CN113736114A - Wear-resistant flexible diffusion film and preparation process thereof - Google Patents
Wear-resistant flexible diffusion film and preparation process thereof Download PDFInfo
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Abstract
The invention discloses a wear-resistant flexible diffusion film and a preparation process thereof, wherein the preparation process comprises the following steps: (1) preparing diffusion particles: taking a silicon source and ammonia water to prepare silicon dioxide microspheres; injecting zinc ions to prepare modified silicon dioxide microspheres; adding urea, sodium tartrate and vinyl trimethoxy silane for reaction; adding polyethylene and an initiator for reaction; (2) preparing a membrane body: taking hydroxyl-terminated polybutadiene to react with glyoxylic acid and react with m-phenylenediamine to prepare modified polybutadiene; reacting with diffusion particles and maleic anhydride, coating, and stretching; (3) preparing a diffusion film: coating the coating on the surface of the diffusion film body, compounding the coating surface and the base film, and curing. The invention forms the layer structure of the base film and the diffusion film body by setting the components of the diffusion film and the preparation process thereof, bonds and fills the base film and the diffusion film body by using the coating, and relative refraction exists between every two diffusion film bodies, thereby effectively increasing light refraction, reducing back scattering and improving the transmittance and haze of the prepared diffusion film.
Description
Technical Field
The invention relates to the technical field of optical films, in particular to a wear-resistant flexible diffusion film and a preparation process thereof.
Background
With the popularization of displays such as LEDs and PCs, the requirements for the luminous efficiency, light diffusibility and color rendering property of displays are increasing. However, the light efficiency, the light diffusivity and the color rendering property are mutually restricted, and the difficulty of realizing high light efficiency and high diffusion is high. For a conventional display, after other materials and properties are determined, the performance of the diffusion film determines the light efficiency and the diffusion rate of the display. . Diffusion membrane materials are mainly classified into two categories according to differences in structure and diffusion principle: the method is characterized in that the ion type and the surface microstructure type are doped in a common method, but the light transmittance and the diffusivity are a pair of contradictory technical indexes, and the relationship of the trade-off exists, so that how to obtain the diffusion film with both high light transmittance and high diffusivity is an important technical hotspot; and with the update and iteration of products, the requirements of people on the flexibility and the wear resistance of the diffusion film are improved. Therefore, we propose a wear-resistant flexible diffusion film and a preparation process thereof.
Disclosure of Invention
The invention aims to provide a wear-resistant flexible diffusion film and a preparation process thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation process of a wear-resistant flexible diffusion film comprises the following steps:
(1) preparing diffusion particles:
mixing a silicon source and ammonia water, adding absolute ethyl alcohol, and stirring for reaction to prepare silicon dioxide microspheres;
taking the silicon dioxide microspheres, injecting zinc ions, and annealing to prepare modified silicon dioxide microspheres;
adding deionized water into modified silicon dioxide microspheres for dispersion, adding urea and sodium tartrate, stirring, adding vinyl trimethoxy silane, adjusting the system to acidity, and heating for reaction; adding polyethylene and an initiator into the reaction product, and heating for reaction to obtain diffusion particles;
(2) preparing a membrane body:
taking hydroxyl-terminated polybutadiene and glyoxylic acid, mixing, and heating for reaction to obtain aldehyde-terminated polybutadiene;
mixing aldehyde-terminated polybutadiene and m-phenylenediamine, and heating for reaction to obtain modified polybutadiene;
soaking a pure titanium substrate in a sodium hydroxide solution, soaking a sodium bicarbonate solution, and boiling in boiling water to obtain a template;
heating and mixing diffusion particles, modified polybutadiene, maleic anhydride and an initiator, coating the mixture on the surface of a template, cooling to form a film, and stretching to obtain a diffusion film body;
(3) preparing a diffusion film:
taking tripropylene glycol diacrylate, urethane acrylate and a photoinitiator to prepare a coating, coating the coating on the surface of a diffusion membrane body, compounding the coating surface with a base membrane, and carrying out ultraviolet curing to prepare the diffusion membrane.
Further, the step (1) comprises the steps of:
mixing tetraethyl orthosilicate and ammonia water, adding absolute ethyl alcohol, stirring at room temperature, reacting for 5-6 h, centrifuging, washing a precipitate with ethanol for 3-5 times, and drying to obtain silicon dioxide microspheres; forming silicon dioxide microspheres by tetraethyl orthosilicate under the action of ammonia water;
taking silicon dioxide microspheres, and injecting zinc ions by using a metal vapor vacuum arc ion implanter, wherein the process comprises the following steps: accelerating voltage of 27-30 kV, and injection amount of 1.2 × 1017～1.8×1017/cm2The energy of zinc ion is 87-140 keV, and the beam density is 2.0-7.0 muA/cm2Annealing, and the process comprises: in an oxygen atmosphere, annealing at 400-900 ℃ for 1-8 h to prepare modified silicon dioxide microspheres; injecting zinc ions by using metal vapor vacuum arc ions, dispersing the zinc ions in the silicon dioxide microspheres, contacting the zinc ions with oxygen to form zinc oxide nanoparticles under the condition of oxygen atmosphere annealing, and oxidizing at high temperatureThe zinc size is reduced to form a compact zinc oxide particle film, so that the wear resistance and the mechanical property of the prepared diffusion film can be improved;
adding deionized water into modified silicon dioxide microspheres, performing ultrasonic dispersion for 50-80 min, adding urea and sodium tartrate, stirring, adding vinyl trimethoxy silane, adjusting the pH value of a system to 3-4, stirring for 50-80 min, reacting at a constant temperature of 175-185 ℃ for 3-4 h, cooling, centrifuging, taking out a precipitate, washing with water for 3-5 times, and drying at a temperature of 70-80 ℃ for 20-27 h; and (3) taking a reaction product, adding polyethylene and an initiator, and reacting at the temperature of 165-200 ℃ for 6-10 hours to obtain the diffusion particles.
