CN112379546A - Polymer disperse dye liquid crystal material, electrochromic dimming film and preparation method - Google Patents
Polymer disperse dye liquid crystal material, electrochromic dimming film and preparation method Download PDFInfo
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Images
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
- G02F1/1334—Constructional arrangements; Manufacturing methods based on polymer dispersed liquid crystals, e.g. microencapsulated liquid crystals
-
- 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
-
- 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
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
- C09K9/02—Organic tenebrescent materials
-
- 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
- G02F1/1514—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 characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1516—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 characterised by the electrochromic material, e.g. by the electrodeposited material comprising organic material
- G02F1/15165—Polymers
-
- 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
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/14—Macromolecular compounds
- C09K2211/1441—Heterocyclic
- C09K2211/145—Heterocyclic containing oxygen as the only heteroatom
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- Materials Engineering (AREA)
- Optics & Photonics (AREA)
- Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Mathematical Physics (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
- Liquid Crystal (AREA)
Abstract
The invention relates to a polymer disperse dye liquid crystal material, an electrochromic dimming film and a preparation method thereof, wherein the polymer disperse dye liquid crystal material comprises a dye liquid crystal composition and thermosetting glue, the dye liquid crystal composition comprises negative liquid crystal and dichroic dye, and the thermosetting glue comprises the following components in percentage by mass: 40-60% of epoxy resin, 1-5% of reactive diluent, 0.5-1% of coupling agent, 5-15% of amine curing agent, 5-15% of imidazole curing agent and 4-10% of curing accelerator. The polymer disperse dye liquid crystal material and the electrochromic dimming film prepared from the same have excellent aging resistance, are transparent when power is off, are frosted when power is on, are shading, can realize roll-to-roll production and laser heating curing, and have high production efficiency.
Description
Technical Field
The invention relates to the technical field of dimming films, in particular to a polymer disperse dye liquid crystal material, an electrochromic dimming film and a preparation method of the electrochromic dimming film.
Background
The PDLC light adjusting film, which is a polymer dispersed liquid crystal light adjusting film, adjusts the transparency of the film by controlling the alignment state of liquid crystals mainly by using a voltage. PDLC membrane of adjusting luminance is usually the outage dull polish, the circular telegram is transparent, and when the outage, the liquid crystal material unordered arrangement in the polymer dispersed liquid crystal layer, the scattering takes place when light passes the film, and the membrane of adjusting luminance is opaque state, and when the circular telegram, the electric field makes liquid crystal material ordered arrangement, and light can directly penetrate the film, and the membrane of adjusting luminance is transparent state. However, the PDLC light control film cannot replace a curtain because the total light transmittance does not change much between the on state and the off state.
Existing films for Electrochromic (EC) and Suspended Particle Devices (SPD) only achieve a change in transmittance, and no change in haze, and therefore can block visible light, but cannot achieve privacy.
Doping the PDLC with dyes can achieve transparency, privacy and light blocking. The existing PDLC commonly uses the light-cured glue, the light-cured glue can be rapidly cured under UV irradiation, the production efficiency of the PDLC film is improved, but the existing bidirectional dye generally has a highly conjugated molecular structure, the absorption of the bidirectional dye to UV is very strong in the curing reaction process of the light-cured glue, the bidirectional dye enters an excited state after absorbing UV, the excited dye and a functional group of the dye are easy to react with and decompose with a free radical of the light-cured glue, the product performance is poor, the fading phenomenon occurs, and the weather resistance is poor.
In summary, there is an urgent need to develop an electrochromic dimming film which can not only realize privacy, but also replace curtains and has good aging performance.
Disclosure of Invention
In view of the defects of the prior art, the first object of the present invention is to provide a polymer disperse dye liquid crystal material, which can be thermally cured, wherein the dye is not easy to react and decompose during the thermal curing process, and the electrochromic material obtained after the thermal curing has good aging resistance, and is suitable for preparing a liquid crystal layer of an electrochromic dimming film, and can be switched between a bright state with transparency and a dark state with privacy and light-shielding properties when power is turned on or off.
