CN112698530A - Quantum dot film with long service life, preparation method thereof and application of quantum dot film in liquid crystal display - Google Patents
Quantum dot film with long service life, preparation method thereof and application of quantum dot film in liquid crystal display Download PDFInfo
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Classifications
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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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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
- C23C14/0652—Silicon nitride
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/10—Glass or silica
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Abstract
The invention provides a quantum dot film with long service life, which comprises a first PET layer, a first water-resistant layer, a quantum dot layer, a second water-resistant layer and a second PET layer which are contacted in sequence; the first water resisting layer comprises a ceramic layer A and a carbon functional layer A; the second water resisting layer comprises a ceramic layer B and a carbon functional layer B; the ceramic layer A and the ceramic layer B are respectively and independently selected from silicon oxide and/or silicon nitride; the carbon functional layer A and the carbon functional layer B respectively and independently comprise graphene and/or carbon nanotubes. The invention utilizes the loose and imperfect structure of the carbon nano-tube and the graphene, can store water vapor, can adjust the water vapor to enter and store on the PET water-blocking and air-blocking layer, can prolong the service life of the quantum dot film, and can disperse heat in a local area without concentrating the heat easily due to the thin film type. The invention provides a preparation method and application of a quantum dot film with long service life.
Description
Technical Field
The invention belongs to the technical field of liquid crystal display, and particularly relates to a quantum dot film with long service life, a preparation method thereof and application thereof in a liquid crystal display.
Background
Liquid Crystal Displays (LCDs) have become the dominant flat panel display technology over half a century of development and research. Since LCDs do not emit light themselves, they require the use of a backlight. Cold Cathode Fluorescent Lamps (CCFLs) were once the most popular backlight, but only achieve 75% NTSC color gamut, so in order to achieve wider color gamut, higher brightness and lower power consumption, researchers have been working on developing newer backlight technologies to ameliorate these problems.
The quantum dot film is as a brand-new nano-material that has unique light characteristic, can be accurate high-efficient with high energy blue light conversion red and green light, and quantum dot can form the one deck film on the LED backlight of LCD display screen, shines with blue LED and just can send full-spectrum light, through carrying out meticulous regulation to being shaded, can promote the colour gamut performance by a wide margin, lets the color more vivid.
The quantum dot display technology has been comprehensively upgraded in various dimensions such as color gamut coverage, color control accuracy, red, green and blue color purity and the like, is regarded as an advanced point of the global display technology, and is also regarded as a revolution of the global display technology. Compared with the traditional LCD display, the color gamut of the quantum dot display screen can reach 110%.
However, due to the sensitivity of the quantum dot material to moisture and oxygen due to its special properties, both moisture and oxygen in the environment can have a negative effect on the service life of the quantum dot film.
Disclosure of Invention
The invention aims to provide a quantum dot film with long service life, a preparation method thereof and application of the quantum dot film in a liquid crystal display.
The invention provides a quantum dot film with long service life, which comprises a first PET layer, a first water-resistant layer, a quantum dot layer, a second water-resistant layer and a second PET layer which are contacted in sequence;
the first water resisting layer comprises a ceramic layer A and a carbon functional layer A; the second water resisting layer comprises a ceramic layer B and a carbon functional layer B;
the ceramic layer A and the ceramic layer B are respectively and independently selected from silicon oxide and/or silicon nitride;
the carbon functional layer A and the carbon functional layer B respectively and independently comprise graphene and/or carbon nanotubes.
Preferably, the ceramic layer A is in contact with the carbon functional layer A; the ceramic layer B is in contact with the carbon functional layer B.
Preferably, the thickness of the ceramic layer A is 50-150 nm, and the thickness of the ceramic layer B is 50-150 nm.
Preferably, the thickness of the carbon functional layer A is 0.5-2.5 μm, and the thickness of the carbon functional layer B is 0.5-2.5 μm.
Preferably, the quantum dot layer is a UV-curable pressure-sensitive adhesive layer dispersed with quantum dot materials,
the quantum dot material comprises CdSe, CdTe, InP, CuInS and CsPbCl3、CsPbBr3And CsPbI3The mass fraction of the quantum dot material in the quantum dot layer is 1-10%.
