CN114114779A - Light valve and method for improving pressure resistance of light valve - Google Patents
Light valve and method for improving pressure resistance of light valve Download PDFInfo
- Publication number
- CN114114779A CN114114779A CN202111437997.3A CN202111437997A CN114114779A CN 114114779 A CN114114779 A CN 114114779A CN 202111437997 A CN202111437997 A CN 202111437997A CN 114114779 A CN114114779 A CN 114114779A
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- CN
- China
- Prior art keywords
- light
- silicon
- och
- light valve
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Classifications
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- 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
- G02F1/1675—Constructional details
- G02F1/16757—Microcapsules
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
- C08F283/122—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to saturated polysiloxanes containing hydrolysable groups, e.g. alkoxy-, thio-, hydroxy-
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
- C08K5/5419—Silicon-containing compounds containing oxygen containing at least one Si—O bond containing at least one Si—C bond
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- C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K5/544—Silicon-containing compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
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- C08K5/00—Use of organic ingredients
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- C08K5/548—Silicon-containing compounds containing sulfur
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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
- G02F1/165—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
- G02F1/1675—Constructional details
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Abstract
The invention provides a light valve, a manufacturing method of the light valve and a dimming glass assembly. The light valve has excellent high-temperature compression resistance and can meet the requirement of the laminating process for subsequently manufacturing the dimming glass assembly.
Description
Technical Field
The invention relates to the field of electronic light control materials, in particular to a light valve with improved pressure resistance and a method for improving the pressure resistance of the light valve.
Background
The light valve is an electronic light control device, mainly a light control layer is arranged between two transparent conductive films, and after an electric field is switched on, the arrangement or the state of materials in the light control layer is changed, so that the light transmission characteristic of the device is changed, such as the conversion from low light transmittance to high light transmittance or the conversion from high light transmittance to low light transmittance. By the action of the electric field, the fast switching between the on-state and the off-state can be realized. Light valves can be classified into suspended particle light valves, polymer dispersed liquid crystal light valves, electrochemical reaction light valves, and the like according to different light control mechanisms of the light control layer.
Depending on the substrate of the light valve, the light valve may have a plastic sheet, such as PET, as the substrate, commonly referred to as a light modulating film; glass may also be used as a substrate, and is generally referred to as a light control glass. The assembly formed by the laminated light control film is generally referred to as a light control glass assembly.
In practical applications, the light adjusting film is sandwiched between two pieces of glass, and the light adjusting film is laminated under a certain temperature and pressure to manufacture a light adjusting glass assembly. However, the color-changing performance of the light modulation film is usually damaged to a greater extent due to higher temperature and pressure in the process of laminating, and the reason for this is mainly that the light modulation film has poor pressure resistance of the light control layer at a high temperature, which greatly affects the preparation of the light modulation glass assembly.
Therefore, for the light modulation film in the prior art, the problem of poor pressure resistance of the light control layer of the light modulation film at a high temperature state is urgently needed to be solved.
Disclosure of Invention
The inventors have unexpectedly found in long-term studies that the problem of poor compression resistance of the light control layer at high temperatures can be effectively solved by using a polymer matrix comprising a siloxane copolymer of the present invention obtained by copolymerizing the following monomers having specific units:
(a) a silicon-containing non-crosslinking monomer, which may be provided in the form of a silicon-containing non-crosslinking monomer and/or an oligomer thereof,
(b) a silicon-containing crosslinkable monomer, and
(c) a silicon-containing monomer having a high-occupancy side chain having the formula:
R-Xm-(CH2)n-SiR1 xR2 yformula (A)
Wherein the content of the first and second substances,
R1is hydroxy or a group which forms a hydroxy group upon hydrolysis, e.g. -Cl or C1-C3 alkoxy, especially R1Selected from-OH, -Cl, -OCH3、-OCH2CH3、-OCH(CH3)2、-OCH2CH2OCH3、-O-C(＝O)-CH3In particular from-OH, -Cl, -OCH3and-OCH2CH3，
R2Is C1-C3 alkyl, especially methyl or ethyl,
x and y are integers from 0 to 3, and x + y is 3, preferably x is 2 or 3,
x is selected from the group consisting of nitrogen, oxygen and sulfur,
m is 0 or 1, n is an integer from 0 to 10, preferably n is 0, 1, 2 or 3, more preferably 2 or 3,
r is a non-polymeric group such as H or a chain or cyclic group R' selected from optionally substituted alkyl, cycloalkyl, aromatic ring, heterocyclic, cycloalkylalkyl, heterocyclylalkyl, aralkyl, carbonyl and carbamoyl groups, said optional substituents being selected from hydroxy, amino, mercapto, acidic groups, alkoxy, aryloxy, alkylthio, arylthio, alkylamino, arylamino, ester groups, halogen and epoxy groups, which may be further optionally substituted.
