CN117301589A - Preparation method of high barrier film for flexible display - Google Patents

Preparation method of high barrier film for flexible display Download PDF

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Publication number
CN117301589A
CN117301589A CN202311445139.2A CN202311445139A CN117301589A CN 117301589 A CN117301589 A CN 117301589A CN 202311445139 A CN202311445139 A CN 202311445139A CN 117301589 A CN117301589 A CN 117301589A
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Prior art keywords
barrier film
flexible display
coating
substrate
oxide
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CN202311445139.2A
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Chinese (zh)
Inventor
辜勇
方元
邹云
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Jiangsu Sile Technology Co ltd
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Jiangsu Sile Technology Co ltd
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Priority to CN202311445139.2A priority Critical patent/CN117301589A/en
Publication of CN117301589A publication Critical patent/CN117301589A/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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D7/00—Producing flat articles, e.g. films or sheets
    • B29D7/01—Films or sheets
    • 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
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin 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
    • 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
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
    • 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
    • B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
    • 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
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • 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
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • 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
    • B32B2255/00—Coating on the layer surface
    • B32B2255/10—Coating on the layer surface on synthetic resin layer or on natural or synthetic rubber layer
    • 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
    • B32B2255/00—Coating on the layer surface
    • B32B2255/20—Inorganic coating
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/546—Flexural strength; Flexion stiffness
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/554—Wear resistance

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention relates to a preparation method of a high barrier film for flexible display, which comprises the following steps: s1, performing heat treatment on a barrier film substrate until shrinkage rates in the TD and MD directions are less than 0.5%; s2, hydroxylating the surface of one side of the barrier film substrate, then sending the barrier film substrate into ALD deposition equipment, carrying a metal oxide precursor by inert gas in a vacuum environment, and alternately growing a metal oxide film by reacting the metal oxide precursor with pure water carried by the inert gas to form a barrier layer; and S3, coating OCA optical cement on the other side surface of the barrier film substrate, and bonding the PET substrate with the AG coating. An OCA gel with UV cut-off and an AG PET with anti-glare and friction resistance were compounded on the barrier film substrate. By combining the characteristics, the product is enough to meet the flexible packaging requirements of OLED (organic light emitting semiconductor), QLED (quantum dot light emitting semiconductor), EPD (electronic paper) and the like.