The second purpose of the invention is to provide an electrochromic light-adjusting film with the material, wherein the film is transparent when power is off, and is frosted when power is on and can shield light.
The third purpose of the invention is to provide a preparation method of the electrochromic light-adjusting film, which has high production efficiency.
In order to achieve the first object of the invention, the invention provides a polymer disperse dye liquid crystal material, which comprises a dye liquid crystal composition and a thermosetting glue, wherein the dye liquid crystal composition comprises a negative liquid crystal and a dichroic dye, and the thermosetting glue is an epoxy resin composition. Preferably, the thermosetting glue comprises the following components in percentage by mass: 40-60% of epoxy resin, 1-5% of reactive diluent, 0.5-1% of coupling agent, 5-15% of amine curing agent, 5-15% of imidazole curing agent and 4-10% of curing accelerator.
Therefore, the electrochromic material with good aging resistance is obtained by combining the epoxy resin composition thermosetting glue with excellent performance and the dye liquid crystal composition with the response characteristic of an external field. The epoxy resin composition can be thermally cured, does not react with dye molecules in the thermal curing process, has excellent heat resistance and corrosion resistance, good insulating property and adhesive force and is easy to process into a film. The liquid crystal adopted in the dye liquid crystal composition is negative liquid crystal, the dye is dichroic dye, the dichroic dye mixed in the liquid crystal can be orderly arranged along the same direction with liquid crystal molecules along with a main transformer, when the negative liquid crystal is vertically arranged, the dichroic dye is vertically arranged along with the liquid crystal, the absorptivity of the material to light is low, so that the material is in a transparent and bright state, when the negative liquid crystal is powered on to be lodging, the dichroic dye is subsequently lodged, and when the negative liquid crystal is powered on, the material is high in light scattering and absorptivity, and is in a frosted and shading state. Specifically, the amine curing agent and the imidazole curing agent are compounded to form the fast-curing composite curing agent, wherein the amine curing agent participates in the curing process of the epoxy resin through an addition reaction, the imidazole curing agent participates in the curing through the reaction mechanism of anionic etherification polymerization, the amine curing agent and the imidazole curing agent are mutually promoted, and meanwhile, the reactive diluent and the promoter are added into the system to form a fast-curing epoxy resin system, so that the epoxy resin system is sufficiently thermally cured in a short time, and the production efficiency is improved. Moreover, the refractive index of the thermosetting glue is consistent with that of the negative liquid crystal, so that the haze is small in a transparent state and the thermosetting glue is very transparent. In addition, the thermosetting glue has good bonding performance, can ensure the bonding force of the dimming film when preparing the dimming film, is beneficial to coating the polymer disperse dye liquid crystal material and preparing the dimming film by a roll-to-roll process, and improves the strength of the prepared film.
Preferably, the epoxy resin is at least one of bisphenol a epoxy resin, bisphenol F epoxy resin, aliphatic epoxy resin, alicyclic epoxy resin, and rubber-modified epoxy resin.
Therefore, the epoxy resin in the thermosetting glue can be selected and combined from various types, wherein the bisphenol A epoxy resin has the advantages of high strength, low cost and the like, the bisphenol F epoxy resin has the advantages of low viscosity, good corrosion resistance and the like, the aliphatic epoxy resin has the advantages of low viscosity, good flexibility and the like, the alicyclic epoxy resin has the advantages of heat resistance, good weather resistance and the like, and the rubber modified epoxy resin has the advantages of good toughness and the like. Preferably, a combination of two or more epoxy resins may be used to obtain good overall properties, such as a combination of an aliphatic epoxy resin and a bisphenol F epoxy resin, or a combination of an aliphatic epoxy resin and a rubber-modified epoxy resin.