Accordingly, based on the above findings, in a first aspect, the present invention provides a light valve having improved pressure resistance, comprising:
a first transparent substrate having a first refractive index,
a first transparent electrode formed on the first transparent substrate,
a second transparent substrate, which is transparent to light,
a second transparent electrode formed on a second transparent substrate, the first and second transparent electrodes being disposed opposite to each other, an
A light control layer disposed between the first transparent electrode and the second transparent electrode; the light management layer includes a polymer matrix;
wherein the polymer matrix is dispersed with suspension medium droplets, and solid light-controlling particles are distributed in the suspension medium droplets, the polymer matrix is obtained by crosslinking and curing at least one siloxane copolymer, and the siloxane copolymer is obtained by copolymerizing monomers comprising the following units:
(a) a silicon-containing non-crosslinking monomer, which may be provided in the form of a silicon-containing non-crosslinking monomer and/or an oligomer thereof,
(b) a silicon-containing crosslinkable monomer, and
(c) a silicon-containing monomer having a high-occupancy side chain having the formula:
R-Xm-(CH2)n-SiR1 xR2 yformula (A)
Wherein the content of the first and second substances,
R1is hydroxy or a group which forms a hydroxy group upon hydrolysis, e.g. -Cl or C1-C3 alkoxy, especially R1Selected from-OH, -Cl, -OCH3、-OCH2CH3、-OCH(CH3)2、-OCH2CH2OCH3、-O-C(＝O)-CH3In particular from-OH, -Cl, -OCH3and-OCH2CH3，
R2Is C1-C3 alkyl, especially methyl or ethyl,
x and y are integers from 0 to 3, and x + y is 3, preferably x is 2 or 3,
x is selected from the group consisting of nitrogen, oxygen and sulfur,
m is 0 or 1, n is an integer from 0 to 10, preferably n is 0, 1, 2 or 3, more preferably 2 or 3,
r is a non-polymeric group such as H or a chain or cyclic group R' selected from optionally substituted alkyl, cycloalkyl, aromatic ring, heterocyclic, cycloalkylalkyl, heterocyclylalkyl, aralkyl, carbonyl and carbamoyl groups, said optional substituents being selected from hydroxy, amino, mercapto, acidic groups, alkoxy, aryloxy, alkylthio, arylthio, alkylamino, arylamino, ester groups, halogen and epoxy groups, which may be further optionally substituted.
The siloxane copolymer of the light valve of the present invention contains units (c) which provide increased compressive strength compared to siloxane copolymers which do not contain units (c).
In some preferred embodiments of the present invention, in formula (A) above, when R-Xm-is-OH, -SH or-NH2When is, R-Xm-(CH2)n-the total number of atoms, excluding hydrogen, is at least 4; when R-Xm-is not-OH, -SH or-NH2When is, R-Xm-(CH2)nThe total number of atoms, not counting hydrogen, is at least 6, and/or
Wherein in formula (A), R-X is when unit (c) comprises only one silicon-containing monomer with a high-occupancy side chainmIs not-NH2Hydroxyl, glycidoxy, acryloxy, methacryloxy and acidic groups. In the present invention, the "acidic group" means a group which can give a proton according to the Lewis acid-base theory, such as a carboxyl group, a sulfonic acid group, a phosphoric acid group.
In some embodiments of the invention, the polymer matrix is formed by cross-linking and curing a polymer matrix precursor synthesized from starting materials comprising,
(a) oligomers of silicon-containing non-crosslinking monomers;
(b) a silicon-containing crosslinkable monomer; and
(c) silicon-containing monomers with high-occupancy side chains.
Preferably, the cross-linking curing of the polymer matrix precursor to form the polymer matrix takes place under thermocatalytic or radiation catalysed conditions, for example a photoinitiator may be added to the polymer matrix precursor to cause polymerisation by irradiation. The photoinitiators may be those commonly used in the art, and may be selected, for example, from 184(CAS number 947-19-3), ITX (CAS number 5495-84-1 or 83846-86-0), 819(CAS number 162881-26-7), 1173(CAS number 7473-98-5), BDK (CAS number 24650-42-8), BP (CAS number 119-61-9), TPO (CAS number 75980-60-8), 369(CAS number 119313-12-1), 907(CAS number 71868-10-5), including any one or any combination thereof.
In some embodiments of the invention, in the light valve, wherein
The oligomer of the silicon-containing non-crosslinking monomer is silicone oil; and/or
The silicon-containing crosslinkable monomer source is a compound of formula (1):
Q-(CH2)m-Si(RnX3-n) Formula (1);
wherein the content of the first and second substances,
q is an acrylate-based polymerizable group;
r is alkyl;
x is hydroxyl or a group which can generate hydroxyl after hydrolysis reaction;
m is a positive integer; n is 0, 1 or 2.
In some embodiments of the invention, in the light valve, wherein
The oligomer of the silicon-containing non-crosslinking monomer is at least one of hydroxyl-terminated silicone oil and methoxyl-terminated silicone oil; and/or
The silicon-containing crosslinkable monomer source is a compound of formula (1):
Q-(CH2)m-Si(RnX3-n) Formula (1);
wherein the content of the first and second substances,
q is methacryloxy or acryloxy;
r is C1-C4 alkyl;
x is-OH, -Cl, -OCH3、-OCH2CH3、-OCH(CH3)2、-OCH2CH2OCH3、-O-C(＝O)-CH3At least one of;
m is an integer of 1 to 10, and n is 0 or 1.
In some embodiments of the invention, the polymer matrix is formed by cross-linking and curing a polymer matrix precursor synthesized from starting materials comprising,
(a) oligomers of silicon-containing non-crosslinking monomers;
(b) a silicon-containing crosslinkable monomer; and
(c) silicon-containing monomers with high-occupancy side chains.
Specifically, the silicon hydroxyl groups and/or the groups capable of forming silicon hydroxyl groups on the units (a), (b), and (c) may be obtained by condensation reaction between silicon hydroxyl groups, or by condensation reaction between silicon hydroxyl groups and groups capable of forming silicon hydroxyl groups, or by condensation reaction between groups capable of forming silicon hydroxyl groups, under certain conditions. The polymer matrix precursor may also be obtained from at least one siloxane copolymer by hydrolyzing the groups capable of forming silicon hydroxyl groups on units (a), (b), (c) to silicon hydroxyl groups in the presence of an acid catalyst and obtaining the siloxane copolymer by condensation reaction between the silicon hydroxyl groups under certain conditions.
More specifically, the organic solvent is at least one of hexane, heptane, octane and toluene, the organic tin catalyst is at least one of stannous 2-ethylhexanoate, stannous octoate, dibutyltin dilaurate, dibutyltin diacetate and dioctyltin dilaurate, and the units (a), (b) and (c) are added to react under reflux conditions. After the reaction is finished, unreacted raw materials, solvent and low-boiling components are removed by means of liquid separation extraction, reduced pressure distillation and the like to obtain siloxane copolymer, and the polymer matrix precursor is obtained from at least one siloxane copolymer.
