CN115097676B - Optical film with full-coverage electrode and light transmittance capable of being controlled in multiple areas and multiple levels and preparation method thereof - Google Patents
Optical film with full-coverage electrode and light transmittance capable of being controlled in multiple areas and multiple levels and preparation method thereof Download PDFInfo
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- CN115097676B CN115097676B CN202210697482.5A CN202210697482A CN115097676B CN 115097676 B CN115097676 B CN 115097676B CN 202210697482 A CN202210697482 A CN 202210697482A CN 115097676 B CN115097676 B CN 115097676B
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- 239000012788 optical film Substances 0.000 title claims abstract description 53
- 238000002834 transmittance Methods 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000004973 liquid crystal related substance Substances 0.000 claims abstract description 80
- 239000004593 Epoxy Substances 0.000 claims abstract description 53
- 229920000106 Liquid crystal polymer Polymers 0.000 claims abstract description 34
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 claims abstract description 34
- 150000002500 ions Chemical class 0.000 claims abstract description 30
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 239000000758 substrate Substances 0.000 claims abstract description 25
- 230000005540 biological transmission Effects 0.000 claims abstract description 16
- 239000000178 monomer Substances 0.000 claims abstract description 16
- 239000011521 glass Substances 0.000 claims abstract description 11
- 239000012952 cationic photoinitiator Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000007151 ring opening polymerisation reaction Methods 0.000 claims abstract description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 11
- 239000010408 film Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000000049 pigment Substances 0.000 claims description 6
- 125000001931 aliphatic group Chemical group 0.000 claims description 4
- 125000003545 alkoxy group Chemical group 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 125000000304 alkynyl group Chemical group 0.000 claims description 4
- 125000003118 aryl group Chemical group 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- -1 cyano, methyl Chemical group 0.000 claims description 4
- 125000004185 ester group Chemical group 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 229910052736 halogen Inorganic materials 0.000 claims description 4
- 150000002367 halogens Chemical class 0.000 claims description 4
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 4
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 claims description 4
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 claims description 4
- 239000004417 polycarbonate Substances 0.000 claims description 3
- 229920000515 polycarbonate Polymers 0.000 claims description 3
- 229920001225 polyester resin Polymers 0.000 claims description 3
- 239000004645 polyester resin Substances 0.000 claims description 3
- 239000012954 diazonium Substances 0.000 claims description 2
- 150000001989 diazonium salts Chemical group 0.000 claims description 2
- 239000002861 polymer material Substances 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- 230000000977 initiatory effect Effects 0.000 abstract 1
- 230000005684 electric field Effects 0.000 description 23
- 229920000642 polymer Polymers 0.000 description 21
- 238000001514 detection method Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 238000007142 ring opening reaction Methods 0.000 description 7
- 239000000975 dye Substances 0.000 description 5
- 238000010030 laminating Methods 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 125000002091 cationic group Chemical group 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 239000003999 initiator Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- KTEFLEFPDDQMCB-UHFFFAOYSA-N 1,4-bis(4-butylanilino)-5,8-dihydroxyanthracene-9,10-dione Chemical compound C1=CC(CCCC)=CC=C1NC(C=1C(=O)C2=C(O)C=CC(O)=C2C(=O)C=11)=CC=C1NC1=CC=C(CCCC)C=C1 KTEFLEFPDDQMCB-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004984 smart glass Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/137—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells characterised by the electro-optical or magneto-optical effect, e.g. field-induced phase transition, orientation effect, guest-host interaction or dynamic scattering
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
- C08G59/22—Di-epoxy compounds
- C08G59/24—Di-epoxy compounds carbocyclic
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/137—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells characterised by the electro-optical or magneto-optical effect, e.g. field-induced phase transition, orientation effect, guest-host interaction or dynamic scattering
- G02F1/13731—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells characterised by the electro-optical or magneto-optical effect, e.g. field-induced phase transition, orientation effect, guest-host interaction or dynamic scattering based on a field-induced phase transition
- G02F1/13737—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells characterised by the electro-optical or magneto-optical effect, e.g. field-induced phase transition, orientation effect, guest-host interaction or dynamic scattering based on a field-induced phase transition in liquid crystals doped with a pleochroic dye
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/137—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells characterised by the electro-optical or magneto-optical effect, e.g. field-induced phase transition, orientation effect, guest-host interaction or dynamic scattering
- G02F1/13775—Polymer-stabilized liquid crystal layers
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- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Liquid Crystal (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses an optical film with a full-coverage electrode, light transmittance of which can be controlled in multiple steps in a region and a preparation method thereof, wherein the optical film comprises a substrate layer, a conductive layer, a parallel orientation layer, a liquid crystal/epoxy liquid crystal polymer composite material layer, a parallel orientation layer, a conductive layer and a substrate layer which are sequentially laminated; the liquid crystal/epoxy liquid crystal polymer composite material layer consists of an epoxy liquid crystal polymer network, ions and negative liquid crystal and is divided into a light transmission area and a scattering area with different dynamic scattering degrees: when not electrified, each area is in a light-transmitting state; when the power is on, the light-transmitting area keeps a light-transmitting state, and other areas are in scattering states with different degrees. The optical film is prepared by uniformly mixing a liquid crystal epoxy monomer, negative liquid crystal and a cationic photoinitiator, and initiating ring-opening polymerization by light through a mask. The optical film can achieve regional regulation and multistage regulation of light transmittance at the same time, can be widely used as an intelligent window in the fields of building glass, automobile glass and the like, and can also be used as a display device.