The invention provides a preparation method of a quantum dot film with long service life, which comprises the following steps:
A) forming a ceramic layer B on the surface of the second PET layer through magnetron sputtering, coating and curing the carbon material slurry B to form a carbon functional layer B, and obtaining the second PET layer compounded with a second water-blocking layer, wherein the ceramic layer B and the carbon functional layer B are formed in no sequence;
forming a ceramic layer A on the surface of the first PET layer through magnetron sputtering, coating and curing the carbon material slurry A to form a carbon functional layer A, and obtaining the first PET layer compounded with the first water-blocking layer, wherein the ceramic layer A and the carbon functional layer A are formed in no sequence;
B) and coating quantum dot glue solution on the surface of the second water blocking layer to form a quantum dot layer, and then bonding the quantum dot layer with the first water blocking layer to obtain the quantum dot film with long service life.
Preferably, the target material of the magnetron sputtering is a silicon target and/or aluminum palladium; the magnetron sputtering uses a mixed gas of argon and oxygen or a mixed gas of argon and nitrogen, and the total gas flow in the magnetron sputtering is 60-120 sccm.
Preferably, the carbon material slurry A is a polyurethane coating liquid of a carbon material, and the mass concentration of the carbon material in the carbon material slurry A is 5-20%;
the carbon material slurry B is a polyurethane coating liquid of a carbon material, and the mass concentration of the carbon material in the carbon material slurry B is 5-20%.
Preferably, the temperature for coating and curing the carbon material slurry A is 100-150 ℃;
the temperature for coating and curing the carbon material slurry B is 100-150 ℃.
Use of a water-gas resistant quantum dot film as described above in a liquid crystal display.
The invention provides a quantum dot film with long service life, which comprises a first PET layer, a first water-resistant layer, a quantum dot layer, a second water-resistant layer and a second PET layer which are contacted in sequence; the first water resisting layer comprises a ceramic layer A and a carbon functional layer A; the second water resisting layer comprises a ceramic layer B and a carbon functional layer B; the ceramic layer A and the ceramic layer B are respectively and independently selected from silicon oxide and/or silicon nitride; the carbon functional layer A and the carbon functional layer B respectively and independently comprise graphene and/or carbon nanotubes. The carbon nano-tubes and graphene have loose and flawed structures, so that water vapor can be stored, the water vapor can be regulated to enter the PET water-blocking and air-blocking layer and then stored, the service life of a quantum dot film can be prolonged, and the heat can be dispersed by the thin film type and is not easy to concentrate in a local area; the compact ceramic material can block water vapor, is a transparent ceramic oxide layer, and is not easy to allow external water vapor to penetrate through PET and enter the structure to be oxidized.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic diagram of the structure of a quantum dot film in one embodiment of the invention;
1 is the first PET layer, 2 is ceramic layer A, 3 is carbon function layer A, 4 is the ultraviolet curing glue film, 5 is the quantum dot layer, 6 is carbon function layer B, 7 is ceramic layer B, 8 is the second PET layer.
Detailed Description
The invention provides a quantum dot film with long service life, which comprises a first PET layer, a first water-resistant layer, a quantum dot layer, a second water-resistant layer and a second PET layer which are contacted in sequence;
the first water resisting layer comprises a ceramic layer A and a carbon functional layer A; the second water resisting layer comprises a ceramic layer B and a carbon functional layer B;
the ceramic layer A and the ceramic layer B are respectively and independently selected from silicon oxide and/or silicon nitride;
the carbon functional layer A and the carbon functional layer B respectively and independently comprise graphene and/or carbon nanotubes.
In the present invention, the first PET layer is preferably a transparent PET film, and the thickness of the first PET layer is preferably 38 to 200 μm, more preferably 38 to 100 μm, and most preferably 100 μm.
In the invention, the first water resisting layer comprises a ceramic layer A and a carbon functional layer A, wherein the ceramic layer A comprises one or more of silicon oxide, silicon nitride, aluminum oxide and aluminum nitride, and SiO is more preferablex，SiNxOne or more of the above; wherein, x is more preferably 1. ltoreq. x.ltoreq.4, and more preferably 2. ltoreq. x.ltoreq.3; the thickness of the ceramic layer A is preferably 50-150 nm, more preferably 70-130 nm, and specifically, the thickness of the ceramic layer A can be 70nm or 130 nm.
