CN111399096B - Optical diffusion film and manufacturing method thereof - Google Patents
Optical diffusion film and manufacturing method thereof Download PDFInfo
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- CN111399096B CN111399096B CN202010252986.7A CN202010252986A CN111399096B CN 111399096 B CN111399096 B CN 111399096B CN 202010252986 A CN202010252986 A CN 202010252986A CN 111399096 B CN111399096 B CN 111399096B
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/02—Diffusing elements; Afocal elements
- G02B5/0205—Diffusing elements; Afocal elements characterised by the diffusing properties
- G02B5/021—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place at the element's surface, e.g. by means of surface roughening or microprismatic structures
- G02B5/0226—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place at the element's surface, e.g. by means of surface roughening or microprismatic structures having particles on the surface
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/02—Diffusing elements; Afocal elements
- G02B5/0268—Diffusing elements; Afocal elements characterized by the fabrication or manufacturing method
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/1336—Illuminating devices
- G02F1/133602—Direct backlight
- G02F1/133606—Direct backlight including a specially adapted diffusing, scattering or light controlling members
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Abstract
The invention discloses an optical diffusion film and a manufacturing method thereof, wherein the optical diffusion film comprises the following steps: the optical diffusion film takes a PET film as a base material, and a light diffusion layer is solidified on the surface of the PET film; the light diffusion layer comprises the following raw materials in parts by mass: 100 parts of urethane acrylate, 25-35 parts of tripropylene glycol diacrylate, 10-30 parts of core-shell light diffusion microspheres and 1-3 parts of photoinitiator; the preparation method of the core-shell type photodiffusion microsphere comprises the following steps: adjusting the pH value of 35-50% (v/v) ethanol solution to 3.0-5.0, adding APS, VTMS and phenyltriethoxysilane, magnetically stirring at 25-40 ℃ for reaction for 2-6 h, adjusting the pH value to 9-11, continuing the reaction for 3-8 h, and adding Zn (NO)3)2·6H2O、Ce(NO3)3·6H2O、Al(NO3)3·9H2O, HTM, magnetically stirring for 0.5-1 h, refluxing for 3-5 h at 80 ℃, cooling to 40-50 ℃, dropwise adding glutaraldehyde for crosslinking modification for 1-2 h, and centrifugally washing and drying. The optical diffusion film disclosed by the invention is uniform and stable, good in weather resistance and durability, and has a visible light transmittance of more than 93%, a haze of more than 85%, an ultraviolet light transmittance of less than 12%, and a 400-480 nm short-wave blue light transmittance of less than 15%.
Description
Technical Field
The invention belongs to the technical field of optical films, and particularly relates to an optical diffusion film and a manufacturing method thereof.
Background
The diffusion film is mainly an optical film applied to a backlight system of an LCD module. The diffusion film takes PET with high transparency as a base material, a layer of randomly dispersed diffusion particles with a micron structure is precisely coated on the surface of acrylic resin, and the diffusion particles are applied to an LCD (liquid crystal display), so that light is subjected to multiple refraction, reflection and diffraction phenomena through a diffusion layer to be corrected into a uniform surface light source, the optical diffusion effect is achieved, and the light is displayed more uniformly and softly.
The light diffusing agent is mainly classified into an inorganic light diffusing agent and an organic light diffusing agent, wherein the former includes silica, alumina, titanium oxide, barium sulfate, calcium carbonate and the like, and the latter includes acrylic polymers, siloxane polymers, polystyrene microspheres and the like. The organic light diffusion particles have high light transmission, ultraviolet rays and short-wave blue light with the wavelength of 400-480 nm can directly penetrate through the diffusion particles, the problems of dazzling and retina radiation damage are easily caused, and the inorganic particles are poor in dispersibility in resin, the agglomeration phenomenon is easily caused, and the stability and the quality of a diffusion film are influenced.
Based on the above, the invention utilizes the hydrolysis polycondensation reaction of aminopropyltrimethoxysilane, vinyltrimethoxysilane and phenyltriethoxysilane to prepare the organic silicon microsphere precursor core, and further grows nano ZnO/CeO in situ on the surface of the organic silicon microsphere precursor core2/Al2O3And the chemical crosslinking action of the glutaraldehyde intermediate and amino is utilized to lead the core-shell type photodiffusion microspheres and the polyurethane acrylate to generate graft copolymerization, thereby obviously improving the stability of the photodiffusion layer.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an optical diffusion film and a manufacturing method thereof.