Description
Technical Field
The invention belongs to the field of application of liquid crystal technology, and relates to an optical film, in particular to an optical film with light transmittance on a full-coverage electrode capable of being controlled in multiple areas and multiple levels and a preparation method thereof.
Background
Liquid crystals are widely used in the fields of display, smart windows, handwriting boards, etc. due to their unique electro-optical response characteristics, which come from their own dielectric anisotropy, optical anisotropy, and their fluidity similar to liquids. In order to realize response of liquid crystal to an electric field, liquid crystal is generally placed between two transparent conductive substrates, and when a voltage is applied to the conductive substrates to form a potential difference (voltage) between the two conductive substrates, different liquid crystals spontaneously align liquid crystal molecules in a specific direction due to the difference of respective dielectric anisotropies. In this process, the propagation properties of the liquid crystal layer to the incident light are changed due to its optical anisotropy, thereby modulating the light. If different areas of the same liquid crystal panel have different effects on light, the conductive layer needs to be divided by processing, and each area of liquid crystal is dynamically scattered by controlling a separate circuit of each area, and related circuit design and preparation are needed. The specific method comprises the steps of etching the conductive layer, performing electromagnetic sputtering on the surface of the substrate under a mask, coating the conductive layer and the like. Although the methods realize independent control of different areas of the same liquid crystal panel, the technology is complex, the cost is high, and only regional control can be realized, so that no technology can realize multi-stage control of the same liquid crystal panel at present.
Disclosure of Invention
The invention aims to provide an optical film with the full-coverage electrode, the light transmittance of which can be controlled in multiple stages in different areas, so as to solve the problem that the current control of the liquid crystal optical film in different areas needs complex and high-cost circuit design treatment, and simultaneously achieve the effect of multiple stages of control;
another object of the present invention is to provide a method for preparing the optical film with the light transmittance on the fully covered electrode being controlled in multiple steps in different areas.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the optical film comprises a first composite layer structure formed by a first substrate layer, a first conductive layer and a first parallel orientation layer which are sequentially laminated along the thickness direction, and a second composite layer structure formed by a second parallel orientation layer, a second conductive layer and a second substrate layer which are sequentially laminated along the thickness direction, and further comprises a liquid crystal/epoxy liquid crystal polymer composite layer, wherein the liquid crystal/epoxy liquid crystal polymer composite layer is laminated between the first parallel orientation layer and the second parallel orientation layer and is integrated with the first composite layer structure and the second composite layer structure, and the liquid crystal/epoxy liquid crystal polymer composite layer is formed by an epoxy liquid crystal polymer network, ions and negative liquid crystal;
the liquid crystal/epoxy liquid crystal polymer composite material layer can be divided into a light transmission area and a scattering area with different dynamic scattering degrees: when not electrified, each area presents a light transmission state; when the power is on, the light-transmitting area keeps a light-transmitting state, other areas show scattering states with different degrees, and the shape, the size, the position and the number of each area can be designed and customized according to requirements.
