WO2021119969A1 - Valve de lumière à particules suspendues ayant une couche de protection - Google Patents

Valve de lumière à particules suspendues ayant une couche de protection Download PDF

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Publication number
WO2021119969A1
WO2021119969A1 PCT/CN2019/125808 CN2019125808W WO2021119969A1 WO 2021119969 A1 WO2021119969 A1 WO 2021119969A1 CN 2019125808 W CN2019125808 W CN 2019125808W WO 2021119969 A1 WO2021119969 A1 WO 2021119969A1
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WO
WIPO (PCT)
Prior art keywords
layer
light valve
protective layer
transparent electrode
light
Prior art date
Application number
PCT/CN2019/125808
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English (en)
Chinese (zh)
Inventor
张达玮
赵世勇
李亚男
肖淑勇
张昱喆
梁斌
Original Assignee
浙江精一新材料科技有限公司
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Priority to CN201980102523.8A priority Critical patent/CN114730109A/zh
Priority to PCT/CN2019/125808 priority patent/WO2021119969A1/fr
Publication of WO2021119969A1 publication Critical patent/WO2021119969A1/fr

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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
    • 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 
    • G02F1/17—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 variable-absorption elements not provided for in groups G02F1/015 - G02F1/169

Definitions

  • the invention relates to a suspended particle light valve. More specifically, it relates to a suspended particle light valve whose protective layer has a single-layer structure or a multi-layer structure.
  • a light valve is a device that can adjust the amount of light passing through a medium, similar to a water valve that can control the flow of water. Curtains can be seen as a kind of light valve.
  • the light valve is a device that can electronically control the light transmittance, and this device is scientifically called an electrochromic device. Depending on the principle of the electrochromic device, it can be further classified into a liquid crystal color changing light valve, an electrochemical color changing light valve and a suspended particle light valve.
  • the suspended particle light valve whose electroactive component is light-controlling particles that can be rearranged in an electromagnetic field applied through two transparent electrodes.
  • a typical suspended particle light valve is shown in Figure 1. It includes a light control layer 1 sandwiched between two transparent electrodes 2.
  • the transparent electrode 2 is composed of a transparent substrate 21 and a transparent conductive film 22 thereon.
  • the light control layer 1 is usually obtained by dispersing a suspension medium 12 containing light control particles 11 into a polymer matrix 13, wherein the light control particles 11 can be rearranged under the action of an electric field. More specifically, in this type of light valve, the light control particles 11 absorb, scatter or reflect light through Brownian motion in a state where no electric field is applied, so incident light cannot penetrate the light valve. When an electric field is applied, because the light control particles 11 have an electric dipole moment, the light control particles 11 are arranged in a direction parallel to the electric field. At this time, the light incident on the light valve can penetrate the light valve. In this, the amount of transmitted light is adjusted by the response of the light control particles 11 to the electric field.
  • the light control layer of the suspended particle light valve made in this way is relatively fragile, and it is easy to wear and break under bending, pressure, friction, etc., and damage will cause the transparent electrodes to contact each other and short-circuit, resulting in irreversible light.
  • the valve is damaged.
  • the chemical properties of the light control layer and its direct adhesion to the transparent electrode are very low, which leads to problems such as inability to smoothly wind up in the industrial production process.
  • suspended particles are nanoparticles, which are very sensitive to humidity, transparent conductive film 22, ultraviolet rays, etc., and require strict protection; therefore, a better technology needs to be invented to effectively improve the stability of the suspended particle light valve. Reduce the damage of external factors to the light valve.
  • the present invention provides a suspended particle light valve with a protective layer, including a first transparent electrode, a second transparent electrode, and a suspended particle light control layer arranged between the first transparent electrode and the second transparent electrode, among them:
  • a first protective layer is provided between the first transparent electrode and the light control layer;
  • a second protective layer is arranged between the second transparent electrode and the light control layer.
  • the first protective layer and the second protective layer have a single-layer or multi-layer structure.
  • the material of any sublayer in the single-layer or multi-layer structure includes one of epoxy resin, polyurethane, polyimide resin, polystyrene resin, acrylic resin, modified acrylic, and silica gel.
  • the material of the sub-layer adjacent to the suspended particle light control layer includes one of the main components of acrylate, modified acrylic, and silica gel.
  • the thickness of the first protective layer and/or the second protective layer is 0.5-10 microns.
  • the thickness of the first protective layer and/or the second protective layer is 0.8-5 microns.
  • the thickness of the first protective layer and/or the second protective layer is 1 to 3 microns.
  • the single-layer or multi-layer structure is 1 layer or 2 layers or 3 layers.