By the process, the surface of the modified silicon dioxide microspheres is coated with the organic siloxane, so that the surface uniformity and the flatness are improved, and then the modified silicon dioxide microspheres are crosslinked with polyethylene, so that the flexibility of the prepared diffusion film is improved, a multi-shell structure with different refractive indexes is formed, multiple scattering can be generated on incident light, and the light diffusion performance of the prepared diffusion film is improved; the difference of the refractive indexes between the adjacent structures in the multi-shell structure is small, so that the backscattering can be effectively reduced, the optical loss is reduced, and the transmittance of the prepared diffusion film is improved; meanwhile, when organic matters are coated on the surface of the modified silicon dioxide microspheres, zinc oxide on the modified silicon dioxide microspheres can cooperate with an initiator to promote the crosslinking reaction between siloxane and polyethylene, so that the mechanical property of the prepared diffusion film body is improved; wherein the initiator can be tert-butyl peroxypivalate, and the dosage is 0.2-0.3 wt%;
furthermore, the mass ratio of the urea, the sodium tartrate and the vinyl trimethoxy silane in the step (1) is 2.1 (0.36-0.40) to (1.9-2.0).
Further, the step (2) comprises the following steps:
mixing hydroxyl-terminated polybutadiene and glyoxylic acid, heating to 100-160 ℃, adding cyclohexane and p-toluenesulfonic acid in a nitrogen atmosphere, heating to 130-160 ℃, reacting for 1-2 h, vacuumizing, reacting for 2-4 h, and purifying with absolute ethanol to obtain aldehyde-terminated polybutadiene;
mixing aldehyde-terminated polybutadiene and m-phenylenediamine, heating to 160-250 ℃, adding acetic acid, stirring, reacting for 6-12 h, centrifuging, washing and drying to obtain modified polybutadiene;
taking a pure titanium substrate, polishing the pure titanium substrate by using metallographic abrasive paper, cleaning the pure titanium substrate by using acetone and absolute ethyl alcohol, drying the pure titanium substrate for 100-140 min at the temperature of 70-80 ℃, cleaning a mixed solution of nitric acid and hydrofluoric acid, and removing scratches left by surface polishing; placing the material in a 1mol/L sodium bromide solution, etching the material for 5-7 min at the solution temperature of 0-1 ℃ and the current density of 500mA/cm to form a surface structure with fluctuation and holes in the fluctuation, soaking the surface structure in a mixed solution of nitric acid and hydrofluoric acid for 1-2 min, weakening the fluctuation structure, and obtaining the holes with the regular hexagon shape;
heating the diffusion particles, modified polybutadiene, maleic anhydride and an initiator to 156-178 ℃, mixing, coating on the surface of a template, hot-pressing for 5-15 min at 65-75 ℃, cooling to form a film, transversely stretching by 30-50 times, and longitudinally stretching by 10-30 times to obtain the diffusion film body.
In the technical scheme, hydroxyl-terminated polybutadiene is used as a raw material and reacts with glyoxylic acid to generate aldehyde-terminated polybutadiene, wherein aldehyde groups react with m-phenylenediamine to generate imine bonds, and modified polybutadiene is obtained; crosslinking with organic matters on the surfaces of the diffusion particles under the action of maleic anhydride and an initiator, preparing a membrane on a template, wherein modified silicon dioxide microspheres in the diffusion particles are self-assembled in holes formed in the template due to the limitation of a physical boundary, so that the prepared membrane has more regular distribution of the diffusion particles, and the uniformity of the prepared diffusion membrane is improved; the holes in the template which are not occupied by the microspheres are filled with organic matters to form nanoscale protrusions with regular hexagons; after stretching, the regular hexagonal bulges are changed into a micron structure, so that the refraction of the prepared diffusion film to incident light is enhanced, and the light diffusion performance is improved; the modified polybutadiene has better tensile property and flexibility, can realize higher-multiple stretching and is beneficial to the flexible embodiment of the prepared diffusion membrane;
furthermore, the molar ratio of hydroxyl in the hydroxyl-terminated polybutadiene to glyoxylic acid, cyclohexane and p-toluenesulfonic acid is 1:1 (0.1-0.2) to (0.06-0.09), the molar ratio of aldehyde groups in the aldehyde-terminated polybutadiene to m-phenylenediamine is 1:0.5, and the mass ratio of the diffusion particles, the modified polybutadiene and the maleic anhydride is (10-15) to 100 (4-6).
Further, the step (3) comprises the following steps:
taking tripropylene glycol diacrylate, urethane acrylate and a photoinitiator to prepare a coating, mixing and stirring uniformly in the absence of light, coating the coating on the surface of a diffusion membrane body, compounding the coating surface with a base membrane, coating the coating on the surface, carrying out ultrasonic treatment for 5-10 min, and curing for 10-15 min under ultraviolet light to prepare the diffusion membrane.