Preferably, the reactive diluent is at least one of ethylene glycol diglycidyl ether, butanediol diglycidyl ether and polypropylene glycol diglycidyl ether.
Therefore, the reactive diluent in the thermal curing glue can be selected and combined from various types, and the reactive diluent can play a role in reducing the viscosity of a system, is beneficial to coating a polymer disperse dye liquid crystal material into a film and can improve the flexibility of the material.
Preferably, the coupling agent is a silane coupling agent.
It can be seen that the coupling agent in the thermosetting glue of the invention can be a silane coupling agent, and the silane coupling agent can promote the dispersion of each component and improve the adhesive force of the polymer disperse dye liquid crystal material, such as the adhesive force with the orientation layer.
Preferably, the amine curing agent is a modified amine curing agent. More preferably, the amine curing agent is selected from one or more of 593 curing agent and 793 curing agent.
Therefore, the amine curing agent in the thermal curing glue can be selected and combined from various types, and the modified amine curing agent has the characteristics of low toxicity, small viscosity, high curing speed, good toughness of cured products and the like.
Preferably, the imidazole curing agent is at least one of 2-ethyl-4-methylimidazole and 2-methylimidazole. More preferably, the imidazole-based curing agent is 2-ethyl-4-methylimidazole.
It can be seen that the imidazole-based curing agent in the thermal curing glue of the present invention can be selected and combined from the above-mentioned various kinds. Wherein, the 2-ethyl-4-methylimidazole is liquid and has the advantages of easy dispersion and the like.
Preferably, the curing accelerator is at least one of dicyanodiamine accelerator and 2, 4, 6-tris (dimethylaminomethyl) phenol.
Therefore, the curing accelerator in the thermal curing glue can be selected and combined from various types, and has a good curing accelerating effect. Among them, the dicyanodiamide accelerator is an accelerator suitable for a dicyanodiamide curing agent, for example, an organic urea accelerator and the like.
Preferably, the dichroic dye is a black dichroic dye; the negative liquid crystal has a birefringence Δ n of 0.07 to 0.25, a refractive index no of 1.47 to 1.53 at a wavelength of 589nm and at 25 ℃, and a dielectric anisotropy Δ ε of-4 to-10 at a frequency of 1KHz and at 25 ℃.
Therefore, the dichroic dye is black and can play a good role in shading light. When the negative liquid crystal has a birefringence, an ordinary refractive index and a dielectric anisotropy in the above ranges, the polymer dispersed dye liquid crystal material has good optical properties and has a suitable threshold voltage.
Preferably, the mass ratio of the dye liquid crystal composition to the thermosetting glue is 90:10 to 60: 40.
Therefore, the mass ratio of the dye liquid crystal composition to the thermosetting glue can be selected within the range, so that the dye liquid crystal composition is well dispersed into a matrix formed by the thermosetting glue.
Preferably, the polymer disperse dye liquid crystal material also comprises microbeads, and the mass of the microbeads is 2-8 per thousand of the total mass of the dye liquid crystal composition and the thermosetting glue.
It can be seen that the polymer disperse dye liquid crystal material preferably further contains microbeads, which can function as spacers and can be used to control the thickness of the polymer disperse dye liquid crystal layer formed after the polymer disperse dye liquid crystal material is coated.
In order to achieve the second object of the present invention, the present invention provides an electrochromic dimming film, which includes a first substrate layer, a first conductive layer, a first vertical alignment layer, a polymer dispersed dye liquid crystal layer, a second vertical alignment layer, a second conductive layer, and a second substrate layer, which are sequentially stacked, wherein the polymer dispersed dye liquid crystal layer is formed by thermally curing the polymer dispersed dye liquid crystal material in any of the above schemes.