The carbon functional layer a preferably includes a carbon material, and the carbon material is preferably graphene and/or carbon nanotubes, and particularly, when the carbon functional layer includes graphene and carbon nanotubes, a mass ratio of the graphene to the carbon nanotubes is preferably 1: 1; the graphene is preferably flaky, the diameter of the flaky graphene is preferably 20-50 nm, and the specific surface area is preferably 400-550 m2(ii)/g; the carbon nano tube is preferably a multi-walled carbon nano tube, the pH value is 7.0-8.0, the diameter of the carbon nano tube is preferably 30-60 nm, and the specific surface area is preferably 60-300 m2/g；The thickness of the carbon functional layer A is preferably 0.5 to 2.5 μm, more preferably 1 to 2 μm, and most preferably 1.2 to 1.3 μm, and specifically, in an embodiment of the present invention, may be 1.2 μm, 1.3 μm, or 2.1 μm.
In the present invention, the ceramic layer a and the carbon functional layer a are preferably in contact, and the stacking order of the ceramic layer a and the carbon functional layer a in the present invention is not particularly limited, and the ceramic layer a may be in contact with the first PET layer, the carbon functional layer a may be in contact with the quantum dot layer, or the ceramic layer a may be in contact with the quantum dot layer, and the carbon functional layer a may be in contact with the first PET layer.
The graphene and the carbon nano-tube have high specific surface area, can have strong adsorption capacity on water vapor, and carbon materials can preferentially attract the water vapor to adhere, thereby playing a role in protecting quantum dots.
In the invention, the quantum dot layer is a UV curing pressure sensitive adhesive layer containing quantum dot materials, and the quantum dot materials are preferably CdSe, CdTe, InP, CuInS and CsPbCl3、CsPbBr3And CsPbI3The mass fraction of the quantum dot material in the quantum dot layer is preferably 1-10%, more preferably 3-8%, and most preferably 5-6%; the main component of the UV curing pressure sensitive adhesive is acrylic acid, and the UV curing pressure sensitive adhesive is UV curing acrylic acid pressure sensitive adhesive. Specifically, in the embodiment of the present invention, CsPbBr may be used3The emission wavelength is 520 +/-10 nm, the half-peak width is less than 20nm, and the CsPbBr is taken as the reference by the volume of the UV-cured acrylic pressure-sensitive adhesive3The amount of (B) was 47.5 mg/mL.
In the present invention, the thickness of the quantum dot layer is preferably 50 to 150 μm, more preferably 80 to 120 μm, and most preferably 90 to 100 μm, and in particular, in an embodiment of the present invention, may be 90 μm.
In the invention, an ultraviolet curing adhesive layer is further arranged between the quantum dot layer and the first water resisting layer, and the thickness of the ultraviolet curing adhesive layer is preferably 5-15 micrometers, and more preferably 8-10 micrometers. In the invention, the second water resisting layer comprises a ceramic layer B and a carbon functional layer B, and the ceramic layer B comprises silicon oxide, silicon nitride,One or more of aluminum oxide and aluminum nitride, more preferably SiOxAnd/or SiNx(ii) a Wherein, x is more preferably 1 to 3, and x is more preferably 2 to 2.5; the thickness of the ceramic layer B is preferably 50-150 nm, more preferably 70-130 nm, and specifically, the thickness of the ceramic layer B can be 70nm or 130 nm.
The carbon functional layer B preferably includes a carbon material, and the carbon material is preferably graphene and/or carbon nanotubes, and specifically, when the carbon functional layer includes graphene and carbon nanotubes, the mass ratio of the graphene to the carbon nanotubes is preferably 1: 1; the graphene is preferably flaky, the diameter of the flaky graphene is preferably 20-50 nm, and the specific surface area is preferably 400-550 m2(ii)/g; the carbon nano tube is preferably a multi-wall carbon nano tube, the pH value is 7.0-8.0, the diameter of the carbon nano tube is preferably 30-60 nm, and the specific surface area is preferably 60-300 m of which position2(ii)/g; the thickness of the carbon functional layer B is preferably 0.5 to 2.5 μm, more preferably 1 to 2 μm, and most preferably 1.2 to 1.3 μm, and specifically, in an embodiment of the present invention, may be 1.2 μm, 1.3 μm, or 2.1 μm.