Description

Preparation method of high barrier film for flexible display
Technical Field
The invention belongs to the technical field of new flexible film materials, and particularly relates to a preparation method of a high barrier film for flexible display.
Background
The water-oxygen barrier film is a core material of flexible packaging of OLED (organic light-emitting semiconductor), QLED (quantum dot light-emitting semiconductor), EPD (electronic paper) and OPV (organic thin film solar cell), and is mainly used for isolating the damage of water vapor and oxygen to organic light-emitting materials, quantum dots and organic light-emitting elements, and is a key factor for limiting the service life of the device. The same water-oxygen isolation effect of the glass package of the inflexible device can be achieved.
At present, most of high-efficiency water-oxygen barrier films in the market adopt preparation technologies including evaporation, sputtering and chemical deposition, wherein the film layer prepared by the evaporation mode is poor in density, low in barrier performance and difficult to meet the high-efficiency water blocking requirement; the density of the sputtering mode is slightly lower than that of chemical vapor deposition, a flat layer is needed to be made on the substrate before coating, and the barrier property can reach-10 < -2 > g/m 2 24h level; the chemical vapor deposition mode has higher density, a flat layer is also required to be made on the substrate during the deposition of the coating film, and the barrier property can reach-10 < -3 > g/m 2 The level 24h, poor bending resistance and slightly higher cost.
At present, with regard to a high barrier film for flexible display, it is reported that sputtering and chemical vapor deposition are mostly adopted, and the two modes have the defects that a substrate needs to be precoated with a flat layer and the like, which undoubtedly increases the production cost, and has the thickness of a coating film and poor flexibility, on the other hand, the density of the film layer is not the best no matter the sputtering and the chemical vapor deposition, and the extremely high barrier performance cannot be achieved in the aspect of barrier performance. In order to improve the service life of the organic light-emitting display product, the flexibility of the end product and the cost requirement on the protective material are lower, an industrialized production method with higher barrier property, better flexibility, lower cost and more convenient production needs to be developed.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention aims to provide the preparation method of the high-efficiency barrier film for the flexible display, which is characterized in that an atomic layer deposition mode is directly adopted on a PET substrate to plate an aluminum oxide film and a zinc oxide film which are alternately combined, the film coating compactness is high, the film coating coverage is strong, a flat layer is not needed, the film layer flexibility is good, and the barrier performance is high.
The aim of the invention can be achieved by the following technical scheme:
a preparation method of a high barrier film for flexible display comprises the following steps:
s1, performing heat treatment on a barrier film substrate until shrinkage rates in the TD and MD directions are less than 0.5%;
s2, hydroxylating the surface of one side of the barrier film substrate, then sending the barrier film substrate into ALD deposition equipment, carrying a metal oxide precursor by inert gas in a vacuum environment, and alternately growing a metal oxide film by reacting the metal oxide precursor with pure water carried by the inert gas to form a barrier layer;
and S3, coating OCA optical cement on the other side surface of the barrier film substrate, and bonding the PET substrate with the AG coating.
Further, the barrier film base material is a PET (polyethylene terephthalate) film, a PP (polypropylene) film or a PI (polyimide) film.
Further, the corona treatment in step S2 is corona, precoating or plasma treatment.
Further, the inert gas in step S2 is nitrogen, argon or helium.
Further, the metal oxide film is formed by stacking one or more of magnesium oxide, zinc oxide, zirconium oxide, titanium oxide, manganese oxide, aluminum oxide, hafnium oxide, iron oxide and calcium oxide according to any proportion.
Further, in the step S2, the refractive index of the barrier layer is between 1.60 and 1.8, the overall thickness of the barrier layer film layer is controlled to be 10nm-100nm, the barrier property of a film coating finished product is less than or equal to 8E-3 g/m2.24h, and the visible light transmittance is more than 88%.
Further, the UV cut-off of the OCA optical adhesive in the step S3 is required to be at the wavelength of 280-380nm, the average transmittance cut-off is less than 1%, and the bonding strength of the OCA optical adhesive to a barrier film substrate is more than or equal to 1.2kg/2.5cm.
Further, in step S3, AG coating is adhered to one surface of the PET substrate with AG coating, and the other surface is adhered to the barrier film substrate by OCA optical adhesive.
Further, the PET substrate with AG coating has a thickness of 50-180 μm, AG coating has a thickness of 2-20 μm, surface hardness > 3H, and haze is required to be 2-20.
The invention has the beneficial effects that:
in view of the full coverage characteristic of the ALD technology, a flattening layer is not needed on the substrate, the process is simple, and the cost is lower than that of other methods. And the film layer is fully covered and has stronger compactness, and the barrier property is more excellent. The thickness of the film layer can be thinner, and the bending resistance is better. An OCA gel with UV cut-off and an AG PET with anti-glare and friction resistance were compounded on the barrier film substrate. By combining the characteristics, the product is enough to meet the flexible packaging requirements of OLED (organic light emitting semiconductor), QLED (quantum dot light emitting semiconductor), EPD (electronic paper) and the like.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic view of the structure of a high barrier film according to the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A preparation method of a high barrier film for flexible display comprises the following steps:
