CN114086135A - Electro-dimming film and preparation method thereof - Google Patents
Electro-dimming film and preparation method thereof Download PDFInfo
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- CN114086135A CN114086135A CN202111310854.6A CN202111310854A CN114086135A CN 114086135 A CN114086135 A CN 114086135A CN 202111310854 A CN202111310854 A CN 202111310854A CN 114086135 A CN114086135 A CN 114086135A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000004973 liquid crystal related substance Substances 0.000 claims abstract description 80
- 239000000178 monomer Substances 0.000 claims abstract description 67
- 239000010410 layer Substances 0.000 claims abstract description 49
- 239000000758 substrate Substances 0.000 claims abstract description 40
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 125000006850 spacer group Chemical group 0.000 claims abstract description 14
- 230000005684 electric field Effects 0.000 claims abstract description 13
- QCDWFXQBSFUVSP-UHFFFAOYSA-N 2-phenoxyethanol Chemical compound OCCOC1=CC=CC=C1 QCDWFXQBSFUVSP-UHFFFAOYSA-N 0.000 claims abstract description 12
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims abstract description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 9
- 229920005989 resin Polymers 0.000 claims abstract description 9
- 230000003287 optical effect Effects 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000004568 cement Substances 0.000 claims abstract description 6
- 239000002344 surface layer Substances 0.000 claims abstract description 6
- 238000005096 rolling process Methods 0.000 claims abstract description 5
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 239000010408 film Substances 0.000 claims description 63
- 239000000843 powder Substances 0.000 claims description 60
- 238000005245 sintering Methods 0.000 claims description 37
- 239000002131 composite material Substances 0.000 claims description 16
- 238000004544 sputter deposition Methods 0.000 claims description 15
- 239000013077 target material Substances 0.000 claims description 14
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 13
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 13
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 13
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 13
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 13
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 13
- 238000000465 moulding Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000004986 Cholesteric liquid crystals (ChLC) Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 239000010409 thin film Substances 0.000 claims description 6
- 239000004974 Thermotropic liquid crystal Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 5
- 239000004988 Nematic liquid crystal Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000005478 sputtering type Methods 0.000 claims description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- -1 alkylbenzene ketone Chemical class 0.000 claims description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 2
- 239000012965 benzophenone Substances 0.000 claims description 2
- 239000011325 microbead Substances 0.000 claims description 2
- 238000002834 transmittance Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 238000005562 fading Methods 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000011514 reflex Effects 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
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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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
- C09K19/04—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit
- C09K19/38—Polymers
- C09K19/3804—Polymers with mesogenic groups in the main chain
- C09K19/3814—Polyethers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
- C09K19/04—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit
- C09K19/38—Polymers
- C09K19/3833—Polymers with mesogenic groups in the side chain
- C09K19/3842—Polyvinyl derivatives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
- C09K19/04—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit
- C09K19/38—Polymers
- C09K19/3833—Polymers with mesogenic groups in the side chain
- C09K19/3842—Polyvinyl derivatives
- C09K19/3852—Poly(meth)acrylate derivatives
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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
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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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
- G02F1/137—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 characterised by the electro-optical or magneto-optical effect, e.g. field-induced phase transition, orientation effect, guest-host interaction or dynamic scattering
- G02F1/13718—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 characterised by the electro-optical or magneto-optical effect, e.g. field-induced phase transition, orientation effect, guest-host interaction or dynamic scattering based on a change of the texture state of a cholesteric liquid crystal
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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
- G02F1/15—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 an electrochromic effect
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- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Liquid Crystal (AREA)
Abstract
The invention relates to a preparation method of an electro-dimming film, which comprises the following steps: step 1: treating the surface of the substrate: step 2: performing magnetron sputtering on the single-side layer of the substrate obtained in the step (1) to plate a conductive film layer; and step 3: fully and uniformly mixing an acrylic liquid crystal resin monomer, an acrylate monomer, a vinyl ether monomer, an ethylene glycol phenyl ether monomer, a photoinitiator and an accelerator in proportion, adding a liquid crystal monomer, mixing and stirring uniformly with a spacer, and defoaming to prepare a liquid crystal layer; and 4, step 4: and (3) clamping the liquid crystal layer obtained in the step (3) by the two substrate coating surfaces obtained in the step (2), rolling the outer side surface layer of the substrate to form a liquid crystal film on the liquid crystal layer, applying an electric field to the liquid crystal film, carrying out ultraviolet curing on the liquid crystal film, and then coating liquid optical cement LOCA on the edge part of the substrate for covering. The dimming film prepared and formed by the invention has lower driving voltage, excellent dimming effect on light transmittance, compact forming and good integral stability and compatibility.