As a limitation, the epoxy liquid crystal polymer network and the negative liquid crystal forming the liquid crystal/epoxy liquid crystal polymer composite layer are aligned in parallel; the content of the epoxy liquid crystal polymer network and the content of ions form concentration gradients between different areas in the layer, and the gradient directions of the epoxy liquid crystal polymer network and the ion content are consistent.
As a further limitation, the substrate layer is composed of a transparent substrate made of glass, polyester resin or polycarbonate; the conductive layer is made of ITO or conductive high polymer material; the parallel alignment layer is made of PVA or PI.
As a further limitation, the thickness of the liquid crystal/epoxy-based liquid crystal polymer composite layer is 0.5 to 100 μm.
As a second limitation, the raw materials of the liquid crystal/epoxy liquid crystal polymer composite material comprise 0.01-40 weight percent: 40 to 99.9: 0.01-10 of liquid crystal epoxy monomer, negative liquid crystal and cationic photoinitiator.
As a further limitation, the liquid crystalline epoxy monomer is at least one of the following compounds I and II:
wherein A is 1 、A 2 、G 1 And G 2 Are all one of C1-C16 alkyl, C1-C16 alkoxy and C1-C16 siloxane groups;
J 1 、J 2 、L 1 、L 2 、M 1 and M 2 Are aromatic or aliphatic rings;
x 1 、x 2 、y 1 、y 2 、z 1 and z 2 Are all integers from 0 to 4;
Q 1 、Q 2 、R 1 、R 2 、T 1 and T 2 All are halogen, cyano, methyl or methoxy;
k 1 、k 2 、m 1 、m 2 、n 1 and n 2 Are all integers from 0 to 4;
D 1 、D 2 、E 1 and E is 2 All are ester groups, alkynyl groups, methylene groups, nitrogen-nitrogen double bonds, ether bonds or direct connection;
the negative liquid crystal is at least one of the following compounds:
wherein A is 3 And G 3 Are all one of C1-C16 alkyl, C1-C16 alkoxy and C1-C16 siloxane groups;
J 3 、L 3 and M 3 Are aromatic or aliphatic rings;
x 3 、y 3 and z 3 Are all integers from 0 to 4;
Q 3 、R 3 and T 3 All are halogen, cyano, methyl or methoxy;
k 3 、m 3 、n 3 are all integers from 0 to 4;
D 3 and E is 3 All are ester groups, alkynyl groups, methylene groups, nitrogen-nitrogen double bonds, ether bonds or direct connection;
the cationic photoinitiator is diazonium salt and iodineSalt or sulfur->And (3) salt.
As a further limitation, the liquid crystal/epoxy liquid crystal polymer composite layer further comprises dye or pigment, and the weight portion of the dye or pigment is 0.01% -10%.
The invention also provides a preparation method of the optical film with the light transmittance of the full-coverage electrode capable of being controlled in a region-by-region and multiple-stage manner, when the dynamic scattering level of the film is n levels, the preparation method comprises the following steps of:
s1, uniformly mixing raw materials of a liquid crystal/epoxy liquid crystal polymer composite material, and adding the raw materials between a first parallel orientation layer and a second parallel orientation layer;
s2, continuously polymerizing the film for n-1 times, placing a mask between the substrate layer and the light source during each polymerization, and performing epoxy photoinitiated ring-opening polymerization for 0.01-10 h to complete the polymerization, wherein the optical film with the light transmittance capable of being controlled in multiple stages and in different areas on the full-coverage electrode can be prepared after the polymerization for n-1 times is completed.
As a limitation, the mask is divided into opaque and transparent areas, and the shape, size, position and number of the two areas can be designed and customized according to the requirements;
starting from the second polymerization, the light-transmitting areas of the mask used in the preparation process cover the light-transmitting areas of the mask in the previous step; alternatively, the light-transmitting areas of the masks used in the preparation process are not coincident.
As a further limitation, the temperature of the epoxy photoinitiated ring-opening polymerization is-20 to 120 ℃.
