CN108873549B - Preparation method of suspended particle type intelligent window and intelligent window - Google Patents
Preparation method of suspended particle type intelligent window and intelligent window Download PDFInfo
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- CN108873549B CN108873549B CN201810563469.4A CN201810563469A CN108873549B CN 108873549 B CN108873549 B CN 108873549B CN 201810563469 A CN201810563469 A CN 201810563469A CN 108873549 B CN108873549 B CN 108873549B
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- G—PHYSICS
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- 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
- G02F1/165—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 translational movement of particles in a fluid under the influence of an applied field
- G02F1/166—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 translational movement of particles in a fluid under the influence of an applied field characterised by the electro-optical or magneto-optical effect
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- E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
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Abstract
The invention discloses a preparation method of a suspended particle type intelligent window, which comprises the following steps: (1) disposing a dielectric layer on a transparent substrate; (2) curing the dielectric layer and carrying out hydrophilic treatment; (3) manufacturing a cracking template on the dielectric layer: (4) forming a cracking network transparent conductive electrode on a transparent substrate; (5) preparing modified nano titanium dioxide sol; (6) and injecting the modified nano titanium dioxide sol between two cracking network transparent conductive electrodes and packaging to obtain the suspended particle type intelligent window. The method has the advantages of simple process, high efficiency, low cost, convenience for mass production and easiness for realizing industrialization. The invention also aims to provide the suspended particle type intelligent window manufactured by the method, which has the advantages of low driving voltage, low power, quick response, accurate control, high light transmittance and good chemical and thermal stability.
Description
Technical Field
The invention belongs to the technical field of intelligent windows, and particularly relates to a preparation method of a suspended particle type intelligent window and the intelligent window.
Background
A Smart window (Smart windows) is an optical device composed of a substrate (glass or other transparent materials and the like) and a light-adjusting substance, and can generate coloring or fading reactions in certain sections of a solar spectrum under the excitation of certain physical and chemical factors (such as illumination, electromagnetic radiation, an electric field, gas and temperature) to cause the change of optical characteristics of the light-adjusting substance, so that the spectrum selectively absorbs or reflects solar radiation, and the purposes of shielding ultraviolet rays, adjusting the intensity of sunlight entering a room and heat exchange between the room and the outside, reducing the energy consumption of refrigeration and heating, reducing carbon emission and the like are achieved. When voltage, light or heat is applied, its light transmission characteristics change, typically from translucent to transparent, from blocking part (or all) of the light wavelength to letting it pass. Smart window technologies include electrochromic, photochromic, thermo-optic dimming, suspended particle, and the like types. The intelligent window can save the cost of heating, air conditioner and illumination, and the intelligent window can also obstruct the ultraviolet ray, reduces the fabric and fades. Key aspects of smart windows include material costs, installation costs, power costs and durability, as well as functional characteristics such as control speed, dimming possibilities and transparency. The following briefly introduces different types of smart windows that are common.
Photochromism and thermochromism are two passive smart windows. Photochromic (photochromysm) means that under the action of light with certain wavelength and intensity, the molecular structure of some compounds can be changed, so that the corresponding change of the absorption peak value of the compounds to the light, namely the color is caused, and the change is generally reversible. Mainly applied to the glasses, can change from a transparent state under the indoor dim condition to a dark state under the outdoor bright condition; the cost is low, the size is large, but the durability problem is difficult to solve, the application field is limited, and the commercial production is not available. Thermal dimming (coherent Light Adjusted) refers to a phenomenon that changes its transmission or absorption characteristics for incident Light depending on the change of ambient temperature. The optical properties of the material are mainly classified into three types, namely thermochromic type, thermotropic scattering type and bifunctional type according to the change of the optical properties with temperature. The thermochromic dimming material can change the absorption characteristic of the thermochromic dimming material to a certain visible light waveband along with the change of temperature, and reversible color conversion is generated; the thermoluminescent scattering type dimming material can present reversible transmittance conversion along with the temperature change; the dual-function light-adjusting material has the functions of the two materials, and transparency transition and color transition occur simultaneously along with temperature change, but the use conditions limit the commercial application and development of the dual-function light-adjusting material. The passive intelligent window can only respond to a single environment variable, and the use condition is harsh, so that the passive intelligent window cannot be well used.
