-section of one embodiment of the barrier assembly of the present invention.
- FIG. 2 is a cross-section of an encapsulated device made using the barrier assembly of the present invention.
- the barrier assembly is supported by a substrate 105 .
- the substrate 105 can be either rigid or flexible.
- a flexible substrate can be any flexible material, including, but not limited to: polymers, for example, polyethylene terephthalate (PET), polyethylene naphthalate (PEN), or high temperature polymers, such as polyether sulfone (PES), polyimides, or TransphanTM (a high glass transition temperature cyclic olefin polymer available from Lofo High Tech Film, GMBH or Weil am Rhein, Germany); metal; paper; fabric; and combinations thereof.
- Rigid substrates are preferably glass, metal, or silicon.
- scratch resistant layers 110 on either side of the substrate 105 to protect it.
- a scratch resistant layer it is preferred that both sides of the substrate have a scratch resistant layer. This helps to balance stresses and prevent deformation of a flexible substrate during processing and use.
- the scratch resistant layer 110 On top of the scratch resistant layer 110 , there is a polymer smoothing layer 115 .
- the polymer smoothing layer decreases surface roughness, and encapsulates surface defects, such as pits, scratches, and digs. This produces a planarized surface which is ideal for subsequent deposition of layers.
- there can be additional layers deposited on the substrate 105 such as organic or inorganic layers, planarizing layers, electrode layers, antireflective coatings, and other functional layers. In this way, the substrate can be specifically tailored to different applications.
- the first barrier stack 120 is adjacent to the polymer smoothing layer 115 .
- the first barrier stack 120 includes a barrier layer 125 and a polymer layer 130 .
- the first barrier layer 125 includes barrier layers 135 and 140 .
- Barrier layers 135 and 140 can be made of the same barrier material or of different barrier materials.
- FIG. 1 shows a barrier stack with two barrier layers and one polymer layer
- the barrier stacks can have one or more polymer layers and one or more barrier layers.
- the important feature is that the barrier stack have at least one polymer layer and at least one barrier layer.
- the barrier layers and polymer layers in the barrier stack can be made of the same material or of a different material.
- the barrier layers are typically about 100-400 ⁇ thick, and the polymer layers are typically about 1000-10,000 ⁇ thick.
- barrier stacks Although only one barrier stack is shown in FIG. 1 , the number of barrier stacks is not limited. The number of barrier stacks needed depends on the substrate material used and the level of permeation resistance needed for the particular application. One or two barrier stacks should provide sufficient barrier properties for some applications. The most stringent applications may require five or more barrier stacks.
- a transparent conductor 145 such as an indium tin oxide layer, adjacent to the first barrier stack 120 .
- a transparent conductor 145 such as an indium tin oxide layer
- additional overcoat layers on top of the barrier stack such as organic or inorganic layers, planarizing layers, transparent conductors, antireflective coatings, or other functional layers, if desired. This allows the barrier assembly to be tailored to the application.
- FIG. 2 shows a barrier assembly being used to encapsulate an environmentally sensitive display device.
- the substrate 205 has an environmentally sensitive display device 210 on it.
- the barrier stack 215 includes a barrier layer 220 and a polymer layer 225 .
- the environmentally sensitive display device 210 can be any display device which is environmentally sensitive.
- environmentally sensitive display devices include, but are not limited to liquid crystal displays (LCDs), light emitting diodes (LEDs), light emitting polymers (LEPs), electronic signage using electrophoretic inks, electroluminescent devices (EDs), and phosphorescent devices.
- LCDs liquid crystal displays
- LEDs light emitting diodes
- LEPs light emitting polymers
- EDs electroluminescent devices
- phosphorescent devices phosphorescent devices.
- These display devices can be made using known techniques, such as those described in U.S. Pat. Nos. 6,025,899, 5,995,191, 5,994,174, 5,956,112 (LCDs); U.S. Pat. Nos. 6,005,692, 5,821,688, 5,747,928 (LEDs); U.S. Pat. Nos.
- a polymer smoothing layer is preferably included to provide a smooth base for the remaining layers. It can be formed by depositing a layer of polymer, for example, an acrylate-containing polymer, onto the substrate or previous layer. The polymer layer can be deposited in vacuum or by using atmospheric processes such as spin coating and/or spraying.