By adopting the technical scheme, compared with the prior art, the invention has the following technical progress:
(1) the optical film with the full-coverage electrode, which has the light transmittance capable of being controlled in the multiple areas, firstly utilizes the mask method to carry out regional epoxy monomer polymerization (the shape, the size, the position and the number of the light transmission area of the mask can be designed and customized according to the requirements), the epoxy liquid crystal polymer network in the liquid crystal/epoxy liquid crystal polymer composite material layer is only formed in the area which is subjected to illumination, and the epoxy liquid crystal polymer network is not formed in the area which is not subjected to illumination, namely the concentration gradient of the polymer network is formed; meanwhile, by utilizing the adsorption effect of a polymer network formed by polymerization on ions (a cationic photoinitiator and a photolysis product thereof), the ions in the liquid crystal/epoxy liquid crystal polymer composite material layer are only distributed in the area subjected to illumination, so that an ion concentration gradient is formed; in the off state, each region of the film presents a consistent transparent state; when the film is electrified, the dynamic scattering of the region containing the polymer network and ions is strong, and the light transmittance is obviously reduced; the area without a polymer network and ions (i.e. the unpolymerized area) is not scattered dynamically, and the transparent state consistent with the off state is maintained, so that the regional regulation and control of the light transmittance of the optical film on the full-coverage electrode is realized;
(2) the optical film with the full-coverage electrode, which is provided by the invention, has the advantages that the light transmittance can be controlled in the multiple areas in the multiple steps, the epoxy monomer can be polymerized by using a plurality of masks according to the requirement, the concentration gradient and the ion concentration gradient of a multi-level polymer network are formed between different areas in the liquid crystal/epoxy liquid crystal polymer composite material layer by using the plurality of masks and continuous multi-step polymerization, and under the off state, each area of the film presents a consistent transparent state; when the film is electrified, the dynamic scattering of the high-molecular network density and ion concentration area is strong, and the light transmittance is low; the dynamic scattering of the areas with low polymer network density and ion concentration is weak, and the light transmittance is high; the area without a polymer network and ions (i.e. the area which is not polymerized all the time) is not scattered dynamically, and the transparent state consistent with the off state is maintained, so that the light transmittance of the optical film on the full-coverage electrode can be regulated and controlled in multiple stages;
(3) the optical film with the full-coverage electrode, which is provided by the invention, has the advantages that the light transmittance can be controlled in the areas in multiple stages, dyes or pigments can be added in the liquid crystal/epoxy liquid crystal polymer composite material layer, at the moment, the optical film with specific color can be prepared, each area of the optical film presents a light transmission state with specific color in an off state, one area maintains the light transmission state with specific color when the power is on, and other areas present scattering states with different degrees with specific color;
(4) according to the preparation method of the optical film with the full-coverage electrode and the regional multi-stage control of the light transmittance, disclosed by the invention, the regional etching or the electromagnetic sputtering and the coating of the conductive layer and the related circuit design preparation are not involved in the preparation process, so that the preparation flow of a liquid crystal device is greatly simplified, and the manufacturing cost of the liquid crystal device is reduced.
The preparation method is suitable for preparing the optical film with the light transmittance of the fully covered electrode capable of being controlled in the different areas and multiple levels, is simple, can achieve the different-area regulation and the multiple-level regulation of the light transmittance at the same time, can be widely used as an intelligent window in the fields of building glass, automobile glass and the like, and can also be used as a display device.
Drawings
FIG. 1 is a schematic diagram of the mask used in example 1;
FIG. 2 is a physical view of the optical film prepared in example 1;
FIG. 3 is a schematic diagram of the mask used in example 2;
FIG. 4 is a physical view of the optical film prepared in example 2;
FIG. 5 is a schematic view of a first mask used in example 3;
FIG. 6 is a schematic diagram of a second mask used in example 3;
FIG. 7 is a physical view of the optical film prepared in example 3;
FIG. 8 is a schematic view of a first mask used in example 4;
FIG. 9 is a schematic diagram of a second mask used in example 4;
FIG. 10 is a physical view of the optical film produced in example 4.
Detailed Description
The invention is further illustrated by the following examples. It should be understood that the described embodiments are only for explaining the present invention and do not limit the present invention.