In some embodiments of the invention, the material forming the droplets of suspension medium is selected from at least one of fluorocarbon organic compounds, phthalates, trimellitates, dodecylbenzenes, polybutylenes oils, polyacrylates, polymethacrylates, epoxidized soybean oils, epoxidized linseed oils. The phthalate ester may be dioctyl terephthalate, di (2-ethylhexyl) isophthalate, dibutyl phthalate, dioctyl phthalate, diisooctyl phthalate, etc.; the trimellitate can be methyl trimesate, trioctyl trimellitate, triisodecyl trimellitate, etc.
In the present invention, the solid light-controlling particles may be optional suitable light-controlling particles. Preferably, the solid light-controlling particles are selected from at least one of oxide nanorods, perovskite nanorods, and polyiodide nanorods.
In the present invention, the first and second transparent substrates may take any suitable form. In some embodiments of the invention, the first transparent substrate and the second transparent substrate are glass plates. In other embodiments of the present invention, the first transparent substrate and the second transparent substrate are transparent plastic sheets.
In the present invention, the first transparent electrode and the second transparent electrode may employ an optional suitable transparent electrode. In some embodiments of the present invention, the first and second transparent electrodes are each independently selected from an ITO conductive layer, an FZO conductive layer, an IZO conductive layer, a GZO conductive layer, an AZO conductive layer, a PEDOT conductive layer, a nano Ag wire conductive layer, a conductive graphene, and a nano Cu wire conductive layer.
Preferably, in the light valve of the present invention, the first transparent electrode and/or the second transparent electrode may be further covered with an insulating layer.
In a second aspect of the present invention, there is provided a privacy glass assembly comprising:
a first glass plate and a second glass plate, and
a light valve (light adjusting film) of the present invention as described above disposed between the first glass plate and the second glass plate.
Preferably, in the dimming glass assembly of the present invention, a first adhesive layer is disposed between the first glass plate and the light valve, and/or a second adhesive layer is disposed between the second glass plate and the light valve.
In the present invention, the types of the first glass plate and the second glass plate are not particularly limited, and may be transparent glass for a conventional light control glass assembly, which is well known to those skilled in the art, and may be common glass such as inorganic glass and organic glass, or functional glass such as UV-blocking glass, IR-blocking glass, Low-E glass, tempered glass, or antibacterial glass.
In the present invention, the types of the first adhesive interlayer and the second adhesive interlayer are not particularly limited, and are known to those skilled in the art as the adhesive interlayer for the conventional dimming glass assembly, and the adhesive interlayer may be an EVA adhesive film, a TPU adhesive film, a PVB adhesive film, or a functional adhesive film, such as a UV-blocking EVA adhesive film, a UV-blocking TPU adhesive film, a UV-blocking PVB adhesive film, and the like.
In the present invention, the manner of manufacturing the dimming glass assembly is not particularly limited, and may be a conventional laminating manner of the dimming glass assembly in the art, such as laminating in a laminating machine, or laminating in an autoclave or a laminating box/furnace.
In a third aspect of the present invention, there is provided a method for improving the pressure resistance of a light valve, comprising:
providing a matrix emulsion of a light control layer;
coating the matrix emulsion of the light control layer on a first transparent electrode to form a wet film of the light control layer;
covering a second transparent electrode on the wet film of the light control layer; and
crosslinking and curing the wet film of the light control layer to obtain the light valve of the invention,
wherein
The light management layer matrix emulsion contains a polymer matrix precursor having dispersed therein droplets of a suspension medium within which are distributed solid light management particles, the polymer matrix precursor containing at least one siloxane copolymer derived from copolymerization of monomers comprising:
(a) a silicon-containing non-crosslinking monomer, which may be provided in the form of a silicon-containing non-crosslinking monomer and/or an oligomer thereof,
(b) a silicon-containing crosslinkable monomer, and
(c) a silicon-containing monomer having a high-occupancy side chain having the formula:
R-Xm-(CH2)n-SiR1 xR2 yformula (A)
Wherein the content of the first and second substances,
R1is hydroxy or a group which forms a hydroxy group upon hydrolysis, e.g. -Cl or C1-C3 alkoxy, especially R1Selected from-OH, -Cl, -OCH3、-OCH2CH3、-OCH(CH3)2、-OCH2CH2OCH3、-O-C(＝O)-CH3In particular from-OH, -Cl, -OCH3and-OCH2CH3，
R2Is C1-C3 alkyl, especially methyl or ethyl,
x and y are integers from 0 to 3, and x + y is 3, preferably x is 2 or 3,
x is selected from the group consisting of nitrogen, oxygen and sulfur,
m is 0 or 1, n is an integer from 0 to 10, preferably n is 0, 1, 2 or 3, more preferably 2 or 3,
r is a non-polymeric group such as H or a chain or cyclic group R' selected from optionally substituted alkyl, cycloalkyl, aromatic ring, heterocyclic, cycloalkylalkyl, heterocyclylalkyl, aralkyl, carbonyl and carbamoyl groups, said optional substituents being selected from hydroxy, amino, mercapto, acidic groups, alkoxy, aryloxy, alkylthio, arylthio, alkylamino, arylamino, ester groups, halogen and epoxy groups, which may be further optionally substituted.
In some embodiments of the present invention relating to the above method for improving the pressure resistance of a light valve, the matrix emulsion of a light management layer is obtained by the steps comprising:
providing a mixture of a suspension medium containing solid light-controlling particles;
providing a polymer matrix precursor; and
mixing an initiator that initiates cross-linking cure of the polymer matrix precursor, the mixture of the suspension medium containing solid light-controlling particles and the polymer matrix precursor.
In the method for improving the pressure resistance of the light valve, the matrix emulsion of the light control layer and the polymer matrix precursor contained in the matrix emulsion are in a liquid state. In the light valve of the present invention, the polymer matrix is in a cross-linked cured solid state.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a light modulation film according to some embodiments of the present invention. Wherein, 1 is a transparent electrode, 2 is a light control layer, 3 is a transparent substrate, 21 is a polymer matrix, 22 is a suspension medium liquid drop containing solid light control particles, and 23 is the solid light control particles.