Therefore, the electrochromic dimming film is prepared by adopting the polymer disperse dye liquid crystal material, the polymer disperse dye liquid crystal is clamped between two vertical orientation layers of two conducting films with substrate layers, conducting layers and vertical orientation layers to form a sandwich structure, so that negative liquid crystal is vertically oriented and a dichroic dye is vertically oriented along with the negative liquid crystal when power is off, and the dimming film is in a transparent state and has the same performance as common glass; when the power is on, the negative liquid crystal falls down and the bidirectional dye falls down, and the dimming film is frosted and in a shading state. The light-adjusting film can be widely applied to occasions using glass, such as building doors and windows, building curtain walls, vehicles and the like. The thermal curing of the polymer disperse dye liquid crystal material can be infrared heating curing or laser heating curing, preferably laser heating curing, the curing time of the laser heating curing is short, and the production efficiency can be improved.
Preferably, the first substrate layer and the second substrate layer are each a colorless or colored PET substrate. When colored, the color is preferably black. The first conductive layer is formed by magnetron sputtering an ITO film on the first base material layer, and the second conductive layer is formed by magnetron sputtering an ITO film on the second base material layer.
As can be seen, the base layer of the light control film of the present invention is preferably a PET base material, and the conductive layer is preferably ITO, which has good light transmittance.
Preferably, the thickness of the polymer disperse dye liquid crystal layer is 3-15 μm.
It can be seen that the thickness of the polymer dispersed dye liquid crystal layer of the present invention can be selected within the above range, which can further improve the optical performance of the light control film. The thickness can be adjusted by beads.
In order to achieve the third object of the present invention, the present invention provides a method for preparing an electrochromic dimming film, comprising the steps of: preparing a conductive film formed by sequentially laminating a substrate layer, a conductive layer and a vertical orientation layer; coating a polymer disperse dye liquid crystal material between vertical orientation layers of two conductive films by adopting a roll-to-roll continuous production method, wherein the polymer disperse dye liquid crystal material is the polymer disperse dye liquid crystal material in any scheme; and carrying out laser thermal curing on the obtained film material. Preferably, the heat curing temperature is 80-160 ℃, and the heat curing time is 1-30 min.
Therefore, the electrochromic dimming film can be continuously produced by a roll-to-roll process, the production efficiency is high, and the production efficiency is further improved by a laser heating curing process. The laser heating solidification is an energy-saving, environment-friendly, convenient and efficient method which is three-dimensional from inside to outside and is heated without contact by the absorption wavelength of glue, and is suitable for various heating solidification glues, especially epoxy resin glue. The light source in the laser heating curing process is generally a point light source emitted from a laser, the common wavelengths are 976nm and 1064nm, the laser power is generally adjustable, and the appropriate thermal curing temperature and thermal curing time can be adjusted according to requirements. The laser has the characteristics of high brightness and good directivity, the energy of the laser light source is concentrated, the thermal diffusion spot is small, the light source can rapidly and thoroughly heat the glue, and the heated glue is liquefied and then is added to enable the resin to be fully contacted and reacted with the curing agent, so that the purpose of rapid adhesion is achieved. Firstly, because the wavelength of laser is easily absorbed by glue, the reflection and scattering of the glue to a light source are relatively less during laser heating and curing, so that the curing efficiency is very high; secondly, the energy of the laser light source is high, so that the curing time is short, and various complex and deep surfaces can be cured; in addition, the laser curing mode has the advantages of simple device, easy realization, good curing effect and the like. In contrast, the conventional infrared heating simply uses air as a good heat conductor, and achieves the purpose of heat curing by transferring heat through air, and the essence of the infrared heating is heat transfer, so that the heat utilization rate is low, the infrared heating time is longer, usually more than 1h, which results in lower production efficiency, and the infrared heating has poor curing effect on corners or hidden surfaces of products due to difficult heat transfer.
Drawings
Fig. 1 is a structural diagram of an electrochromic light-adjusting film prepared in an example of the present invention.
