CN112255844A - Optical diaphragm and preparation method and application thereof - Google Patents
Optical diaphragm and preparation method and application thereof Download PDFInfo
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- CN112255844A CN112255844A CN202011324483.2A CN202011324483A CN112255844A CN 112255844 A CN112255844 A CN 112255844A CN 202011324483 A CN202011324483 A CN 202011324483A CN 112255844 A CN112255844 A CN 112255844A
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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
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/14—Protective coatings, e.g. hard coatings
Abstract
The invention relates to an optical diaphragm and a preparation method and application thereof, wherein the optical diaphragm comprises a first water-blocking oxygen-isolating film, a quantum dot sol layer and a second water-blocking oxygen-isolating film which are sequentially stacked, and edge sealing films which coat the edges of the first water-blocking oxygen-isolating film, the quantum dot sol layer and the second water-blocking oxygen-isolating film. The quantum dot sol layer in the optical membrane ensures that the quantum dot ligand and the quantum dot material are both in a solution and sol state, and when the optical membrane is eroded by the external environment, the separated ligand can be bonded with the quantum dot material again, so that the protection of the quantum dot material is recovered, a self-repairing mechanism is formed, and the service life of the product is greatly prolonged. According to the invention, the edges of the first water-blocking and oxygen-isolating film, the quantum dot sol layer and the second water-blocking and oxygen-isolating film are subjected to edge sealing treatment, so that the invasion of external moisture and oxygen to quantum dots is prevented to a great extent, and the reliability of the product is improved.
Description
Technical Field
The invention relates to the technical field of display, in particular to an optical membrane and a preparation method and application thereof.
Background
With the rapid progress of society, the development of display technology is more and more closely related to the quality of life of people, and one of the focuses of research in the display technology is the color gamut value of the display. The color gamut of the traditional liquid crystal display NTSC is generally about 70%, and the color gamut of the OLED display NTSC which emits light by itself can reach 100%. Therefore, it is important to improve the product competitiveness of the LCD to study how to improve the color gamut of the LCD.
The color gamut is improved mainly by backlight improvement, for example, the color gamut can be improved to 80-90% by using fluoride and nitride fluorescent powder. However, the fluoride phosphor has the characteristics of being not moisture-proof and high temperature-resistant, which makes the application of fluoride in wide color gamut LCDs very limited. The quantum dot material is an inorganic nano semiconductor crystal, has the characteristics of narrow emission wavelength, adjustable wavelength and the like, is applied to the field of LCD backlight sources in recent years, and can improve the color gamut to more than 100%.
The quantum dot backlight source which is commercialized at present adopts a quantum dot film product, and the quantum dot film generally adopts a sandwich structure: the quantum dot layer is clamped between the two water-oxygen barrier films, and the quantum dot layer contains red and green quantum dots and cured packaging glue.
CN105425463A discloses a display device, a backlight module, a quantum dot optical film and a preparation method thereof, the quantum dot optical film includes: the quantum dot layer, the first composite water-oxygen barrier layer coated on the surface of the light incident side of the quantum dot layer and the second composite water-oxygen barrier layer coated on the surface of the light emergent side of the quantum dot layer; the first composite water-oxygen barrier layer and the second composite water-oxygen barrier layer are of one or the combination of any two of a first film structure, a second film structure and a third film structure; wherein the first film structure is a composite water-oxygen barrier layer composed of polyethylene terephthalate (PET) and graphene; the second thin film structure is a graphene layer; the third film structure is a water oxygen barrier layer composed of PET and alumina. Compared with the traditional optical film, the water-oxygen barrier property, the light transmittance and the structural stability of the quantum dot optical film are obviously improved, but the packaging glue of the quantum dot layer is in a curing state, and the separated ligand cannot be bonded with a quantum dot material again, so that permanent failure is caused, and the use of the optical film is influenced.
