CN110591471B - Pre-coating liquid for enhancing surface adhesion of transparent PI (polyimide) substrate and application method thereof - Google Patents
Pre-coating liquid for enhancing surface adhesion of transparent PI (polyimide) substrate and application method thereof Download PDFInfo
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- CN110591471B CN110591471B CN201910924826.XA CN201910924826A CN110591471B CN 110591471 B CN110591471 B CN 110591471B CN 201910924826 A CN201910924826 A CN 201910924826A CN 110591471 B CN110591471 B CN 110591471B
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- 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
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D129/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
- C09D129/02—Homopolymers or copolymers of unsaturated alcohols
- C09D129/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/08—Homopolymers or copolymers of acrylic acid esters
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/18—Homopolymers or copolymers of nitriles
- C09D133/20—Homopolymers or copolymers of acrylonitrile
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/24—Homopolymers or copolymers of amides or imides
- C09D133/26—Homopolymers or copolymers of acrylamide or methacrylamide
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- 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
- C08J2429/00—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 at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08J2431/00—Characterised by the use of copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, or carbonic acid, or of a haloformic acid
- C08J2431/02—Characterised by the use of omopolymers or copolymers of esters of monocarboxylic acids
- C08J2431/04—Homopolymers or copolymers of vinyl acetate
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
- C08J2433/08—Homopolymers or copolymers of acrylic acid esters
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
- C08J2433/18—Homopolymers or copolymers of nitriles
- C08J2433/20—Homopolymers or copolymers of acrylonitrile
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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
- C08J2433/24—Homopolymers or copolymers of amides or imides
- C08J2433/26—Homopolymers or copolymers of acrylamide or methacrylamide
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- C08J2439/00—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 at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Derivatives of such polymers
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Abstract
The invention belongs to the technical field of pre-coating liquid for transparent polyimide hardened films, and particularly relates to pre-coating liquid for enhancing surface adhesion of a transparent PI (polyimide) substrate and an application method thereof, wherein the pre-coating liquid comprises the following components in parts by weight: 100 parts of polar polymer, 1-25 parts of fluorine-containing additive and 5000 parts of solvent. According to the invention, the polar polymer and the fluorine-containing additive are added, and the similar intermiscibility between the fluoride in the fluorine-containing additive and the fluorine modified transparent PI base material and the strong polarity of the polar polymer are utilized, so that the precoating liquid can be favorably permeated into the transparent PI base material and mutually interpenetrated with the base material, the precoating liquid is firmly attached to the surface of the base material after being crosslinked and cured, the problem of poor adhesive force caused by fluorine modification of the base material is effectively avoided, the hardened layer is firmly attached to the precoating layer, and the binding force between the hardened layer and the base material can be effectively improved; the adhesive force is improved by the precoating layer between the base material and the hardened layer, and the comprehensive properties of the hardened layer, such as optical transparency, hardness, wear resistance and the like, are not influenced.
Description
Technical Field
The invention belongs to the technical field of pre-coating liquid for a transparent polyimide hardened film, and particularly relates to pre-coating liquid for enhancing surface adhesion of a transparent PI (polyimide) substrate and an application method thereof.
Background
In recent years, with the vigorous development of the electronic information industry and the raw material industry thereof, flexible and foldable mobile phones and other flexible electronic devices become the key point of research and development in the industry. The cover plate can meet the folding requirement, and the glass is difficult to achieve the bending effect, so that the industry searches for adopting a transparent plastic film to replace the glass, and the transparent Polyimide (PI) film has high transparency, good weather resistance and high hardness, and becomes a preferred substitute for the cover plate glass. However, the molecular chain of the transparent polyimide film contains fluorine element in a large proportion, so that the adhesion of the surface hardening film to the transparent polyimide film is poor, and the improvement of the adhesion becomes a research focus in the aspect of flexible and foldable screens.
In the existing transparent PI hardened film product, the transparency of the transparent PI substrate is generally improved by fluorine modification, and the fluorine modification can cause the problem that a hardened layer on the surface of the transparent PI substrate is difficult to adhere. Therefore, there is a need to develop a pre-coating solution that can effectively improve the surface adhesion of the transparent PI substrate so that the transparent PI hardened film can maintain good performance after long-term use.
Disclosure of Invention
In order to solve the problems, the invention discloses a pre-coating liquid for enhancing the surface adhesion of a transparent PI substrate and an application method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the precoating liquid for enhancing the surface adhesion of the transparent PI base material comprises the following components in parts by weight:
polar Polymer 100 parts
1-25 parts of fluorine-containing additive
100 portions of solvent and 5000 portions.