- an acrylate-containing monomer, oligomer, or resin is deposited and then polymerized in situ to form the polymer layer.
- the term acrylate-containing monomer, oligomer, or resin includes acrylate-containing monomers, oligomers, and resins, methacrylate-containing monomers, oligomers, and resins, and combinations thereof.
- the barrier stack is then placed on the substrate.
- the barrier stack includes at least one barrier layer and at least one polymer layer.
- the barrier stacks are preferably made by vacuum deposition.
- the barrier layer can be vacuum deposited onto the polymer smoothing layer, the substrate, or the previous layer.
- the polymer layer is then deposited on the barrier layer, preferably by flash evaporating acrylate-containing monomers, oligomers, or resins, condensing on the barrier layer, and polymerizing in situ in a vacuum chamber.
- U.S. Pat. Nos. 5,440,446 and 5,725,909 which are incorporated herein by reference, describe methods of depositing thin film, barrier stacks.
- Vacuum deposition includes flash evaporation of acrylate-containing monomer, oligomer, or resin with in situ polymerization under vacuum, plasma deposition and polymerization of acrylate-containing monomer, oligomer, or resin, as well as vacuum deposition of the barrier layers by sputtering, chemical vapor deposition, plasma enhanced chemical vapor deposition, evaporation, sublimation, electron cyclotron resonance-plasma enhanced vapor deposition (ECR-PECVD), and combinations thereof.
- ECR-PECVD electron cyclotron resonance-plasma enhanced vapor deposition
- the barrier assembly is preferably manufactured so that the barrier layers are not directly contacted by any equipment, such as rollers in a web coating system, to avoid defects that may be caused by abrasion over a roll or roller. This can be accomplished by designing the deposition system such that the barrier layers are always covered by polymer layers prior to contacting or touching any handling equipment.
- the substrate When the barrier stack is being used to encapsulate an environmentally sensitive display device, the substrate can be prepared as described above, and the environmentally sensitive display device placed on the substrate. Alternatively, the environmentally sensitive display device can be placed directly on a substrate (or on a substrate with functional layers, such as planarizing layers, scratch resistant layers, etc.).
- the environmentally sensitive display device can be placed on the substrate by deposition, such as vacuum deposition. Alternatively it can be placed on the substrate by lamination.
- the lamination can use an adhesive, glue, or the like, or heat to seal the environmentally sensitive display device to the substrate.
- a barrier stack is then placed over the environmentally sensitive display device to encapsulate it.
- the second barrier stack can be placed over the environmentally sensitive display device by deposition or lamination.
- the barrier layers in the first and second barrier stacks may be any barrier material.
- the barrier layers in the first and second barrier stacks can be made of the same material or a different material.
- multiple barrier layers of the same or different barrier materials can be used in a barrier stack.
- the barrier layers can be transparent or opaque, depending on the design of the packaging, and application for which it is to be used.
- Preferred transparent barrier materials include, but are not limited to, metal oxides, metal nitrides, metal carbides, metal oxynitrides, metal oxyborides, and combinations thereof.
- the metal oxides are preferably selected from silicon oxide, aluminum oxide, titanium oxide, indium oxide, tin oxide, indium tin oxide, tantalum oxide, zirconium oxide, niobium oxide, and combinations thereof.
- the metal nitrides are preferably selected from aluminum nitride, silicon nitride, boron nitride, and combinations thereof.
- the metal oxynitrides are preferably selected from aluminum oxynitride, silicon oxynitride, boron oxynitride, and combinations thereof.
- Opaque barrier layers can be also be used in some barrier stacks.
- Opaque barrier materials include, but are not limited to, metals, ceramics, polymers, and cermets.
- opaque cermets include, but are not limited to, zirconium nitride, titanium nitride, hafnium nitride, tantalum nitride, niobium nitride, tungsten disilicide, titanium diboride, and zirconium diboride.
- the polymer layers of the first and second barrier stacks are preferably acrylate-containing monomers, oligomers, or resins.
- the polymer layers in the first and second barrier stacks can be the same or different.
- the polymer layers within each barrier stack can be the same or different.