CN107102384A discloses a quantum dot optical film, which comprises a quantum dot adhesive layer containing quantum dots, wherein two sides of the quantum dot adhesive layer are provided with a composite film layer, and the end face of the quantum dot optical film is provided with an end face protective coating. The composite film layer is formed by compounding an ethylene/vinyl alcohol copolymer film (EVOH) and a polyolefin film, and the quantum dot glue layer is connected with the EVOH film. The invention adopts a multilayer structure, the quantum dot glue layer is wrapped on two composite films, wherein the EVOH layer has high oxygen barrier rate, the polyolefin layer has high water barrier rate, and the end face of the quantum dot glue layer is coated with a protective coating with high barrier property, so that gas can be prevented from permeating from the end face of the quantum dot film. However, because quantum dot materials are fragile, ligands are generally bonded around red and green quantum dot materials to protect the red and green quantum dot materials. Under the action of light, water vapor and oxygen, the bond between the quantum dot ligand and the quantum dot material in the cured adhesive film is easily destroyed, so that the ligand is separated from the quantum dot material, and the quantum dot loses the ligand protection, thereby causing the performance degradation.
Therefore, it is important to develop a quantum dot optical film with high reliability and durability.
Disclosure of Invention
The invention provides an optical diaphragm and a preparation method and application thereof, and particularly relates to a self-repairing quantum dot optical diaphragm and a preparation method and application thereof. The optical film has the excellent characteristics of high reliability and durability.
In order to achieve the purpose, the invention adopts the following technical scheme:
one objective of the present invention is to provide an optical film, which includes a first water-blocking oxygen-blocking film, a quantum dot sol layer, a second water-blocking oxygen-blocking film, and an edge-sealing film covering edges of the first water-blocking oxygen-blocking film, the quantum dot sol layer, and the second water-blocking oxygen-blocking film, which are sequentially stacked.
The quantum dot sol layer in the optical membrane ensures that the quantum dot ligand and the quantum dot material are both in a solution and sol state, and when the optical membrane is eroded by the external environment, the separated ligand can be bonded with the quantum dot material again, so that the protection of the quantum dot material is recovered, a self-repairing mechanism is formed, and the service life of the product is greatly prolonged.
According to the invention, the edges of the first water-blocking and oxygen-isolating film, the quantum dot sol layer and the second water-blocking and oxygen-isolating film are subjected to edge sealing treatment, so that the invasion of external moisture and oxygen to quantum dots is prevented to a great extent, and the reliability of the product is improved.
Preferably, the thickness of the quantum dot sol layer is 10-150 μm, such as 30 μm, 50 μm, 80 μm, 100 μm, 120 μm, 140 μm, and the like.
Preferably, the quantum dot sol layer contains a quantum dot material, scattering particles and a sol solvent.
Preferably, the mass ratio of the quantum dot material, the scattering particles and the sol solvent is (0.5-5): 1-10): 85-98.5, for example, (0.5-5) may specifically be 1, 2, 3, 4, etc., (1-10) may specifically be 2, 4, 6, 8, etc., (85-98.5) may specifically be 86, 88, 90, 92, 94, 96, 98, etc.
Preferably, the scattering particles comprise any one of barium sulfate, barium carbonate, silica, styrene, or acrylic resin, or a combination of at least two thereof, with a typical but non-limiting combination being: barium sulfate and barium carbonate, silicon dioxide and styrene, barium sulfate, barium carbonate, silicon dioxide, styrene and acrylic resin, and the like, and the size of the scattering particles is nano-scale or micro-scale particles.
Preferably, the scattering particles have a refractive index > 1.4, such as 1.5, 1.6, 1.7, 1.8, etc.
Preferably, the quantum dot material comprises any one of or a combination of at least two of a red light quantum dot material, a green light quantum dot material, or a blue light quantum dot material, wherein typical but non-limiting combinations are: the combination of red light quantum dot material and green light quantum dot material, the combination of red light quantum dot material and blue light quantum dot material, the combination of green light quantum dot material and blue light quantum dot material, the combination of red light quantum dot material, green light quantum dot material and blue light quantum dot material, etc.
Preferably, the peak wavelength of the emission light of the red light quantum dot material is 600-660nm, such as 610nm, 620nm, 630nm, 640nm, 650nm and the like.
Preferably, the peak wavelength of the emitted light of the green light quantum dot material is 510-550nm, such as 520nm, 530nm, 540nm and the like.
Preferably, the peak wavelength of the emitted light of the blue light quantum dot material is 420-485nm, such as 430nm, 440nm, 450nm, 460nm, 470nm, 480nm, and the like.