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Detailed Description
Example 1
The electrochromic dimming film of this example was prepared by the following steps:
the method comprises the following steps: a colorless and transparent PET base material with the thickness of 125 mu m is selected, the visible light transmittance of the transparent PET base material is 89%, and the haze is 0.6%;
step two: an ITO film is plated on a colorless and transparent PET substrate in a magnetron sputtering mode, the sheet resistance is 100 omega/□, the visible light transmittance is 82%, and the haze is 0.7%;
step three: coating an alignment layer on the ITO film, wherein the alignment layer is made of polyimide materials, the thermosetting temperature is 120 ℃, the curing time is 5min, and the thickness of the cured alignment layer is 50 nm;
step four: preparing a dye liquid crystal material, wherein the color of the dye liquid crystal is black, the birefringence index delta n is 0.11, the ordinary light refractive index no (589nm,25 ℃) is 1.478, and the dielectric anisotropy delta epsilon (1KHz,25 ℃) of the liquid crystal is-5.8;
step five: preparing thermosetting glue, wherein the glue consists of 20-25 wt% of bisphenol F epoxy resin, 30-35 wt% of aliphatic epoxy resin, 3 wt% of butanediol diglycidyl ether, 1 wt% of silane active coupling agent, 10-13 wt% of 593 curing agent, 5-8 wt% of 2-ethyl-4-methylimidazole and 5-8 wt% of dicyandiamide accelerator;
step six: mixing the dye liquid crystal material and the thermosetting glue according to the mass ratio of 80:20, and then uniformly stirring at normal temperature to obtain polymer dispersed dye liquid crystal;
step seven: adding microbeads with the diameter of 10 mu m into the polymer disperse dye liquid crystal, wherein the adding proportion is 3 wt% of the polymer disperse dye liquid crystal;
step eight: continuously laminating by using a roll-to-roll mode, and then curing by using laser thermocuring equipment, wherein the curing temperature is 100 ℃, the curing time is 6min, and the electrochromic dimming film is produced;
step nine: manufacturing an electrode, and carrying out photoelectric performance test to obtain that the visible light transmittance of the electrochromic dimming film is 50%, the haze is 4%, the visible light transmittance of the electrochromic dimming film is 10% and the haze is 75% in a power-off state and a 36V power-on state;
step ten: performing an aging test, and irradiating for 240 hours by using a xenon lamp without obvious color change; the change rate of each index of 240h of high temperature and high humidity is less than 10 percent.
As shown in fig. 1, the electrochromic light-modulating film prepared in this embodiment includes seven layers of materials stacked in sequence, where the first layer 1 is a PET substrate, the second layer 2 is an ITO conductive layer, the third layer 3 is a vertical alignment layer, the fourth layer 4 is a polymer dispersed dye liquid crystal material layer, the fifth layer 5 is a vertical alignment layer, the sixth layer 6 is an ITO conductive layer, and the seventh layer 7 is a PET substrate.
Comparative example 1
The film of this comparative example was prepared by the following steps:
the method comprises the following steps: a colorless transparent PET substrate with the thickness of 125 mu m is selected, the visible light transmittance of the transparent PET substrate is 89%, and the haze is 0.6%;
step two: an ITO film is plated on a colorless and transparent PET substrate in a magnetron sputtering mode, the sheet resistance is 100 omega/□, the visible light transmittance is 82%, and the haze is 0.7%;
step three: coating an alignment layer on the ITO film, wherein the alignment layer is made of polyimide materials, the thermosetting temperature is 120 ℃, the curing time is 5min, and the thickness of the cured alignment layer is 50 nm;
step four: preparing a dye liquid crystal material, wherein the color of the dye liquid crystal is black, the birefringence index delta n is 0.11, no (589nm,25 ℃) is 1.478, and delta epsilon (1KHz,25 ℃) is-5.8;
step five: preparing photocuring glue, wherein the glue is prepared by mixing 30-35 wt% of isobornyl acrylate, 20-25 wt% of methacrylate, 10-15 wt% of 2-hydroxyethyl methacrylate, 24-28 wt% of acrylic acid and 1 wt% of photoinitiator TPO in proportion;
step six: mixing the dye liquid crystal material and the photocuring glue according to the mass ratio of 80:20, and then uniformly stirring at normal temperature to obtain polymer dispersed dye liquid crystal;
step seven: adding microbeads with the diameter of 10 mu m into the polymer disperse dye liquid crystal, wherein the adding proportion is 3 wt% of the polymer disperse dye liquid crystal;
step eight: continuously laminating the liquid crystal film in a roll-to-roll manner, and then carrying out ultraviolet curing on the liquid crystal film, wherein the UV light intensity is 6mw/cm2The curing temperature is 23 ℃, and the curing time is 4 min;
step nine: manufacturing an electrode, and carrying out a photoelectric performance test, wherein the visible light transmittance is 51%, the haze is 3.5% in a power-off state, the visible light transmittance is 8% in a 36V power-on state, and the haze is 55%;
step ten: and (4) carrying out an aging test, and obviously changing the film into yellow brown after the xenon lamp irradiates for 144 h.