Detailed Description
Term(s) for
In the present invention, the following terms are used with the meanings defined below.
Light valve:
the light valve is an electronic light control device, mainly a light control layer is arranged between two transparent conductive films, and after an electric field is switched on, the arrangement or the state of materials in the light control layer is changed, so that the light transmission characteristics of the device are changed, such as the conversion from low light transmittance to high light transmittance or the conversion from high light transmittance to low light transmittance.
And (3) crosslinking:
cross-linking refers to the polymerization of reactive groups on the side chains of the unit monomers in the polymer matrix precursor, said side chains referring to the structures covalently linked to silicon atoms other than the silicon hydroxyl groups and the groups that can form silicon hydroxyl groups. Crosslinking is sometimes referred to herein as crosslinking cure, i.e., occurs under thermocatalytic or radiation catalyzed conditions, such as the addition of a photoinitiator to a polymer matrix precursor to cause polymerization by radiation. Silicon-containing non-crosslinking monomer:
monomer units (a) forming a polymer matrix precursor, which have side chains not participating in the crosslinking reaction, said side chains being structures covalently linked to silicon atoms other than silicon hydroxyl groups and groups capable of forming silicon hydroxyl groups. Silicon-containing crosslinkable monomer:
monomer units (b) forming a polymer matrix precursor having reactive groups on side chains which are structures covalently bonded to silicon atoms other than silicon hydroxyl groups and groups capable of forming silicon hydroxyl groups, to participate in a crosslinking reaction.
Silicon-containing monomers with high-occupancy side chains:
and (c) a monomer unit (c) forming a polymer matrix precursor, which does not contain a group capable of participating in polymerization in a side chain, and which has a large steric hindrance in the side chain, said side chain being a structure covalently bonded to a silicon atom other than a silicon hydroxyl group and a group capable of forming a silicon hydroxyl group.
Silicone oil:
a linear polysiloxane which remains in a liquid state at room temperature.
Acrylate-based polymerizable group:
refers to a group containing a methacryloxy group or an acryloxy group.
Alkyl groups:
refers to a branched or straight chain saturated aliphatic hydrocarbon group having the specified number of carbon atoms. For example, "C1-C3 alkyl" represents an alkyl group having 1 to 3 carbon atoms. Examples of alkyl groups include, but are not limited to, methyl (Me), ethyl (Et), propyl (e.g., n-propyl and isopropyl), butyl (e.g., n-butyl, isobutyl, tert-butyl), and pentyl (e.g., n-pentyl, isopentyl, neopentyl).
The present invention provides a light valve with improved pressure resistance, wherein the polymer matrix precursor is composed of at least one siloxane copolymer, both terms of siloxane copolymer and polymer matrix precursor being equivalent when the polymer matrix precursor is composed of only one siloxane copolymer.
The invention provides a light valve with improved compressive property, which can effectively solve the problem of poor compressive property of a light control layer at a high temperature by adopting a polymer matrix precursor obtained by copolymerizing monomers of specific units and then crosslinking the polymer matrix precursor to form a polymer matrix. In particular, the present invention can effectively achieve an improvement in the compressive resistance relative to the absence of unit (c) by employing unit (c) of the following structural formula (a), i.e., a silicon-containing monomer having a high-occupancy side chain:
R-Xm-(CH2)n-SiR1 xR2 yformula (A)
See fig. 1. The polymer matrix precursor contains functional groups that can be cross-linked and cured to form polymer matrix 21 via a cross-linking reaction. The suspension medium is dispersed in the polymer matrix in the form of droplets, the droplets formed being referred to as suspension medium droplets 22.
To better illustrate the present invention, the following specific examples, including various preparation examples (including preparation of solid light-controlling particles, preparation of liquid suspending medium, preparation of polymer matrix precursor, preparation of light-adjusting film) and anti-pressure effect test examples, are now provided.
Example 1 preparation of solid light-controlling particles 23
Into a 250mL three-necked round bottom glass flask was charged 30g of isoamyl acetate solution containing 21.2 wt% nitrocellulose (model SS 1/4sec), 6g I270g of isoamyl acetate and 4g of anhydrous CaI2And heated to 42 ℃. Etc. I2After dissolution, 6g of anhydrous methanol, 0.8g of distilled water and 4g of 2, 5-pyrazinedicarboxylic acid dihydrate were charged into the above three-necked round-bottomed glass flask, and the mixture was reacted with heating at 42 ℃ for 4 hours with stirring, followed by natural cooling. The resulting reaction solution was centrifuged at 1350g for 0.5h to remove large particle products, and the supernatant was centrifuged at 18000g for 5h to discard the supernatant, yielding solid light-controlling particles 23. The solid light-controlling particles 23 were thoroughly dispersed with 250ml of isoamyl acetate.
Example 2 preparation of a liquid suspension Medium
24.4 g of dodecyl methacrylate, 2.0 g of hydroxyethyl methacrylate, 2.3 g of 1-hexanethiol and 20mL of toluene were each charged into a 250mL three-neck round-bottom glass flask. The middle of the three-neck round bottom glass flask is equipped with a mechanical stirring device, one side of the three-neck round bottom glass flask is connected with a condenser pipe, and the other side of the three-neck round bottom glass flask is provided with a thermometer and is communicated with argon. Before starting the heating, argon was introduced into the round-bottom glass flask for about 10 minutes to completely displace the air in the round-bottom glass flask. The flask was then heated to 60 ℃. At this temperature, 0.20g of azobisisobutyronitrile in 10mL of toluene was added to the flask. The reaction temperature was maintained at 60 ℃ for 21 hours, and the reaction temperature was raised again to reflux the reaction solution for 3 hours. The reaction was stopped. The reaction mixture was then treated by a rotary evaporator at 100 ℃ for 3 hours to remove toluene and unreacted starting materials to give a liquid suspension medium.
