CN108034066B - Preparation method of wear-resistant bending-resistant high-transmittance film for flexible display - Google Patents
Preparation method of wear-resistant bending-resistant high-transmittance film for flexible display Download PDFInfo
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- C08J2327/00—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 halogen; Derivatives of such polymers
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- 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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Abstract
The invention relates to a flexible display surface protection technology, and aims to provide a preparation method of a wear-resistant bending-resistant high-light-transmission film for a flexible display. The method comprises the steps of mixing and grinding vinyl chloride-vinyl acetate-vinyl alcohol terpolymer resin, polybutylene terephthalate resin, polyisobutylene, nano alumina, nano yttrium oxide and nano mullite, casting into a film, and irradiating by ultraviolet light, continuously soaking in nano montmorillonite aqueous dispersion, continuously soaking in polyvinyl alcohol aqueous solution and continuously soaking in glutaraldehyde aqueous solution to finally obtain the product. The invention solves the problems that the high-strength glass protection surface layer can not be applied to the flexible display field and the wear resistance of the high-molecular protection surface layer is poor; meanwhile, the wear-resistant bending-resistant high-transmittance film for the flexible display has better light transmittance and bending resistance compared with a glass protection surface layer and a polymer protection surface layer.
Description
Technical Field
The invention relates to a flexible display surface protection technology, in particular to a preparation method of a wear-resistant bending-resistant high-light-transmission film for a flexible display.
Background
The flexible display refers to a flat display device having flexibility manufactured on a flexible substrate such as plastic, metal foil, or the like. In recent years, the potential advantages of flexible displays have become increasingly prominent, such as light weight, flexibility, and impact resistance. The flexible display can be applied to mobile phones, notebook computers, electronic books, automobile instrument panels and the like. By utilizing the bendable characteristic of the flexible display, the engineering is not limited to planarization, and the display mode with diversified appearances can be realized.
But flexible displays present new problems compared to rigid display systems; rigid display can adopt high-strength glass as a transparent protective surface layer, but the protective surface layer cannot be applied to the field of flexible display, so that a flexible bending-resistant transparent film needs to be developed to serve as the protective surface layer of the flexible display.
In the prior art, a large amount of inorganic components are added into a system for realizing high surface hardness of the transparent film for the protective surface layer, but the light transmittance and flexibility of the film are obviously reduced due to the addition of too much inorganic components, and the application advantages of the film in flexible display are lost. Therefore, how to achieve both high surface hardness and light transmittance and flexibility of the film is an urgent problem to be solved.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art and provides a preparation method of a wear-resistant bending-resistant high-light-transmission film for a flexible display.
In order to solve the technical problem, the solution of the invention is as follows:
the preparation method of the wear-resistant bending-resistant high-light-transmission film for the flexible display comprises the following steps:
(1) weighing the following raw material components in parts by weight:
100 parts of vinyl chloride-vinyl acetate-vinyl alcohol ternary copolymer resin, 20-40 parts of polybutylene terephthalate resin, 1-5 parts of polyisobutylene, 3-6 parts of nano alumina, 0.1-0.5 part of nano yttrium oxide and 1-5 parts of nano mullite;
weighing dimethyl adipate, vinyl chloride-vinyl acetate-vinyl alcohol ternary copolymer resin, polybutylene terephthalate resin and polyisobutylene according to the mass ratio of the mass sum of the dimethyl adipate to the dimethyl adipate being 0.05-0.25: 1;
(2) adding vinyl chloride-vinyl acetate-vinyl alcohol terpolymer resin, polybutylene terephthalate resin and polyisobutylene into dimethyl adipate, and fully stirring until the materials are completely dissolved to obtain a mixture I;
(3) adding the nano alumina, the nano yttrium oxide and the nano mullite into the first mixture, and stirring for 1-3 hours at 400-;
(4) adding the mixture II into a three-roll grinder, grinding for 30-70 times, and cooling to room temperature to obtain a mixture III;
(5) preparing a film with the thickness of 50 microns by casting the mixture tee into a film, and marking as a film I;
(6) irradiating the surface of the first film for 30-60 minutes by adopting ultraviolet light with the wavelength of 300 nanometers to obtain a second film;
(7) immersing the second film into 0.5-1.5% of nano montmorillonite water dispersion, continuously immersing for 5-10 minutes, taking out, and drying at 60-80 ℃ for 30-60 minutes to obtain a third film;
(8) immersing the third film into a polyvinyl alcohol aqueous solution with the mass fraction of 1-3%, continuously immersing for 5-10 minutes, taking out, and drying at 60-80 ℃ for 30-60 minutes to obtain a fourth film;
(9) and immersing the film IV into a glutaraldehyde aqueous solution with the mass fraction of 25-55%, continuously immersing for 24-72 hours, taking out, and drying at 80-90 ℃ for 3-6 hours to obtain the wear-resistant bending-resistant high-light-transmittance film for the flexible display.