In the present invention, the ceramic layer B and the carbon functional layer B are preferably in contact, and the stacking order of the ceramic layer B and the carbon functional layer B in the present invention is not particularly limited, and the ceramic layer B may be in contact with the first PET layer, the carbon functional layer B may be in contact with the quantum dot layer, or the ceramic layer B may be in contact with the quantum dot layer, and the carbon functional layer B may be in contact with the first PET layer.
In the present invention, the stacking order of the ceramic layer a and the carbon functional layer a in the first water-resistant layer may be the same as or different from the stacking order of the ceramic layer B and the carbon functional layer B in the second water-resistant layer, and the stacking order of the ceramic layer a and the carbon functional layer a in the first water-resistant layer may be the same as or different from the thickness of the ceramic layer B and the carbon functional layer B in the second water-resistant layer. That is, the specific film layer structures of the first and second water-blocking layers on both sides of the quantum dot layer, which is centered on the quantum dot layer, may be arranged in a symmetrical structure or an asymmetrical structure.
In the present invention, the second PET layer is a transparent PET layer, and the thickness of the second PET layer is preferably 38-200 μm, more preferably 38-100 μm, and most preferably 100 μm.
In the invention, the distance between the edge of the quantum dot layer and the packaging edge of the quantum dot film is 1-10 mm, generally speaking, the quantum dot film has two packaging edges, the width of the quantum dot layer in the packaging edge direction is 2-20 mm smaller than the width of the quantum dot film (1-10 mm smaller on both sides), the 1-10 mm gap is filled with an ultraviolet curing glue layer in contact with the quantum dot film, and the main purpose of the structural design is to prevent edge oxidation.
The invention also provides a preparation method of the quantum dot film with long service life, which comprises the following steps:
A) forming a ceramic layer B on the surface of the second PET layer through magnetron sputtering, coating and curing the carbon material slurry B to form a carbon functional layer B, and obtaining the second PET layer compounded with a second water-blocking layer, wherein the ceramic layer B and the carbon functional layer B are formed in no sequence;
forming a ceramic layer A on the surface of the first PET layer through magnetron sputtering, coating and curing the carbon material slurry A to form a carbon functional layer A, and obtaining the first PET layer compounded with the first water-blocking layer, wherein the ceramic layer A and the carbon functional layer A are formed in no sequence;
B) and coating quantum dot glue solution on the surface of the second water blocking layer to form a quantum dot layer, and then bonding the quantum dot layer with the first water blocking layer to obtain the quantum dot film with long service life.
According to the invention, first water-resistant layers are respectively formed on the surfaces of the first PET layers, second water-resistant layers are formed on the surfaces of the second PET layers, then quantum dot layers are formed on the surfaces of the second water-resistant layers, and finally, the surfaces of the quantum dot layers of the second PET layers with the quantum dot layers are bonded with the second water-resistant layers through adhesives, so that the quantum dot film with long service life is obtained.
Wherein the step of forming the first water blocking layer comprises forming a ceramic layer A by a magnetron sputtering method and forming a carbon functional layer A by a carbon material slurry coating method; the step of forming the second water blocking layer includes forming a ceramic layer B by a magnetron sputtering method and forming a carbon functional layer B by a carbon material slurry coating method.
The formation of the first water-resistant layer and the formation of the second water-resistant layer are not in sequence, the formation of the ceramic layer B and the formation of the carbon functional layer B are not in sequence, and the formation of the ceramic layer A and the formation of the carbon functional layer A are not in sequence.
Specifically, the present invention takes one of the structures as an example to illustrate a specific preparation process of the quantum dot film in the present invention, that is, taking a quantum dot film having a structure of a first PET layer, a ceramic layer a, a carbon functional layer A, UV glue layer, a quantum dot layer, a carbon functional layer B, a ceramic layer B and a second PET layer in contact in sequence as an example, the preparation steps of the quantum dot film in the present invention are as follows:
A) forming a ceramic layer B on the surface of the second PET layer by magnetron sputtering, and then coating the carbon material slurry B on the surface of the ceramic layer B to form a carbon functional layer B to obtain a lower PET layer compounded with a second water-resistant layer;
forming a ceramic layer A on the surface of the first PET layer by magnetron sputtering, and then coating the carbon material slurry A on the surface of the ceramic layer A to form a carbon functional layer A, so as to obtain a lower PET layer compounded with a first water-resistant layer;
the preparation of the second PET layer compounded with the second water-resistant layer and the preparation of the first PET layer compounded with the first water-resistant layer are not in sequence;
B) and coating quantum dot glue solution on the surface of the second water blocking layer to form a quantum dot layer, and then bonding the quantum dot layer with the first water blocking layer to obtain the quantum dot film with long service life.