Preferably, the molecular weight of the polar polymer is 1000-50000.
Preferably, the polar polymer is one or more of polyvinyl alcohol, polyvinyl pyrrolidone, polyvinyl acetate, polyacrylate, polyacrylamide and polyacrylonitrile.
Preferably, the fluorine-containing additive is one or more of polyether modified polytetrafluoroethylene, fluoroalkyl trimethyl siloxane and acrylic modified fluororesin.
Preferably, the solvent is one or more of methanol, ethanol, isopropanol, butanone, cyclohexanone, toluene and xylene.
The application method of the pre-coating liquid for enhancing the surface adhesion of the transparent PI base material comprises the following steps:
(1) uniformly coating the pre-coating liquid on a transparent PI substrate, and performing thermocuring to obtain a pre-coating layer;
(2) and uniformly coating a layer of hardening liquid on the surface of the precoating layer, solidifying to obtain a hardened layer, and attaching a protective film after the hardened layer is cooled.
Preferably, the conditions for heat curing in the step (1) are as follows: 50-120 deg.C, 1-5 min.
Preferably, the step (1) is preceded by a pretreatment step, wherein the pretreatment step comprises: and (3) placing the transparent PI base material in an alkali liquor for soaking for 0.5-25h, then washing with deionized water for 1-3 times, and drying.
Preferably, the alkali liquor is a mixture of sodium hydroxide, potassium hydroxide, water and ethanol, wherein the mass ratio of the sodium hydroxide to the potassium hydroxide to the water to the ethanol is 1:0-2:10-50: 0-50; the drying condition in the pretreatment step is drying at 50-100 ℃ for 0.5-5 min.
Preferably, the thickness of the precoat layer is 2 to 500nm, preferably 50 to 200 nm.
The invention has the following beneficial effects: (1) the precoating liquid is added with the polar polymer and the fluorine-containing additive, the similar intermiscibility between the fluoride in the fluorine-containing additive and the fluorine modified transparent PI base material and the strong polarity of the polar polymer are utilized, so that the precoating liquid can be favorably permeated into the transparent PI base material and mutually interpenetrated with the base material, and the precoating liquid is stabbed into the base material after being crosslinked and cured, so that the precoating liquid is firmly attached to the surface of the base material, the problem of poor adhesive force caused by fluorine modification of the base material is effectively avoided, the hardened layer is firmly attached to the precoating layer with good adhesive force, and the binding force between the hardened layer and the base material can be effectively improved;
(2) according to the invention, the adhesion is improved by a method of coating the pre-coating liquid between the transparent PI substrate and the hardened layer to obtain the pre-coating layer, the comprehensive performances such as optical transparency, hardness, wear resistance and the like of the hardened layer are not influenced, and the substrate, the pre-coating layer and the hardened layer have higher transparency, so that the CPI (transparent polyimide) hardened film has higher integral transparency;
(3) the polar polymer adopts low molecular substances with the molecular weight of 1000-50000, and is easier to permeate into the transparent PI base material, so that the adhesive force is further improved;
(4) the transparent PI base material is pretreated by the alkali liquor before the coating of the pre-coating liquid, so that the surface of the base material can be activated, the permeation of the pre-coating liquid to the inside of the base material in the later period is facilitated, and the adhesion is increased.
Detailed Description
The present invention will now be described in further detail with reference to examples.
The preparation method of the pre-coating liquid for enhancing the surface adhesion of the transparent PI base material comprises the following steps: weighing the components in proportion, and mixing uniformly.
The application method of the pre-coating liquid for enhancing the surface adhesion of the transparent PI base material comprises the following steps:
(1) uniformly coating the pre-coating liquid on a transparent PI substrate, and performing thermocuring to obtain a pre-coating layer;
(2) and uniformly coating a layer of hardening liquid on the surface of the precoating layer, solidifying to obtain a hardened layer, and attaching a protective film after the hardened layer is cooled.
Wherein, the conditions of the thermal curing in the step (1) are as follows: 50-120 deg.C, 1-5 min.
A pretreatment step is also carried out before the step (1), and the pretreatment step comprises the following steps: putting the transparent PI base material into alkali liquor to be soaked for 0.5-25h, then washing with deionized water for 1-3 times, and drying; the alkali liquor is a mixture of sodium hydroxide, potassium hydroxide, water and ethanol, and the mass ratio of the sodium hydroxide to the potassium hydroxide to the water to the ethanol is 1:0-2:10-50: 0-50; the drying condition in the pretreatment step is drying at 50-100 ℃ for 0.5-5 min.