The main difference between the comparative example 1 and the example 1 is that the comparative example 1 adopts the photo-curing glue, the photo-curing glue in the polymer disperse dye liquid crystal material is cured in an ultraviolet light curing mode, and the component usage, operation and process parameters in the other preparation steps are the same as those in the example 1. The comparison shows that the aging resistance of the electrochromic film of example 1 is better.
Example 2
The electrochromic dimming film of this example was prepared by the following steps:
the method comprises the following steps: selecting a black transparent PET substrate with the thickness of 50 mu m, wherein the visible light transmittance of the transparent PET substrate is 60 percent, and the haze is 0.9 percent;
step two: an ITO film is plated on a black transparent PET substrate in a magnetron sputtering mode, the sheet resistance is 150 omega/□, the visible light transmittance is 54%, and the haze is 0.9%;
step three: coating an alignment layer on the ITO film, wherein the alignment layer is made of polyimide, the thermosetting temperature is 100 ℃, the curing time is 6min, and the thickness of the cured alignment layer is 10 nm;
step four: preparing a dye liquid crystal material, wherein the color of the dye liquid crystal is black, the birefringence index delta n is 0.18, the ordinary light refractive index no (589nm,25 ℃) is 1.50, and the dielectric anisotropy delta epsilon (1KHz,25 ℃) of the liquid crystal is-8.2;
step five: preparing thermosetting glue, wherein the glue consists of 35-40 wt% of aliphatic epoxy resin, 15-20 wt% of rubber modified epoxy resin, 3.5-4.5 wt% of ethylene glycol diglycidyl ether, 0.3-0.5 wt% of silane active coupling agent, 793 curing agent, 12-15 wt% of 2-ethyl-4-methylimidazole and 5-8 wt% of DMP-30;
step six: mixing the dye liquid crystal material and the thermosetting glue according to the mass ratio of 65:35, and then uniformly stirring at normal temperature to obtain polymer dispersed dye liquid crystal;
step seven: adding microbeads with the diameter of 12 microns into the polymer disperse dye liquid crystal, wherein the adding proportion is 3 wt% of the polymer disperse dye liquid crystal;
step eight: continuously laminating by using a roll-to-roll mode, and then curing by using laser thermocuring equipment, wherein the curing temperature is 110 ℃, the curing time is 5min, and the electrochromic dimming film is produced;
step nine: manufacturing an electrode, and carrying out photoelectric performance test to obtain that the visible light transmittance of the electrochromic dimming film in a power-off state is 48%, the haze is 5%, the visible light transmittance of the electrochromic dimming film in a 36V power-on state is 6%, and the haze is 90%;
step ten: performing an aging test, and irradiating for 240 hours by using a xenon lamp without obvious color change; the change rate of each index of 240h of high temperature and high humidity is less than 10 percent.