  • each sub-layer in the single-layer or multi-layer structure is 0.5-10 microns.
  • each sub-layer in the single-layer or multi-layer structure is 0.6-5 microns.
  • each sub-layer in the single-layer or multi-layer structure is 0.8-2 microns.
  • the first protective layer and the second protective layer are formed as follows: the protective layer polymer precursor RP is respectively coated on the conductive sides of the first transparent electrode and the second transparent electrode to form a glue protective layer; The glue protective layer on the first transparent electrode and the second transparent electrode are respectively irradiated with ultraviolet UV or thermally cured to form the protective layer on the first transparent electrode and the protective layer on the second electrode.
  • the light control layer is formed by coating a light valve matrix emulsion containing polymer precursor PPM, suspension medium SM, light control particles LCP and photoinitiator PI on the protective layer side of the transparent electrode containing the protective layer.
  • Valve matrix emulsion layer is formed by coating a light valve matrix emulsion containing polymer precursor PPM, suspension medium SM, light control particles LCP and photoinitiator PI on the protective layer side of the transparent electrode containing the protective layer.
  • Valve matrix emulsion layer is formed by coating a light valve matrix emulsion containing polymer precursor PPM, suspension medium SM, light control particles LCP and photoinitiator PI.
  • the thickness of the light valve matrix emulsion layer is 10-100 microns.
  • the length of the light control particle LCP is in the range of 100-500 nm, and the diameter thereof is 20-100 nm.
  • the composition of the light control particle LCP is at least one of titanium dioxide (TiO 2 ), polyhalides and chloroapatite.
  • the mass amount of the photoinitiator accounts for 0.1%-1% of the light valve matrix emulsion.
  • the photoinitiator is selected from at least one of 184, ITX, 819, 1173, BDK, BP, TPO, 369, and 907.
  • the light valve matrix emulsion further includes a stabilizer and/or emulsifier.
  • the method for adding a protective layer to the suspended particle light valve of the present invention has a simple structure and obvious effects, and has the following advantages:
  • the first advantage is that it can prevent the entire light valve device from being short-circuited and damaged due to a small amount of flaws in the light valve causing the transparent electrode to contact, thereby improving the product qualification rate.
  • the protective layer material is a high-viscosity material and has similar chemical properties to the light control layer
  • the protective layer can bond the transparent electrode and the light control layer more firmly, thereby making the light valve device more difficult to break, abrasion resistance, and bending resistance
  • the physical properties such as folding are improved.
  • the protective layer is a transparent material with a dense structure, good hydrophobicity, and low dielectric constant, which can effectively prevent moisture and oxygen from penetrating into the light control layer, effectively protect the light control particles, and increase the service life of the light valve.
  • the protective layer effectively blocks the contact between the transparent electrode and the light control layer, it blocks the catalytic decomposition of the metal oxide layer, that is, the transparent conductive film 22', on the light control layer, thereby increasing the service life of the light valve.
  • the multi-layer structure of the protective layer avoids the limitations of the single-layer material, and through synergy, greatly improves the service life of the suspended particle light valve.
  • Figure 1 A schematic diagram of the structure of a suspended particle light valve in the prior art
  • FIG. 2 The structure diagram of the protective layer on the transparent conductive film 22 of the transparent electrode 2 in the present invention.
  • Figure 3 A schematic diagram of the suspension particle light valve matrix emulsion applied to the protective layer side of the transparent electrode containing a protective layer in the present invention to form a suspended particle light valve matrix emulsion layer;
  • Figure 4 is a schematic diagram of the structure of the suspended particle light valve containing a protective layer in the present invention.
  • the preparation method of the protective layer is as follows.
  • the glue is applied to the transparent conductive film 22 of the transparent electrode to form the protective glue layer 3a, which is cured by ultraviolet UV radiation or thermal curing.
  • the protective layer 3a is formed, and another glue solution is applied to the protective layer 3a to form a protective glue layer 3b.
  • the protective layer 3b is formed by ultraviolet UV radiation or thermal curing.
  • the protective layers 3a, 3b are collectively referred to as the protective layer 3.
  • the protective layer includes the protective layer 3a and the protective layer 3b, which is a two-layer structure protective layer.
  • the main function of 3a sublayer is barrier function
  • the main function of 3b sublayer is viscosity function
  • the protective layer may be a single layer or a three-layer or more layer structure.
  • the barrier effect and viscosity effect represent the main functions that the material of the layer can achieve, and the barrier sublayer can achieve better water barrier, oxygen barrier, barrier organic solvent penetration, and isolation of the metal oxide layer (ie the transparent conductive film 22' );
  • the adhesive sub-layer can achieve better adhesion to the light control layer.
  • the material used in each sublayer here is not a single function.