As one of the active smart windows that are very common today, electrochromic (electrochromic) devices respond to voltage by changing the transmission characteristics of light, thereby controlling the transfer of light and heat. In electrochromic glazing, the electrochromic material changes its opacity, which changes between a transparent and a colored state. Changing its opacity requires a large amount of power, but once changed, no power is required to maintain the particular shadow that has been reached. Recent developments in electrochromic materials involving transition metal hydrides have led to the development of reflective hydrides, the generation of which is reflective rather than absorptive, thus enabling switching states between transparent and specular. The development of modified porous nanocrystalline films has led to the development of electrochromic display technology in recent years, where a single substrate display structure is composed of several laminated porous layers that can be printed on a substrate of a transparent conductor (e.g., ITO or PEDOT: PSS). These color-changing substances change color through a reduction or oxidation process. However, the electrochromic device has a slow response speed, high power consumption and a long service life, so that a new design of a smart window is urgently needed.
Suspended Particle Devices (SPDs) have become an area of interest for smart windows as a means for controlling the transmission of electromagnetic radiation because of their advantages of immediate, accurate light control and cost effectiveness. Smart windows can be controlled by a variety of media, such as automatic light sensors and motion detectors, smart phone applications, smart building and vehicle systems, knobs or light switches. The operating principle of the SPD technology is that particles having oriented light absorption characteristics are dispersed in a suspension, and when power is off, the particles are randomly arranged due to brownian motion, and can absorb more than 99% of visible light. When an alternating voltage of 110V is applied to the SPD film, the particles are aligned under the action of an electric field, and light is transmitted. The intelligent light control technology increases the control of the user to the environment, provides better comfort and happiness for the user, and improves the energy efficiency. Data published by metsdes-gallo shows that suspended particle device technology can reduce the in-vehicle temperature by 10 ℃, other advantages include reduced carbon emissions and elimination of the need for expensive window decoration, and suspended particle device smart windows are patented by the market companies at the research front. However, the traditional SPD needs larger driving voltage, and the safety problem cannot be ignored.
Disclosure of Invention
The invention aims to provide a preparation method of a suspended particle type intelligent window, which has the advantages of simple process, high efficiency, low cost, convenience for mass production and easiness in realizing industrialization.
The invention also aims to provide the suspended particle type intelligent window manufactured by the method, which has the advantages of low driving voltage, low power, quick response, accurate control, high light transmittance and good chemical and thermal stability.
The first object of the present invention is achieved by the following technical solutions: a preparation method of a suspended particle type intelligent window comprises the following steps:
(1) selecting a transparent substrate, and arranging a dielectric layer on the transparent substrate;
(2) curing the dielectric layer and carrying out hydrophilic treatment;
(3) setting a cracking film on the cured dielectric layer, and controlling the heating temperature and the heat preservation time to enable the cracking film to naturally crack to form a cracking template;
(4) removing the dielectric layer which is not covered by the cracking template by adopting plasma, forming a cracking network on the transparent substrate, and removing the cracking template on the cracking network by adopting a cleaning solvent to form a cracking network transparent conductive electrode;
(5) selecting nano titanium dioxide, carrying out lipophilic modification by adopting a surfactant, and dispersing in a dispersing agent to prepare modified nano titanium dioxide sol;
(6) and arranging the modified nano titanium dioxide sol between at least two crack network transparent conductive electrodes and carrying out packaging treatment to obtain the suspended particle type intelligent window.
In the preparation method of the suspended particle type smart window, the steps of:
the material of the transparent substrate in the step (1) includes, but is not limited to, at least one of tin-doped indium oxide (ITO), fluorine-doped tin oxide (FTO), and aluminum-doped zinc oxide (AZO).
The transparent substrate is preferably subjected to a cleaning process before use, wherein one preferred embodiment of the cleaning process is: and (3) ultrasonically treating the transparent substrate for 15 minutes by using acetone, ultrasonically treating the transparent substrate for 15 minutes by using ethanol, ultrasonically treating the transparent substrate for 15 minutes by using deionized water, and blow-drying the transparent substrate by using nitrogen.
The material of the dielectric layer in step (1) includes, but is not limited to, at least one of CYTOP (1-butyl vinyl ether) polymer, AF1600 (Teflon @ AF1600 from dupont), and PAA (polyimide acid, english name is polymic acid), and the thickness of the dielectric layer is 200 to 800 nm.
As a preferred embodiment of the present invention, the dielectric layer is preferably coated on the transparent substrate by spin coating to ensure uniform thickness and smooth surface.