Description
Technical Field
The invention relates to the technical field of dimming films, in particular to an electro-dimming film and a preparation method thereof.
Background
The film of adjusting luminance is when applying the electric field, applys operating voltage promptly, can demonstrate the transparent state, presents the scattering state after getting rid of the electric field, refracts and reflects light, hinders light and follows original route propagation, makes the formation of image fuzzy, can realize people and pierce through the dual requirement with the protection privacy to glass, even when opaque, daylighting is still fine, and this is all curtains all can not realize to the heat energy of light has insulating reflex action, makes indoor warm in winter and cool in summer, environmental protection and energy saving. Generally, a dimming thin film shields light in a transmission range by using the beneficial optical and electrical characteristics of liquid crystal, and an ITO thin film is a thin film having high conductivity, visible light transmittance, and mechanical hardness.
In the prior art, an ITO film has better light transmittance, but the adjustment of the light transmittance is lacked, and the compatibility also has an optimization space. For example, patent application No. 201811015139.8 discloses a method for preparing a low temperature resistant high resistivity ITO conductive film, which improves the resistance of the ITO conductive film by increasing the content of tin oxide in the ITO target. After the resistance is improved, the heat productivity of the ITO conductive film is improved when the ITO conductive film is used, the ambient temperature is improved, the ITO conductive film can enable the liquid crystal display to normally work at a low temperature, instant imaging is realized, the working temperature range of the liquid crystal display is greatly improved, the integral driving voltage is high, the surface resistance and the uniformity are poor, energy consumption is high, heat is easily accumulated on a film layer to damage the film, the stable compatibility is poor, the phase change temperature is easily influenced by the temperature at an overhigh temperature, imaging is fuzzy, the light transmittance is influenced, and the ITO conductive film does not have the dimming effect.
Disclosure of Invention
In order to solve the problems in the background art, the invention provides an electro-dimming thin film and a preparation method thereof, the prepared and formed dimming thin film has low driving voltage, excellent dimming effect on light transmittance, compact formation and good strength.
The invention provides the following technical scheme:
a preparation method of an electro-dimming film comprises the following steps:
step 1: treating the surface of the substrate:
respectively and sequentially carrying out ultrasonic cleaning on the substrate for 5min by using hydrogen peroxide, ultrapure water, acetone and ethanol, and drying to obtain a cleaned substrate;
step 2: performing magnetron sputtering on the single-side layer of the substrate obtained in the step 1 to plate a conductive film layer:
manufacturing a target material: uniformly mixing indium tin oxide powder, nickel oxide powder, tungsten oxide powder and lithium oxide powder with uniform granularity by a wet method, heating to prepare prefabricated composite powder, granulating and screening the prefabricated composite powder, performing cold press molding on the composite powder with effective grain size, and sintering at high temperature to prepare an ITO target material;
sputtering: ionizing to generate electrons to bombard the ITO target material, and depositing to prepare an ITO conductive film layer;
and step 3: under the shading condition, fully and uniformly mixing an acrylic liquid crystal resin monomer, an acrylate monomer, a vinyl ether monomer, an ethylene glycol phenyl ether monomer, a photoinitiator and an accelerator in proportion, adding a liquid crystal monomer, mixing and stirring uniformly with a spacer, and defoaming to prepare a liquid crystal layer;
and 4, step 4: and (3) clamping the liquid crystal layer obtained in the step (3) by the two substrate coating surfaces obtained in the step (2), rolling the outer side surface layer of the substrate to form a liquid crystal film on the liquid crystal layer, applying an electric field to the liquid crystal film to orient liquid crystal molecules, performing ultraviolet curing on the liquid crystal film, and then coating liquid optical cement LOCA on the edge part of the substrate for covering.