The technical scheme of the invention is summarized as follows:
an optical diffusion film: the optical diffusion film takes a PET film as a base material, and a light diffusion layer is solidified on the surface of the PET film; the light diffusion layer comprises the following raw materials in parts by mass:
the preparation method of the core-shell type photodiffusion microsphere comprises the following steps: h is to be2SO4Adding the solution into 35-50% (v/v) ethanol solution, adjusting the pH to 3.0-5.0, adding aminopropyltrimethoxysilane, vinyltrimethoxysilane and phenyltriethoxysilane, magnetically stirring at 25-40 ℃ for reaction for 2-6 h, adding NaOH solution to adjust the pH to 9-11, and continuing to react for 3-8 h to obtain organic silicon microsphere suspension;
adding Zn (NO) into the obtained organosilicon microsphere suspension3)2·6H2O、Ce(NO3)2·6H2O、Al(NO3)3·9H2O and hexamethylenetetramine are magnetically stirred for 0.5-1 h, the mixture is refluxed for 3-5 h at the temperature of 80 ℃, is reduced to 40-50 ℃, is dropwise added with glutaraldehyde for crosslinking modification for 1-2 h, is reduced to room temperature, is centrifuged to obtain a precipitate, is alternately washed for 2-3 times by deionized water and ethanol, and is dried in vacuum to obtain the core-shell type light diffusion microsphere;
in each 100mL of 35-50% (v/v) ethanol solution, the dosage of each reaction raw material is as follows: 2-3 mL of aminopropyltrimethoxysilane, 1-2 mL of vinyltrimethoxysilane, 0.5-1 mL of phenyltriethoxysilane, and Zn (NO)3)2·6H2O 0.1～0.2g、Ce(NO3)2·6H2O 0.2～0.3g、Al(NO3)3·9H20.1-0.2 g of O, 0.8-1.2 g of hexamethylenetetramine and 1.5-3 mL of glutaraldehyde.
Preferably, the thickness of the PET film is 45-60 mu m.
Preferably, the thickness of the light diffusion layer is 8-10 μm.
Preferably, the photoinitiator is one or more of a photoinitiator 1173, a photoinitiator 184, a photoinitiator 907 and a photoinitiator 1490.
Preferably, said H2SO4The concentration of the solution is 0.5-2 mol/L.
Preferably, the concentration of the NaOH solution is 0.2-1 mol/L.
A manufacturing method of an optical diffusion film comprises the following steps:
s1: preparing a light diffusion layer coating: under the condition of no light, uniformly stirring urethane acrylate, tripropylene glycol diacrylate, core-shell light diffusion microspheres and a photoinitiator to obtain a light diffusion layer coating;
s2: ultraviolet light imprinting: at a wavelength of 365nm and an intensity of 420mJ cm-2Under the radiation of ultraviolet rays, coating the light diffusion layer coating on the PET film, impressing the PET film by utilizing the PDMS stamper, and demolding after complete curing to obtain the optical diffusion film.
The invention has the beneficial effects that:
1. the invention firstly utilizes the hydrolytic polycondensation reaction of aminopropyl trimethoxy silane, vinyl trimethoxy silane and phenyl triethoxy silane to prepare an organosilicon microsphere precursor core, and further grows nano ZnO/CeO on the surface of the organosilicon microsphere precursor core in an uneven and in-situ manner2/Al2O3And the chemical crosslinking action of the glutaraldehyde intermediate and amino is utilized to lead the core-shell type photodiffusion microspheres and the polyurethane acrylate to generate graft copolymerization, thereby obviously improving the stability of the photodiffusion layer.
2. Because of the nanometer ZnO/CeO2/Al2O3The organic silicon microspheres are distributed on the surface of the organic silicon microsphere in a non-uniform way, so that when light is projected into the light diffusion layer, refraction and diffuse reflection phenomena in different angles and different directions occur, the diffusion performance of the diffusion film on visible light is obviously improved, and meanwhile, the nano ZnO/CeO2/Al2O3Effectively improves the haze of the light diffusion microspheres, has obvious shielding effect on ultraviolet rays and 400-480 nm short-wave blue light, and prevents dazzling and short-wave radiation from stimulating and damaging the retina.