Furthermore, the mass ratio of the tripropylene glycol diacrylate, the urethane acrylate and the photoinitiator is 5 (15-19) to 0.4-0.5.
Further, the base film is polyethylene terephthalate, the base film is subjected to surface treatment by oxygen plasma, and the ratio of the thickness of the diffusion film to the thickness of the diffusion film body is (2-3): 1.
In the technical scheme, the initiator can be cumene peroxide, and the base membrane is subjected to surface treatment by oxygen plasma to form oxygen-containing polar groups; the tripropylene glycol diacrylate, the urethane acrylate and the photoinitiator are mixed to obtain a coating, the coating is coated on the surfaces of the base film and the diffusion film body to improve the cohesiveness between the tripropylene glycol diacrylate and the urethane acrylate, holes formed in the diffusion film body are filled, the surface flatness of the prepared diffusion film is improved, relative refraction exists among the base film, the diffusion film body and the coating, the difference between every two refraction indexes is small, the light refraction can be effectively increased, the back scattering is reduced, and the transmittance and the haze of the prepared diffusion film are improved; the bending fatigue resistance of the prepared diffusion film is improved, and the flexibility of the diffusion film is reflected; the thickness ratio of the diffusion film and the diffusion film body is limited, and the high transmittance and the high haze of the diffusion film body are ensured.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the wear-resistant flexible diffusion film and the preparation process thereof, the base film and the diffusion film body layer structure are formed by arranging the diffusion film components and the preparation process thereof, the base film and the diffusion film body layer structure are bonded and filled by using the coating, and relative refraction exists between every two diffusion film components, so that light refraction can be effectively increased, back scattering is reduced, and the transmittance and haze of the prepared diffusion film are improved.
2. According to the wear-resistant flexible diffusion film and the preparation process thereof, the silicon dioxide-zinc oxide-organic silicon crosslinked polyethylene multi-shell structure is formed by arranging the diffusion particle components and the preparation process thereof, the difference of the refractive indexes between adjacent structures is small, the backscattering can be effectively reduced, and the transmittance of the prepared diffusion film is improved; wherein, the zinc oxide permeates and wraps the silicon dioxide, the wear resistance and the mechanical property of the prepared diffusion film are improved, and the flexibility of the prepared diffusion film body can be improved by the organosilicon crosslinked polyethylene.
3. According to the wear-resistant flexible diffusion membrane and the preparation process thereof, the diffusion particles and the modified polybutadiene are coated on the template in a cross-linking manner through the arrangement of the components of the diffusion membrane body and the preparation process thereof, and are stretched, organic matters such as the modified polybutadiene and the like and the diffusion particles are self-assembled in holes in the template, so that the diffusion particles in the prepared membrane body are uniformly distributed, the stretched organic matters form a micron convex structure, and the refraction of the prepared diffusion membrane to incident light is enhanced; the modified polybutadiene has better tensile property and flexibility, can realize higher-multiple stretching, is beneficial to the flexible embodiment of the prepared diffusion film, and positions the diffusion particles to prevent the diffusion particles from drifting.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The components, thickness and preparation process of the following basement membranes are the same.
Example 1
(1) Preparing diffusion particles:
mixing tetraethyl orthosilicate and ammonia water, adding absolute ethyl alcohol, stirring at room temperature, reacting for 5 hours, centrifuging, taking precipitate, washing for 3 times by using the ethanol, and drying to obtain silicon dioxide microspheres;
taking silicon dioxide microspheres, and utilizing metal steamThe empty arc ion implanter injects zinc ions, and the process comprises the following steps: acceleration voltage 27kV, injection amount 1.2X 1017/cm2Zinc ion energy 87keV, beam density 2.0 muA/cm2Annealing, and the process comprises: preparing modified silicon dioxide microspheres in oxygen atmosphere at the annealing temperature of 600 ℃ for 1 h;
adding deionized water into modified silicon dioxide microspheres, performing ultrasonic dispersion for 50min, adding urea and sodium tartrate, stirring, adding vinyl trimethoxy silane, adjusting the pH of the system to 4, stirring for 50min, reacting at a constant temperature of 175 ℃ for 3h, cooling, centrifuging, washing the precipitate with water for 3 times, and drying at a temperature of 70 ℃ for 20 h; wherein the mass ratio of urea to sodium tartrate to vinyl trimethoxy silane is 2.1:0.36: 1.9;
adding polyethylene and an initiator into the reaction product, and reacting at 165 ℃ for 6 hours to obtain diffusion particles;
(2) preparing a membrane body:
mixing hydroxyl-terminated polybutadiene and glyoxylic acid, heating to 100 ℃, adding cyclohexane and p-toluenesulfonic acid in a nitrogen atmosphere, heating to 130 ℃ for reaction for 1h, vacuumizing for reaction for 2h, and purifying with absolute ethanol to obtain aldehyde-terminated polybutadiene, wherein the molar ratio of hydroxyl in the hydroxyl-terminated polybutadiene to the glyoxylic acid, the cyclohexane and the p-toluenesulfonic acid is 1:1:0.1: 0.06;