Preferably, in step 2, the target raw materials are prepared according to the mass ratio:
preferably, in the step 2, the pressure of the cold press molding of the composite powder is 210-300MPa, the high-temperature sintering can adopt normal-pressure sintering or pressure sintering, the sintering temperature is 1100-1680 ℃, and the sintering time is 2-12 h.
Preferably, in step 3, the liquid crystal layer is prepared by the following raw materials in percentage by mass:
the spacer is rigid microbead with diameter of 20-35 μm.
Preferably, the liquid crystal monomer is a thermotropic liquid crystal monomer, the thermotropic liquid crystal monomer is nematic liquid crystal or cholesteric liquid crystal, preferably negative cholesteric liquid crystal, and the dielectric constant of the thermotropic liquid crystal monomer is less than zero (delta epsilon < 0).
Preferably, the sputtering type is direct current sputtering, the sputtering pressure is 3-5Pa, and the sputtering atmosphere is a mixed gas of argon and oxygen.
Preferably, the photoinitiator comprises at least one of methacrylate, alkylbenzene ketone and benzophenone, and the accelerator is a silane coupling agent.
Preferably, in the step 4, the applied voltage is 15-115V, the frequency of the applied voltage is 0-800 Hz, the intensity of ultraviolet light is 30-90 mw/cm2, and the irradiation time of the ultraviolet light is 240-3600 s.
Preferably, in step 1, the substrate is a glass layer; further, the thickness of the substrate is 0.4-1.2 mm.
An electro-dimming film is prepared by the preparation method.
The invention has the beneficial effects that:
the preparation method provided by the invention cleans the substrate and removes the electrical impedance impurities of the surface layer; wet mixing indium tin oxide powder, nickel oxide powder, tungsten oxide powder and lithium oxide powder, heating and dehumidifying to prepare prefabricated composite powder, granulating and screening, performing cold press molding on the composite powder with effective particle size, and sintering at high temperature to prepare an ITO target material which has uniform components and is beneficial to sputtering to form an integral balanced and reliable ITO conductive film layer and promoting the conductivity of the ITO target material; the liquid crystal monomer can adopt nematic liquid crystal or cholesteric liquid crystal, the spacer is matched with the liquid crystal monomer to be mixed, the mixing of the dispersed liquid crystal monomer and the early-stage material can be accelerated, the flowing of the liquid crystal layer is promoted by utilizing the reliable diluting capability and the low viscosity characteristic of the vinyl ether monomer and the ethylene glycol phenyl ether monomer, the liquid crystal layer is fully homogenized, the liquid crystal layer is oriented by an electric field and is compact after being subjected to ultraviolet curing, the driving voltage of the prepared and formed dimming film is lower, and the dimming effect of the linear light transmittance is excellent;
molecules such as indium tin oxide, nickel oxide, tungsten oxide, lithium oxide and the like contained in the ITO conductive film layer have certain resistance, the resistance of the ITO conductive film layer is higher than that of the inner liquid crystal film layer, the outer heat is transmitted through the substrate, the temperature influence on the phase change of the molecules in the liquid crystal film layer can be avoided, the light transmission and dimming are unreliable, and the whole stability and compatibility of the dimming film are good.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
Fig. 1 is a schematic structural diagram of the present invention, in which fig. 1 is a substrate, 2 is an ITO conductive film layer, 3 is a liquid crystal film, and 4 is a liquid optical cement LOCA.