3. The optical diffusion film disclosed by the invention is uniform and stable, good in weather resistance and durability, and has a visible light transmittance of more than 93%, a haze of more than 85%, an ultraviolet light transmittance of less than 12%, and a 400-480 nm short-wave blue light transmittance of less than 15%.
Drawings
FIG. 1 is a flow chart of a method for fabricating an optical diffusion film according to the present invention.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
Example 1
S1: preparing core-shell light diffusion microspheres: 0.5mol/L H2SO4Adding the solution into 1000mL of 35% (v/v) ethanol solution, adjusting pH to 3.5, adding 20mL of aminopropyltrimethoxysilane, 10mL of vinyltrimethoxysilane and 5mL of phenyltriethoxysilane, magnetically stirring at 25 deg.C for reaction for 3h, adding 0.2mol/L NaOH solution to adjust pH to 10, continuing reaction for 3h,obtaining an organic silicon microsphere suspension;
adding 1g Zn (NO) into the obtained organosilicon microsphere suspension3)2·6H2O、2g Ce(NO3)3·6H2O、1g Al(NO3)3·9H2Magnetically stirring O and 8g of hexamethylenetetramine for 0.5h, refluxing for 3h at 80 ℃, reducing the temperature to 40 ℃, dropwise adding 15mL of glutaraldehyde for crosslinking modification for 1h, reducing the temperature to room temperature, centrifuging to obtain a precipitate, alternately washing with deionized water and ethanol for 2 times, and drying in vacuum to obtain the core-shell type light diffusion microsphere;
s2: preparing a light diffusion layer coating: weighing 100g of urethane acrylate, 25g of tripropylene glycol diacrylate, 10g of core-shell light diffusion microspheres and 11731 g of photoinitiator, and uniformly stirring in the absence of light to obtain a light diffusion layer coating;
s3: ultraviolet light imprinting: at a wavelength of 365nm and an intensity of 420mJ cm-2Under the radiation of ultraviolet rays, coating the light diffusion layer coating on a 60-mu mPE film, wherein the thickness of the light diffusion layer coating is 10 mu m, stamping the light diffusion layer coating by utilizing a PDMS (polydimethylsiloxane) die, and demolding after the light diffusion layer coating is completely cured to obtain the optical diffusion film.
Example 2
S1: preparing core-shell light diffusion microspheres: 1.5mol/L H2SO4Adding the solution into 1000mL of 35-50% (v/v) ethanol solution, adjusting the pH to 4.0, adding 25mL of aminopropyltrimethoxysilane, 15mL of vinyltrimethoxysilane and 7.5mL of phenyltriethoxysilane, magnetically stirring at 30 ℃ for reaction for 4 hours, adding 0.5mol/L of NaOH solution, adjusting the pH to 10, and continuing the reaction for 6 hours to obtain an organic silicon microsphere suspension;
then 1.5g Zn (NO) is added into the obtained organosilicon microsphere suspension3)2·6H2O、2.5gCe(NO3)3·6H2O、1.5g Al(NO3)3·9H2Stirring O and 10g of hexamethylenetetramine by magnetic force for 1h, refluxing for 4h at 80 ℃, reducing the temperature to 45 ℃, dropwise adding 20mL of glutaraldehyde for crosslinking modification for 1-2 h, reducing the temperature to room temperature, centrifuging to obtain a precipitate, alternately washing with deionized water and ethanol for 2-3 times, and drying in vacuum to obtain the core-shell type light diffusion microsphere;
s2: preparing a light diffusion layer coating: weighing 100g of urethane acrylate, 20g of tripropylene glycol diacrylate, 15g of core-shell light diffusion microspheres and 11731-3 g of photoinitiator, and uniformly stirring in the absence of light to obtain a light diffusion layer coating;
s3: ultraviolet light imprinting: at a wavelength of 365nm and an intensity of 420mJ cm-2Under the radiation of ultraviolet rays, coating the light diffusion layer coating on a 60-mu mPE film, wherein the thickness of the light diffusion layer coating is 10 mu m, stamping the light diffusion layer coating by utilizing a PDMS (polydimethylsiloxane) die, and demolding after the light diffusion layer coating is completely cured to obtain the optical diffusion film.