40 g of the resulting suspension medium was added in portions to a 250ml round bottom glass flask, and the isoamyl acetate dispersion of the solid light-controlling particles 23 prepared in example 1 was added, and the isoamyl acetate was removed by a rotary evaporator, and finally, the treatment was continued at 80 ℃ for 3 hours using the rotary evaporator to obtain a mixture of the liquid suspension medium containing the solid light-controlling particles 23.
Example 3 preparation of siloxane copolymer
To a 500mL three neck round bottom glass flask was added (a) silicon containing non-crosslinked oligomer: 54g of hydroxyl-terminated dimethyldiphenylpolysiloxane and 190mL of n-heptane. One side of the three-neck round bottom glass flask is connected with a water separator and a condenser pipe, the middle part is provided with a mechanical stirrer, and the other side is provided with a thermometer. The reaction solution in a three-neck round bottom glass flask was heated to reflux for 30min and a solution of 0.13g stannous octoate in 10mL n-heptane was added. Then dropwise adding (b) a silicon-containing crosslinkable monomer: 3g of hydrolyzed 3-acryloxypropylmethyldimethoxysilane, and (c) a silicon-containing monomer with a high occupancy side chain: 1.8g of a mixture of hydrolyzed 3-glycidoxypropylmethyldimethoxysilanes was added dropwise over a period of about 5 minutes. Then reacting for 2 hours under the reflux condition, and immediately adding 30mL of trimethyl methoxy silane as a reaction terminator; the reaction was terminated for 2h and then rapidly cooled to room temperature. 50mL of ethanol and the reaction solution which had been cooled were mixed and stirred in a 1L beaker, and the reaction flask was rinsed with 30mL of heptane and poured into the beaker. After mixing well, 200mL of methanol was added and stirred for 15 min. Pouring the obtained mixture into a 1L separating funnel, standing for several hoursDelamination occurred. Taking out the lower layer liquid, treating at 70 deg.C for 3 hr by rotary evaporator to remove low boiling point substances to obtain the final productSiloxane copolymers。
And (3) hydrolysis reaction: one side of a three-neck round bottom glass flask is connected with a condenser pipe, the middle part is provided with a mechanical stirrer, and the other side is provided with a thermometer. In a 250mL three-necked round-bottomed glass flask, 0.1g of acetic acid, 5.5g of water, 44.5g of 3-acryloyloxypropylmethyldimethoxysilane, or 44.5g of 3-glycidyloxypropylmethyldimethoxysilane and 35mL of anhydrous ethanol were sequentially charged, and the hydrolysis reaction was carried out at 65 ℃ for 5 hours. And after the reaction is finished, removing the solvent, the residual water and the acid by using a rotary evaporator to obtain a hydrolysate.
Example 4 preparation of siloxane copolymer
As in example 3, except that unit (c)) a silicon-containing monomer with a high-occupancy side chain: the hydrolyzed 3-glycidoxypropylmethyldimethoxysilane was replaced with 3-piperazinylpropylmethyldimethoxysilane.
EXAMPLE 5 preparation of siloxane copolymer
As in example 3, except that unit (c) a silicon-containing monomer with a high occupancy side chain: hydrolyzed 3-glycidoxypropylmethyldimethoxysilane was replaced with isooctyltrimethoxysilane.
Example 6 preparation of siloxane copolymer
The same as example 3, except that the unit (c) is a silicon-containing monomer having a non-crosslinked side chain: the hydrolyzed 3-glycidoxypropylmethyldimethoxysilane was replaced with 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane.
Example 7 preparation of siloxane copolymer
The same as example 3, except that the unit (b) silicon-containing crosslinkable monomer: the hydrolyzed 3-acryloxypropylmethyldimethoxysilane was replaced with 3-methacryloxypropyltrimethoxysilane;
at the same time, unit (c) a silicon-containing monomer with a high-occupancy side chain: the hydrolyzed 3-glycidoxypropylmethyldimethoxysilane was replaced with 3- (N-cyclohexylamino) propyltrimethoxysilane.
Example 8 preparation of siloxane copolymer
The same as example 7, except that unit (c) a silicon-containing monomer with a high occupancy side chain: 3- (N-cyclohexylamino) propyltrimethoxysilane was replaced with 3-mercaptopropyltrimethoxysilane.
Example 9 preparation of siloxane copolymer
The same as example 7, except that unit (c) a silicon-containing monomer with a high occupancy side chain: 3- (N-cyclohexylamino) propyltrimethoxysilane was replaced with 3-ureidopropyltriethoxysilane.
EXAMPLE 10 preparation of siloxane copolymer
The same as example 7, except that unit (c) a silicon-containing monomer with a high occupancy side chain: 3- (N-cyclohexylamino) propyltrimethoxysilane was replaced with cyclohexyltrimethoxysilane.
Example 11 preparation of siloxane copolymer
The same as example 7, except that unit (c) a silicon-containing monomer with a high occupancy side chain: 3- (N-cyclohexylamino) propyltrimethoxysilane was replaced with 1H,1H,2H, 2H-perfluorooctyltrimethoxysilane.
Example 12 preparation of siloxane copolymer
The same as example 7, except that unit (c) a silicon-containing monomer with a high occupancy side chain: 3- (N-cyclohexylamino) propyltrimethoxysilane was replaced with benzoyloxypropyltrimethoxysilane.
Example 13 preparation of a siloxane copolymer
The same as example 7, except that unit (c) a silicon-containing monomer with a high occupancy side chain: 3- (N-cyclohexylamino) propyl trimethoxy silane is replaced by (trimethoxysilyl) methyl propionate.
Example 14 preparation of siloxane copolymer
The same as example 7, except that unit (c) a silicon-containing monomer with a high occupancy side chain: the 3- (N-cyclohexylamino) propyltrimethoxysilane was replaced with 9-anthracenyl (trimethoxy) silane.
Example 15 preparation of siloxane copolymer
The same as example 7, except that unit (c) a silicon-containing monomer with a high occupancy side chain: 3- (N-cyclohexylamino) propyltrimethoxysilane was replaced with trimethoxysilylpropoxypolyethyleneoxide methyl ether.