Preferably, the quantum dot material comprises axMyEzSystem materials, said x is 0.3 to 2.0, such as 0.5, 0.8, 1.0, 1.2, 1.4, 1.6, 1.8, etc., y is 0.5 to 3.0, such as 1.0, 1.5, 2.0, 2.5, etc., and z is 0 to 4.0, such as 0.5, 1.0, 1.5, 2.0, 2.5, 3.0, 3.5, etc.;
a is any one of Ba, Ag, Na, Fe, In, Cd, Zn, Ga, Mg, Pb or Cs;
m is any one of S, Cl, O, As, N, P, Se, Te, Ti, Zr or Pb;
and E is any one of S, As, Se, O, Cl, Br or I.
Preferably, A isxMyEzThe system material comprises any one or the combination of at least two of CdSe, InP or CsPbBr 3.
Preferably, the particle size of the red light quantum dot material is 7-12nm, such as 8nm, 9nm, 10nm, 11nm and the like.
Preferably, the particle size of the green light quantum dot material is 3-7nm, such as 4nm, 5nm, 6nm, 7nm, and the like.
Preferably, the particle size of the blue light quantum dot material is 1-3nm, such as 1nm, 2nm, 3nm, and the like.
Preferably, the viscosity of the sol solvent is 100-6500 mPas, such as 500 mPas, 1000 mPas, 1500 mPas, 2500 mPas, 3500 mPas, 4500 mPas, 5500 mPas, etc.
The viscosity of the sol solvent is 100-6500 mPa.s, the viscosity of the sol solvent is too low, so that the fluidity of the quantum dot sol layer is too high, the preparation difficulty of the optical membrane is increased, and the bonding capability of a quantum dot ligand and a quantum dot material is poor when the optical membrane is corroded by the outside, so that the self-repairing performance of the optical membrane is influenced.
Preferably, the sol solvent comprises any one or a combination of at least two of cyclohexane, n-hexane, octadecene, hexadecene, tetradecene, dodecene, toluene, chloroform, silicone, epoxy, or acrylic, preferably n-hexane and/or toluene, with a typical but non-limiting combination being: a combination of cyclohexane and toluene, a combination of n-hexane and silicone resin, a combination of octadecene, chloroform and epoxy resin, a combination of n-hexane, toluene, chloroform and acrylic acid, and the like.
N-hexane and/or toluene are preferred in the present invention because quantum dots are more soluble in this solvent combination.
Preferably, the silica gel comprises any one of or a combination of at least two of a methyl phenyl silicone resin, a methyl silicone resin, an amino silicone resin, a fluoro-silicone resin or a vinyl silicone resin, wherein a typical but non-limiting combination is: combinations of methylphenyl silicone resin and methyl silicone resin, combinations of amino silicone resin and fluorosilicone resin, methylphenyl silicone resin, methyl silicone resin, amino silicone resin, fluorosilicone resin and vinyl silicone resin, and the like.
Preferably, the epoxy resin includes any one of or a combination of at least two of glycidyl ether epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, or alicyclic epoxy resin, wherein a typical but non-limiting combination is: a combination of glycidyl ether epoxy resin and glycidyl ester epoxy resin, a combination of glycidyl amine epoxy resin and alicyclic epoxy resin, glycidyl ether epoxy resin, glycidyl ester epoxy resin, a combination of glycidyl amine epoxy resin and alicyclic epoxy resin, and the like.
Preferably, the sol solvent contains a viscosity modifier.
Preferably, the viscosity modifier comprises SiO2、TiO2Or NaOH, or a combination of at least two, with typical but non-limiting combinations being: SiO 22And TiO2Combinations of (A) and (B), TiO2And NaOH, SiO2、TiO2And NaOH, and the like.
Preferably, the mass ratio of the viscosity modifier in the sol solvent is 0 to 3%, for example, 0.5%, 1%, 1.5%, 2%, 2.5%, etc.
Preferably, the first and second water and oxygen barrier films each independently have a thickness of 1-30 μm, such as 5 μm, 10 μm, 15 μm, 20 μm, 25 μm, and the like.
Preferably, the first water and oxygen blocking film and the second water and oxygen blocking film each independently comprise any one or a combination of at least two of metal compounds, nonmetal compounds or metal organic salts.
Preferably, the metal compound comprises alumina.
Preferably, the non-metallic compound comprises silicon nitride and/or silicon carbide.
Preferably, the metal organic salt comprises any one or a combination of at least two of octadecyl titanate, zirconium citrate or titanium ethyl-1-hexanoate, wherein typical but non-limiting combinations are: combinations of octadecyl titanate and zirconium citrate salt, zirconium citrate salt and titanium ethyl-1-hexanoate, combinations of octadecyl titanate, zirconium citrate salt and titanium ethyl-1-hexanoate, and the like.