And (3) heating in the step (2) to solidify the dielectric layer, wherein the heating temperature is 80-120 ℃, and the heat preservation time is 5-15 min.
In the step (2), the hydrophilic treatment is preferably carried out for 50-100 s by adopting a plasma cleaning machine, and the power of the plasma cleaning machine is preferably 180-220 w.
The cracking film in the step (3) includes but is not limited to TiO2At least one of sol, egg white sol and nail polish, wherein the heating temperature is 40-100 ℃, and the heat preservation time is 5-10 min.
In a preferred embodiment of the present invention, the cracking liquid is coated on the dielectric layer in step (3), and the coating is uniform to obtain a cracking film, and different cracking materials are suitable for different temperature conditions, and the material naturally cracks after heat preservation for 5-10 min at approximately 40-100 ℃.
By reasonably controlling the fluidity and the adhesiveness of the cracking film, the cracking film can be cracked to form a net, and the transparent substrate can be protected from plasma bombardment treatment, and is easy to clean in the subsequent process.
And (4) removing the dielectric layer which is not covered by the cracking template by adopting plasma, wherein the specific process is as follows: at least one of argon, oxygen, and nitrogen, including but not limited to, is plasmatized and then bombarded to remove dielectric layers not covered by the crack template.
The invention adopts plasma treatment, namely, argon, oxygen, nitrogen or other molecules are ionized and then bombard the surface of a sample, and only the dielectric layer at the crack is bombarded and deepened because most areas have the protection function of a cracking template.
Argon is preferred as one of the preferred embodiments of the invention, and the duration of the bombardment is preferably 300 s.
The cleaning solvent in the step (4) comprises at least one of deionized water and absolute ethyl alcohol, and the deionized water and/or the absolute ethyl alcohol can be used for further removing the cracking template on the cracking network.
The surfactant in step (5) includes, but is not limited to, span80 (span 80), dodecyltrimethoxysilane or KH570 (gamma- (methacryloyloxy) propyltrimethoxysilane); the dispersant includes, but is not limited to, at least one of n-hexadecane and tetrachloroethylene; the particle size of the modified nano titanium dioxide particles is 60-100 nm.
The nano titanium dioxide in the invention is preferably hydrophilic nano titanium dioxide, preferably purchased from Aladdin company.
As a preferred embodiment of the invention, the modification process comprises the following steps: selecting hydrophilic titanium dioxide, adding absolute ethyl alcohol and a surfactant, fully mixing by ultrasonic to obtain a mixed colloid, putting the mixed colloid into a centrifuge tube, putting the centrifuge tube into a centrifuge, centrifuging, taking out the centrifuge tube, pouring out supernatant, drying the lower precipitate to obtain modified titanium dioxide particles, adding a dispersing agent into the modified titanium dioxide particles, putting the modified titanium dioxide particles into an ultrasonic cell crusher for dispersing, and taking out the colloid to obtain the modified nano titanium dioxide sol.
Therefore, the hydrophilic nano titanium dioxide in the invention needs to be modified to change the hydrophilicity into lipophilicity, so that the occurrence of agglomeration can be reduced, and the occurrence of water can be prevented.
And (6) arranging and sealing an encapsulation adhesive tape between the two opposite side edges of the at least two cracking network transparent conductive electrodes, injecting modified nano titanium dioxide sol from the opening positions of the remaining two opposite side edges, and sealing the opening of the remaining two opposite side edges by adopting at least one of UV (ultraviolet) glue and photoresist to obtain the intelligent window, wherein the thickness of the encapsulation adhesive tape is preferably 30-200 mu m.
As a preferred embodiment of the present invention, in the step (6) of the present invention, the modified nano titanium dioxide particles are dropped between the contact gaps of the two ITO transparent conductive electrodes, and due to the capillary force of the glass, the colloid can be uniformly distributed between the two crack network transparent conductive electrodes.
By controlling the concentration of the nano titanium dioxide sol, the size of a gap between two crack network transparent conductive electrodes, selecting packaging tapes (30-50 mu m is better) with different thicknesses and the like, different initial transmittances, response voltages and response speeds can be obtained.
And coating at least one of UV (ultraviolet) glue and photoresist on gaps which are not sealed at the other two ends, and exposing (preferably 30s) under an ultraviolet exposure machine to complete the manufacture of the intelligent window.