Finally, it should be emphasized that the above-described embodiments are merely preferred examples of the invention, which is not intended to limit the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The polymer disperse dye liquid crystal material is characterized by comprising a dye liquid crystal composition and thermosetting glue, wherein the dye liquid crystal composition comprises negative liquid crystal and dichroic dye, and the thermosetting glue comprises the following components in percentage by mass:
40 to 60 percent of epoxy resin,
1-5% of active diluent,
0.5 to 1 percent of coupling agent,
5 to 15 percent of amine curing agent,
5 to 15 percent of imidazole curing agent,
4-10% of a curing accelerator.
2. The polymer dispersed dye liquid crystal material of claim 1, characterized in that said dichroic dye is a black dichroic dye; the negative liquid crystal has a birefringence delta n of 0.07-0.25, an ordinary refractive index no of 1.47-1.53 at a wavelength of 589nm and at 25 ℃, and a dielectric anisotropy delta epsilon of-4-10 at a frequency of 1KHz and at 25 ℃.
3. The polymer disperse dye liquid crystal material according to claim 1 or 2, characterized in that:
the epoxy resin is at least one of bisphenol A epoxy resin, bisphenol F epoxy resin, aliphatic epoxy resin, alicyclic epoxy resin and rubber modified epoxy resin;
the reactive diluent is at least one of ethylene glycol diglycidyl ether, butanediol diglycidyl ether and polypropylene glycol diglycidyl ether;
the coupling agent is a silane coupling agent;
the amine curing agent is a modified amine curing agent;
the imidazole curing agent is at least one of 2-ethyl-4-methylimidazole and 2-methylimidazole;
the curing accelerator is at least one of dicyandiamide accelerator and 2, 4, 6-tris (dimethylaminomethyl) phenol.
4. The polymer dispersed dye liquid crystal material of claim 3, wherein:
the amine curing agent is one or more of 593 curing agent and 793 curing agent;
the imidazole curing agent is 2-ethyl-4-methylimidazole.
5. The polymer dispersed dye liquid crystal material according to claim 1 or 2, characterized in that the mass ratio of the dye liquid crystal composition to the thermosetting glue is 90:10 to 60: 40.
6. The polymer dispersed dye liquid crystal material according to claim 1 or 2, wherein the polymer dispersed dye liquid crystal material further comprises microbeads, and the mass of the microbeads is 2-8% of the total mass of the dye liquid crystal composition and the thermosetting glue.
7. An electrochromic dimming film, comprising a first substrate layer, a first conductive layer, a first vertical alignment layer, a polymer dispersed dye liquid crystal layer, a second vertical alignment layer, a second conductive layer and a second substrate layer which are sequentially stacked, wherein the polymer dispersed dye liquid crystal layer is formed by thermally curing the polymer dispersed dye liquid crystal material according to any one of claims 1 to 6.
8. The electrochromic dimming film of claim 7, wherein:
the first substrate layer and the second substrate layer are colorless or colored PET substrates respectively;
the first conducting layer is formed on the first base material layer through magnetron sputtering of an ITO film, and the second conducting layer is formed on the second base material layer through magnetron sputtering of an ITO film;
the thickness of the polymer disperse dye liquid crystal layer is 3-15 mu m.
9. The preparation method of the electrochromic dimming film is characterized by comprising the following steps of:
preparing a conductive film formed by sequentially laminating a substrate layer, a conductive layer and a vertical orientation layer;
applying a polymer dispersed dye liquid crystal material between the vertical alignment layers of the two conductive films using a roll-to-roll continuous production method, the polymer dispersed dye liquid crystal material being the polymer dispersed dye liquid crystal material according to any one of claims 1 to 6;
and carrying out laser thermal curing on the obtained film material.
10. The method for preparing the electrochromic dimming film according to claim 9, wherein the laser thermal curing temperature is 80-160 ℃ and the laser thermal curing time is 1-30 min.
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