Detailed Description
The embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1:
referring to fig. 1, in the present embodiment, a liquid crystal film 3 is formed by sandwiching two substrates 1 and rolling a liquid crystal layer, the liquid crystal layer is homogenized sufficiently and formed compactly, the ITO conductive film layer 2 and the liquid crystal film 3 are used for dimming and conducting together to improve the conductive performance of the dimming film, reduce the driving voltage and promote energy saving, the outer substrate 1 can form reliable protection for the conductive structure of the inner layer, the bonding edge of the substrate 1 and the liquid crystal film 3 is coated by liquid optical adhesive LOCA4 to promote the tight connection of the structure, and the strength is good.
Example 2:
an electro-dimming film and a preparation method thereof specifically comprise the following steps:
step 1: treating the surface of the substrate:
respectively and sequentially carrying out ultrasonic cleaning on the substrate for 5min by using hydrogen peroxide, ultrapure water, acetone and ethanol, and drying to obtain a cleaned substrate;
step 2: performing magnetron sputtering on the single-side layer of the substrate obtained in the step 1 to plate a conductive film layer:
manufacturing a target material: uniformly mixing indium tin oxide powder, nickel oxide powder, tungsten oxide powder and lithium oxide powder with uniform granularity by a wet method, wherein the mass ratio of the indium tin oxide powder to the nickel oxide powder to the tungsten oxide powder to the lithium oxide powder is 35:25:20:10, heating to prepare prefabricated composite powder, granulating and screening the prefabricated composite powder, performing cold press molding on the composite powder with effective particle size, wherein the pressure of the cold press molding is 250MPa, and then sintering at high temperature, namely pressure sintering; sintering at 1300 ℃ for 4h to obtain the ITO target material;
sputtering: ionizing to generate electrons to bombard the ITO target, and depositing to prepare an ITO conductive film layer, wherein the sputtering type is direct current sputtering, the sputtering pressure is 4Pa, and the sputtering atmosphere is mixed gas of argon and oxygen (the volume ratio is 9: 1);
and step 3: under the shading condition, fully and uniformly mixing an acrylic liquid crystal resin monomer, an acrylate monomer, a vinyl ether monomer, an ethylene glycol phenyl ether monomer, a photoinitiator and an accelerator in proportion, wherein the mass ratio of the acrylic liquid crystal resin monomer, the acrylate monomer, the vinyl ether monomer, the ethylene glycol phenyl ether monomer, the photoinitiator, the accelerator and a spacer is 24:12:8:6:1.2:0.4:48:0.4, the photoinitiator is methacrylate, the accelerator is a silane coupling agent, the liquid crystal monomer and the spacer are added and uniformly mixed, the liquid crystal monomer is cholesteric liquid crystal, and a liquid crystal layer is prepared after defoaming;
and 4, step 4: and (3) sandwiching the liquid crystal layer in the step (3) by the two substrate coating surfaces in the step (2), rolling the outer side surface layer of the substrate to enable the liquid crystal layer to form a liquid crystal film, applying an electric field to the liquid crystal film, applying a voltage of 80V, applying a voltage frequency of 700Hz, orienting liquid crystal molecules, performing ultraviolet curing on the liquid crystal film, wherein the ultraviolet light intensity is 70mw/cm2, the ultraviolet light irradiation time is 900s, and then coating liquid optical cement LOCA on the edge part of the substrate for covering.
Example 3:
this example differs from example 2 in that:
in the step 2: the mass ratio of indium tin oxide powder to nickel oxide powder to tungsten oxide powder to lithium oxide powder is 40:22:20: 8; the pressure of cold press molding is 280MPa, and then high-temperature sintering is carried out, wherein the high-temperature sintering is pressure sintering; the sintering temperature is 1100 ℃, and the sintering time is 3 h.