Example 3
S1: preparing core-shell light diffusion microspheres: 2mol/L H2SO4Adding the solution into 1000mL of 35-50% (v/v) ethanol solution, adjusting the pH to 4.5, adding 30mL of aminopropyltrimethoxysilane, 20mL of vinyltrimethoxysilane and 10mL of phenyltriethoxysilane, magnetically stirring at 40 ℃ for reaction for 6 hours, adding 1mol/L of NaOH solution, adjusting the pH to 10, and continuing to react for 8 hours to obtain an organic silicon microsphere suspension;
2g Zn (NO) was added to the resulting suspension of silicone microspheres3)2·6H2O、3g Ce(NO3)3·6H2O、2g Al(NO3)3·9H2Stirring O and 10g of hexamethylenetetramine by magnetic force for 1h, refluxing for 5h at 80 ℃, reducing the temperature to 50 ℃, dropwise adding 30mL of glutaraldehyde for crosslinking modification for 2h, reducing the temperature to room temperature, centrifuging to obtain a precipitate, alternately washing the precipitate for 3 times by using deionized water and ethanol, and drying in vacuum to obtain the core-shell type light diffusion microsphere;
s2: preparing a light diffusion layer coating: weighing 100g of urethane acrylate, 35g of tripropylene glycol diacrylate, 30g of core-shell light diffusion microspheres and 1843 g of photoinitiator, and uniformly stirring in the absence of light to obtain a light diffusion layer coating;
s3: ultraviolet light imprinting: at a wavelength of 365nm and an intensity of 420mJ cm-2Under the radiation of ultraviolet rays, coating the photodiffusion layer coating on a 60 mu mPE film, wherein the thickness of the photodiffusion layer coating is 10 mu m, imprinting the photodiffusion layer coating by utilizing a PDMS stamper, and demolding after completely curing to obtain the photodiffusion layer coatingThe optical diffusion film.
Comparative example 1: the same as in example 1, except that: directly centrifuging, washing and vacuum drying the organic silicon microsphere suspension to obtain the organic silicon microspheres, and replacing core-shell type photodiffusion microspheres with the organic silicon microspheres.
Comparative example 2: the same as in example 1, except that: mixing organosilicon microsphere with nanometer ZnO and CeO2Nano Al2O3Mixing at a mixing ratio of 3:0.1:0.15:0.1, and replacing the core-shell type light-diffusing microspheres with the obtained mixed light-diffusing particles.
Comparative example 3: the same as in example 1, except that: and no glutaraldehyde is added dropwise for crosslinking modification.
The optical performance indexes of the optical diffusion films prepared in examples 1 to 3 and comparative examples 1 to 3 are shown in the following table:
as can be seen from the above table, the optical diffusion film of the invention has uniform and stable quality, good weather resistance and durability, and has a transmittance of more than 93% for visible light, a haze of more than 85%, an ultraviolet transmittance of less than 12%, and a short-wave blue light transmittance of 400-480 nm of less than 15%.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (7)
1. An optical diffusion film characterized in that: the optical diffusion film takes a PET film as a base material, and a light diffusion layer is solidified on the surface of the PET film; the light diffusion layer comprises the following raw materials in parts by mass:
the preparation method of the core-shell type photodiffusion microsphere comprises the following steps: h is to be2SO4Adding the solution into 35-50% (v/v) ethanol solution, adjusting the pH to 3.0-5.0, adding aminopropyltrimethoxysilane, vinyltrimethoxysilane and phenyltriethoxysilane, magnetically stirring at 25-40 ℃ for reaction for 2-6 h, adding NaOH solution to adjust the pH to 9-11, and continuing to react for 3-8 h to obtain organic silicon microsphere suspension;
adding Zn (NO) into the obtained organosilicon microsphere suspension3)2·6H2O、Ce(NO3)3·6H2O、Al(NO3)3·9H2O and hexamethylenetetramine are magnetically stirred for 0.5-1 h, the mixture is refluxed for 3-5 h at the temperature of 80 ℃, is reduced to 40-50 ℃, is dropwise added with glutaraldehyde for crosslinking modification for 1-2 h, is reduced to room temperature, is centrifuged to obtain a precipitate, is alternately washed for 2-3 times by deionized water and ethanol, and is dried in vacuum to obtain the core-shell type light diffusion microsphere;
in each 100mL of 35-50% (v/v) ethanol solution, the dosage of each reaction raw material is as follows: 2-3 mL of aminopropyltrimethoxysilane, 1-2 mL of vinyltrimethoxysilane, 0.5-1 mL of phenyltriethoxysilane, and Zn (NO)3)2·6H2O 0.1～0.2g、Ce(NO3)3·6H2O 0.2～0.3g、Al(NO3)3·9H20.1-0.2 g of O, 0.8-1.2 g of hexamethylenetetramine and 1.5-3 mL of glutaraldehyde.