The second objective of the present invention is to provide a method for preparing an optical film, which comprises the following steps: coating a quantum dot sol layer on a first water-blocking oxygen-insulating film, then coating a second water-blocking oxygen-insulating film on the quantum dot sol layer, spraying packaging glue on the edges of the first water-blocking oxygen-insulating film, the quantum dot sol layer and the second water-blocking oxygen-insulating film, and curing to obtain the optical membrane.
Preferably, the curing comprises thermal curing or uv curing.
Preferably, the encapsulation glue comprises any one or a combination of at least two of silicone, epoxy or polyurethane, wherein a typical but non-limiting combination is: combinations of silicone and epoxy, silicone and polyurethane, silicone, epoxy and polyurethane, and the like. The encapsulation glue of the invention is the same as the silicon resin and the epoxy resin in the sol solvent.
Preferably, the preparation of the quantum dot sol layer comprises the following steps: and mixing the quantum dot material with a sol solvent, and then mixing with scattering particles to obtain the quantum dot sol layer.
Preferably, the preparation of the quantum dot material comprises the following steps: and dissolving the quantum dot material, and purifying for the first time to obtain a quantum dot material solution.
Preferably, the first purification comprises: firstly, carrying out centrifugal precipitation on the quantum dot material solution, removing the supernatant for the first time, adding the solvent for centrifugation, removing the supernatant for the second time, and repeating the steps for 5-10 times, such as 6 times, 7 times, 8 times, 9 times and the like.
Preferably, the preparation of the quantum dot material further comprises the steps of adding a coating material into the quantum dot material solution for coating reaction and secondary purification.
The coating reaction refers to that under the conditions of temperature of 120-320 ℃ and pH value of 5.5-11, the raw materials of the coating material are gradually added to be dissolved and then react with each other, and the uniform precipitation growth is carried out outside the quantum dot core material. The contact surface of the cladding material and the quantum dot core material can react to generate a transition layer, the transition layer is a quantum dot and a composite material or solid solution generated by the reaction of a new material and the cladding material, such as CdSe quantum dot cladded with CdS material, and CdSe can be produced in the middle of the transition layer by reactionySz。
Preferably, the cladding material comprises silicon dioxide (SiO)2) Propylene glycol methyl ether acetate (PMA) orAny one or a combination of at least two of polyvinylidene fluoride (PVDF), with typical but non-limiting combinations being: SiO 22Combination with PMA, combination of PMA and PVDF, SiO2Combinations of PMA and PVDF, and the like.
Preferably, the second purification comprises: firstly, centrifugally precipitating the quantum dot material solution after the coating reaction, removing supernatant for the third time, adding a solvent for centrifugation, removing supernatant for the fourth time, and repeating for 5-10 times, such as 6 times, 7 times, 8 times, 9 times and the like.
Preferably, the temperature of the coating reaction is 120 ℃ to 320 ℃, such as 150 ℃, 200 ℃, 250 ℃, 300 ℃ and the like.
As a preferred technical scheme, the preparation method comprises the following steps:
(1) dissolving the quantum dot material, then carrying out centrifugal precipitation, removing supernatant for the first time, adding the solvent for centrifugation, removing the supernatant for the second time, and repeating for 5-10 times to obtain a quantum dot material solution;
(2) adding a coating layer material into the quantum dot material solution, carrying out coating reaction at 120-320 ℃, then carrying out centrifugal precipitation, removing supernatant for the third time, adding a solvent for centrifugation, removing supernatant for the fourth time, repeating for 5-10 times, and then sequentially mixing with a sol solvent and scattering particles to obtain the quantum dot sol layer;
(3) coating the quantum dot sol layer on a first water-blocking oxygen-insulating film, then coating a second water-blocking oxygen-insulating film on the quantum dot sol layer, spraying packaging glue on the edges of the first water-blocking oxygen-insulating film, the quantum dot sol layer and the second water-blocking oxygen-insulating film, and performing thermocuring or ultraviolet curing to obtain the optical membrane.
The invention also aims to provide application of the optical film in quantum dot backlight.
Compared with the prior art, the invention has the following beneficial effects:
(1) the quantum dot sol layer in the optical membrane ensures that the quantum dot ligand and the quantum dot material are both in a solution and sol state, and when the optical membrane is eroded by the external environment, the separated ligand can be bonded with the quantum dot material again, so that the protection of the quantum dot material is recovered, a self-repairing mechanism is formed, and the service life of the product is greatly prolonged.