The hardening liquid can be directly selected from the hardening liquids for PI hardening films sold in the market, and the specific curing conditions are based on the requirements of the selected hardening liquid sold in the market.
The components of the precoat liquids used in examples 1 to 5 and comparative examples 1 to 8, their amounts by weight, and curing conditions are detailed in Table 1.
TABLE 1
Comparative example 9, comparative example 9 is substantially the same as example 4 except that comparative example 9 does not apply the pre-coating liquid on the transparent PI substrate.
The results of various property tests on the PI hardened films prepared using the precoat liquids prepared in examples 1 to 5 and comparative examples 1 to 8 and the PI hardened film of comparative example 9 are shown in Table 2.
TABLE 2
The conditions of uv damp heat ageing in the hundred cells after uv damp heat ageing in table 2 are: strong ultraviolet at 340nm, 60 deg.C, relative humidity of 90%, 72 hr.
Since the precoating liquid is applied between the transparent PI base material and the surface hardened layer, the optical transparency hardness, the abrasion resistance, the yellowing resistance and the like of the hardened layer are not affected.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (7)
1. The precoating liquid for enhancing the surface adhesion of the transparent PI base material is characterized in that: the composition comprises the following components in parts by weight:
polar Polymer 100 parts
1-25 parts of fluorine-containing additive
100 portions of solvent and 5000 portions;
the solvent is one or more of methanol, ethanol, isopropanol, butanone, cyclohexanone, toluene and xylene;
the molecular weight of the polar polymer is 1000-50000;
the polar polymer is one or more of polyvinyl alcohol, polyvinylpyrrolidone, polyvinyl acetate, polyacrylate, polyacrylamide and polyacrylonitrile;
the fluorine-containing additive is one or more of polyether modified polytetrafluoroethylene, fluoroalkyl trimethyl siloxane and acrylic acid modified fluororesin.
2. The method of using the pre-coating solution for enhancing the surface adhesion of the transparent PI substrate as claimed in claim 1, wherein the pre-coating solution comprises the following steps: the method comprises the following steps:
(1) uniformly coating the pre-coating liquid on a transparent PI substrate, and performing thermocuring to obtain a pre-coating layer;
(2) and uniformly coating a layer of hardening liquid on the surface of the precoating layer, solidifying to obtain a hardened layer, and attaching a protective film after the hardened layer is cooled.
3. The method of applying the pre-coating solution for enhancing the surface adhesion of transparent PI substrates according to claim 2, wherein: the conditions of thermal curing in the step (1) are as follows: 50-120 deg.C, 1-5 min.
4. The method of applying the pre-coating solution for enhancing the surface adhesion of transparent PI substrates according to claim 2, wherein: a pretreatment step is also carried out before the step (1), and the pretreatment step comprises the following steps: and (3) placing the transparent PI base material in an alkali liquor for soaking for 0.5-25h, then washing with deionized water for 1-3 times, and drying.
5. The method of applying the pre-coating solution for enhancing the surface adhesion of transparent PI substrates of claim 4, wherein: the alkali liquor is a mixture of sodium hydroxide, potassium hydroxide, water and ethanol, and the mass ratio of the sodium hydroxide to the potassium hydroxide to the water to the ethanol is 1:0-2:10-50: 0-50; the drying condition in the pretreatment step is drying at 50-100 ℃ for 0.5-5 min.
6. The method of applying the pre-coating solution for enhancing the surface adhesion of transparent PI substrates according to claim 2, wherein: the thickness of the precoat layer is 2-500 nm.
7. The method of applying the pre-coating solution for enhancing the surface adhesion of transparent PI substrates of claim 6 wherein: the thickness of the precoat layer is 50-200 nm.
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| CN113292921A (en) * | 2021-05-26 | 2021-08-24 | 广东电网有限责任公司 | Composite insulator coating, preparation method and spraying process |
| CN114181420B (en) * | 2021-12-09 | 2023-06-23 | 宁波惠之星新材料科技股份有限公司 | Additional coating for transparent polyimide film, application method of additional coating and cover plate film |
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| CN102236113B (en) * | 2010-05-01 | 2015-02-11 | 中国航天科技集团公司第四研究院第四十二所 | Ultraviolet-cured hard coating and application thereof |
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