- the barrier stack includes a polymer layer and two barrier layers.
- the two barrier layers can be made from the same barrier material or from different barrier materials.
- the thickness of each barrier layer in this embodiment is about one half the thickness of the single barrier layer, or about 50 to 200 ⁇ . There are no limitations on the thickness, however.
- the barrier layers When the barrier layers are made of the same material, they can be deposited either by sequential deposition using two sources or by the same source using two passes. If two deposition sources are used, deposition conditions can be different for each source, leading to differences in microstructure and defect dimensions. Any type of deposition source can be used. Different types of deposition processes, such as magnetron sputtering and electron beam evaporation, can be used to deposit the two barrier layers.
- the microstructures of the two barrier layers are mismatched as a result of the differing deposition sources/parameters.
- the barrier layers can even have different crystal structure.
- Al 2 O 3 can exist in different phases (alpha, gamma) with different crystal orientations.
- the mismatched microstructure can help decouple defects in the adjacent barrier layers, enhancing the tortuous path for gases and water vapor permeation.
- two deposition sources are needed. This can be accomplished by a variety of techniques. For example, if the materials are deposited by sputtering, sputtering targets of different compositions could be used to obtain thin films of different compositions. Alternatively, two sputtering targets of the same composition could be used but with different reactive gases. Two different types of deposition sources could also be used. In this arrangement, the lattices of the two layers are even more mismatched by the different microstructures and lattice parameters of the two materials.
- a single pass, roll-to-roll, vacuum deposition of a three layer combination on a PET substrate i.e., PET substrate/polymer layer/barrier layer/polymer layer
- PET substrate/polymer layer/barrier layer/polymer layer can be more than five orders of magnitude less permeable to oxygen and water vapor than a single oxide layer on PET alone.
- permeation rates in the roll-to-roll coated oxide-only layers were found to be conductance limited by defects in the oxide layer that arose during deposition and when the coated substrate was wound up over system idlers/rollers. Asperities (high points) in the underlying substrate are replicated in the deposited inorganic barrier layer. These features are subject to mechanical damage during web handling/take-up, and can lead to the formation of defects in the deposited film. These defects seriously limit the ultimate barrier performance of the films.
- the first acrylic layer planarizes the substrate and provides an ideal surface for subsequent deposition of the inorganic barrier thin film.
- the second polymer layer provides a robust “protective” film that minimizes damage to the barrier layer and also planarizes the structure for subsequent barrier layer (or environmentally sensitive display device) deposition.
- the intermediate polymer layers also decouple defects that exist in adjacent inorganic barrier layers, thus creating a tortuous path for gas diffusion.
- the permeability of the barrier stacks used in the present invention is shown in Table 1.
- the barrier stacks of the present invention on polymeric substrates, such as PET, have measured oxygen transmission rate (OTR) and water vapor transmission rate (WVTR) values well below the detection limits of current industrial instrumentation used for permeation measurements (Mocon OxTran 2/20L and Permatran).
- Table 1 shows the OTR and WVTR values (measured according to ASTM F 1927-98 and ASTM F 1249-90, respectively) measured at Mocon (Minneapolis, Minn.) for several barrier stacks on 7 mil PET, along with reported values for other materials.
- the barrier stacks of the present invention provide oxygen and water vapor permeation rates several orders of magnitude better than PET coated with aluminum, silicon oxide, or aluminum oxide.
- Typical oxygen permeation rates for other barrier coatings range from 1 to about 0.1 cc/m 2 /day.
- the oxygen transmission rate for the barrier stacks of the present invention is less than 0.005 cc/m 2 /day at 23° C. and 0% relative humidity, and at 38° C. and 90% relative humidity.
- the water vapor transmission rate is less than 0.005 g/m 2 /day at 38° C. and 100% relative humidity. The actual transmission rates are lower, but cannot be measured with existing equipment.
- the barrier assemblies were also tested by encapsulating organic light emitting devices using the barrier stacks of the present invention.
- the organic light emitting devices are extremely sensitive to water vapor, and they are completely destroyed in the presence of micromole quantities of water vapor.
- Experimentation and calculations suggest that the water vapor transmission rate through the encapsulation film must be on the order of about 10 ⁇ 6 to 10 ⁇ 5 g/m 2 /day to provide sufficient barrier protection for acceptable device lifetimes.