2. The optical diffuser film as claimed in claim 1, wherein the thickness of the PET film is 45-60 μm.
3. The optical diffusion film according to claim 1, wherein the thickness of the light diffusion layer is 8 to 10 μm.
4. The optical diffuser film of claim 1, wherein the photoinitiator is one or more of photoinitiator 1173, photoinitiator 184, photoinitiator 907 and photoinitiator 1490.
5. The optical diffuser film of claim 1, wherein the H is2SO4The concentration of the solution is 0.5-2 mol/L.
6. The optical diffusion film according to claim 1, wherein the concentration of the NaOH solution is 0.2-1 mol/L.
7. The method for manufacturing an optical diffusion film according to any one of claims 1 to 6, comprising the steps of:
s1: preparing a light diffusion layer coating: under the condition of no light, uniformly stirring urethane acrylate, tripropylene glycol diacrylate, core-shell light diffusion microspheres and a photoinitiator to obtain a light diffusion layer coating;
s2: ultraviolet light imprinting: at a wavelength of 365nm and an intensity of 420mJ cm-2Under the radiation of ultraviolet rays, coating the light diffusion layer coating on the PET film, impressing the PET film by utilizing the PDMS stamper, and demolding after complete curing to obtain the optical diffusion film.
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| CN111730792B (en) * | 2020-08-05 | 2020-12-18 | 上海鲲游光电科技有限公司 | Integrally-formed resin light homogenizing element and manufacturing method thereof |
| CN113736114A (en) * | 2021-06-23 | 2021-12-03 | 江苏怡丽科姆新材料股份有限公司 | Wear-resistant flexible diffusion film and preparation process thereof |
| CN113667337B (en) * | 2021-08-30 | 2022-06-28 | 宁波惠之星新材料科技有限公司 | Optical hard coating liquid and preparation method thereof, optical hard coating film and preparation method thereof |
| CN113897194B (en) * | 2021-09-16 | 2023-02-03 | 宁波东旭成新材料科技有限公司 | Light diffusion particle and preparation method and application thereof |
| CN114539586B (en) * | 2022-04-27 | 2022-07-19 | 河南银金达新材料股份有限公司 | Surface treatment production and detection process of polymer film |
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| CN101812220A (en) * | 2010-03-02 | 2010-08-25 | 江苏工业学院 | Light diffusion agent mother material used for light diffusion film, preparation method and application thereof |
| CN104592905A (en) * | 2013-10-31 | 2015-05-06 | 藤森工业株式会社 | Light-diffusing adhesive layer and light-diffusing adhesive film |
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| CN108976338A (en) * | 2018-07-10 | 2018-12-11 | 东南大学 | A kind of novel display optical material and preparation method thereof |
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| EP3047313B1 (en) * | 2013-09-16 | 2021-01-20 | CoeLux S.r.l. | Light diffuser comprising a composite system comprising a polymer matrix and core-shell nanoparticles, and process for preparing it |
| US20160178814A1 (en) * | 2014-12-18 | 2016-06-23 | Eastman Chemical Company | Light diffusion composition and articles made therefrom |
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| CN101812220A (en) * | 2010-03-02 | 2010-08-25 | 江苏工业学院 | Light diffusion agent mother material used for light diffusion film, preparation method and application thereof |
| CN104592905A (en) * | 2013-10-31 | 2015-05-06 | 藤森工业株式会社 | Light-diffusing adhesive layer and light-diffusing adhesive film |
| CN104730605A (en) * | 2015-03-04 | 2015-06-24 | 东南大学 | Light diffusion membrane for display and preparation method thereof |
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Address after: 230012 first floor of phase I plant of Boxun photoelectric technology (Hefei) Co., Ltd., intersection of yuhuangshan road and Dayu Road, Xinzhan District, Hefei City, Anhui Province Patentee after: Hefei Xingchen New Materials Co.,Ltd. Address before: 230012 plant of Hanbo high tech materials (Hefei) Co., Ltd., north of Tianshui Road, Xinzhan District, Hefei City, Anhui Province Patentee before: HEFEI HANBOGAOXIN NEW MATERIAL CO.,LTD. |