In the step 3: the mass ratio of an acrylic liquid crystal resin monomer, an acrylate monomer, a vinyl ether monomer, an ethylene glycol phenyl ether monomer, a photoinitiator, an accelerator and a liquid crystal monomer to a spacer is 30:25:10:7:0.8:0.3:26: 0.9;
in the step 4: the voltage applied by the electric field is 80V, the frequency of the applied voltage is 600Hz, the intensity of ultraviolet light is 60mw/cm2, and the irradiation time of the ultraviolet light is 1200 s.
Example 4:
this example differs from example 2 in that:
in the step 2: the mass ratio of the indium tin oxide powder to the nickel oxide powder to the tungsten oxide powder to the lithium oxide powder is 35:25:20: 10; the pressure of cold press molding is 300MPa, and then high-temperature sintering is carried out, wherein the high-temperature sintering is normal-pressure sintering; the sintering temperature is 1300 ℃, the sintering time is 4h,
in the step 3: the mass ratio of the acrylic liquid crystal resin monomer, the acrylate monomer, the vinyl ether monomer, the ethylene glycol phenyl ether monomer, the photoinitiator, the accelerator and the liquid crystal monomer to the spacer is 35:8:5:5:0.4:0.1:46: 0.5;
in the step 4: the voltage applied by the electric field is 80V, the frequency of the applied voltage is 800Hz, the intensity of ultraviolet light is 70mw/cm2, and the irradiation time of the ultraviolet light is 1200 s.
Example 5:
this example differs from example 2 in that:
in the step 2: the mass ratio of the indium tin oxide powder to the nickel oxide powder to the tungsten oxide powder to the lithium oxide powder is 35:25:20: 10; the pressure of cold press molding is 210MPa, and then high-temperature sintering is carried out, wherein the high-temperature sintering is normal-pressure sintering; the sintering temperature is 1680 ℃, the sintering time is 10h,
in the step 3: the mass ratio of the acrylic liquid crystal resin monomer, the acrylate monomer, the vinyl ether monomer, the ethylene glycol phenyl ether monomer, the photoinitiator, the accelerator and the liquid crystal monomer to the spacer is 15:25:15:10:1:0.2:33: 0.8;
in the step 4: the voltage applied by the electric field is 100V, the frequency of the applied voltage is 800Hz, the intensity of ultraviolet light is 60mw/cm2, and the irradiation time of the ultraviolet light is 2400 s.
Example 6:
this example differs from example 2 in that:
in the step 2: the mass ratio of the indium tin oxide powder to the nickel oxide powder to the tungsten oxide powder to the lithium oxide powder is 35:25:20: 10; the pressure of cold press molding is 230MPa, and then high-temperature sintering is carried out, wherein the high-temperature sintering is normal-pressure sintering; the sintering temperature is 1600 ℃, the sintering time is 12h,
in the step 3: the mass ratio of the acrylic liquid crystal resin monomer, the acrylate monomer, the vinyl ether monomer, the ethylene glycol phenyl ether monomer, the photoinitiator, the accelerator and the liquid crystal monomer to the spacer is 32:15:20:9:1.5:0.5:21: 1;
in the step 4: the voltage applied by the electric field is 80V, the frequency of the applied voltage is 700Hz, the intensity of ultraviolet light is 90mw/cm2, and the irradiation time of the ultraviolet light is 2400 s.