(2) According to the invention, the edges of the first water-blocking and oxygen-isolating film, the quantum dot sol layer and the second water-blocking and oxygen-isolating film are subjected to edge sealing treatment, so that the invasion of external moisture and oxygen to quantum dots is prevented to a great extent, and the reliability of the product is improved.
(3) The optical film has excellent comprehensive performance, and is particularly characterized in that the light conversion efficiency is more than 88%, the color gamut value of a display is more than 118%, and the service life of L70 is more than 25700 hours.
Drawings
FIG. 1 is a schematic structural diagram of an optical film provided by an embodiment of the present invention;
10-a quantum dot sol layer, 201-a first water-blocking oxygen-insulating film, 202-a second water-blocking oxygen-insulating film and 30-a sealing film.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides an optical film, as shown in fig. 1, which includes a first water-blocking oxygen-blocking film 201 (silicon nitride, with a thickness of 15 μm), a quantum dot sol layer 10 (with a thickness of 100 μm), a second water-blocking oxygen-blocking film 202 (silicon nitride, with a thickness of 15 μm), and an edge-sealing film 30 (with a thickness of 3 μm) coated on edges of the first water-blocking oxygen-blocking film, the quantum dot sol layer, and the second water-blocking oxygen-blocking film, which are sequentially stacked.
The quantum dot sol layer contains 2 weight parts of red light quantum dot material (specifically InP with particle diameter of 10nm and peak wavelength of emitted light of 628nm) and 3 weight parts of green light quantum dot material (specifically CsPbBr)3Particle size of 5nm and emission peak wavelength of 530nm), 10 parts by weight of scattering particles (styrene, refractive index of 2.7) and 85 parts by weight of sol solvent (40% n-hexane, 58% toluene and 2% SiO2Viscosity of3000 mPas).
The edge sealing film is formed by curing methyl phenyl silicone resin.
The preparation method of the optical film comprises the following steps:
(1) 2 parts by weight of InP and 3 parts by weight of CsPbBr3Dissolving, then carrying out centrifugal precipitation, removing supernatant for the first time, adding a solvent for centrifugation, removing supernatant for the second time, and repeating for 5 times to obtain a quantum dot material solution;
(2) adding PVDF into the quantum dot material solution, carrying out coating reaction at 200 ℃, then carrying out centrifugal precipitation, removing supernatant liquor for the third time, adding a solvent for centrifugation, removing supernatant liquor for the fourth time, repeating the steps for 5 times, mixing with 34 parts by weight of n-hexane and 49.3 parts by weight of toluene (with the viscosity of 3000mPa & s), mixing with 10 parts by weight of styrene with the refractive index of 1.5, adding 1.7 parts by weight of SiO2Obtaining a 100 mu m quantum dot sol layer;
(3) coating the quantum dot sol layer on silicon nitride with the thickness of 15 microns, then coating the silicon nitride with the thickness of 15 microns on the quantum dot sol layer, spraying methyl phenyl silicone resin water on the edges of the first layer of silicon nitride, the quantum dot sol layer and the second layer of silicon nitride, and performing thermal curing at 120 ℃ to obtain the optical membrane.
Example 2
The embodiment provides an optical film, as shown in fig. 1, including a first water-blocking oxygen-blocking film 201 (aluminum oxide octadecyl titanate, thickness of 1 μm), a quantum dot sol layer 10 (thickness of 10 μm), a second water-blocking oxygen-blocking film 202 (thickness of 1 μm), and an edge-sealing film 30 (thickness of 2 μm) coated on the edges of the first water-blocking oxygen-blocking film, the quantum dot sol layer, and the second water-blocking oxygen-blocking film, which are sequentially stacked.
The quantum dot sol layer contains 0.2 parts by weight of red light quantum dot material (specifically CdSe with particle size of 7nm and emission peak wavelength of 600nm), 0.3 parts by weight of green light quantum dot material (specifically InP with particle size of 3nm and emission peak wavelength of 510nm), 1 part by weight of scattering particles (barium sulfate with refractive index of 1.5) and 98.5 parts by weight of sol solvent (55% cyclohexane, 44% acrylic solvent and 1% TiO)2The viscosity was 100 mPas).