In the invention, the molecular weight of the chloroethylene-vinyl acetate-vinyl alcohol ternary copolymer resin is 20000-30000, and the mass ratio of chloroethylene/vinyl acetate/vinyl alcohol in the resin is 80: 15: 5; the molecular weight of the polybutylene terephthalate is 30000-100000, and the molecular weight of the polyisobutylene is 110000-400000.
In the invention, the grain diameter of the nano alumina is 5-15 nm; the grain size of the nano yttrium oxide is 2-4 nm; the grain diameter of the nano mullite is 3-7 nanometers.
In the invention, in the step (8), the size of the montmorillonite sheet layer in the nano montmorillonite water dispersion liquid is 50-150 nm.
In the present invention, in the step (8), the molecular weight of the polyvinyl alcohol in the aqueous solution of polyvinyl alcohol is 60000-120000.
Compared with the prior art, the invention has the following beneficial effects:
the invention solves the problems that the high-strength glass protection surface layer can not be applied to the flexible display field and the wear resistance of the high-molecular protection surface layer is poor; meanwhile, the wear-resistant bending-resistant high-transmittance film for the flexible display has better light transmittance and bending resistance compared with a glass protection surface layer and a polymer protection surface layer.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1:
a wear-resistant bending-resistant high-light-transmission film for a flexible display comprises the following components in parts by weight: vinyl chloride-vinyl acetate-vinyl alcohol terpolymer resin: 100 parts of (A); polybutylene terephthalate resin: 20 parts of (1); polyisobutylene: 1 part; nano alumina: 3 parts of a mixture; nano yttrium oxide: 0.1 part; nano mullite: 1 part;
the molecular weight of the chloroethylene-vinyl acetate-vinyl alcohol ternary copolymer resin is 20000, and the mass ratio of chloroethylene/vinyl acetate/vinyl alcohol is as follows: 80/15/5, respectively; the molecular weight of polybutylene terephthalate is 30000; the molecular weight of the polyisobutene is 110000; the grain diameter of the nano alumina is 5-10 nanometers; the grain diameter of the nano yttrium oxide is 2-3 nanometers; the grain diameter of the nano mullite is 3-5 nm.
The preparation method of the film sequentially comprises the following steps:
(1) adding vinyl chloride-vinyl acetate-vinyl alcohol terpolymer resin, polybutylene terephthalate resin and polyisobutylene into dimethyl adipate in proportion, and fully stirring until the materials are completely dissolved to obtain a mixture I; the mass ratio of the sum of the mass of the vinyl chloride-vinyl acetate-vinyl alcohol terpolymer resin, the mass of the polybutylene terephthalate resin and the mass of the polyisobutylene to the mass of the dimethyl adipate is 0.05: 1;
(2) adding the nano alumina, the nano yttrium oxide and the nano mullite into the first mixture in proportion, and stirring for 1 hour at 400 revolutions per minute to obtain a second mixture;
(3) adding the mixture II into a three-roll grinder to grind for 30 times, and cooling to room temperature to obtain a mixture III;
(4) preparing a film with the thickness of 50 microns by casting the mixture tee into a film, and marking as a film I;
(5) irradiating the surface of the first film for 30 minutes by adopting ultraviolet light with the wavelength of 300 nanometers to obtain a second film;
(6) immersing the second film into 0.5 mass percent of nano montmorillonite water dispersion, continuously immersing for 5 minutes, taking the second film out of the solution, and drying for 30 minutes at 60 ℃ to obtain a third film;
(7) immersing the film III into a polyvinyl alcohol aqueous solution with the mass fraction of 1%, continuously immersing for 5 minutes, taking the film out of the solution, and drying for 30 minutes at 60 ℃ to obtain a film IV;
(8) soaking the film IV into a glutaraldehyde aqueous solution with the mass fraction of 25%, continuously soaking for 24 hours, taking the film out of the solution, and drying at 80 ℃ for 3 hours to obtain the wear-resistant bending-resistant high-light-transmission film for the flexible display;
the molecular weight of polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 60000; the size of montmorillonite layer in the nano montmorillonite water dispersion liquid is 50-100 nm.