mixing aldehyde-terminated polybutadiene and m-phenylenediamine, wherein the molar ratio of aldehyde to m-phenylenediamine in the aldehyde-terminated polybutadiene is 1:0.5, heating to 160 ℃, adding acetic acid, stirring, reacting for 6 hours, centrifuging, washing and drying to obtain modified polybutadiene;
taking a pure titanium substrate, polishing the pure titanium substrate by using metallographic abrasive paper, cleaning the pure titanium substrate by using acetone and absolute ethyl alcohol, drying the pure titanium substrate for 100min at the temperature of 70 ℃, and cleaning a mixed solution of nitric acid and hydrofluoric acid; placing in 1mol/L sodium bromide solution with the solution temperature of 1 deg.C, etching at 500mA/cm current density for 5min, and soaking in mixed solution of nitric acid and hydrofluoric acid for 1min to obtain template;
taking diffusion particles, modified polybutadiene, maleic anhydride and an initiator, wherein the mass ratio of the diffusion particles to the modified polybutadiene to the maleic anhydride is 10:100:4, heating to 156 ℃, mixing, coating on the surface of a template, hot-pressing at 65 ℃ for 5min, cooling to form a film, transversely stretching by 30 times, and longitudinally stretching by 10 times to obtain a diffusion film body;
(3) preparing a diffusion film:
taking tripropylene glycol diacrylate, polyurethane acrylate and a photoinitiator, wherein the mass ratio of the tripropylene glycol diacrylate to the polyurethane acrylate to the photoinitiator is 5:15:0.4, preparing a coating, mixing and stirring uniformly in the absence of light, coating the coating on the surface of a diffusion membrane body, compounding the coating surface with a base membrane, coating the surface with the coating, carrying out ultrasonic treatment for 5min, and curing for 10min under ultraviolet light to obtain the diffusion membrane.
The base film is polyethylene terephthalate subjected to surface treatment by oxygen plasma, and the ratio of the thickness of the diffusion film to the thickness of the diffusion film body is 2: 1.
Example 2
(1) Preparing diffusion particles:
mixing tetraethyl orthosilicate and ammonia water, adding absolute ethyl alcohol, stirring at room temperature, reacting for 5.5 hours, centrifuging, washing the precipitate with ethanol for 4 times, and drying to obtain silicon dioxide microspheres;
taking silicon dioxide microspheres, and injecting zinc ions by using a metal vapor vacuum arc ion implanter, wherein the process comprises the following steps: acceleration voltage 28kV, injection amount 1.5 × 1017/cm2Zinc ion energy 107keV, beam density 4.5 muA/cm2Annealing, and the process comprises: preparing modified silicon dioxide microspheres in an oxygen atmosphere at the annealing temperature of 800 ℃ for 4 hours;
adding deionized water into modified silicon dioxide microspheres, performing ultrasonic dispersion for 65min, adding urea and sodium tartrate, stirring, adding vinyl trimethoxy silane, adjusting the pH of the system to 3.5, stirring for 65min, reacting at a constant temperature of 180 ℃ for 3.5h, cooling, centrifuging, washing the precipitate with water for 4 times, and drying at a temperature of 75 ℃ for 24 h; wherein the mass ratio of urea to sodium tartrate to vinyl trimethoxy silane is 2.1:0.38: 1.9;
adding polyethylene and an initiator into the reaction product, and reacting at the temperature of 183 ℃ for 8 hours to obtain diffusion particles;
(2) preparing a membrane body:
mixing hydroxyl-terminated polybutadiene and glyoxylic acid, heating to 130 ℃, adding cyclohexane and p-toluenesulfonic acid in a nitrogen atmosphere, heating to 145 ℃ to react for 1.5h, vacuumizing to react for 3h, and purifying with absolute ethanol to obtain aldehyde-terminated polybutadiene, wherein the molar ratio of hydroxyl in the hydroxyl-terminated polybutadiene to the glyoxylic acid, the cyclohexane and the p-toluenesulfonic acid is 1:1:0.1: 0.07;
mixing aldehyde-terminated polybutadiene and m-phenylenediamine, wherein the molar ratio of aldehyde to m-phenylenediamine in the aldehyde-terminated polybutadiene is 1:0.5, heating to 205 ℃, adding acetic acid, stirring, reacting for 8 hours, centrifuging, washing and drying to obtain modified polybutadiene;
taking a pure titanium substrate, polishing the pure titanium substrate by using metallographic abrasive paper, cleaning the pure titanium substrate by using acetone and absolute ethyl alcohol, drying the pure titanium substrate for 120min at the temperature of 75 ℃, and cleaning a mixed solution of nitric acid and hydrofluoric acid; placing in 1mol/L sodium bromide solution with the solution temperature of 0 deg.C, etching at 500mA/cm current density for 6min, and soaking in mixed solution of nitric acid and hydrofluoric acid for 1.5min to obtain template;
taking diffusion particles, modified polybutadiene, maleic anhydride and an initiator, wherein the mass ratio of the diffusion particles to the modified polybutadiene to the maleic anhydride is 12:100:5, heating to 167 ℃, mixing, coating on the surface of a template, hot-pressing at 70 ℃ for 10min, cooling to form a film, transversely stretching by 40 times, and longitudinally stretching by 20 times to obtain a diffusion film body;
(3) preparing a diffusion film:
taking tripropylene glycol diacrylate, polyurethane acrylate and a photoinitiator, wherein the mass ratio of the tripropylene glycol diacrylate to the polyurethane acrylate to the photoinitiator is 5:17:0.4, preparing a coating, mixing and stirring uniformly in the absence of light, coating the coating on the surface of a diffusion membrane body, compounding the coating surface with a base membrane, coating the coating on the surface, carrying out ultrasonic treatment for 7min, and curing for 12min under ultraviolet light to obtain the diffusion membrane.