Table 1 shows the quality ratio of the raw materials for preparing the composite powder
| Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Indium tin oxide powder | 30 | 40 | 45 | 38 | 50 |
| Nickel oxide powder | 35 | 32 | 25 | 32 | 20 |
| Tungsten oxide powder | 20 | 20 | 15 | 25 | 18 |
| Lithium oxide powder | 15 | 8 | 15 | 5 | 12 |
Table 2 shows the mass ratio of the raw materials for preparing the liquid crystal layer
| Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Acrylic resin monomer | 24 | 30 | 35 | 15 | 32 |
| Acrylate monomer | 12 | 25 | 8 | 25 | 15 |
| Vinyl ether monomer | 8 | 10 | 5 | 15 | 20 |
| Ethylene glycol phenyl ether monomer | 6 | 7 | 5 | 10 | 9 |
| Photoinitiator | 1.2 | 0.8 | 0.4 | 1 | 1.5 |
| Accelerator | 0.4 | 0.3 | 0.1 | 0.2 | 0.5 |
| Liquid crystal monomer | 48 | 26 | 46 | 33 | 21 |
| Spacer | 0.4 | 0.9 | 0.5 | 0.8 | 1 |
Table 3 is a table comparing the properties of examples 2 to 6
| Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Fading transmittance | 72％ | 75％ | 60％ | 70％ | 70％ |
| Colored transmittance | 5％ | 5％ | 8％ | 8％ | 10％ |
| Surface resistance | 90Ω | 82Ω | 105Ω | 98Ω | 115Ω |
| Uniformity of surface resistance | <8％ | <7％ | <10％ | <8％ | <10％ |
| Operating voltage | 48V | 48V | 48V | 48V | 48V |
| Saturation voltage | <32V | <30V | <40V | <38V | <40V |
| Power of | ＜6W/M2 | ＜5W/M2 | ＜7W/M2 | ＜6W/M2 | ＜8W/M2 |
| Response time (Power on) | 40ms | 36ms | 48ms | 45ms | 66ms |
The invention firstly cleans the substrate to remove the electrical impedance impurities on the surface layer; sputtering and coating a single-side layer of a substrate, mixing indium tin oxide powder, nickel oxide powder, tungsten oxide powder and lithium oxide powder by a wet method, heating and dehumidifying to prepare prefabricated composite powder, granulating and screening, performing cold press molding on the composite powder with effective particle size, and sintering at high temperature to prepare an ITO target material which has uniform target material components, is beneficial to sputtering to form an integrally balanced and reliable ITO conductive film layer and promotes the conductivity of the ITO target material; in the modulated liquid crystal layer, the liquid crystal monomer can adopt nematic liquid crystal or cholesteric liquid crystal, and the spacer is mixed with the liquid crystal monomer, so that the mixing of the dispersed liquid crystal monomer and the early-stage material can be accelerated, and the reliable diluting capability and the low viscosity characteristic of the vinyl ether monomer and the ethylene glycol phenyl ether monomer are utilized to promote the flowing of the liquid crystal layer, so that the wettability is strong, and the liquid crystal layer is fully homogenized; the two substrates are clamped, the liquid crystal layer is rolled to form a liquid crystal film, electric field orientation and ultraviolet light curing are carried out, liquid optical cement is coated on the edges of the substrates and the liquid crystal film, the liquid crystal film is formed compactly after being subjected to electric field orientation and ultraviolet curing, the formed dimming film is low in driving voltage, and the dimming effect of excellent light transmittance is achieved; molecules such as indium tin oxide, nickel oxide, tungsten oxide and lithium oxide contained in the ITO conductive film layer have certain resistance, the resistance is higher than that of the inner liquid crystal film, the outer heat is transmitted through the substrate, the phase change of the molecules in the liquid crystal film due to temperature influence can be avoided, light transmission and dimming are unreliable, and the overall stability and compatibility of the dimming film are good.
Through the tests of the embodiments 2-6, the working voltage is 48V, the surface resistances of the embodiments 2-5 are less than or equal to 105 omega, the surface resistance uniformity of the embodiments 2-6 is less than 10 percent, the saturation voltage is less than 40 percent, the electrical property is good, the response time is short, the conductive capability is excellent, the power consumption is low, and the energy-saving effect is achieved; in terms of optics, the fading transmittance of the examples 2 to 6 is less than or equal to 75 percent, the coloring transmittance of the examples 2 to 5 is less than or equal to 8 percent, and the dimming effect is good.