Example 2:
a wear-resistant bending-resistant high-light-transmission film for a flexible display comprises the following components in parts by weight: vinyl chloride-vinyl acetate-vinyl alcohol terpolymer resin: 100 parts of (A); polybutylene terephthalate resin: 40 parts of a mixture; polyisobutylene: 5 parts of a mixture; nano alumina: 6 parts of (1); nano yttrium oxide: 0.5 part; nano mullite: 5 parts of a mixture;
the molecular weight of the vinyl chloride-vinyl acetate-vinyl alcohol ternary copolymer resin is 30000, and the mass ratio of vinyl chloride/vinyl acetate/vinyl alcohol is as follows: 80/15/5, respectively; the molecular weight of polybutylene terephthalate is 100000; the molecular weight of the polyisobutylene is 400000; the grain diameter of the nano alumina is 10-15 nm; the grain diameter of the nano yttrium oxide is 3-4 nm; the grain diameter of the nano mullite is between 5 and 7 nanometers.
The preparation method of the film sequentially comprises the following steps:
(1) adding vinyl chloride-vinyl acetate-vinyl alcohol terpolymer resin, polybutylene terephthalate resin and polyisobutylene into dimethyl adipate in proportion, and fully stirring until the materials are completely dissolved to obtain a mixture I; the mass ratio of the sum of the mass of the vinyl chloride-vinyl acetate-vinyl alcohol terpolymer resin, the mass of the polybutylene terephthalate resin and the mass of the polyisobutylene to the mass of the dimethyl adipate is 0.25: 1;
(2) adding the nano alumina, the nano yttrium oxide and the nano mullite into the mixture I obtained in the step 1 according to the proportion, and stirring for 3 hours at 1000 revolutions per minute to obtain a mixture II;
(3) adding the mixture II into a three-roll grinder, grinding for 70 times, and cooling to room temperature to obtain a mixture III;
(4) preparing the mixture three-way by a casting film forming mode to obtain a film with the film thickness of 50 microns, and marking as a film I
(5) Irradiating the surface of the first film for 1 hour by adopting ultraviolet light with the wavelength of 300 nanometers to obtain a second film;
(6) immersing the second film into 1.5% of nano montmorillonite water dispersion liquid by mass fraction, continuously immersing for 10 minutes, taking the second film out of the solution, and drying for 1 hour at 80 ℃ to obtain a third film;
(7) immersing the film III into a polyvinyl alcohol aqueous solution with the mass fraction of 3%, continuously immersing for 10 minutes, taking the film out of the solution, and drying for 1 hour at 80 ℃ to obtain a film IV;
(8) soaking the film IV into 55% glutaraldehyde water solution by mass fraction for 72 hours, taking out the film from the solution, and drying at 90 ℃ for 6 hours to obtain a wear-resistant bending-resistant high-light-transmission film for the flexible display;
the molecular weight of polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 120000; the size of montmorillonite layer in the nano montmorillonite water dispersion liquid is 100-150 nm.