s1, performing heat treatment on a barrier film substrate until shrinkage rates in the TD and MD directions are less than 0.5%;
s2, hydroxylating the surface of one side of the barrier film substrate, then sending the barrier film substrate into ALD deposition equipment, carrying a metal oxide precursor by inert gas in a vacuum environment, and alternately growing a metal oxide film by reacting the metal oxide precursor with pure water carried by the inert gas to form a barrier layer;
and S3, coating OCA optical cement on the other side surface of the barrier film substrate, and bonding the PET substrate with the AG coating.
The barrier film base material is PET polyester film.
The corona treatment in step S2 is corona.
The inert gas in the step S2 is nitrogen.
The metal oxide thin film is magnesium oxide.
In the step S2, the refractive index of the barrier layer is between 1.60 and 1.8, the overall thickness of the barrier layer film layer is controlled to be 10nm, and the barrier property of a coated finished product is less than or equal to 8E-3g/m 2 24 hours, the visible light transmittance is more than 88%.
The UV cut-off of the OCA optical adhesive in the step S3 is required to be at the wavelength of 280nm, the average transmittance cut-off is less than 1%, and the bonding strength of the OCA optical adhesive to a barrier film substrate is more than or equal to 1.2kg/2.5cm.
And in the step S3, the AG coating is adhered to one side surface of the PET substrate with the AG coating, and the other side surface is adhered to the barrier film substrate through OCA optical cement.
The PET substrate with AG coating has the thickness of 50 mu m, AG coating has the thickness of 2 mu m, surface hardness of more than 3H and haze of 2.
Example 2
A preparation method of a high barrier film for flexible display comprises the following steps:
s1, performing heat treatment on a barrier film substrate until shrinkage rates in the TD and MD directions are less than 0.5%;
s2, hydroxylating the surface of one side of the barrier film substrate, then sending the barrier film substrate into ALD deposition equipment, carrying a metal oxide precursor by inert gas in a vacuum environment, and alternately growing a metal oxide film by reacting the metal oxide precursor with pure water carried by the inert gas to form a barrier layer;
and S3, coating OCA optical cement on the other side surface of the barrier film substrate, and bonding the PET substrate with the AG coating.
The barrier film base material is a PET (polyethylene terephthalate) film, a PP (polypropylene) film or a PI (polyimide) film.
The corona treatment in step S2 is corona, precoating or plasma treatment.
The inert gas in the step S2 is nitrogen, argon or helium.
The metal oxide film is formed by stacking one or more of magnesium oxide, zinc oxide, zirconium oxide, titanium oxide, manganese oxide, aluminum oxide, hafnium oxide, iron oxide and calcium oxide according to any proportion.
In the step S2, the refractive index of the barrier layer is between 1.60 and 1.8, the overall thickness of the barrier layer film layer is controlled to be 150nm, and the barrier property of a coated finished product is less than or equal to 8E-3g/m 2 24 hours, the visible light transmittance is more than 88%.
The UV cut-off of the OCA optical adhesive in the step S3 is required to be at 320nm wavelength, the average transmittance cut-off is less than 1%, and the bonding strength of the OCA optical adhesive to a barrier film substrate is more than or equal to 1.2kg/2.5cm.
And in the step S3, the AG coating is adhered to one side surface of the PET substrate with the AG coating, and the other side surface is adhered to the barrier film substrate through OCA optical cement.
The PET substrate with AG coating has the thickness of 100 mu m, AG coating has the thickness of 10 mu m, surface hardness of more than 3H and haze of 10.
Example 3
A preparation method of a high barrier film for flexible display comprises the following steps:
s1, performing heat treatment on a barrier film substrate until shrinkage rates in the TD and MD directions are less than 0.5%;
s2, hydroxylating the surface of one side of the barrier film substrate, then sending the barrier film substrate into ALD deposition equipment, carrying a metal oxide precursor by inert gas in a vacuum environment, and alternately growing a metal oxide film by reacting the metal oxide precursor with pure water carried by the inert gas to form a barrier layer;
and S3, coating OCA optical cement on the other side surface of the barrier film substrate, and bonding the PET substrate with the AG coating.
The barrier film base material is a PET (polyethylene terephthalate) film, a PP (polypropylene) film or a PI (polyimide) film.
The corona treatment in step S2 is corona, precoating or plasma treatment.
The inert gas in the step S2 is nitrogen, argon or helium.
The metal oxide film is formed by stacking one or more of magnesium oxide, zinc oxide, zirconium oxide, titanium oxide, manganese oxide, aluminum oxide, hafnium oxide, iron oxide and calcium oxide according to any proportion.
In the step S2, the refractive index of the barrier layer is between 1.60 and 1.8, the whole thickness of the barrier layer film layer is controlled to be 100nm, and the barrier property of a coated finished product is less than or equal to 8E-3g/m 2 24 hours, the visible light transmittance is more than 88%.
The UV cut-off requirement of the OCA optical adhesive in the step S3 is that the average transmittance cut-off rate is less than 1% at 380nm wavelength, and the bonding strength of the OCA optical adhesive to a barrier film substrate is more than or equal to 1.2kg/2.5cm.
And in the step S3, the AG coating is adhered to one side surface of the PET substrate with the AG coating, and the other side surface is adhered to the barrier film substrate through OCA optical cement.
The PET substrate with AG coating has a thickness of 180 mu m, AG coating has a thickness of 2-20 mu m, surface hardness is more than 3H, and haze is required to be 20.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.