The principle of the invention is as follows: the cracking liquid is coated on the surface of the transparent substrate coated with the dielectric layer to form a cracking film, the cracking film loses moisture due to heating in the air, the film shrinks to generate stress concentration, so that cracks are generated, the grains are fine and dense, and in the plasma cleaning process, the dielectric layer below the cracking template is bombarded by plasma, so that the grains are carved, and the cracking grains covered by the dielectric layer are formed. In the initial state, the titanium dioxide colloid particles have strong reflection and scattering effects, so that the transmittance of light can be reduced. The titanium dioxide colloid particles are white inorganic pigment, have non-toxicity, optimal opacity, optimal whiteness and brightness, and the nano-scale titanium dioxide has small particle size and high activity, can reflect and scatter ultraviolet rays and absorb ultraviolet rays, thereby having stronger blocking capability on the ultraviolet rays. The existence of the dielectric layer is to protect the transparent conductive electrode, and the transparent conductive electrode is made into a special cracking grid shape, so that titanium dioxide colloid particles are adsorbed on the grid, and the visible light transmittance of the intelligent window is improved. When voltage is applied to two ends of the substrate, the charged titanium dioxide colloid particles are attached to the exposed transparent conductive electrode from a dispersed state under the action of electric field force, so that grid-shaped titanium dioxide colloid particles are formed, and the transmissivity is improved.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, the cracking liquid is arranged on the dielectric layer to form a cracking film, the cracking film naturally cracks to form a cracking template, and the cracking network transparent conductive electrode is further prepared, and is used as a fractal structure, so that the filling of nano titanium dioxide particles is easy, the transmission change rate is improved, and the nano titanium dioxide is non-toxic, tasteless, non-decomposition, non-deterioration, strong in ultraviolet absorption capacity, and capable of shielding long waves and medium waves, and the nano titanium dioxide is white, so that the coloring can be adjusted, and the preparation of intelligent windows with different colors can be met;
(2) the nano titanium dioxide adopted in the invention has valuable optical properties, high chemical stability and thermal stability, ultraviolet ray resistance, antibiosis, self-cleaning and anti-aging performance, and is very important for the further development of commercialization and durability of the intelligent window;
(3) the nano titanium dioxide has higher surface charge potential and smaller particle size, and can realize low power, quick reaction and accurate control of transmittance;
(4) the intelligent window prepared by the method has low requirements on equipment, the raw materials are green and pollution-free, the process is simple, the production efficiency can be effectively improved, the production cost is reduced, and the industrialization is easy to realize;
(5) the crack grid based suspended particle type intelligent window can remarkably reduce the production investment of the intelligent window, simplifies the production process flow, can be widely suitable for specific requirements of various environments, has good environmental stability and high transparency switching rate, can shield ultraviolet bands and the like, can be used for high-end civil use and the like, and has strong market competitiveness.
Drawings
FIG. 1 is a step of applying a dielectric layer on a transparent substrate according to examples 1-3 of the present invention, wherein 1 is a dielectric layer, 2 is a transparent substrate, and 3 is a spin coater;
FIG. 2 shows the hydrophilic treatment step of the dielectric layer in examples 1-3 of the present invention, wherein 4 is a plasma cleaning agent and 5 is a drying oven;
FIG. 3 shows the steps of making a cracking template in examples 1-3 of the present invention, wherein 6 is a cracking liquid and 7 is a wire rod;
FIG. 4 illustrates the step of plasma-laying in examples 1-3 of the present invention, wherein 8 is absolute ethanol or deionized water;
FIG. 5 shows the modification steps of the nano-titania in examples 1-3 of the present invention, wherein 9 is nano-titania particles, and 10 is lipophilic group-CH3Etc.;
FIG. 6 shows the steps of assembling the nano-titania device in examples 1 to 3 of the present invention, in which 11 is modified nano-TiO2Particle, 12 is packaging tape;
fig. 7 is a magnified image of a crazing-grid-based suspended particle smart window of examples 1-3 of the present invention before voltage is applied under an optical microscope;
fig. 8 is a magnified image of a crazing grid based suspended particle smart window of examples 1-3 of the present invention after applying a voltage under an optical microscope;
fig. 9 is a graph of a change curve of a transmission value of a smart window before and after a voltage is applied to the smart window based on a suspended particle type of a crack grid in examples 1 to 3 of the present invention;
fig. 10 is a theoretical simulation picture of a suspended particle type smart window in embodiments 1 to 3 of the present invention, in which a is opaque, B is translucent, and C is transparent.
Detailed Description
Unless otherwise specified, the following starting materials are all commercially available products.