Example 1 optical film with totally covered electrode and light transmittance capable of being controlled in two-region and two-stage manner, preparation method and performance detection
(one) preparing a sample:
s1, selecting a transparent substrate made of glass, and preparing a liquid crystal box formed by sequentially laminating a substrate layer, a conductive layer and a parallel orientation layer, wherein the distance between the liquid crystal boxes is 20 mu m; wherein the conductive layer is made of ITO material, and the parallel orientation layer is made of PVA material;
s2, uniformly mixing 4g of liquid crystal epoxy monomer E6M, 95.8g of negative liquid crystal HNG726200-100 and 0.2g of cationic photoinitiator UV 6976, filling into a liquid crystal box, placing a mask shown in figure 1 between the liquid crystal box and an ultraviolet light source after parallel orientation is formed (wherein a black area can not transmit 365nm ultraviolet light and a white area can transmit 365nm ultraviolet light), and then using 50mW/cm at 25 DEG C 2 The ultraviolet light of 365nm irradiates for 120min, so that E6M is subjected to ring-opening homopolymerization, and an optical film with the light transmittance capable of being controlled in two areas and two stages on a full-coverage electrode is prepared, and is marked as T1;
wherein, the molecular structure of the liquid crystal epoxy monomer E6M is as follows:
the molecular structure of the cationic photoinitiator UV 6976 is:
(II) performance detection:
as shown in fig. 2, when no electric field is applied, each part of the prepared optical film exhibits a light-transmitting state; when a square wave electric field of 80V and 100Hz is applied, the area which is not irradiated by ultraviolet light in the middle does not contain a polymer network and ions, so that dynamic scattering does not occur, a light transmission state is kept consistent with that when no electric field is applied, and the area which is irradiated by ultraviolet light in the periphery contains the polymer network and ions, so that dynamic scattering occurs under the electric field, a scattering state is presented, and the light transmittance is obviously reduced.
Example 2 optical film with four-region two-stage control of light transmittance on fully covered electrode, preparation method and performance detection
The preparation method comprises the following steps:
s1, selecting a transparent substrate made of glass, and preparing a liquid crystal box formed by sequentially laminating a substrate layer, a conductive layer and a parallel orientation layer, wherein the distance between the liquid crystal boxes is 20 mu m; wherein the conductive layer is made of ITO material, and the parallel orientation layer is made of PVA material;
s2, uniformly mixing 4g of liquid crystal epoxy monomer E6M, 95.8g of negative liquid crystal HNG726200-100 and 0.2g of cationic initiator UV 6976, filling into a liquid crystal box, placing a mask shown in figure 3 between the liquid crystal box and an ultraviolet light source after the parallel orientation is formed (wherein a black area can not transmit 365nm ultraviolet light and a white area can transmit 365nm ultraviolet light), and then using 50mW/cm at 25 DEG C 2 The ultraviolet light of 365nm irradiates for 120min, so that E6M is subjected to ring-opening homopolymerization, and an optical film with the light transmittance capable of being controlled in four areas in two stages on the full-coverage electrode is prepared, and is marked as T2.
(II) performance detection:
as shown in fig. 4, when no electric field is applied, each part of the prepared optical film exhibits a light-transmitting state; when a square wave electric field of 80V and 100Hz is applied, the middle three small rectangular areas irradiated by ultraviolet light contain polymer networks and ions, so that dynamic scattering occurs under the electric field, a scattering state is shown, the light transmittance is obviously reduced, and the rest areas not irradiated by the ultraviolet light do not contain the polymer networks and the ions, so that the dynamic scattering does not occur, the light transmission state is kept consistent with the situation when no electric field is applied.
Example 3 optical film with three-region three-level control of light transmittance on fully covered electrode, preparation method and performance detection
The preparation method comprises the following steps:
s1, selecting a transparent substrate made of glass, and preparing a liquid crystal box formed by sequentially laminating a substrate layer, a conductive layer and a parallel orientation layer, wherein the distance between the liquid crystal boxes is 20 mu m; wherein the conductive layer is made of ITO material, and the parallel orientation layer is made of PVA material;
s2, uniformly mixing 4g of liquid crystal epoxy monomer E6M, 95.8g of negative liquid crystal HNG726200-100 and 0.2g of cationic initiator UV 6976, and filling the mixture into a liquidA cell, after parallel alignment has been established, a first mask as shown in FIG. 5 (in which the black region is opaque to 365nm UV light and the white region is transparent to 365nm UV light) is placed between the cell and the UV light source, followed by a 50mW/cm exposure at 25deg.C 2 Irradiating the E6M for 120min by ultraviolet light at 365nm to enable ring-opening homopolymerization of the E6M to occur;
s3, replacing the first mask with a second mask as shown in FIG. 6 (wherein the black region is impermeable to 365nm ultraviolet light and the white region is permeable to 365nm ultraviolet light), and then using 50mW/cm at 25deg.C 2 The ultraviolet light of 365nm irradiates for 120min, so that E6M is subjected to ring-opening homopolymerization, and an optical film with three-region three-level control of light transmittance based on a fully covered electrode can be prepared, and is marked as T3.