Example 16 preparation of a siloxane copolymer
The same as example 7, except that unit (c) a silicon-containing monomer with a high occupancy side chain: 3- (N-cyclohexylamino) propyltrimethoxysilane was replaced with 3- (phenylamino) propyltrimethoxysilane.
EXAMPLE 17 preparation of light-adjusting film and compression test
The initiator that initiates the cross-linking cure of the polymer matrix precursor, the mixture of the suspension medium containing the solid light-controlling particles 23 and the polymer matrix precursor are mixed homogeneously, and the resulting mixture is referred to as the light-controlling layer matrix emulsion.
The initiator that initiates the crosslinking curing of the polymer matrix precursor is preferably a photoinitiator, specifically photoinitiator 819 in the present example; the kind of the photoinitiator may be selected according to actual needs, and is not particularly limited, and the initiator for initiating the crosslinking curing of the polymer matrix precursor is preferably at least one of 184(CAS number 947-19-3), ITX (CAS number 5495-84-1 or 83846-86-0), 819(CAS number 162881-26-7), 1173(CAS number 7473-98-5), BDK (CAS number 24650-42-8), BP (CAS number 119-61-9), TPO (CAS number 75980-60-8), 369(CAS number 119313-12-1), 907(CAS number 71868-10-5). The amount (mass%) of the photoinitiator is preferably 0.05% to 1%, more preferably 0.1% to 0.6%, and still more preferably 0.2% to 0.5% of the polymer matrix precursor.
0.03 g of photoinitiator 819, 3.0 g of a mixture of liquid suspension medium containing solid light-controlling particles 23 prepared in example 2 and prepared in example 3Siloxane copolymers7.0 g of the mixture is uniformly mixed to obtain the matrix emulsion of the light control layer.
Controlling the lightThe layer matrix emulsion was coated on the ITO/PET transparent conductive film with a thickness of 80 μm using a doctor blade type automatic film coater (MSK-AFA-III, MTI Corporation), and another layer of the ITO/PET transparent conductive film was coated on the light control layer matrix emulsion wet film to obtain a wet film containing a light control layer. Curing the mixture for 1 minute in an X200-150 UV curing machine manufactured by Aventk company with a UV power of 700W/m under a nitrogen atmosphere2And obtaining the light adjusting film.
In this embodiment, a transparent conductive film (transparent electrode) is formed on a base of a plastic sheet.
The polymer matrix precursor forms a polymer matrix after crosslinking and curing.
In this application, the pressure resistance of a light valve is characterized by the relative rate of change Δ T of the light valve transmittance T.
And the relative change rate of delta T is [ (Ton before compression test Ton-Toff before compression test) - (Ton after compression test Ton-Toff after compression test) ]/(Ton before compression test Ton-Toff before compression test) x 100%, wherein Ton refers to the electrified light transmittance of the light valve, Toff refers to the non-electrified light transmittance of the light valve, and the electric field intensity of Ton before compression test is the same as that of Ton after compression test.
It is clear that a smaller value of the relative rate of change of deltat indicates a better pressure resistance of the light valve.
The transmittance of the light-modulating film was measured by an LS116 transmittance meter (Shenzhen Lin technologies Co., Ltd.). When no voltage is applied (off state), the light transmittance Toff of the light-adjusting film is 0.5%. When a 60 hz 220 v ac (on state) is applied, the total light transmittance Ton of the light-adjusting film is 59.5%.
And (3) compression resistance test:
and clamping the light modulation film between two pieces of glass, and carrying out a compression resistance test in a laminating machine. The test conditions were: and (3) vacuumizing for 10min at the temperature of 110 ℃, gradually pressurizing to 350kPa, delaying for 30min, then cooling to room temperature, and testing the change of the light transmittance of the light-adjusting film. When no voltage is applied (off state), the light transmittance Toff of the light-adjusting film is 0.5%. When a 60 hz 220 v ac (on state) is applied, the total light transmittance Ton of the light-adjusting film is 56.1%.
Specific results are shown in table 1.
ExamplesPreparation and compression resistance test of 18 light adjusting film
The same as example 17 except that the siloxane copolymer prepared in alternative example 3 was the siloxane copolymer prepared in example 4. The pressure resistance test condition is that the temperature is 110 ℃, the vacuum is pumped for 10min, the pressure is gradually increased to 300kPa, and the time delay is 30 min.
EXAMPLE 19 preparation of light-adjusting film and compression test
The same as example 17 except that the siloxane copolymer prepared in alternative example 3 was the siloxane copolymer prepared in example 5. The pressure resistance test condition is that the temperature is 120 ℃, the vacuum pumping is carried out for 10min, the pressure is gradually increased to 300kPa, and the time delay is 30 min.
EXAMPLE 20 preparation of light-adjusting film and compression test
The same as in example 17 except that the siloxane copolymer prepared in alternative example 3 was the siloxane copolymer prepared in example 6. The pressure resistance test condition is that the temperature is 115 ℃, the vacuum is pumped for 10min, the pressure is gradually increased to 300kPa, and the time delay is 30 min.
EXAMPLE 21 preparation of light-adjusting film and compression test
The same as in example 17 except that the siloxane copolymer prepared in alternative example 3 was the siloxane copolymer prepared in example 7. The replacement laminator was an autoclave, the compression test condition was 125 ℃, the pressure was gradually increased to 350kPa, and the time was extended for 30 min.
EXAMPLE 22 preparation of light-adjusting film and compression test
The same as in example 21, except that the siloxane copolymer prepared in alternative example 7 was the siloxane copolymer prepared in example 8.
EXAMPLE 23 preparation of light-adjusting film and compression test
The same as in example 21, except that the siloxane copolymer prepared in alternative example 7 was the siloxane copolymer prepared in example 9.
EXAMPLE 24 preparation of light-adjusting film and compression resistance test
The same as in example 21, except that the siloxane copolymer prepared in alternative example 7 was the siloxane copolymer prepared in example 10.