The edge sealing film is formed by curing glycidyl ether epoxy resin.
The preparation method of the optical film comprises the following steps:
(1) dissolving 0.2 weight part of CdSe and 0.3 weight part of InP, centrifuging and precipitating, removing supernatant for the first time, adding a solvent for centrifuging, removing supernatant for the second time, and repeating for 10 times to obtain a quantum dot material solution;
(2) adding PMA into the quantum dot material solution, performing coating reaction at 150 ℃, then performing centrifugal precipitation, removing supernatant for the third time, adding a solvent for centrifugation, removing supernatant for the fourth time, repeating for 10 times, mixing with 54.18 parts by weight of cyclohexane and 43.34 parts by weight of tetradecene, mixing with 1 part by weight of barium sulfate with a refractive index of 1.5, adding 9.85 parts by weight of TiO2Obtaining a 10 mu m quantum dot sol layer;
(3) coating the quantum dot sol layer on aluminum oxide octadecyl titanate with the thickness of 1 mu m, then coating silicon nitride with the thickness of 1 mu m on the quantum dot sol layer, spraying glycidyl ether epoxy resin on the edges of the aluminum oxide octadecyl titanate, the quantum dot sol layer and the silicon nitride, and carrying out ultraviolet curing to obtain the optical membrane.
Example 3
The embodiment provides an optical film, as shown in fig. 1, including a first water-blocking oxygen-blocking film 201 (zirconium citrate and ethyl-1-titanium hexanoate, thickness of 30 μm), a quantum dot sol layer 10 (thickness of 150 μm), a second water-blocking oxygen-blocking film 202 (zirconium citrate and ethyl-1-titanium hexanoate, thickness of 30 μm), and an edge-sealing film 30 (thickness of 4 μm) coated on the edges of the first water-blocking oxygen-blocking film, the quantum dot sol layer, and the second water-blocking oxygen-blocking film, which are sequentially stacked.
The quantum dot sol layer contains 2.5 weight parts of blue light quantum dot material (specifically CsPbBr)3Emission peak wavelength of 420nm, particle size of 2nm), 7.5 parts by weight of scattering particles (acrylate, refractive index of 1.7) and 90 parts by weight of sol solvent (35% octadecene, 32% glycidyl ester epoxy, 30% aminosilicone and 3% NaOH, viscosity of 6500mPa · s).
The edge sealing film is formed by solidifying polyurethane.
The preparation method of the optical film comprises the following steps:
(1) 2.5 parts by weight of CsPbBr3Dissolving, then carrying out centrifugal precipitation, removing supernatant for the first time, adding a solvent for centrifugation, removing supernatant for the second time, and repeating for 8 times to obtain a quantum dot material solution;
(2) mixing SiO2Adding PVDF and the quantum dot material solution into the quantum dot material solution, performing coating reaction at 300 ℃, then performing centrifugal precipitation, removing supernatant for the third time, adding a solvent for centrifugation, removing the supernatant for the fourth time, repeating the steps for 8 times, mixing the supernatant with 31.5 parts by weight of octadecene, 28.8 parts by weight of glycidyl ester epoxy resin and 27 parts by weight of amino silicone resin (the viscosity is 100mPa & s), mixing the mixture with 7.5 parts by weight of acrylic ester with the refractive index of 1.7, and adding 2.7 parts by weight of NaOH to obtain a 150 mu m quantum dot sol layer;
(3) coating the quantum dot sol layer on 30 mu m of zirconium citrate and ethyl-1-titanium hexanoate, coating the 30 mu m of zirconium citrate and ethyl-1-titanium hexanoate on the quantum dot sol layer, spraying polyurethane on the edges of the first layer of zirconium citrate and ethyl-1-titanium hexanoate, the quantum dot sol layer and the second layer of zirconium citrate and ethyl-1-titanium hexanoate, and performing thermocuring at 160 ℃ to obtain the optical film.
Examples 4 to 5
The difference from example 1 was a sol solvent having a viscosity of 3000 mPas (40% n-hexane, 58% toluene and 2% SiO)2) Replacement with equal mass of a sol solvent having a viscosity of 50 mPas (40% n-hexane, 58% toluene and 0.5% SiO)2) Example 4 Sol solvent with viscosity of 7500 mPas (40% n-hexane, 58% toluene and 3% SiO) with equal mass2) (example 5).