- the experiments/calculations are based on the detrimental hydrolysis reaction of water vapor with the extremely thin (less than 10 nm), low work function, cathode materials (Ca, Mg, Li, LiF). Hydrolysis of the cathode leads to the formation of non-conductive reaction products (such as hydroxides and oxides) that delaminate or blister away from the electron transport layers of the organic light emitting devices, resulting in the formation of dark spots on the device.
- non-conductive reaction products such as hydroxides and oxides
- the organic light emitting devices encapsulated in the barrier stacks of the present invention have been in operation for over six months and without measurable degradation.
- the extrapolated lifetime for the encapsulated devices exceeds the required 10,000 hours necessary to satisfy industry standards.
- the barrier stacks are extremely effective in preventing oxygen and water penetration to the underlying components, substantially outperforming other thin-film barrier coatings on the market.
- the preferred deposition process is compatible with a wide variety of substrates. Because the preferred process involves flash evaporation of a monomer and magnetron sputtering, deposition temperatures are well below 100° C., and stresses in the coating can be minimized. Multilayer coatings can be deposited at high deposition rates. No harsh gases or chemicals are used, and the process can be scaled up to large substrates and wide webs.
- the barrier properties of the coating can be tailored to the application by controlling the number of layers, the materials, and the layer design.
- the present invention provides a barrier stack with the exceptional barrier properties necessary for hermetic sealing of an environmentally sensitive display device, or other environmentally sensitive device. It permits the production of an encapsulated environmentally sensitive display device.
Abstract
Description
TABLE 1 | |||||
Oxygen | Water Vapor | ||||
Permeation Rate | Permeation | ||||
(cc/m2/day) | (g/m2/day)* | ||||
Sample | 23° C. | 38° C. | 23° C. | 38° C. | |
Native 7 mil PET | 7.62 | — | — | — | ||
1-barrier stack | <0.005 | <0.005* | — | 0.46* | ||
1-barrier stack | <0.005 | <0.005* | — | 0.011* | ||
with ITO | ||||||
2-barrier stacks | <0.005 | <0.005* | — | <0.005* | ||
2-barrier stacks | <0.005 | <0.005* | — | <0.005* | ||
with ITO | ||||||
5-barrier stacks | <0.005 | <0.005* | — | <0.005* | ||
5-barrier stacks | <0.005 | <0.005* | — | <0.005* | ||
with ITO | ||||||
DuPont film1 | 0.3 | — | — | — | ||
(PET/Si3N4 or | ||||||
PEN/Si3N4) | ||||||
Polaroid3 | <1.0 | — | — | — | ||
PET/Al2 | 0.6 | — | 0.17 | — | ||
PET/silicon | 0.7-1.5 | — | 0.15-0.9 | — | ||
oxide2 | ||||||
Teijin LCD film | <2 | — | <5 | — | ||
(HA grade- | ||||||
TN/STN)3 | ||||||
*38° C., 90% RH, 100% O2 | ||||||
*38° C., 100% RH | ||||||
1P. F. Carcia, 46th International Symposium of the American Vacuum Society, October 1999 | ||||||
2Langowski, H. C., 39th Annual Technical Conference Proceedings, SVC, pp. 398-401 (1996) | ||||||
3Technical Data Sheet |
Claims (25)
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US09/427,138 US6522067B1 (en) | 1998-12-16 | 1999-10-25 | Environmental barrier material for organic light emitting device and method of making |
US09/553,188 US6413645B1 (en) | 2000-04-20 | 2000-04-20 | Ultrabarrier substrates |
US10/890,437 USRE40531E1 (en) | 1999-10-25 | 2004-07-12 | Ultrabarrier substrates |
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US09/553,188 Reissue US6413645B1 (en) | 1999-10-25 | 2000-04-20 | Ultrabarrier substrates |
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USRE40531E1 true USRE40531E1 (en) | 2008-10-07 |
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US6413645B1 (en) | 2002-07-02 |
WO2001081649A1 (en) | 2001-11-01 |
AU2001241893A1 (en) | 2001-11-07 |
TW575671B (en) | 2004-02-11 |
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