(II) performance detection:
as shown in fig. 7, when no electric field is applied, each part of the prepared optical film assumes a light-transmitting state; when a square wave electric field of 80V and 100Hz is applied, the polymer network density and the ion concentration of the right small rectangular area are highest due to longer polymerization time, and the dynamic scattering is strongest, so that the light transmittance is lowest; the polymer network density and the ion concentration of the left small rectangular area are low due to the short polymerization time, the dynamic scattering is weak, and the light transmittance is low; the rest of the areas which are not subjected to ultraviolet polymerization do not contain polymer network and ions, so that dynamic scattering does not occur, and the same light transmission state is maintained as when no electric field is applied.
Example 4 optical film with three-region three-level control of light transmittance on fully covered electrode, preparation method and performance detection
The preparation method comprises the following steps:
s1, selecting a transparent substrate made of glass, and preparing a liquid crystal box formed by sequentially laminating a substrate layer, a conductive layer and a parallel orientation layer, wherein the distance between the liquid crystal boxes is 20 mu m; wherein the conductive layer is made of ITO material, and the parallel orientation layer is made of PVA material;
s2, uniformly mixing 4g of liquid crystal epoxy monomer E6M, 95.8g of negative liquid crystal HNG726200-100 and 0.2g of cationic initiator UV 6976, and filling into a liquid crystal box to form a parallel alignmentAfter this, a first mask as shown in FIG. 8 (in which the black region is opaque to 365nm UV light and the white region is transparent to 365nm UV light) was placed between the cell and the UV light source, followed by a 50mW/cm exposure at 25℃ 2 Irradiating the E6M for 120min by ultraviolet light at 365nm to enable ring-opening homopolymerization of the E6M to occur;
s3, replacing the first mask with a second mask as shown in FIG. 9, (wherein the black region can not transmit 365nm ultraviolet light and the white region can transmit 365nm ultraviolet light), and then using 50mW/cm at 25deg.C 2 The ultraviolet light of 365nm irradiates for 120min, so that E6M is subjected to ring-opening homopolymerization, and an optical film with three-region three-level control of light transmittance based on a fully covered electrode can be prepared, and is marked as T4.
(II) performance detection:
as shown in fig. 10, when no electric field is applied, each part of the prepared optical film assumes a light-transmitting state; when a square wave electric field of 80V and 100Hz is applied, the polymer network density and the ion concentration of the right small rectangular area are highest due to longer polymerization time, and the dynamic scattering is strongest, so that the light transmittance is lowest; the small rectangular area on the left side consumes epoxy monomer in the first polymerization, so that the concentration of polymerizable monomer is reduced, and therefore, the density and ion concentration of a polymer network formed in the small rectangular area are low in the second polymerization, the dynamic scattering is weak, and the light transmittance is low; the rest of the areas which are not subjected to ultraviolet polymerization do not contain polymer network and ions, so that dynamic scattering does not occur, and the same light transmission state is maintained as when no electric field is applied.
Example 5A green full-covered electrode optical film with light transmittance capable of being controlled in two regions and two stages, preparation method and performance detection
The preparation method comprises the following steps:
s1, selecting a transparent substrate made of glass, and preparing a liquid crystal box formed by sequentially laminating a substrate layer, a conductive layer and a parallel orientation layer, wherein the distance between the liquid crystal boxes is 20 mu m; wherein the conductive layer is made of ITO material, and the parallel orientation layer is made of PVA material;
s2, taking 4g of liquid crystal epoxy monomer E6M, 95.8g of negative liquid crystal HNG726200-100, 0.2g of cationic initiator UV 6976 and 0.5g of dye solvent green 28 are mixed uniformly and then poured into a liquid crystal box, after parallel orientation is formed, a mask as shown in figure 1 (wherein a black region can not transmit 365nm ultraviolet light and a white region can transmit 365nm ultraviolet light) is placed between the liquid crystal box and an ultraviolet light source, and then 50mW/cm of the mask is used at 25 DEG C 2 The ultraviolet light of 365nm irradiates for 120min, so that E6M is subjected to ring-opening homopolymerization, and the green optical film with the light transmittance capable of being controlled in four areas and two stages based on the full-coverage electrode is prepared, and is marked as T5.