In the present invention, the magnetron sputtering conditions for forming the ceramic layer B are as follows:
the target material is silicon and/or aluminum, the gas is a mixed gas of argon and oxygen or a mixed gas of argon and nitrogen, when the magnetron sputtering is carried out in an oxygen atmosphere, the total gas flow is preferably 50-100 sccm, more preferably 60-90 sccm, most preferably 70-80 sccm, and the volume ratio of the argon to the oxygen is preferably 1: (0.5 to 2), more preferably 1: (1 to 1.5), and most preferably 1: 1.
when the magnetron sputtering is performed in a nitrogen atmosphere, the total gas flow is preferably 50-100 sccm, more preferably 60-90 sccm, and most preferably 70-90 sccm, and the volume ratio of argon to oxygen is preferably 1: (0.5 to 2), more preferably 1: (1 to 1.5), and most preferably 1: 1.25.
the power of the magnetron sputtering is preferably 1-5 kW/m2More preferably 2 to 4kW/m2Most preferably 3kW/m2DC direct current sputtering is preferably used in the present invention.
The invention preferably uses a roll-to-roll magnetron sputtering coating device to prepare the ceramic layer B, and the thickness of the ceramic layer B can be controlled by controlling the speed of a roll-to-roll machine. The speed of the roll-to-roll machine is preferably 5-20 m/min, and more preferably 8-15 m/min.
In the present invention, the coating conditions for forming the carbon functional layer B are as follows:
and coating the carbon material slurry B on the surface of the ceramic layer B by adopting a gravure coating method, and performing thermosetting to obtain the carbon functional layer B.
The carbon material slurry B comprises a carbon material and polyurethane glue, the carbon material is preferably graphene and/or carbon nano tubes, and the mass fraction of the carbon material in the carbon material slurry is preferably 5-20%, and more preferably 8-15%;
the coating speed is preferably 30-45 m/min, more preferably 35-40 m/min, and most preferably 37 m/min; the heat curing temperature is preferably 100-150 ℃, more preferably 110-140 ℃, most preferably 120-130 ℃, and the heat curing time is 10-30 seconds, more preferably 15-26 seconds, most preferably 20-26 seconds.
Under a certain coating speed, the thickness of the carbon functional layer B can be adjusted by adjusting the solid content of the carbon material slurry, namely the content of the carbon material.
In the present invention, the magnetron sputtering conditions for forming the ceramic layer a are as follows:
the target material is silicon and/or aluminum, the gas is a mixed gas of argon and oxygen or a mixed gas of argon and nitrogen, when the magnetron sputtering is carried out in an oxygen atmosphere, the total gas flow is preferably 50-100 sccm, more preferably 60-90 sccm, most preferably 70-80 sccm, and the volume ratio of the argon to the oxygen is preferably 1: (0.5 to 2), more preferably 1: (1 to 1.5), and most preferably 1: 1.
when the magnetron sputtering is performed in a nitrogen atmosphere, the total gas flow is preferably 50-100 sccm, more preferably 60-90 sccm, and most preferably 70-90 sccm, and the volume ratio of argon to oxygen is preferably 1: (0.5 to 2), more preferably 1: (1 to 1.5), and most preferably 1: 1.25.
the power of the magnetron sputtering is preferably 1-5 kW/m2More preferably 2 to 4kW/m2Most preferably 3kW/m2DC direct current sputtering is preferably used in the present invention.
The ceramic layer A is prepared by preferably using roll-to-roll magnetron sputtering coating equipment, and the thickness of the ceramic layer A can be controlled by controlling the speed of a roll-to-roll machine. The speed of the roll-to-roll machine is preferably 5-20 m/min, and more preferably 8-15 m/min.
In the present invention, the coating conditions for forming the carbon functional layer a are as follows:
and coating the carbon material slurry A on the surface of the ceramic layer B by adopting a gravure coating method, and performing thermosetting to obtain the carbon functional layer A.