Claims (9)

1. The preparation method of the high barrier film for the flexible display is characterized by comprising the following steps of:
s1, performing heat treatment on a barrier film substrate until shrinkage rates in the TD and MD directions are less than 0.5%;
s2, hydroxylating the surface of one side of the barrier film substrate, then sending the barrier film substrate into ALD deposition equipment, carrying a metal oxide precursor by inert gas in a vacuum environment, and alternately growing a metal oxide film by reacting the metal oxide precursor with pure water carried by the inert gas to form a barrier layer;
and S3, coating OCA optical cement on the other side surface of the barrier film substrate, and bonding the PET substrate with the AG coating.
2. The method for preparing the high barrier film for flexible display according to claim 1, wherein the barrier film substrate is a PET polyester film, a PP polypropylene film or a PI polyimide film.
3. The method for producing a high barrier film for flexible display according to claim 1, wherein the corona treatment in step S2 is corona, precoating or plasma treatment.
4. The method for producing a high barrier film for flexible display according to claim 1, wherein the inert gas in step S2 is nitrogen, argon or helium.
5. The method for producing a high barrier film for flexible display according to claim 1, wherein one or more of magnesium oxide, zinc oxide, zirconium oxide, titanium oxide, manganese oxide, aluminum oxide, hafnium oxide, iron oxide and calcium oxide are stacked in an arbitrary ratio.
6. The method for preparing the high barrier film for flexible display according to claim 1, wherein in the step S2, the refractive index of the barrier layer is between 1.60 and 1.8, the whole thickness of the barrier layer film layer is controlled to be between 10nm and 100nm, and the barrier property of a coated finished product is less than or equal to 8E-3g/m 2 24 hours, the visible light transmittance is more than 88%.
7. The method for preparing a high barrier film for flexible display according to claim 1, wherein the UV cut-off of the OCA optical adhesive in step S3 is required to be in a wavelength of 280-380nm, the average transmittance cut-off is less than 1%, and the adhesive strength to the barrier film substrate is not less than 1.2kg/2.5cm.
8. The method for preparing a high barrier film for flexible display according to claim 1, wherein in the step S3, the AG coating is adhered to one surface of the PET substrate with AG coating, and the other surface is adhered to the barrier film substrate by OCA optical adhesive.
9. The method for preparing the high barrier film for flexible display according to claim 8, wherein the PET substrate with AG coating has a thickness of 50-180 μm, AG coating has a thickness of 2-20 μm, surface hardness > 3H, and haze requirement of 2-20.
CN202311445139.2A 2023-11-02 2023-11-02 Preparation method of high barrier film for flexible display Pending CN117301589A (en)

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