Example 1
The embodiment provides a preparation method of a suspended particle type smart window, which comprises the following steps:
(1) disposing a dielectric layer on a transparent substrate;
(2) curing the dielectric layer and carrying out hydrophilic treatment;
(3) manufacturing a cracking template on the dielectric layer:
(4) forming a cracking network transparent conductive electrode on a transparent substrate;
(5) preparing modified nano titanium dioxide sol;
(6) and injecting the modified nano titanium dioxide sol between two cracking network transparent conductive electrodes and packaging to obtain the suspended particle type intelligent window.
It comprises four main steps: firstly, preparing dielectric material and cracking liquid, and secondly, modifying nano TiO2Preparing sol, changing water solubility into oil solubility, preparing a dielectric layer, depositing a cracking solution, cracking, removing the dielectric layer, cleaning a cracking template and the surface of a sample, and modifying nano TiO2And injecting the sol and packaging the smart window to obtain a suspended particle type smart window sample.
The detailed process of each step is as follows:
dielectric material, cracking liquid and preparation thereof
The dielectric layer used in the smart window may be CYTOP, PAA, AF1600, etc., and the crack fluid may include titanium dioxide colloid, egg white, nail polish, etc.
The embodiment mainly uses egg white sol, which has larger cracking blocks, thinner cracking lines, good light transmittance, low cost and biodegradability compared with other cracking liquids.
The dielectric layer of the embodiment uses AF1600, and has low price and good dielectric property.
This example uses span80 as the TiO2The modifier of the nano particles prevents the nano particles from agglomerating and improves the dispersibility.
The process for preparing a sol formed from egg white and deionized water is described in detail herein.
(1) Adding 3mL of deionized water into the beaker A, adding 9mL of egg white, and preparing a solution A1；
(2) Mixing the solution A1The mixed solution is put into an ultrasonic cleaning machine for ultrasonic oscillation for 20min, and then is put into a centrifuge for 5min at 5000r/min, and supernatant is taken as a crack colloid.
The method of preparing the dielectric layer solution is detailed herein.
(1) Adding 3.0mL of AF1600 diluent into the beaker B, and then adding 1.0mL of LAF1600 solution to prepare solution B1；
(2) Mixing the solution B1The mixed solution is placed into an ultrasonic cleaning machine for ultrasonic oscillation for 30min, and the obtained solution is the dielectric layer solution.
(II) modified nano TiO2Preparation of colloids
In this example, 10g of hydrophilic TiO with a particle size of 60nm was taken2(Allatin) is placed in a beaker C, 100mL of absolute ethyl alcohol (analytically pure) is poured into the beaker, 1mL of span80 (sorbitan fatty acid ester) is added into the beaker, the beaker is placed in an ultrasonic cleaning machine to vibrate for 20min, then the beaker is placed in a centrifuge to centrifuge at 8000r/min for 10min, then supernatant is poured out, the precipitate is placed in a drying box to be dried for 8h at 60 ℃, 40mL of n-hexadecane or tetrachloroethylene is injected into a centrifuge tube, the centrifuge tube is placed in an ultrasonic cell crusher to be ultrasonically treated for 1h at 25 ℃ with 40% power after being shaken for 1min, and then the modified nano titanium dioxide sol is obtained, wherein the modified nano titanium dioxide sol is shown in figure 5.
(III) preparation of the dielectric layer and deposition of the cracking liquid, and cracking
Dripping the prepared AF1600 dielectric layer solution on a purchased ITO transparent conductive electrode, spin-coating by a spin coater at the rotating speed of 3000r/min, placing on a hot bench at the temperature of 120 ℃, and curing for 10min to obtain a dielectric layer, wherein the thickness of the dielectric layer is 200-800 nm, as shown in figure 1;
putting a sample into a plasma cleaning machine for hydrophilic treatment, wherein the plasma cleaning machine cleans the sample for 50-100 s during the hydrophilic treatment, and the power of the plasma cleaning machine is 180-220 w, as shown in FIG. 2;
coating egg white colloid on the surface, heating on a hot table at 60 deg.C for 10min to crack, as shown in FIG. 3;
and then placing the cracked sample in a plasma cleaning machine for 300s (the specific process is that at least one of argon, oxygen and nitrogen is subjected to plasma treatment, and then the dielectric layer which is not covered by the cracking template is removed through bombardment), and then removing the cracking layer by using deionized water to obtain the transparent conductive electrode with the prepared cracking grids, as shown in fig. 4.