The carbon material slurry A comprises a carbon material and polyurethane glue, the carbon material is preferably graphene and/or carbon nano tubes, and the mass fraction of the carbon material in the carbon material slurry is preferably 5-20%, and more preferably 8-15%;
the coating speed is preferably 30-45 m/min, more preferably 35-40 m/min, and most preferably 37 m/min; the heat curing temperature is preferably 100-150 ℃, more preferably 110-140 ℃, most preferably 120-130 ℃, and the heat curing time is preferably 10-30 s, more preferably 15-26 s, most preferably 20-26 s.
Under a certain coating speed, the thickness of the carbon functional layer A can be adjusted by adjusting the solid content of the carbon material slurry A, namely the content of the carbon material. For example, according to the above-mentioned production conditions, the content of the carbon material in the carbon material slurry was 8% in the production of the carbon functional layer having the thickness of 1.2 μm and 1.3 μm, and the content of the carbon material in the carbon material slurry was 15% in the production of the carbon functional layer having the thickness of 2.1 μm.
After the second PET compounded with the second water-resistant layer is obtained, the quantum dot glue solution is further coated on the surface of the second water-resistant layer (namely the surface of the carbon functional layer B) to prepare the quantum dot layer.
In the invention, the quantum dot adhesive solution comprises a quantum dot material and a UV-curable acrylic pressure-sensitive adhesive, and the mass fraction of the quantum dot material in the quantum dot adhesive solution is preferably 1-10%, more preferably 3-8%, and most preferably 5-6%. The quantum dot colloidal solution is preferably coated using a doctor blade.
Finally, the invention uses ultraviolet curing pressure sensitive adhesive (UV-PSA) to bond the quantum dot layer and the carbon functional layer A together, so as to obtain the quantum dot film with long service life.
The invention also provides the application of the water-gas-blocking quantum dot film in the liquid crystal display.
The invention provides a quantum dot film with long service life, which comprises a first PET layer, a first water-resistant layer, a quantum dot layer, a second water-resistant layer and a second PET layer which are contacted in sequence; the first water resisting layer comprises a ceramic layer A and a carbon functional layer A; the second water resisting layer comprises a ceramic layer B and a carbon functional layer B; the ceramic layer A and the ceramic layer B are respectively and independently selected from silicon oxide and/or silicon nitride; the carbon functional layer A and the carbon functional layer B respectively and independently comprise graphene and/or carbon nanotubes. The carbon nano-tubes and graphene have loose and flawed structures, so that water vapor can be stored, the water vapor can be regulated to enter the PET water-blocking and air-blocking layer and then stored, the service life of a quantum dot film can be prolonged, and the heat can be dispersed by the thin film type and is not easy to concentrate in a local area; the compact ceramic material can block water vapor, is a transparent ceramic oxide layer, and is not easy to allow external water vapor to penetrate through PET and enter the structure to be oxidized.
In order to further illustrate the present invention, the following examples are provided to describe the water-gas blocking quantum dot film, the preparation method thereof and the application thereof in the liquid crystal display in detail, but should not be construed as limiting the scope of the present invention.
Example 1
Taking a PET transparent film with the thickness of 38 mu m, forming a SiO layer on the surface of the PET transparent film through magnetron sputtering, wherein the target material is a silicon target, the gas is a mixed gas of argon and oxygen, the flow of the argon is 40sccm, the flow of the oxygen is 40sccm, and the sputtering power is 3kW/m2The speed of a reel-to-reel machine is 8m/min, and a SiO layer with the thickness of 130nm is obtained;
mixing graphene with polyurethane glue solution to obtain graphene coating solution with the graphene content of 8%, then carrying out gravure coating on the surface of the SiO layer, and carrying out thermosetting at 120 ℃ to obtain a graphene layer with the thickness of 1.2 mu m;
another 38-micron-thick PET white film is taken, and a 70 nm-thick SiO layer (the speed of a roll-to-roll machine is 15m/min) and a 1.2-micron-thick graphene layer are formed on the surface of the white film according to the method;
CsPbBr with the mass fraction of 5 percent is coated on the graphene layer (PET white film)3The thickness of the UV curing type acrylic pressure-sensitive adhesive liquid is 90 mu m;
and bonding the quantum dot layer and the graphene layer (PET transparent film) by using UV-PSA ultraviolet curing adhesive to obtain the quantum dot film.