EXAMPLE 25 preparation of light-adjusting film and compression test
The same as in example 21, except that the siloxane copolymer prepared in alternative example 7 was the siloxane copolymer prepared in example 11.
EXAMPLE 26 preparation of light-adjusting film and compression test
The same as in example 21, except that the siloxane copolymer prepared in alternative example 7 was the siloxane copolymer prepared in example 12.
EXAMPLE 27 preparation of light-adjusting film and compression test
The same as in example 21, except that the siloxane copolymer prepared in alternative example 7 was the siloxane copolymer prepared in example 13.
EXAMPLE 28 preparation of light-adjusting film and compression test
The same as in example 21, except that the siloxane copolymer prepared in alternative example 7 was the siloxane copolymer prepared in example 14.
EXAMPLE 29 preparation of light-adjusting film and compression test
The same as in example 21, except that the siloxane copolymer prepared in alternative example 7 was the siloxane copolymer prepared in example 15.
EXAMPLE 30 preparation of light-adjusting film and compression test
The same as in example 21, except that the siloxane copolymer prepared in alternative example 7 was the siloxane copolymer prepared in example 16.
Comparative example 1 preparation of a catalyst composition containing(c)Siloxane copolymers of
The same as example 3 except that (c) the silicon-containing monomer with a high occupancy side chain was not added.
Comparative example 2 preparation of a composition containing(c)Siloxane copolymers of
The same as example 7, except that (c) the silicon-containing monomer with a high occupancy side chain was not added.
Comparative example 3 preparation of light-adjusting film and compression resistance test
The same as in example 17, except that the siloxane copolymer prepared in comparative example 1 was used in place of the siloxane copolymer prepared in example 3, and no pressure was applied, only vacuum was pulled.
Comparative example 4 preparation of light-adjusting film and compression resistance test
The same as in example 17 except that the siloxane copolymer prepared in comparative example 1 was used in place of the siloxane copolymer prepared in example 3.
Comparative example 5 preparation of light-adjusting film and compression resistance test
The same as example 21 except that the siloxane copolymer prepared in comparative example 2 was used in place of the siloxane copolymer prepared in example 7.
The results of examples 17 to 30 and comparative examples 3 to 5 described above are shown in Table 1 below.
TABLE 1
As can be seen from the comparison of comparative examples 3-5 with examples 17-30 in table 1, by adding (c) at least one silicon-containing monomer with a high occupancy side chain, the high occupancy side chain moiety has an unexpectedly significant property of improving the compressive strength of the light management layer, and the relative rate of change Δ T is much less than the light management film prepared without the addition of (c) a polymer matrix precursor of the at least one silicon-containing monomer with a high occupancy side chain. The proposal can completely meet the requirement of the laminating process for manufacturing the dimming glass component by adopting a laminating machine or an autoclave subsequently.
The present invention has been described above by way of example with a light valve having a transparent plastic sheet as a substrate, i.e., a light adjusting film. It is obvious that the inventive idea is also fully applicable to light valves with glass as substrate, i.e. dimming glasses. The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (17)
1. A light valve having increased compressive strength, comprising:
a first transparent substrate having a first refractive index,
a first transparent electrode formed on the first transparent substrate,
a second transparent substrate, which is transparent to light,
a second transparent electrode formed on a second transparent substrate, the first and second transparent electrodes being disposed opposite to each other, an
A light control layer disposed between the first transparent electrode and the second transparent electrode; the light management layer includes a polymer matrix;
wherein the polymer matrix is dispersed with suspension medium droplets, and solid light-controlling particles are distributed in the suspension medium droplets, the polymer matrix is obtained by crosslinking and curing at least one siloxane copolymer, and the siloxane copolymer is obtained by copolymerizing monomers comprising the following units:
(a) a silicon-containing non-crosslinking monomer, which may be provided in the form of a silicon-containing non-crosslinking monomer and/or an oligomer thereof,
(b) a silicon-containing crosslinkable monomer, and
(c) a silicon-containing monomer having a high-occupancy side chain having the formula:
R-Xm-(CH2)n-SiR1 xR2 yformula (A)
Wherein the content of the first and second substances,
R1is hydroxy or a group which forms a hydroxy group upon hydrolysis, e.g. -Cl or C1-C3 alkoxy, especially R1Selected from-OH, -Cl, -OCH3、-OCH2CH3、-OCH(CH3)2、-OCH2CH2OCH3、-O-C(＝O)-CH3In particular from-OH, -Cl, -OCH3and-OCH2CH3，
R2Is C1-C3 alkyl, especially methyl or ethyl,
x and y are integers from 0 to 3, and x + y is 3, preferably x is 2 or 3,
x is selected from the group consisting of nitrogen, oxygen and sulfur,
m is 0 or 1, n is an integer from 0 to 10, preferably n is 0, 1, 2 or 3, more preferably 2 or 3,
r is a non-polymeric group such as H or a chain or cyclic group R' selected from optionally substituted alkyl, cycloalkyl, aromatic ring, heterocyclic, cycloalkylalkyl, heterocyclylalkyl, aralkyl, carbonyl and carbamoyl groups, said optional substituents being selected from hydroxy, amino, mercapto, acidic groups, alkoxy, aryloxy, alkylthio, arylthio, alkylamino, arylamino, ester groups, halogen and epoxy groups, which may be further optionally substituted.
2. A light valve according to claim 1 wherein in formula (a), when R-Xm-is-OH, -SH or-NH2When is, R-Xm-(CH2)n-the total number of atoms, excluding hydrogen, is at least 4; when R-Xm-is not-OH, -SH or-NH2When is, R-Xm-(CH2)nThe total number of atoms, not counting hydrogen, is at least 6, and/or
Wherein in formula (A), R-X is when unit (c) comprises only one silicon-containing monomer with a high-occupancy side chainmIs not-NH2A hydroxyl group, a glycidoxy group, an acryloxy group, a methacryloxy group, or an acidic group.