(IV) Nano TiO2Injection of glue and encapsulation of smart windows
Attaching packaging adhesive tape with thickness of 35 μm to the prepared electrode surface, compacting the two electrodes, packaging, and injecting modified nanometer TiO from the two sides2And (3) dissolving the sol, coating UV (ultraviolet) glue on two sides of the unpackaged gap, and exposing for 30 seconds by using an ultraviolet exposure machine to obtain the suspended particle type intelligent window, as shown in figure 6.
Example 2
This example provides a smart window of suspended particle type, which differs from example 1 in that nail polish (model CA600, a commercially available product) is mainly used as a crack liquid, CYTOP is used as a dielectric layer, and KH-570 is used as TiO2A modifier for nanoparticles comprising the steps of:
dielectric material, cracking liquid and preparation thereof
The method of preparing the fracturing fluid is described in detail herein.
Adding 10mL of CA600 into a beaker, placing the beaker into an ultrasonic cleaning machine, vibrating for 20min, placing the beaker into a centrifuge for 5min at 5500r/min, taking out the solution, removing the lower-layer precipitate, and taking the supernatant as the solution;
the method of preparing the dielectric layer solution is detailed herein.
Adding 1.0mL of CYTOP diluent into the beaker B, adding 1.0mL of 9% wt CYTOP solution, placing into an ultrasonic cleaning machine, and vibrating for 20min to prepare solution B1;
(II) modified nano TiO2Preparation of colloids
In this example, 10g of the polymer had a particle size of80nm hydrophilic TiO2(Aladdin) is put in a beaker, 100mL of absolute ethyl alcohol (analytically pure) is poured into the beaker, 2mL of gamma- (methacryloyloxy) propyl trimethoxy silane (KH-570 silane coupling agent) is added into the beaker, the beaker is placed in an ultrasonic cleaning machine to be vibrated for 30min, then is stirred for 6h at 60 ℃ at 1000r/min, then is placed in a centrifuge to be centrifuged for 10min at 8000r/min, then the supernatant is poured out, the precipitate is repeatedly centrifuged and washed for 3 times by deionized water and absolute ethyl alcohol, is placed in a drying box to be dried for 8h at 60 ℃, then is injected with 40mL of n-hexadecane or tetrachloroethylene into a centrifugal tube, is shaken for 1min and then is placed in an ultrasonic cell crusher to be subjected to ultrasonic treatment for 1h at 40% power and 25 ℃, and then the colloid is taken out, as shown in figure 5.
The modification principle is shown in the following chemical formula:
(III) preparation of the dielectric layer and deposition of the cracking liquid, and cracking
Dripping the prepared CYTOP dielectric layer solution onto a purchased ITO transparent conductive electrode, spin-coating at the rotating speed of 3000r/min, placing on a hot bench at the temperature of 80 ℃, and curing for 10min to obtain a dielectric layer, wherein the thickness of the dielectric layer is 200-800 nm, as shown in figure 1;
putting a sample into a plasma cleaning machine for hydrophilic treatment, wherein the plasma cleaning machine cleans the sample for 50-100 s during the hydrophilic treatment, and the power of the plasma cleaning machine is 180-220 w, as shown in FIG. 2;
coating CA600 colloid on the template, and heating on a hot table at 80 deg.C for 2min to crack to obtain cracked template, as shown in FIG. 3;
and then placing the cracked sample in a plasma cleaning machine for 300s (the specific process is that at least one of argon, oxygen and nitrogen is subjected to plasma treatment, and then the dielectric layer which is not covered by the cracking template is removed through bombardment), and then removing the cracking template by using deionized water to obtain the transparent conductive electrode with the prepared cracking grids, as shown in fig. 4.
(IV) Nano TiO2Injection of glue and encapsulation of smart windows
Attaching packaging adhesive tape with thickness of 50 μm to the prepared electrode surface, compacting the two electrodes, packaging, and injecting nano TiO from the two sides2And coating UV (ultraviolet) glue on two sides of the unpackaged gap, and exposing for 30 seconds by using an ultraviolet exposure machine to obtain the suspended particle type intelligent window, as shown in figure 6.
Example 3
The difference between the smart window in this embodiment and the smart window in this embodiment is that, in this embodiment, the egg white cracking solution, the PAA dielectric layer and DTMS (dodecyl trimethoxy silane) are mainly used as TiO2Modification of nanoparticles comprising the steps of:
dielectric material, cracking liquid and preparation thereof
The method of preparing the fracturing fluid is described in detail herein.