Examples 2 to 12
Quantum dot films were prepared as in example 1, except that they were prepared according to the structural parameters in table 1:
TABLE 1 film thickness of examples 1 to 12 (transparent PET film for both top and bottom)
Wherein, in the preparation of the SiO layer with the thickness of 130nm, the speed of a roll-to-roll machine is 8m/min, and in the preparation of the SiO layer with the thickness of 70nm, the speed of the roll-to-roll machine is 15 m/min.
In the preparation of the carbon functional layer having the thickness of 1.2 μm and 1.3 μm, the content of the carbon material in the carbon material slurry was 8%, and in the preparation of the carbon functional layer having the thickness of 2.1 μm, the content of the carbon material in the carbon material slurry was 15%.
The quantum dot films prepared in examples 1 to 12 were tested for variations in the reflectance x and y values as shown in table 2, using a blue-violet lamp (backlight for LED) x-0.2931 y-0.1523 and a voltage of 24V/0.04A.
The test method specifically comprises the following steps: (1) high-temperature high-light intensity test: the average light intensity of blue light with the wavelength of 447.5nm at the surface of the film is 300mW/cm at the temperature of 85 DEG C2And a test period: 1000 h;
(2) high temperature high humidity test (60 ℃/95% RH/1000 h): performing high-temperature and high-humidity test by using a high-temperature furnace, and continuously testing for 1000 hours at the temperature of 60 ℃ and the relative humidity of 95% RH;
(3) high temperature storage test (80 ℃/1000 h): performing high-temperature storage test for 1000 hours at 80 ℃ by adopting a high-temperature furnace; )
(4) Cold and hot impact (100 times): the oxidation reference IEC 60068-2-14:2009 Na or GB/T2423.22-2012 Na of the cold and hot impact test is that the quantum dot film is operated once at the interval of 30min between the temperature of-40 ℃ and the temperature of 80 ℃ for 100 times of continuous tests.
The test conditions are the in-line specification of the optical film of the LCD backlight module, and refer to GB/T1740-2007 or ISO 4611:2010,
TABLE 2 variation in reflectance of Quantum dot films in inventive examples 1-12
As can be seen from table 2, the luminance of example 12 exhibited the best, and then examples 5 and 10, and again example 11, and the change in Δ x Δ y in the performance in terms of high temperature storage, high temperature and high humidity, and cold heat shock was judged, and then the performance was the best in example 12, and the performances of examples 5 and 10 and example 11 were comparable.
Examples 13 to 24
Quantum dot films were prepared as in example 1, except that they were prepared according to the structural parameters in table 3:
TABLE 3 film thickness of examples 13-24
The quantum dot films prepared in examples 13 to 24 were subjected to a high temperature test, a high temperature and high humidity test, and a cold thermal shock test in the above-described manner, and the results of the tests on the change in reflectance are shown in table 4.
TABLE 4 variation in reflectance of quantum dot films in inventive examples 13-24
As can be seen from table 4, the luminance of examples 17 and 24 performed best, next example 22, and next example 23, and the performance of Δ x Δ y was judged to change in terms of high temperature storage, high temperature and high humidity, and cold heat shock, and then example 24 performed best, next example 23, and next example 17.
Examples 25 to 36
Quantum dot films were prepared as in example 1, except that they were prepared according to the structural parameters in table 5:
TABLE 5 film thickness of examples 25-36
In the preparation of the SiN layer, the magnetron sputtering atmosphere is argon and nitrogen, the argon flow is 40sccm, and the nitrogen flow is 50 sccm. In the preparation of the SiN layer with a thickness of 130nm, the reel-to-reel speed was 8m/min, and in the preparation of the SiO layer with a thickness of 70nm, the reel-to-reel speed was 15 m/min.
In the preparation of the carbon functional layer having the thickness of 1.2 μm and 1.3 μm, the content of the carbon material in the carbon material slurry was 8%, and in the preparation of the carbon functional layer having the thickness of 2.1 μm, the content of the carbon material in the carbon material slurry was 15%.
The quantum dot films prepared in examples 25 to 36 were subjected to a high temperature test, a high temperature and high humidity test, and a cold thermal shock test in the above-described manner, and the change in reflectance (550nm) was measured, and the results are shown in table 6.