The base film was polyethylene terephthalate surface-treated with oxygen plasma, and the ratio of the thickness of the diffusion film to the thickness of the diffusion film body was 2.5: 1.
Example 3
(1) Preparing diffusion particles:
mixing tetraethyl orthosilicate and ammonia water, adding absolute ethyl alcohol, stirring at room temperature, reacting for 6 hours, centrifuging, taking precipitate, washing for 5 times by using the ethanol, and drying to obtain silicon dioxide microspheres;
taking silicon dioxide microspheres, and injecting zinc ions by using a metal vapor vacuum arc ion implanter, wherein the process comprises the following steps: accelerating voltage of 30kV and injection amount of 1.8 × 1017/cm2Zinc ion energy 140keV, beam density 7.0 muA/cm2Annealing, and the process comprises: preparing modified silicon dioxide microspheres in an oxygen atmosphere at the annealing temperature of 900 ℃ for 2 hours;
adding deionized water into modified silicon dioxide microspheres, performing ultrasonic dispersion for 80min, adding urea and sodium tartrate, stirring, adding vinyl trimethoxy silane, adjusting the pH value of the system to 3, stirring for 80min, reacting at the constant temperature of 185 ℃ for 4h, cooling, centrifuging, washing the precipitate for 5 times, and drying at the temperature of 80 ℃ for 27 h; wherein the mass ratio of urea to sodium tartrate to vinyl trimethoxy silane is 2.1:0.40: 2.0;
adding polyethylene and an initiator into a reaction product, and reacting at the temperature of 200 ℃ for 10 hours to obtain diffusion particles;
(2) preparing a membrane body:
mixing hydroxyl-terminated polybutadiene and glyoxylic acid, heating to 160 ℃, adding cyclohexane and p-toluenesulfonic acid in a nitrogen atmosphere, heating to 160 ℃ to react for 2 hours, vacuumizing to react for 4 hours, and purifying with absolute ethanol to obtain aldehyde-terminated polybutadiene, wherein the molar ratio of hydroxyl in the hydroxyl-terminated polybutadiene to the glyoxylic acid, the cyclohexane and the p-toluenesulfonic acid is 1:1:0.2: 0.09;
mixing aldehyde-terminated polybutadiene and m-phenylenediamine, wherein the molar ratio of aldehyde to m-phenylenediamine in the aldehyde-terminated polybutadiene is 1:0.5, heating to 250 ℃, adding acetic acid, stirring, reacting for 12 hours, centrifuging, washing and drying to obtain modified polybutadiene;
taking a pure titanium substrate, polishing the pure titanium substrate by using metallographic abrasive paper, cleaning the pure titanium substrate by using acetone and absolute ethyl alcohol, drying the pure titanium substrate for 140min at the temperature of 80 ℃, and cleaning a mixed solution of nitric acid and hydrofluoric acid; placing in 1mol/L sodium bromide solution with the solution temperature of 0 deg.C, etching at 500mA/cm current density for 7min, and soaking in mixed solution of nitric acid and hydrofluoric acid for 2min to obtain template;
taking the diffusion particles, the modified polybutadiene, the maleic anhydride and the initiator, wherein the mass ratio of the diffusion particles to the modified polybutadiene to the maleic anhydride is 15:100:6, heating to 178 ℃, mixing, coating on the surface of a template, hot-pressing at 75 ℃ for 15min, cooling to form a film, transversely stretching by 50 times, and longitudinally stretching by 30 times to obtain a diffusion film body;
(3) preparing a diffusion film:
taking tripropylene glycol diacrylate, polyurethane acrylate and a photoinitiator, wherein the mass ratio of the tripropylene glycol diacrylate to the polyurethane acrylate to the photoinitiator is 5:19:0.5, preparing a coating, mixing and stirring uniformly in the absence of light, coating the coating on the surface of a diffusion membrane body, compounding the coating surface with a base membrane, coating the coating on the surface, carrying out ultrasonic treatment for 10min, and curing for 15min under ultraviolet light to obtain the diffusion membrane.
The base film is polyethylene terephthalate subjected to surface treatment by oxygen plasma, and the ratio of the thickness of the diffusion film to the thickness of the diffusion film body is 3: 1.
Comparative example 1
(1) Preparing diffusion particles:
mixing tetraethyl orthosilicate and ammonia water, adding absolute ethyl alcohol, stirring at room temperature, reacting for 5.5 hours, centrifuging, washing the precipitate with ethanol for 4 times, and drying to obtain silicon dioxide microspheres;
adding deionized water into the silica microspheres, performing ultrasonic dispersion for 65min, adding urea and sodium tartrate, stirring, adding vinyl trimethoxy silane, adjusting the pH of the system to 3.5, stirring for 65min, reacting at a constant temperature of 180 ℃ for 3.5h, cooling, centrifuging, washing the precipitate with water for 4 times, and drying at a temperature of 75 ℃ for 24 h; wherein the mass ratio of urea to sodium tartrate to vinyl trimethoxy silane is 2.1:0.38: 1.9;
adding polyethylene and an initiator into the reaction product, and reacting at the temperature of 183 ℃ for 8 hours to obtain diffusion particles;
the other preparation process was the same as in example 2, and a diffusion film was prepared.