(1) Adding 3mL of deionized water into the beaker A, adding 9mL of egg white, and preparing a solution A1；
(2) Mixing the solution A1The mixed solution is put into an ultrasonic cleaning machine for ultrasonic oscillation for 20min, and then is put into a centrifuge for 5min at 5000r/min, and supernatant is taken as a crack colloid.
(II) modified nano TiO2Preparation of colloids
In this example, 10g of hydrophilic TiO was taken at 100nm2(Allatin) is put into a beaker, 100mL of absolute ethyl alcohol (analytically pure) is removed and poured into the beaker, 5mL of dodecyl trimethoxy silane (DTMS) is added into the beaker, the beaker is placed in an ultrasonic cleaning machine to vibrate for 30min, then is stirred for 24h at the temperature of 40 ℃ at 1000r/min, then is placed in a centrifuge to centrifuge for 10min at 8000r/min, then the supernatant is poured out, the precipitate is repeatedly centrifuged and washed for 3 times by deionized water and absolute ethyl alcohol, is placed in a drying box to be dried for 8h at the temperature of 60 ℃, then is injected with 40mL of n-hexadecane or tetrachloroethylene into a centrifuge tube, is placed in an ultrasonic cell crusher to be subjected to ultrasonic treatment for 1h at the power of 40 percent and the temperature of 25 ℃ after being shaken for 1min, and then the colloid is taken out, as shown in figure 5.
(III) preparation of the dielectric layer and deposition of the cracking liquid, and cracking
Dripping PAA dielectric layer solution on a purchased FTO transparent conductive electrode, spin-coating at the rotating speed of 2000-4000 r/min, placing on a hot table at 80 ℃, and curing for 15min to obtain a dielectric layer, wherein the thickness of the dielectric layer is 200-800 nm, as shown in figure 1;
putting a sample into a plasma cleaning machine for hydrophilic treatment, wherein the plasma cleaning machine cleans the sample for 50-100 s during the hydrophilic treatment, and the power of the plasma cleaning machine is 180-220 w, as shown in FIG. 2;
coating egg white colloid on the surface, heating on a hot table at 60 deg.C for 10min to crack, as shown in FIG. 3;
and then placing the cracked sample in a plasma cleaning machine for 300s (the specific process is that at least one of argon, oxygen and nitrogen is subjected to plasma treatment, and then the dielectric layer which is not covered by the cracking template is removed through bombardment), and then removing the cracking layer by using absolute ethyl alcohol to obtain the transparent conductive electrode with the prepared cracking grids, as shown in figure 4.
(IV) Nano TiO2Injection of glue and encapsulation of smart windows
Attaching 100 μm packaging adhesive tape to the prepared electrode surface, compacting the two electrodes, packaging, and injecting nano TiO from the two sides2And coating UV (ultraviolet) glue or photoresist on two sides of the unencapsulated gap, and exposing for 30 seconds by using an ultraviolet exposure machine to obtain the suspended particle type intelligent window, as shown in FIG. 6.
The effect graphs before and after applying voltage under a light mirror of the suspended particle type intelligent window prepared by the cracking template obtained in the examples 1 to 3 are shown in fig. 7 and 8, the change curve of transmission and wavelength under the driving of the voltage is shown in fig. 9, the transmission change rate reaches 37.37 percent, the window can be used as the switch between transparent and non-transparent, and the principle of the transmission change is shown in fig. 10.
The above embodiment example 1 is a preferred embodiment of the present invention, but the embodiment of the present invention is not limited by the above embodiment, for example, besides ITO, other cheap transparent conductive electrode materials (AZO, FTO, etc.) can be used for manufacturing the substrate for preparing the sample, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be regarded as equivalent substitutions, and all are included in the protection scope of the present invention.