Example 6
The difference from example 1 is that a sol solvent (40% n-hexane, 58% toluene and 2% SiO)2Viscosity of 3000 mPas) was replaced with equal mass of sol solvent (97% chloroform and 3% SiO)2And a viscosity of 3000 mPas).
Example 7
The difference from example 1 is that n-hexane was replaced by toluene of equal mass.
Example 8
The difference from example 1 is that toluene was replaced by an equal mass of n-hexane.
Comparative example 1
The difference from example 1 is that the quantum dot sol layer is replaced by the non-sol quantum dot material layer, that is, the preparation method of the optical film of the comparative example is as follows:
the quantum dot material of example 1 was mixed in an acrylate and directly uv cured without edge sealing.
Performance testing
(1) Testing the light conversion efficiency: light conversion efficiency is the output light power/incident light power.
(2) Display device color gamut value: according to the NTSC standard.
(3) Optical film L70 lifetime: that is, the luminance parameter nit of the display device is used with an operating time which is maintained until the light emission intensity decays to 70% of the initial value at the normal temperature lighting (25 ℃).
The above test results are shown in table 1:
TABLE 1
As can be seen from Table 1, the optical film provided by the invention has the advantages of light conversion efficiency of more than 88%, color gamut of a display device of more than 18%, service life of the film L70 of more than 25700 hours, high reliability and excellent durability.
Comparing examples 4-5 with example 1, it was found that the optical film obtained with the sol solvent outside the range of 100-6500 mPas was inferior in performance.
Example 6 in comparison with example 1, it was found that the sol solvent selected a combination of n-hexane and toluene resulted in an optical film having better performance than other solvents.
Examples 7-8 in comparison to example 1 show that the combination of n-hexane and toluene selected as the sol solvent provides optical films with better performance than n-hexane and toluene alone.
Comparison of comparative example 1 with example 1 shows that the optical film obtained by using the quantum dot sol layer has better performance.
The present invention is illustrated in detail by the examples described above, but the present invention is not limited to the details described above, i.e., it is not intended that the present invention be implemented by relying on the details described above. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The utility model provides an optical diaphragm, its characterized in that, optical diaphragm is including the first oxygen membrane, the quantum dot sol layer of blocking water that stack gradually the setting and the second blocks water and separates the oxygen membrane to and the cladding is in the first oxygen membrane, the quantum dot sol layer of blocking water and the second blocks water and separates the banding membrane at oxygen membrane edge.
2. The optical film according to claim 1, wherein the quantum dot sol layer has a thickness of 10-150 μ ι η;
preferably, the quantum dot sol layer contains a quantum dot material, scattering particles and a sol solvent;
preferably, the mass ratio of the quantum dot material to the scattering particles to the sol solvent is (0.5-5) to (1-10) to (85-98.5);
preferably, the scattering particles include any one of barium sulfate, barium carbonate, silica, styrene, or acrylic resin or a combination of at least two thereof;
preferably, the scattering particles have a refractive index > 1.4.
3. The optical film according to claim 2, wherein the quantum dot material comprises any one of or a combination of at least two of a red light quantum dot material, a green light quantum dot material or a blue light quantum dot material;
preferably, the peak wavelength of the emitted light of the red light quantum dot material is 600-660 nm;
preferably, the peak wavelength of the emitted light of the green light quantum dot material is 510-550 nm;
preferably, the peak wavelength of the emitted light of the blue light quantum dot material is 420-485 nm.
4. An optical film as recited in claim 2 or 3, wherein the quantum dot material comprises AxMyEzThe system material comprises x is 0.3-2.0, y is 0.5-3.0, and z is 0-4.0;
a is any one of Ba, Ag, Na, Fe, In, Cd, Zn, Ga, Mg, Pb or Cs;
m is any one of S, Cl, O, As, N, P, Se, Te, Ti, Zr or Pb;
e is any one of S, As, Se, O, Cl, Br or I;
preferably, A isxMyEzThe system material comprises any one or the combination of at least two of CdSe, InP or CsPbBr 3;
preferably, the particle size of the red light quantum dot material is 7-12 nm;
preferably, the particle size of the green light quantum dot material is 3-7 nm;
preferably, the particle size of the blue light quantum dot material is 1-3 nm.