Comparative example 2
(1) Preparing diffusion particles:
mixing tetraethyl orthosilicate and ammonia water, adding absolute ethyl alcohol, stirring at room temperature, reacting for 5.5 hours, centrifuging, washing the precipitate with ethanol for 4 times, and drying to obtain silicon dioxide microspheres;
taking silicon dioxide microspheres, and injecting zinc ions by using a metal vapor vacuum arc ion implanter, wherein the process comprises the following steps: acceleration voltage 28kV, injection amount 1.5 × 1017/cm2Zinc ion energy 107keV, beam density 4.5 muA/cm2Annealing, and the process comprises: preparing modified silicon dioxide microspheres in an oxygen atmosphere at the annealing temperature of 800 ℃ for 4 hours;
adding deionized water into modified silicon dioxide microspheres, performing ultrasonic dispersion for 65min, adding urea and sodium tartrate, stirring, adding vinyl trimethoxy silane, adjusting the pH of the system to 3.5, stirring for 65min, reacting at a constant temperature of 180 ℃ for 3.5h, cooling, centrifuging, washing the precipitate with water for 4 times, and drying at a temperature of 75 ℃ for 24 h; wherein the mass ratio of urea to sodium tartrate to vinyl trimethoxy silane is 2.1:0.38: 1.9;
adding polyethylene and an initiator into the reaction product, and reacting at the temperature of 183 ℃ for 8 hours to obtain diffusion particles;
(2) preparing a diffusion film:
taking tripropylene glycol diacrylate, polyurethane acrylate, a photoinitiator and diffusion particles, wherein the mass ratio of the tripropylene glycol diacrylate to the polyurethane acrylate to the photoinitiator to the diffusion particles is 5:17:0.4:2, preparing a coating, mixing and stirring uniformly in the absence of light, coating the coating on the surface of a diffusion film body, compounding the coating surface and a base film, coating the coating on the surface, carrying out ultrasonic treatment for 7min, and curing for 12min under ultraviolet light to obtain the diffusion film.
The base film was polyethylene terephthalate surface-treated with oxygen plasma, and the ratio of the thickness of the diffusion film to the thickness of the diffusion film body was 2.5: 1.
Comparative example 3
(1) Preparing diffusion particles:
mixing tetraethyl orthosilicate and ammonia water, adding absolute ethyl alcohol, stirring at room temperature, reacting for 5.5 hours, centrifuging, washing the precipitate with ethanol for 4 times, and drying to obtain silicon dioxide microspheres;
taking silicon dioxide microspheres, and injecting zinc ions by using a metal vapor vacuum arc ion implanter, wherein the process comprises the following steps: acceleration voltage 28kV, injection amount 1.5 × 1017/cm2Zinc ion energy 107keV, beam density 4.5 muA/cm2Annealing, and the process comprises: preparing modified silicon dioxide microspheres in an oxygen atmosphere at the annealing temperature of 800 ℃ for 4 hours;
adding deionized water into modified silicon dioxide microspheres, performing ultrasonic dispersion for 65min, adding urea and sodium tartrate, stirring, adding vinyl trimethoxy silane, adjusting the pH of the system to 3.5, stirring for 65min, reacting at a constant temperature of 180 ℃ for 3.5h, cooling, centrifuging, washing the precipitate with water for 4 times, and drying at a temperature of 75 ℃ for 24 h; wherein the mass ratio of urea to sodium tartrate to vinyl trimethoxy silane is 2.1:0.38: 1.9;
adding polyethylene and an initiator into the reaction product, and reacting at the temperature of 183 ℃ for 8 hours to obtain diffusion particles;
(2) preparing a membrane body:
taking diffusion particles, polybutadiene, maleic anhydride and an initiator, wherein the mass ratio of the diffusion particles to the modified polybutadiene to the maleic anhydride is 12:100:5, heating to 167 ℃, mixing, coating on the surface of a template, hot-pressing at 70 ℃ for 10min, cooling to form a film, transversely stretching by 40 times, and longitudinally stretching by 20 times to obtain a diffusion film body;
(3) preparing a diffusion film:
taking tripropylene glycol diacrylate, polyurethane acrylate and a photoinitiator, wherein the mass ratio of the tripropylene glycol diacrylate to the polyurethane acrylate to the photoinitiator is 5:17:0.4, preparing a coating, mixing and stirring uniformly in the absence of light, coating the coating on the surface of a diffusion membrane body, compounding the coating surface with a base membrane, coating the coating on the surface, carrying out ultrasonic treatment for 7min, and curing for 12min under ultraviolet light to obtain the diffusion membrane.
The base film was polyethylene terephthalate surface-treated with oxygen plasma, and the ratio of the thickness of the diffusion film to the thickness of the diffusion film body was 2.5: 1.