  • the main components of the barrier sublayer include epoxy resins, polyurethanes, polyimide resins, polystyrene resins, and modified acrylic.
  • the main components of the adhesive sublayer include acrylates, modified acrylics, and silica gels. one of a kind.
  • the above materials are only examples.
  • the materials used in the barrier sub-layer and the adhesive sub-layer include but are not limited to the above materials. Other materials that can achieve similar functions can be used.
  • the preparation method of the protective layer suspended particle light valve is to apply the suspended particle light valve matrix emulsion containing the polymer precursor PPM, the suspension medium SM, the light control particle LCP and the photoinitiator PI to the transparent electrode containing the protective layer
  • a suspended particle light valve matrix emulsion layer is formed on the protective layer, and the suspended particle light valve matrix emulsion layer is cured by ultraviolet UV radiation to form a light control layer;
  • the part of the transparent electrode and the light control layer containing the protective layer is combined with Another transparent electrode containing a protective layer is pressed together to obtain a complete suspended particle light valve containing a protective layer.
  • the thickness of the protective layer is 0.5-10 micrometers, preferably 0.8-5 micrometers, more preferably 1-3 micrometers, and the thickness of the light valve matrix emulsion layer is 10-100 micrometers.
  • the thickness of each of the "sublayers" included in the protective layer is 0.5-10 microns, more preferably 0.6-5 microns, and most preferably 0.8-2 microns.
  • this light valve containing suspended particles with a protective layer can prevent the entire light valve device from being short-circuited and damaged due to a small amount of defects in the light valve causing the transparent electrode to contact.
  • the protective layer material is a high-viscosity material and has similar chemical properties to the light control layer, the protective layer can bond the transparent electrode and the light control layer more firmly, making the light valve device more difficult to break, more resistant to friction, and resistant to bending The physical performance is greatly improved.
  • the protective layer material is a good hydrophobic, dense, low-dielectric constant transparent material, which can effectively prevent moisture and oxygen from penetrating into the light control layer, and effectively protect the light control particles LCP.
  • the protective layer effectively blocks the contact between the transparent electrode and the light control layer, and isolates the metal oxide layer, that is, the transparent conductive film 22', from the catalytic decomposition of the light control layer, thereby increasing the service life of the light valve.
  • the protective layer is composed of at least one of an epoxy resin layer, an acrylic resin layer, a polyurethane layer, a polyimide resin layer, a polystyrene resin layer, a modified acrylic layer, and a silica gel layer.
  • Adhesion reflects the stability of the structure of the suspended particle light valve against physical external forces.
  • the adhesion force is measured by the adhesion force measuring instrument STROGRAPH ES (Toyo Seiki Seisakusho Ltd).
  • the test method is that the light control layer is slowly peeled off the transparent electrode with a vertical 90° tension, where the load is 50N, the pull rate is 50mm/min, and the value is recorded. It is the size of adhesion.
  • Stability reflects the change of light transmittance of the light valve under long-term high humidity, high temperature and strong light and the change of its own appearance color.
  • the test method is to store the light valve in an environmental box with a 500W/m 2 xenon lamp, an air temperature of 55 degrees Celsius, a light valve surface temperature of 60 degrees Celsius, and an ambient humidity of 50%. Compare different light valves for 100 hours. After 500 hours, the light valve is transparent. The light rate changes to compare stability.
  • the polymer precursor PPM can be a silicon-containing UV optical glue (such as Dow Corning VE-6001, etc.).
  • the suspension medium SM 12 can be fluorocarbon organic compounds, plasticizers (dioctyl phthalate, dibutyl phthalate, dioctyl phthalate and triisodecyl trimellitate, Dioctyl terephthalate, etc.), dodecylbenzene, polybutene oil, etc.
  • the light control particles LCP 11 can be nanorods with a length of 0.1 to 1.0 microns, such as metal oxides, polyhalides, and chloroapatite.
  • the photoinitiator is selected from at least one of 184, ITX, 819, 1173, BDK, BP, TPO, 369, and 907.
  • the transparent electrode 2' can be ITO conductive glass, ITO/PET conductive film, nano Ag wire/PET conductive film, nano Cu wire/PET conductive film, etc.
  • the epoxy resin glue Permabond ET515A was coated on the ITO/PET transparent conductive film with a doctor blade type automatic film coating machine (MSK-AFA-III type, MTI Corporation), with a thickness of 1 micron. Put it in a vacuum oven at 100 degrees and heat it for 1 hour to obtain ITO/PET coated with epoxy resin layer.
  • MSK-AFA-III type MTI Corporation
  • modified acrylic light-curing adhesive Permabond's TA436 is used instead of epoxy resin, and cured with X200-150 UV curing machine produced by Aventk, the power is adjusted to 700W/m 2 , and the curing time is 5s.
  • the epoxy resin glue Permabond ET515A was coated on the ITO/PET transparent conductive film with a doctor blade type automatic film coating machine (MSK-AFA-III type, MTI Corporation), with a thickness of 2 microns. Put it in a vacuum oven at 100 degrees and heat it for 1 hour to obtain ITO/PET coated with epoxy resin layer.