Example 3:
a wear-resistant bending-resistant high-light-transmission film for a flexible display comprises the following components in parts by weight: vinyl chloride-vinyl acetate-vinyl alcohol terpolymer resin: 100 parts of (A); polybutylene terephthalate resin: 30 parts of (1); polyisobutylene: 3 parts of a mixture; nano alumina: 4.5 parts; nano yttrium oxide: 0.3 part; nano mullite: 3 parts of a mixture;
the molecular weight of the vinyl chloride-vinyl acetate-vinyl alcohol ternary copolymer resin is 25000, and the mass ratio of vinyl chloride/vinyl acetate/vinyl alcohol is as follows: 80/15/5, respectively; the molecular weight of polybutylene terephthalate is 60000; the molecular weight of the polyisobutylene is 250000; the grain diameter of the nano alumina is 7-12 nm; the grain diameter of the nano yttrium oxide is 2.5-3.5 nm; the grain diameter of the nano mullite is 4-6 nanometers.
The preparation method of the film sequentially comprises the following steps:
(1) adding vinyl chloride-vinyl acetate-vinyl alcohol terpolymer resin, polybutylene terephthalate resin and polyisobutylene into dimethyl adipate in proportion, and fully stirring until the materials are completely dissolved to obtain a mixture I; the mass ratio of the sum of the mass of the vinyl chloride-vinyl acetate-vinyl alcohol terpolymer resin, the mass of the polybutylene terephthalate resin and the mass of the polyisobutylene to the mass of the dimethyl adipate is 0.15: 1;
(2) adding the nano alumina, the nano yttrium oxide and the nano mullite into the mixture I obtained in the step 1 according to the proportion, and stirring for 2 hours at 700 revolutions per minute to obtain a mixture II;
(3) adding the mixture II into a three-roll grinder, grinding for 50 times, and cooling to room temperature to obtain a mixture III;
(4) preparing a film with the thickness of 50 microns by a compound tee through a casting film forming mode, and marking as a film I
(5) Irradiating the surface of the first film for 45 minutes by adopting ultraviolet light with the wavelength of 300 nanometers to obtain a second film;
(6) immersing the second film into 1.0 mass percent of nano montmorillonite water dispersion, continuously immersing for 8 minutes, taking the second film out of the solution, and drying for 45 minutes at 70 ℃ to obtain a third film;
(7) immersing the film III into a polyvinyl alcohol aqueous solution with the mass fraction of 2%, continuously immersing for 8 minutes, taking the film out of the solution, and drying for 45 minutes at 70 ℃ to obtain a film IV;
(8) soaking the film IV into 40% glutaraldehyde water solution by mass fraction for 48 hours, taking out the film from the solution, and drying at 85 ℃ for 5 hours to obtain the wear-resistant bending-resistant high-light-transmission film for the flexible display;
the molecular weight of polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 90000; the size of montmorillonite layer in the nano montmorillonite water dispersion liquid is 75-125 nm.
Test for verifying the Effect of the invention
1. The wear-resistant, bending-resistant and high-transmittance film for the flexible display obtained in the embodiments 1, 2 and 3 is respectively marked as a first sample, a second sample and a third sample;
2. the pure polycarbonate film was designated sample four;
3. the third generation of gorilla glass (
Glass 3 coloring corporation) as sample five;
4. the light transmission, surface hardness and impact resistance tests were carried out according to ATSM D1003-07, GB/T6739-.