Claims (8)
1. A preparation method of a suspended particle type intelligent window is characterized by comprising the following steps:
(1) selecting a transparent substrate, and arranging a dielectric layer on the transparent substrate;
(2) curing the dielectric layer and carrying out hydrophilic treatment;
(3) setting a cracking film on the cured dielectric layer, and controlling the heating temperature and the heat preservation time to enable the cracking film to naturally crack to form a cracking template;
(4) removing the dielectric layer which is not covered by the cracking template by adopting plasma, forming a cracking network on the transparent substrate, and removing the cracking template on the cracking network by adopting a cleaning solvent to form a cracking network transparent conductive electrode;
(5) selecting nano titanium dioxide, carrying out lipophilic modification by adopting a surfactant, and dispersing in a dispersing agent to prepare modified nano titanium dioxide sol;
(6) arranging the modified nano titanium dioxide sol between at least two crack network transparent conductive electrodes and carrying out encapsulation treatment to obtain a suspended particle type intelligent window;
the material of the transparent substrate in the step (1) includes but is not limited to at least one of tin-doped indium oxide, fluorine-doped tin oxide and aluminum-doped zinc oxide;
the surfactant in step (5) includes, but is not limited to, span80, dodecyltrimethoxysilane, or KH 570; the dispersant includes, but is not limited to, at least one of n-hexadecane and tetrachloroethylene; the particle size of modified nano titanium dioxide particles in the modified nano titanium dioxide sol is 60-100 nm.
2. The method of making a suspended particle smart window of claim 1, wherein: the material of the dielectric layer in the step (1) comprises but is not limited to at least one of CYTOP, AF1600 and PAA, and the thickness of the dielectric layer is 200-800 nm.
3. The method of making a suspended particle smart window of claim 1, wherein: heating in the step (2) to cure the dielectric layer, wherein the heating temperature is 80-120 ℃, and the heat preservation time is 5-15 min; the hydrophilic treatment is carried out for 50-100 s by adopting a plasma cleaning machine, and the power of the plasma cleaning machine is 180-220 w.
4. The method of making a suspended particle smart window of claim 1, wherein: the material of the cracking film in the step (3) includes but is not limited to TiO2At least one of sol, egg white sol and nail polish, wherein the heating temperature is 40-100 ℃, and the heat preservation time is 5-10 min.
5. The method of making a suspended particle smart window of claim 1, wherein: and (4) removing the dielectric layer which is not covered by the cracking template by adopting plasma, wherein the specific process is as follows: at least one of argon, oxygen, and nitrogen, including but not limited to, is plasmatized and then bombarded to remove dielectric layers not covered by the crack template.
6. The method of making a suspended particle smart window of claim 1, wherein: the cleaning solvent in the step (4) comprises at least one of deionized water and absolute ethyl alcohol.
7. The method of making a suspended particle smart window of claim 1, wherein: and (6) arranging and sealing an encapsulation adhesive tape between the two opposite side edges of the at least two cracking network transparent conductive electrodes, injecting modified nano titanium dioxide sol from the opening positions of the remaining two opposite side edges, and sealing the opening of the remaining two opposite side edges by adopting at least one of UV (ultraviolet) glue and photoresist to obtain the intelligent window, wherein the thickness of the encapsulation adhesive tape is 30-200 mu m.
8. The utility model provides a suspended particle formula smart window, characterized by: prepared by the method of any one of claims 1 to 7.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013148744A (en) * | 2012-01-20 | 2013-08-01 | Konica Minolta Inc | Light control film, and method of manufacturing light control film |
| CN106159040A (en) * | 2016-08-24 | 2016-11-23 | 华南师范大学 | A kind of Whote-wet method prepares the method for flexible metal network transparency electrode |
| CN106244989A (en) * | 2016-07-26 | 2016-12-21 | 华南师范大学 | Produce the method and apparatus of flexible micro-nano metalolic network transparent conductive film continuously |
| CN106782879A (en) * | 2016-11-30 | 2017-05-31 | 华南师范大学 | A kind of method that low cost plasma body bombardment prepares metalolic network transparency conductive electrode |
| CN107533268A (en) * | 2015-03-30 | 2018-01-02 | 东进控股股份有限公司 | Smart window |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013148744A (en) * | 2012-01-20 | 2013-08-01 | Konica Minolta Inc | Light control film, and method of manufacturing light control film |
| CN107533268A (en) * | 2015-03-30 | 2018-01-02 | 东进控股股份有限公司 | Smart window |
| CN106244989A (en) * | 2016-07-26 | 2016-12-21 | 华南师范大学 | Produce the method and apparatus of flexible micro-nano metalolic network transparent conductive film continuously |
| CN106159040A (en) * | 2016-08-24 | 2016-11-23 | 华南师范大学 | A kind of Whote-wet method prepares the method for flexible metal network transparency electrode |
| CN106782879A (en) * | 2016-11-30 | 2017-05-31 | 华南师范大学 | A kind of method that low cost plasma body bombardment prepares metalolic network transparency conductive electrode |
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