  • MSK-AFA-III type MTI Corporation
  • the light control particle LCP 11 was prepared. Into a 250 ml three-neck round-bottom glass flask was added 30 g of isoamyl acetate solution containing 21.2wt% nitrocellulose (SS 1/4sec), 6 g of I2, 70 g of isoamyl acetate, 4 g of anhydrous CaI2 and 4 grams P25, and heat to 42°C. After I2 was dissolved, 6 grams of anhydrous methanol, 0.8 grams of distilled water and 4 grams of 2,5-PDA ⁇ 2H2O (2,5-pyrazine dicarboxylic acid dihydrate) were added to a three-necked round bottom glass flask.
  • the reaction was heated and stirred at 42°C for 4 hours, and then cooled naturally.
  • the reaction solution was centrifuged at 1350G for 0.5 hours to remove large particulate products.
  • the supernatant was centrifuged at 18000G for 5 hours, the supernatant was discarded, and the light control particles 11 were obtained.
  • the suspension medium SM 12 is dioctyl terephthalate.
  • the catalyst stannous octoate solution (0.13 g dissolved in 10 ml of heptane) was added. Then a mixture of 3 grams of hydrolyzed acryloxypropyltrimethoxysilane and 1.8 grams of hydrolyzed glycidyltrimethicone was added dropwise for about 5 minutes. The condensation reaction takes about 5 hours, and immediately after that, 30 ml of trimethylmethoxysilane is added as a reaction terminator. The reaction was terminated for 2 hours, and then rapidly cooled to room temperature.
  • 0.3 g of photoinitiator 819, 3.0 g of light control particle LCP, 26.9 g of suspension medium SM and 70.0 g of polymer precursor PPM are mixed uniformly to obtain a suspended particle light valve matrix emulsion.
  • the suspended particle light valve matrix emulsion was coated with a doctor blade type automatic film coating machine (MSK-AFA-III type, MTI Corporation) on the transparent electrode with a protective layer prepared in [Example 1], with a thickness of 60 microns.
  • Table 1 Table 2, and Table 3 list the different performance test results of each suspended particle light valve.
  • each material represents a sub-layer, and the arrangement direction from left to right corresponds to from the electrode side to the corresponding light control layer side.
  • Example 14 represents that the protective layer has a three-layer structure, and the material of the sub-layer close to the light control layer is modified acrylic.
  • Example 8, Example 9, and Example 11 represent that the protective layer has a two-layer structure, and the material of the sub-layer near the light control layer is acrylate.
  • Example 13 represents a single protective layer.
  • the adhesion of the protective layer-containing suspended particle light valve produced by the method of the present invention is far better than that of the prior art 1.
  • the adhesion quality High, and high bonding quality means strong bonding force between the light control layer and the protective layer and the transparent electrode, which is more suitable for commercial products.
  • each material shown represents a sublayer, and the arrangement direction from left to right corresponds to from the electrode side to the corresponding light control layer side.
  • Example 14 represents a three-layer protective layer structure, and the material of the sub-layer close to the corresponding light control layer is modified acrylic.
  • Example 8, Example 9, Example 10, Example 11, and Example 12 represent a 2-layer structure protective layer, and Example 13 represents a single-layer protective layer.
  • the suspended particle light valve made in Examples 8-14 in the environmental box can greatly slow down the dark state fading speed and the bright state performance degradation of the light valve under high humidity, strong light, and high temperature conditions. It can be seen that the protective layer plays a great role in isolating humidity and avoiding contact between the light control layer and the metal oxide layer.
  • the light valve manufactured by the technical method of the present invention can greatly improve the stability of the light valve, and the performance of the light valve is much better than that of the suspended particle light valve manufactured by using the prior art.
  • the method for preparing a suspended particle light valve containing a protective layer designed in the present invention greatly increases the viscosity and stability of the light valve device, increases the life of the suspended particle light valve, and effectively prevents the performance of the light valve. attenuation. At the same time, it is ensured that the addition of a protective layer has only a weak effect on the performance of the light valve itself.
  • the protective layer of the above-mentioned embodiment has a two-layer structure. Single-layer or three-layer or more layer structures are also possible, all of which can achieve the above-mentioned effects.
  • protective layers can be provided on the transparent conductive film sides of the two transparent electrodes.
  • the protective layer on the transparent conductive film side of each transparent electrode can be a single-layer or multi-layer structure, and the number of protective layers can be the same or different. .
  • the protective layer on the transparent conductive film side of the first transparent electrode and the protective layer on the transparent conductive film side of the second transparent electrode may both have a two-layer structure, or the protective layer of the first transparent electrode may have a two-layer structure and the protection of the second transparent electrode
  • the layer is a 3-layer structure.
  • the protective layer may be provided on the transparent conductive film side of the first transparent electrode, and the protective layer may not be provided on the transparent conductive film side of the second transparent electrode.