The test results are given in the following table:
| sample (I) | Light transmittance | Surface hardness | Impact strength |
| Sample No | 94％ | 6H | 819J/m |
| Sample No. 2 | 93％ | 6H | 773J/m |
| Sample No. three | 94％％ | 6H | 802J/m |
| Sample No. 4 | 90％ | 3H | 500J/m |
| Sample five | 86％ | 6H | 224J/m |
From the above table, it can be seen that the abrasion-resistant, bending-resistant and high-transmittance film for the flexible display provided by the invention has higher transmittance and higher impact strength compared with a pure polycarbonate film and third generation gorilla glass, and meanwhile, the surface hardness of the film provided by the invention also reaches the same level as the third generation gorilla glass.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (5)
1. A preparation method of a wear-resistant bending-resistant high-light-transmission film for a flexible display is characterized by comprising the following steps:
(1) weighing the following raw material components in parts by weight:
100 parts of vinyl chloride-vinyl acetate-vinyl alcohol ternary copolymer resin, 20-40 parts of polybutylene terephthalate resin, 1-5 parts of polyisobutylene, 3-6 parts of nano alumina, 0.1-0.5 part of nano yttrium oxide and 1-5 parts of nano mullite;
weighing dimethyl adipate, vinyl chloride-vinyl acetate-vinyl alcohol ternary copolymer resin, polybutylene terephthalate resin and polyisobutylene according to the mass ratio of the mass sum of the dimethyl adipate to the dimethyl adipate being 0.05-0.25: 1;
(2) adding vinyl chloride-vinyl acetate-vinyl alcohol terpolymer resin, polybutylene terephthalate resin and polyisobutylene into dimethyl adipate, and fully stirring until the materials are completely dissolved to obtain a mixture I;
(3) adding the nano alumina, the nano yttrium oxide and the nano mullite into the first mixture, and stirring for 1-3 hours at 400-;
(4) adding the mixture II into a three-roll grinder, grinding for 30-70 times, and cooling to room temperature to obtain a mixture III;
(5) preparing a film with the thickness of 50 microns by casting the mixture tee into a film, and marking as a film I;
(6) irradiating the surface of the first film for 30-60 minutes by adopting ultraviolet light with the wavelength of 300 nanometers to obtain a second film;
(7) immersing the second film into 0.5-1.5 wt% of nano montmorillonite water dispersion, continuously immersing for 5-10 min, taking out, and soaking at 60-80%oC, drying for 30-60 minutes to obtain a third film;
(8) immersing the third film into 1-3% polyvinyl alcohol aqueous solution by mass percent for a long timeSoaking for 5-10 min, taking out, and soaking at 60-80 deg.CoC, drying for 30-60 minutes to obtain a film IV;
(9) immersing the membrane IV into 25-55% glutaraldehyde aqueous solution, continuously immersing for 24-72 hours, taking out, and soaking at 80-90%oAnd C, drying for 3-6 hours to obtain the wear-resistant bending-resistant high-light-transmittance film for the flexible display.
2. The method as claimed in claim 1, wherein the molecular weight of the vinyl chloride-vinyl acetate-vinyl alcohol terpolymer resin is 20000-30000, and the mass ratio of vinyl chloride/vinyl acetate/vinyl alcohol in the resin is 80: 15: 5; the molecular weight of the polybutylene terephthalate is 30000-100000, and the molecular weight of the polyisobutylene is 110000-400000.
3. The method of claim 1, wherein the nano-alumina has a particle size of 5 to 15 nm; the grain size of the nano yttrium oxide is 2-4 nm; the grain diameter of the nano mullite is 3-7 nanometers.
4. The method of claim 1, wherein in the step (7), the size of the montmorillonite layer in the nano montmorillonite aqueous dispersion is 50 nm-150 nm.
5. The method as claimed in claim 1, wherein in step (8), the molecular weight of the polyvinyl alcohol in the aqueous solution of polyvinyl alcohol is 60000-120000.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214687A (en) * | 2013-05-15 | 2013-07-24 | 上海冠旗电子新材料股份有限公司 | High-strength wear-resistant high-transmission polycarbonate film |
| CN105514188A (en) * | 2015-12-25 | 2016-04-20 | 中国科学院上海高等研究院 | Antireflection and self-cleaning thin film and preparation method thereof |
| KR20160136605A (en) * | 2015-05-20 | 2016-11-30 | 재단법인대구경북과학기술원 | Method for manufacturing transparent electrode |
| CN106297952A (en) * | 2016-08-09 | 2017-01-04 | 苏州极地实业有限公司 | A kind of flexible conductive film |
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2017
- 2017-12-09 CN CN201711299575.8A patent/CN108034066B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214687A (en) * | 2013-05-15 | 2013-07-24 | 上海冠旗电子新材料股份有限公司 | High-strength wear-resistant high-transmission polycarbonate film |
| KR20160136605A (en) * | 2015-05-20 | 2016-11-30 | 재단법인대구경북과학기술원 | Method for manufacturing transparent electrode |
| CN105514188A (en) * | 2015-12-25 | 2016-04-20 | 中国科学院上海高等研究院 | Antireflection and self-cleaning thin film and preparation method thereof |
| CN106297952A (en) * | 2016-08-09 | 2017-01-04 | 苏州极地实业有限公司 | A kind of flexible conductive film |
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