Although the preferred embodiments of the present patent have been described in detail, the present patent is not limited to the above embodiments, and various changes and modifications can be made without departing from the spirit of the present patent within the knowledge of those skilled in the art.
Claims (10)
1. The preparation method of the electro-dimming film is characterized by comprising the following steps of:
step 1: treating the surface of the substrate:
respectively and sequentially carrying out ultrasonic cleaning on the substrate for 5min by using hydrogen peroxide, ultrapure water, acetone and ethanol, and drying to obtain a cleaned substrate;
step 2: performing magnetron sputtering on the single-side layer of the substrate obtained in the step 1 to plate a conductive film layer:
manufacturing a target material: uniformly mixing indium tin oxide powder, nickel oxide powder, tungsten oxide powder and lithium oxide powder with uniform granularity by a wet method, heating to prepare prefabricated composite powder, granulating and screening the prefabricated composite powder, performing cold press molding on the composite powder with effective grain size, and sintering at high temperature to prepare an ITO target material;
sputtering: ionizing to generate electrons to bombard the ITO target material, and depositing to prepare an ITO conductive film layer;
and step 3: under the shading condition, fully and uniformly mixing an acrylic liquid crystal resin monomer, an acrylate monomer, a vinyl ether monomer, an ethylene glycol phenyl ether monomer, a photoinitiator and an accelerator in proportion, adding a liquid crystal monomer, mixing and stirring uniformly with a spacer, and defoaming to prepare a liquid crystal layer;
and 4, step 4: and (3) clamping the liquid crystal layer obtained in the step (3) by the two substrate coating surfaces obtained in the step (2), rolling the outer side surface layer of the substrate to form a liquid crystal film on the liquid crystal layer, applying an electric field to the liquid crystal film to orient liquid crystal molecules, performing ultraviolet curing on the liquid crystal film, and then coating liquid optical cement LOCA on the edge part of the substrate for covering.
2. The method of claim 1, wherein the step of forming the electro-optic film comprises: in step 2, the mass ratio of the raw materials for manufacturing the target material is as follows:
3. the method of claim 1, wherein the step of forming the electro-optic film comprises: in the step 2, the pressure of the composite powder cold press molding is 210-300MPa, the high-temperature sintering can adopt normal-pressure sintering or pressure sintering, the sintering temperature is 1100-1680 ℃, and the sintering time is 2-12 h.
4. The method of claim 1, wherein the step of forming the electro-optic film comprises: in step 3, the liquid crystal layer is prepared from the following raw materials in percentage by mass:
the spacer is rigid microbead with diameter of 20-35 μm.
5. The method of claim 1, wherein the step of forming the electro-optic film comprises: the liquid crystal monomer is a thermotropic liquid crystal monomer, and the thermotropic liquid crystal monomer is nematic liquid crystal or cholesteric liquid crystal.
6. The method of claim 1, wherein the step of forming the electro-optic film comprises: the sputtering type is direct current sputtering, the sputtering pressure is 3-5Pa, and the sputtering atmosphere is mixed gas of argon and oxygen.
7. The method of claim 1, wherein the step of forming the electro-optic film comprises: the photoinitiator comprises at least one of methacrylate, alkylbenzene ketone and benzophenone, and the accelerator is a silane coupling agent.
8. The method of claim 1, wherein the step of forming the electro-optic film comprises: in the step 4, the applied voltage is 15-115V, the applied voltage frequency is 0-800 Hz, the ultraviolet light intensity is 30-90 mw/cm2, and the ultraviolet light irradiation time is 240-3600 s.
9. The method of claim 1, wherein the step of forming the electro-optic film comprises: in step 1, the substrate is a glass layer.
10. An electro-dimming thin film prepared by the preparation method of any one of claims 1 to 9.
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