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  • Physics & Mathematics (AREA)
  • Nonlinear Science (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Mathematical Physics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)

Abstract

L'invention concerne une valve de lumière comprenant : une première électrode transparente (22) ; une seconde électrode transparente (22) ; et une couche de régulation de lumière contenant des particules en suspension (1) disposée entre la première électrode transparente (22) et la seconde électrode transparente (22), une première couche de protection (3) étant disposée entre la première électrode transparente (22) et la couche de commande de lumière (1), et/ou une seconde couche de protection (3) étant disposée entre la seconde électrode transparente (22) et la couche de commande de lumière (1).
PCT/CN2019/125808 2019-12-17 2019-12-17 Valve de lumière à particules suspendues ayant une couche de protection WO2021119969A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201980102523.8A CN114730109A (zh) 2019-12-17 2019-12-17 一种具有保护层的悬浮粒子光阀
PCT/CN2019/125808 WO2021119969A1 (fr) 2019-12-17 2019-12-17 Valve de lumière à particules suspendues ayant une couche de protection

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2019/125808 WO2021119969A1 (fr) 2019-12-17 2019-12-17 Valve de lumière à particules suspendues ayant une couche de protection

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WO2021119969A1 true WO2021119969A1 (fr) 2021-06-24

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WO2023197231A1 (fr) * 2022-04-14 2023-10-19 浙江精一新材料科技有限公司 Modulateur de lumière et verre commutable

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