Comparative example 4
(2) Preparing a membrane body:
mixing hydroxyl-terminated polybutadiene and glyoxylic acid, heating to 130 ℃, adding cyclohexane and p-toluenesulfonic acid in a nitrogen atmosphere, heating to 145 ℃ to react for 1.5h, vacuumizing to react for 3h, and purifying with absolute ethanol to obtain aldehyde-terminated polybutadiene, wherein the molar ratio of hydroxyl in the hydroxyl-terminated polybutadiene to the glyoxylic acid, the cyclohexane and the p-toluenesulfonic acid is 1:1:0.1: 0.07;
mixing aldehyde-terminated polybutadiene and m-phenylenediamine, wherein the molar ratio of aldehyde to m-phenylenediamine in the aldehyde-terminated polybutadiene is 1:0.5, heating to 205 ℃, adding acetic acid, stirring, reacting for 8 hours, centrifuging, washing and drying to obtain modified polybutadiene;
taking a pure titanium substrate, polishing the pure titanium substrate by using metallographic abrasive paper, cleaning the pure titanium substrate by using acetone and absolute ethyl alcohol, drying the pure titanium substrate for 120min at the temperature of 75 ℃, and cleaning a mixed solution of nitric acid and hydrofluoric acid; placing in 1mol/L sodium bromide solution with the solution temperature of 0 deg.C, etching at 500mA/cm current density for 6min, and soaking in mixed solution of nitric acid and hydrofluoric acid for 1.5min to obtain template;
taking diffusion particles and modified polybutadiene, wherein the mass ratio of the diffusion particles to the modified polybutadiene is 12:100, heating to 167 ℃, mixing, coating on the surface of a template, hot-pressing at 70 ℃ for 10min, cooling to form a film, transversely stretching by 40 times, and longitudinally stretching by 20 times to obtain a diffusion film body;
the other preparation process was the same as in example 2, and a diffusion film was prepared.
Comparative example 5
Step (1) and step (2) are the same as in example 2;
(3) preparing a diffusion film:
and placing a diffusion film body on the surface of a base film, and carrying out hot pressing to obtain the diffusion film, wherein the base film is polyethylene terephthalate subjected to surface treatment by oxygen plasma, and the ratio of the thickness of the diffusion film to the thickness of the diffusion film body is 2.5: 1.
Comparative example 6
And taking the base film as a diffusion film.
Experiment of
Samples were prepared from the diffusion films obtained in examples 1 to 3 and comparative examples 1 to 6, and the light transmittance, haze, abrasion resistance, and flexibility were measured and the measurement results were recorded:
wear resistance test: taking an abrasive wear testing machine to test the wear resistance of a sample, wherein the size of the sample is 40mm multiplied by 25mm, carrying out rotary sliding friction on the surface of a fixed sample by using a No. 45 steel ring with a chromium-plated surface at room temperature and 65% relative humidity, applying a load of 180N, clockwise rotating a steel wheel at a rotation speed of 200r/min for 2h, measuring the mass of the sample before and after wear by using an electronic balance after the test, and calculating the wear loss with the precision of 0.1 mg;
flexibility experiment: testing the flexibility of the test sample by using a repeated bending machine, repeatedly bending the test sample at the frequency of 1 time/s, and testing the light transmittance and haze of the test sample after bending for 5 ten thousand times;
from the data in the table above, it is clear that the following conclusions can be drawn:
the diffusion films obtained in examples 1 to 3 were compared with the diffusion films obtained in comparative examples 1 to 6, and the results of the tests showed that:
1. compared with the diffusion film obtained in the comparative example 6, the diffusion film obtained in the examples 1 to 3 has the advantages that the haze data are obviously improved, the transmittance and wear rate data are better, and the transmittance and haze data after repeated bending are better represented, which fully indicates that the diffusion film prepared by the invention has better bending fatigue resistance and wear resistance while keeping better light diffusion performance;
2. compared with the diffusion film obtained in example 2, zinc ions are not injected into the silica microspheres in comparative example 1, modified polydibutene is not added in comparative example 2, polybutadiene is not modified in comparative example 3, the diffusion particles are not crosslinked with the modified polybutadiene in comparative example 4, and the coating is not arranged in comparative example 5, so that the transmittance, haze and wear rate data, the transmittance and haze data after repeated bending are changed, and the overall performance orientation is degraded.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Furthermore, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process method article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process method article or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A preparation process of a wear-resistant flexible diffusion film is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing diffusion particles:
mixing a silicon source and ammonia water, adding absolute ethyl alcohol, and stirring for reaction to prepare silicon dioxide microspheres;
taking the silicon dioxide microspheres, injecting zinc ions, and annealing to prepare modified silicon dioxide microspheres;
adding deionized water into modified silicon dioxide microspheres for dispersion, adding urea and sodium tartrate, stirring, adding vinyl trimethoxy silane, adjusting the system to acidity, and heating for reaction; adding polyethylene and an initiator into the reaction product, and heating for reaction to obtain diffusion particles;
(2) preparing a membrane body:
taking hydroxyl-terminated polybutadiene and glyoxylic acid, mixing, and heating for reaction to obtain aldehyde-terminated polybutadiene;
mixing aldehyde-terminated polybutadiene and m-phenylenediamine, and heating for reaction to obtain modified polybutadiene;
soaking a pure titanium substrate in a sodium hydroxide solution, soaking a sodium bicarbonate solution, and boiling in boiling water to obtain a template;
heating and mixing diffusion particles, modified polybutadiene, maleic anhydride and an initiator, coating the mixture on the surface of a template, cooling to form a film, and stretching to obtain a diffusion film body;
(3) preparing a diffusion film:
taking tripropylene glycol diacrylate, urethane acrylate and a photoinitiator to prepare a coating, coating the coating on the surface of a diffusion membrane body, compounding the coating surface with a base membrane, and carrying out ultraviolet curing to prepare the diffusion membrane.