5. The optical film according to any one of claims 2 to 4, wherein the viscosity of the sol solvent is 100-6500 mPa-s;
preferably, the sol solvent comprises any one or a combination of at least two of cyclohexane, n-hexane, octadecene, hexadecene, tetradecene, dodecene, toluene, chloroform, silicone, epoxy resin or acrylic acid, preferably n-hexane and/or toluene;
preferably, the silicone resin comprises any one of methyl phenyl silicone resin, methyl silicone resin, amino silicone resin, fluorosilicone resin or vinyl silicone resin or a combination of at least two of the methyl phenyl silicone resin, the methyl silicone resin, the amino silicone resin, the fluorosilicone resin or the vinyl silicone resin;
preferably, the epoxy resin comprises any one of or a combination of at least two of glycidyl ether epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin or alicyclic epoxy resin;
preferably, the sol solvent contains a viscosity modifier;
preferably, the viscosity modifier comprises SiO2、TiO2Or NaOH, or a combination of at least two of the above;
preferably, the mass ratio of the viscosity modifier in the sol solvent is 0 to 3%.
6. The optical film according to any one of claims 1 to 5, wherein the first and second water-and oxygen-blocking films each independently have a thickness of 1 to 30 μm;
preferably, the first water and oxygen blocking film and the second water and oxygen blocking film respectively and independently comprise any one or a combination of at least two of metal compounds, nonmetal compounds or metal organic salts;
preferably, the metal compound comprises alumina;
preferably, the non-metallic compound comprises silicon nitride and/or silicon carbide;
preferably, the metal organic salt comprises any one of or a combination of at least two of octadecyl titanate, zirconium citrate or titanium ethyl-1-hexanoate.
7. A method of manufacturing an optical film according to any one of claims 1 to 6, comprising the steps of: coating a quantum dot sol layer on a first water-blocking oxygen-insulating film, then coating a second water-blocking oxygen-insulating film on the quantum dot sol layer, spraying packaging glue on the edges of the first water-blocking oxygen-insulating film, the quantum dot sol layer and the second water-blocking oxygen-insulating film, and curing to obtain the optical membrane.
8. The method of claim 7, wherein the curing comprises thermal curing or ultraviolet curing;
preferably, the encapsulation glue comprises any one or a combination of at least two of silicone resin, epoxy resin or polyurethane;
preferably, the preparation of the quantum dot sol layer comprises the following steps: mixing a quantum dot material with a sol solvent, and then mixing with scattering particles to obtain a quantum dot sol layer;
preferably, the preparation of the quantum dot material comprises the following steps: dissolving the quantum dot material, and purifying for the first time to obtain a quantum dot material solution;
preferably, the first purification comprises: firstly, centrifugally precipitating the quantum dot material solution, removing supernatant for the first time, adding a solvent for centrifugation, removing the supernatant for the second time, and repeating the steps for 5-10 times;
preferably, the preparation of the quantum dot material further comprises the steps of adding a coating material into the quantum dot material solution for coating reaction and secondary purification;
preferably, the second purification comprises: firstly, centrifugally precipitating the quantum dot material solution after the coating reaction, removing supernatant for the third time, adding a solvent for centrifugation, removing the supernatant for the fourth time, and repeating for 5-10 times;
preferably, the coating material comprises any one or a combination of at least two of silicon dioxide, propylene glycol methyl ether acetate or polyvinylidene fluoride;
preferably, the temperature of the coating reaction is 120 ℃ to 320 ℃.
9. The method according to any one of claims 7 or 8, characterized by comprising the steps of:
(1) dissolving the quantum dot material, then carrying out centrifugal precipitation, removing supernatant for the first time, adding the solvent for centrifugation, removing the supernatant for the second time, and repeating for 5-10 times to obtain a quantum dot material solution;
(2) adding a coating layer material into the quantum dot material solution, carrying out coating reaction at 120-320 ℃, then carrying out centrifugal precipitation, removing supernatant for the third time, adding a solvent for centrifugation, removing supernatant for the fourth time, repeating for 5-10 times, and then sequentially mixing with a sol solvent and scattering particles to obtain the quantum dot sol layer;
(3) coating the quantum dot sol layer on a first water-blocking oxygen-insulating film, then coating a second water-blocking oxygen-insulating film on the quantum dot sol layer, spraying packaging glue on the edges of the first water-blocking oxygen-insulating film, the quantum dot sol layer and the second water-blocking oxygen-insulating film, and performing thermocuring or ultraviolet curing to obtain the optical membrane.
10. Use of an optical film according to any one of claims 1 to 6 in a quantum dot backlight.
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