(II) performance detection:
when no electric field is applied, all parts of the prepared optical film are in a green light transmission state; when a square wave electric field of 80V and 100Hz is applied, the area which is not irradiated by ultraviolet light in the middle does not contain a polymer network and ions, so that dynamic scattering does not occur, a green light transmission state is kept consistent with that when no electric field is applied, and the area which is irradiated by ultraviolet light in the periphery contains a polymer network and ions, so that dynamic scattering occurs under the electric field, a green scattering state is presented, and the light transmittance is obviously reduced.
Examples 6 to 12 optical thin film with double-region two-stage control of light transmittance on full-coverage electrode
Examples 6 to 12 prepared several optical films with totally covered electrodes and light transmittance capable of being controlled in two areas and two stages, and the preparation method is basically the same as example 1, except that the raw materials and part of the process parameters are different, and the specific details are shown in the following table:
table 1 liquid crystalline epoxy monomer structures and marking codes in examples 6 to 12
Table 2 negative liquid Crystal Structure and marking code in examples 6 to 12
TABLE 3 raw materials and part of process parameters in examples 6-12
Through detection, the optical films T6-T12 with the light transmittance being controlled in two areas and two stages on the full-coverage electrode show a light transmission state when no electric field is applied; when a square wave electric field of 80V and 100Hz is applied, the area which is not irradiated by ultraviolet light in the middle does not contain polymer network and ions, so that dynamic scattering does not occur, a light transmission state is kept consistent with that when no electric field is applied, the area which is irradiated by ultraviolet light in the periphery contains polymer network and ions, thus the dynamic scattering occurs under the electric field, a scattering state is displayed, the light transmittance is obviously reduced, and the light transmission states and the scattering states of T7, T10, T11 and T12 display corresponding colors due to the addition of pigment or dye.
According to the knowledge of the person skilled in the art, when the optical film is made of a flexible material substrate such as polyester resin or polycarbonate, a roll-to-roll (roll-to-roll) processing technology can be adopted as required.
Claims (7)
1. The optical film is characterized in that the liquid crystal/epoxy liquid crystal polymer composite material layer is laminated between the first parallel orientation layer and the second parallel orientation layer and is integrated with the first composite layer structure and the second composite layer structure, and the liquid crystal/epoxy liquid crystal polymer composite material layer is composed of an epoxy liquid crystal polymer network, ions and negative liquid crystal;
the liquid crystal/epoxy liquid crystal polymer composite material layer can be divided into a light transmission area and a scattering area with different dynamic scattering degrees, and the shape, the size, the position and the number of each area can be designed and customized according to requirements;
the epoxy liquid crystal polymer network and the negative liquid crystal forming the liquid crystal/epoxy liquid crystal polymer composite material layer are aligned in parallel; the content of the epoxy liquid crystal polymer network and the content of ions form concentration gradients between different areas in the layer, and the gradient directions of the epoxy liquid crystal polymer network and the ion form a consistent gradient;
the liquid crystal/epoxy liquid crystal polymer composite material comprises the following raw materials in percentage by weight of 0.01-40: 40-99.9: 0.01-10 parts of liquid crystal epoxy monomer, negative liquid crystal and cationic photoinitiator;
the liquid crystal epoxy monomer is at least one of the following compounds I and II:
（I）
（II）
wherein A is 1 、A 2 、G 1 And G 2 Are all one of C1-C16 alkyl, C1-C16 alkoxy and C1-C16 siloxane groups;
J 1 、J 2 、L 1 、L 2 、M 1 and M 2 Are aromatic or aliphatic rings;
x 1 、x 2 、y 1 、y 2 、z 1 and z 2 Are all integers of 0 to 4;
Q 1 、Q 2 、R 1 、R 2 、T 1 and T 2 All are halogen, cyano, methyl or methoxy;
k 1 、k 2 、m 1 、m 2 、n 1 and n 2 Are all integers of 0 to 4;
D 1 、D 2 、E 1 and E is 2 All are ester groups, alkynyl groups, methylene groups, nitrogen-nitrogen double bonds, ether bonds or direct connection;
the negative liquid crystal is at least one of the following compounds:
wherein A is 3 And G 3 Are all one of C1-C16 alkyl, C1-C16 alkoxy and C1-C16 siloxane groups;
J 3 、L 3 and M 3 Are aromatic or aliphatic rings;
x 3 、y 3 and z 3 Are all integers of 0 to 4;
Q 3 、R 3 and T 3 All are halogen, cyano, methyl or methoxy;
k 3 、m 3 、n 3 are all integers of 0 to 4;
D 3 and E is 3 All are ester groups, alkynyl groups, methylene groups, nitrogen-nitrogen double bonds, ether bonds or direct connection;
the cationic photoinitiator is diazonium salt,。
2. The optical film with the full-coverage electrode, which has the light transmittance capable of being controlled in the multiple stages in the area, according to claim 1, wherein the substrate layer is composed of a transparent substrate made of glass, polyester resin or polycarbonate;
the conductive layer is made of ITO or conductive high polymer material;
the parallel alignment layer is made of PVA or PI.