2. The process of claim 1 for preparing a wear resistant flexible diffusion membrane, wherein: the step (1) comprises the following steps:
mixing tetraethyl orthosilicate and ammonia water, adding absolute ethyl alcohol, stirring at room temperature, reacting for 5-6 h, centrifuging, washing a precipitate with ethanol for 3-5 times, and drying to obtain silicon dioxide microspheres;
taking silicon dioxide microspheres, and injecting zinc ions by using a metal vapor vacuum arc ion implanter, wherein the process comprises the following steps: accelerating voltage of 27-30 kV, and injection amount of 1.2 × 1017～1.8×1017/cm2The energy of zinc ion is 87-140 keV, and the beam density is 2.0-7.0 muA/cm2Annealing, and the process comprises: in an oxygen atmosphere, annealing at 400-900 ℃ for 1-8 h to prepare modified silicon dioxide microspheres;
adding deionized water into modified silicon dioxide microspheres, performing ultrasonic dispersion for 50-80 min, adding urea and sodium tartrate, stirring, adding vinyl trimethoxy silane, adjusting the pH value of a system to 3-4, stirring for 50-80 min, reacting at a constant temperature of 175-185 ℃ for 3-4 h, cooling, centrifuging, taking out a precipitate, washing with water for 3-5 times, and drying at a temperature of 70-80 ℃ for 20-27 h;
and (3) taking a reaction product, adding polyethylene and an initiator, and reacting at the temperature of 165-200 ℃ for 6-10 hours to obtain the diffusion particles.
3. The process of claim 2 for preparing a wear resistant flexible diffusion membrane, wherein: in the step (1), the mass ratio of urea to sodium tartrate to vinyltrimethoxysilane is 2.1 (0.36-0.40) to 1.9-2.0.
4. The process of claim 1 for preparing a wear resistant flexible diffusion membrane, wherein: the step (2) comprises the following steps:
mixing hydroxyl-terminated polybutadiene and glyoxylic acid, heating to 100-160 ℃, adding cyclohexane and p-toluenesulfonic acid in a nitrogen atmosphere, heating to 130-160 ℃, reacting for 1-2 h, vacuumizing, reacting for 2-4 h, and purifying with absolute ethanol to obtain aldehyde-terminated polybutadiene;
mixing aldehyde-terminated polybutadiene and m-phenylenediamine, heating to 160-250 ℃, adding acetic acid, stirring, reacting for 6-12 h, centrifuging, washing and drying to obtain modified polybutadiene;
taking a pure titanium substrate, polishing the pure titanium substrate by using metallographic abrasive paper, cleaning the pure titanium substrate by using acetone and absolute ethyl alcohol, drying the pure titanium substrate for 100-140 min at the temperature of 70-80 ℃, and cleaning a mixed solution of nitric acid and hydrofluoric acid; placing the template in a 1mol/L sodium bromide solution, etching the template for 5-7 min at the solution temperature of 0-1 ℃ and the current density of 500mA/cm, and soaking the template in a mixed solution of nitric acid and hydrofluoric acid for 1-2 min to obtain the template;
heating the diffusion particles, modified polybutadiene, maleic anhydride and an initiator to 156-178 ℃, mixing, coating on the surface of a template, hot-pressing for 5-15 min at 65-75 ℃, cooling to form a film, transversely stretching by 30-50 times, and longitudinally stretching by 10-30 times to obtain the diffusion film body.
5. The process of claim 4, wherein the flexible diffusion membrane is prepared by: the molar ratio of hydroxyl in the hydroxyl-terminated polybutadiene to glyoxylic acid, cyclohexane and p-toluenesulfonic acid is 1:1 (0.1-0.2) to (0.06-0.09), the molar ratio of aldehyde group in the aldehyde-terminated polybutadiene to m-phenylenediamine is 1:0.5, and the mass ratio of the diffusion particles, the modified polybutadiene and the maleic anhydride is (10-15) to 100 (4-6).
6. The process of claim 1 for preparing a wear resistant flexible diffusion membrane, wherein: the step (3) comprises the following steps:
taking tripropylene glycol diacrylate, urethane acrylate and a photoinitiator to prepare a coating, mixing and stirring uniformly in the absence of light, coating the coating on the surface of a diffusion membrane body, compounding the coating surface with a base membrane, coating the coating on the surface, carrying out ultrasonic treatment for 5-10 min, and curing for 10-15 min under ultraviolet light to prepare the diffusion membrane.
7. The process of claim 6, wherein the diffusion membrane is prepared by the following steps: the mass ratio of the tripropylene glycol diacrylate, the urethane acrylate and the photoinitiator is 5 (15-19) to 0.4-0.5.
8. The process of claim 1 for preparing a wear resistant flexible diffusion membrane, wherein: the base film is made of polyethylene terephthalate and is subjected to surface treatment by oxygen plasma, and the ratio of the thickness of the diffusion film to the thickness of the diffusion film body is (2-3): 1.
9. A wear resistant flexible diffusion membrane made by a process of making a wear resistant flexible diffusion membrane according to any of claims 1-8.
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Application publication date: 20211203 |