TABLE 6 variation in reflectance of quantum dot films in inventive examples 25 to 36
As can be seen from table 6, the luminance of example 36 performed best, next example 34, and again example 39, and when the performance of Δ x Δ y was judged to change in terms of high-temperature storage, high-temperature high-humidity, and cold-heat shock, the luminance performed best in example 36, next example 29, and next example 34.
Examples 37 to 48
Quantum dot films were prepared as in example 1, except that they were prepared according to the structural parameters in table 7:
TABLE 7 film thickness of examples 37-48
The quantum dot films obtained in examples 37 to 48 were subjected to a high temperature test, a high temperature and high humidity test, and a cold thermal shock test in the above-described manner, and the results of the tests on the change in reflectance are shown in table 8.
TABLE 8 variation in reflectance of quantum dot films in inventive examples 37-48
As can be seen from table 8, the luminance of example 48 is best represented, and next, example 46 and again, example 41 show that, when the change in the expression Δ x Δ y is judged in terms of high-temperature storage, high-temperature high-humidity, and cold-heat shock, the expression of example 48 is best represented, and the expressions of examples 41 and 46 and example 47 are equivalent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A quantum dot film with long service life comprises a first PET layer, a first water-resistant layer, a quantum dot layer, a second water-resistant layer and a second PET layer which are contacted in sequence;
the first water resisting layer comprises a ceramic layer A and a carbon functional layer A; the second water resisting layer comprises a ceramic layer B and a carbon functional layer B;
the ceramic layer A and the ceramic layer B are respectively and independently selected from silicon oxide and/or silicon nitride;
the carbon functional layer A and the carbon functional layer B respectively and independently comprise graphene and/or carbon nanotubes.
2. The long-life quantum dot film according to claim 1, wherein the ceramic layer a and the carbon functional layer a are in contact; the ceramic layer B is in contact with the carbon functional layer B.
3. The long-life quantum dot film according to claim 1, wherein the thickness of the ceramic layer A is 50 to 150nm, and the thickness of the ceramic layer B is 50 to 150 nm.
4. The long-life quantum dot film according to claim 1, wherein the thickness of the carbon functional layer A is 0.5-2.5 μm, and the thickness of the carbon functional layer B is 0.5-2.5 μm.
5. The moisture-blocking quantum dot film of claim 1, wherein said quantum dot layer is a UV-curable pressure sensitive adhesive layer dispersed with a quantum dot material,
the quantum dot material comprises CdSe, CdTe, InP, CuInS and CsPbCl3、CsPbBr3And CsPbI3The mass fraction of the quantum dot material in the quantum dot layer is 1-10%.
6. A method for preparing a quantum dot film with long service life according to any one of claims 1 to 5, comprising the following steps:
A) forming a ceramic layer B on the surface of the second PET layer through magnetron sputtering, coating and curing the carbon material slurry B to form a carbon functional layer B, and obtaining the second PET layer compounded with a second water-blocking layer, wherein the ceramic layer B and the carbon functional layer B are formed in no sequence;
forming a ceramic layer A on the surface of the first PET layer through magnetron sputtering, coating and curing the carbon material slurry A to form a carbon functional layer A, and obtaining the first PET layer compounded with the first water-blocking layer, wherein the ceramic layer A and the carbon functional layer A are formed in no sequence;
B) and coating quantum dot glue solution on the surface of the second water blocking layer to form a quantum dot layer, and then bonding the quantum dot layer with the first water blocking layer to obtain the quantum dot film with long service life.
7. The preparation method according to claim 6, wherein the target material for magnetron sputtering is a silicon target and/or aluminum palladium; the magnetron sputtering uses a mixed gas of argon and oxygen or a mixed gas of argon and nitrogen, and the total gas flow in the magnetron sputtering is 60-120 sccm.
8. The preparation method according to claim 6, wherein the carbon material slurry A is a polyurethane coating liquid of a carbon material, and the mass concentration of the carbon material in the carbon material slurry A is 5-20%;
the carbon material slurry B is a polyurethane coating liquid of a carbon material, and the mass concentration of the carbon material in the carbon material slurry B is 5-20%.
9. The production method according to claim 6, wherein the temperature for coating and curing the carbon material slurry A is 100 to 150 ℃;
the temperature for coating and curing the carbon material slurry B is 100-150 ℃.
10. The use of the water-blocking quantum dot film of any one of claims 1 to 5 in a liquid crystal display.
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