3. The optical film with the light transmittance capable of being controlled in multiple stages in a zoned manner on the fully covered electrode according to claim 2, wherein the thickness of the liquid crystal/epoxy liquid crystal polymer composite layer is 0.5-100 μm.
4. The optical film with the full-coverage electrode, which can be controlled in a zoned and multistage mode, is characterized in that the liquid crystal/epoxy liquid crystal polymer composite material layer further comprises dye or pigment, and the weight portion of the dye or pigment is 0.01% -10%.
5. The method for preparing an optical film with a light transmittance of a fully covered electrode capable of being controlled in multiple areas according to any one of claims 1 to 4, wherein when the dynamic scattering progression of the film is n, the method comprises the following steps in sequence:
s1, uniformly mixing raw materials of a liquid crystal/epoxy liquid crystal polymer composite material, and adding the raw materials between a first parallel orientation layer and a second parallel orientation layer;
s2, continuously polymerizing the film for n-1 times, placing a mask between the substrate layer and the light source during each polymerization, and performing epoxy photoinitiated ring-opening polymerization for 0.01-10 hours to complete the polymerization, wherein the optical film with the light transmittance capable of being controlled in multiple stages and in different areas on the full-coverage electrode can be prepared after the polymerization for n-1 times is completed.
6. The method for preparing the optical film with the light transmittance capable of being controlled in the multiple stages in the divided areas on the fully covered electrode according to claim 5, wherein the mask is divided into two areas which are opaque and transparent, and the shape, the size, the position and the number of the two areas can be designed and customized according to the requirements;
starting from the second polymerization, the light-transmitting areas of the mask used in the preparation process cover the light-transmitting areas of the mask in the previous step; alternatively, the light-transmitting areas of the masks used in the preparation process are not coincident.
7. The method for preparing the optical film with the full-coverage electrode and the regional multi-stage controllable light transmittance is characterized in that the temperature of the epoxy photoinitiated ring-opening polymerization is-20-120 ℃.
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| CN106094338A (en) * | 2016-08-11 | 2016-11-09 | 京东方科技集团股份有限公司 | A kind of double-side display device and electronic equipment |
| CN113272726A (en) * | 2019-10-24 | 2021-08-17 | 京东方科技集团股份有限公司 | Display panel, display device and display panel manufacturing method |
| CN113917729A (en) * | 2021-10-21 | 2022-01-11 | 北京大学 | Trans-form dimming glass based on electric response and preparation method thereof |
| CN114002867A (en) * | 2021-10-08 | 2022-02-01 | 北京大学 | Trans-mode light adjusting film based on liquid crystal epoxy photoinitiated ring-opening polymerization and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106094338A (en) * | 2016-08-11 | 2016-11-09 | 京东方科技集团股份有限公司 | A kind of double-side display device and electronic equipment |
| CN113272726A (en) * | 2019-10-24 | 2021-08-17 | 京东方科技集团股份有限公司 | Display panel, display device and display panel manufacturing method |
| CN114002867A (en) * | 2021-10-08 | 2022-02-01 | 北京大学 | Trans-mode light adjusting film based on liquid crystal epoxy photoinitiated ring-opening polymerization and preparation method thereof |
| CN113917729A (en) * | 2021-10-21 | 2022-01-11 | 北京大学 | Trans-form dimming glass based on electric response and preparation method thereof |
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