3. A light valve according to claim 1 or 2 wherein the polymer matrix is formed by cross-linking curing of a polymer matrix precursor, the polymer matrix precursor being synthesized from starting materials comprising,
(a) oligomers of silicon-containing non-crosslinking monomers;
(b) a silicon-containing crosslinkable monomer; and
(c) silicon-containing monomers with high-occupancy side chains.
4. A light valve according to claim 3 wherein the cross-linking cure takes place under thermocatalytic or radiation catalysed conditions, for example by adding a photoinitiator to the polymer matrix precursor to cause polymerisation by irradiation.
5. A light valve according to claim 4 wherein the photoinitiator is selected from at least one of 184, ITX, 819, 1173, BDK, BP, TPO, 369, 907.
6. A light valve according to any one of claims 1 to 5,
the oligomer of the silicon-containing non-crosslinking monomer is silicone oil; and/or
The silicon-containing crosslinkable monomer source is a compound of formula (1):
Q-(CH2)m-Si(RnX3-n) Formula (1);
wherein the content of the first and second substances,
q is an acrylate-based polymerizable group;
r is alkyl;
x is hydroxyl or a group which can generate hydroxyl after hydrolysis reaction;
m is a positive integer; n is 0, 1 or 2.
7. A light valve according to any one of claims 1 to 6,
the oligomer of the silicon-containing non-crosslinking monomer is at least one of hydroxyl-terminated silicone oil and methoxyl-terminated silicone oil; and/or
The silicon-containing crosslinkable monomer source is a compound of formula (1):
Q-(CH2)m-Si(RnX3-n) Formula (1);
wherein the content of the first and second substances,
q is methacryloxy or acryloxy;
r is C1-C4 alkyl;
x is-OH, -Cl, -OCH3、-OCH2CH3、-OCH(CH3)2、-OCH2CH2OCH3、-O-C(＝O)-CH3At least one of;
m is an integer of 1 to 10, and n is 0 or 1.
8. A light valve according to any one of claims 1 to 7, wherein the suspension medium droplets are formed from a material selected from at least one of a fluorocarbon organic compound, a phthalate, a trimellitate, a dodecylbenzene, a polybutyleneoil, a polyacrylate, a polymethacrylate, an epoxidized soyabean oil, and an epoxidized linseed oil.
9. A light valve according to any one of claims 1 to 8, wherein the solid light-controlling particles are selected from at least one of oxide nanorods, perovskite nanorods, polyiodide nanorods.
10. A light valve according to any one of claims 1 to 9 wherein the first and second transparent substrates are glass plates.
11. A light valve according to any one of claims 1 to 10 wherein the first and second transparent substrates are transparent plastic sheets.
12. A light valve according to any one of claims 1 to 11, wherein the first and second transparent electrodes are each independently selected from an ITO conductive layer, an FZO conductive layer, an IZO conductive layer, a GZO conductive layer, an AZO conductive layer, a PEDOT conductive layer, a nano Ag wire conductive layer, a conductive graphene, and a nano Cu wire conductive layer.
13. A light valve according to any one of claims 1 to 12 wherein the first and/or second transparent electrodes are covered with an insulating layer.
14. A light control glass assembly comprising
A first glass plate and a second glass plate, and
a light valve as claimed in any one of claims 1 to 13 disposed between the first and second glass plates.
15. The privacy glass assembly of claim 14, wherein a first adhesive layer is disposed between the first glass plate and the light valve, and/or a second adhesive layer is disposed between the second glass plate and the light valve.
16. A method of improving the crush resistance of a light valve, comprising:
providing a matrix emulsion of a light control layer;
coating the matrix emulsion of the light control layer on a first transparent electrode to form a wet film of the light control layer;
covering a second transparent electrode on the wet film of the light control layer; and
crosslinking and curing the wet film of the light management layer to obtain a light valve according to any of claims 1 to 13,
wherein
The light management layer matrix emulsion contains a polymer matrix precursor having dispersed therein droplets of a suspension medium within which are distributed solid light management particles, the polymer matrix precursor containing at least one siloxane copolymer derived from copolymerization of monomers comprising:
(a) a silicon-containing non-crosslinking monomer, which may be provided in the form of a silicon-containing non-crosslinking monomer and/or an oligomer thereof,
(b) a silicon-containing crosslinkable monomer, and
(c) a silicon-containing monomer having a high-occupancy side chain having the formula:
R-Xm-(CH2)n-SiR1 xR2 yformula (A)
Wherein the content of the first and second substances,
R1is hydroxy or a group which forms a hydroxy group upon hydrolysis, e.g. -Cl or C1-C3 alkoxy, especially R1Selected from-OH, -Cl, -OCH3、-OCH2CH3、-OCH(CH3)2、-OCH2CH2OCH3、-O-C(＝O)-CH3In particular from-OH, -Cl, -OCH3and-OCH2CH3，
R2Is C1-C3 alkyl, especially methyl or ethyl,
x and y are integers from 0 to 3, and x + y is 3, preferably x is 2 or 3,
x is selected from the group consisting of nitrogen, oxygen and sulfur,
m is 0 or 1, n is an integer from 0 to 10, preferably n is 0, 1, 2 or 3, more preferably 2 or 3,
r is a non-polymeric group such as H or a chain or cyclic group R' selected from optionally substituted alkyl, cycloalkyl, aromatic ring, heterocyclic, cycloalkylalkyl, heterocyclylalkyl, aralkyl, carbonyl and carbamoyl groups, said optional substituents being selected from hydroxy, amino, mercapto, acidic groups, alkoxy, aryloxy, alkylthio, arylthio, alkylamino, arylamino, ester groups, halogen and epoxy groups, which may be further optionally substituted.
17. The method of claim 16, wherein the matrix emulsion of light management layers is obtained by a step comprising:
providing a mixture of a suspension medium containing solid light-controlling particles;
providing a polymer matrix precursor; and
mixing an initiator that initiates cross-linking cure of the polymer matrix precursor, the mixture of the suspension medium containing solid light-controlling particles and the polymer matrix precursor.
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