CN106707593B - A kind of polymer dispersion bistable state smectic C liquid crystal film and preparation method thereof - Google Patents
A kind of polymer dispersion bistable state smectic C liquid crystal film and preparation method thereof Download PDFInfo
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- CN106707593B CN106707593B CN201510792210.3A CN201510792210A CN106707593B CN 106707593 B CN106707593 B CN 106707593B CN 201510792210 A CN201510792210 A CN 201510792210A CN 106707593 B CN106707593 B CN 106707593B
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1334—Constructional arrangements; Manufacturing methods based on polymer dispersed liquid crystals, e.g. microencapsulated liquid crystals
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
- C09K19/52—Liquid crystal materials characterised by components which are not liquid crystals, e.g. additives with special physical aspect: solvents, solid particles
- C09K19/54—Additives having no specific mesophase characterised by their chemical composition
- C09K19/542—Macromolecular compounds
- C09K19/544—Macromolecular compounds as dispersing or encapsulating medium around the liquid crystal
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Abstract
The invention discloses a kind of polymer dispersion bistable state smectic C liquid crystal films and preparation method thereof, it the described method comprises the following steps: smectic C liquid crystal that ultraviolet light polymerisable monomer, dielectric anisotropy are positive, ionic liquid, photoinitiator, glass microballoon being mixed according to the ratio and is placed on two panels and is coated between indium tin oxide films, it is squeezed into film, ultraviolet light polymerize to obtain polymer dispersion bistable state smectic C liquid crystal film.The film of this method preparation is provided simultaneously with that excellent in stability, response modes are simple, the higher advantage of contrast, is a kind of good energy conservation and environmental protection material, build and automobile door and window, flexible electronic paper in terms of have broad application prospects.
Description
Technical field
The invention belongs to liquid crystal applications technical fields, and specifically, the present invention provides a kind of polymer dispersion bistable state is close
Brilliant A phase liquid crystal film and preparation method thereof, the thin-film material of preparation can be widely used for the fields such as building pad pasting.
Background technique
Polymer dispersed liquid crystals (PDLC) material, is the composite material of a kind of polymer and liquid crystal, a variety of function may be implemented
Energy, application value are high.PDLC thin-film material on the market at present, it is general there are two types of state, scattering states with penetrate state, both
In state, usually there is the state that one is normalities, i.e., maintain without power-up, and another kind is switched on state, i.e., need to continue to be powered on to come
It maintains.For the PDLC film of usual positivity liquid crystal in the case where applying voltage, dispersing liquid crystal droplet in a polymer matrix can field therewith
Orientation is caused, field causes refractive index and polymeric matrix index matching under alignment state, then shows a kind of state that light penetrates, otherwise
State of orientation is caused in no electric field, liquid-crystal refractive-index and polymeric matrix refractive index mismatch, and light scattering states are presented.Prepare PDLC
Mode have Polymerizing phase splitting method, temperature split-phase method, solution split-phase method etc., wherein ultraviolet polymerization causes the split-phase method for preparing PDLC
It is the most commonly used in the application of market.As can be seen that PDLC film on the market has a state that lasting power-up is needed to maintain at present,
Meanwhile the liquid crystal in PDLC material in the market, logical the most commonly used is the nematic liquid crystals that dielectric anisotropy is positive, for SmA
The PDLC product of phase liquid crystal yet there are no.
Bi-stable type liquid crystal material, there are two types of normalities, i.e., there are two types of without being powered on the state maintained, this is for realizing energy conservation
Environment protection significance is great.Smectic A (SmA) phase liquid crystal has the property for preparing bistable liquid crystal film.SmA phase liquid crystal material is realized double
The principle of steady-state performance are as follows: under a certain size high frequency voltage effect, ionic liquid cannot be moved further along direction of an electric field,
But concussion in situ occurs, therefore SmA phase liquid crystal molecule will not be disturbed, prolong direction of an electric field arrangement because being positive dielectric properties,
The final light that presents penetrates state;Under the voltage effect of a certain size low frequency, ionic liquid is moved along direction of an electric field, is moved through
Cheng Zhongyu liquid crystal molecule collides, and generates upset effect, shows the scattering state of light.Again since SmA phase liquid crystal itself glues
Larger, state of the meeting when maintain application voltage after cancelling voltage is spent, therefore realizes bistable state.Above-mentioned SmA phase liquid crystal material
The principle that scattering states can be presented is commonly referred to as dynamic scattering, and this dynamic scattering effect is commonly done in negativity nematic phase liquid
In brilliant material, and at present without this phenomenon in positivity Nematic phase liquid crystal material.Yet there are no currently on the market will be provided with bistability
In a polymer matrix, the bistable state PDLC thin-film material having is made in the SmA phase liquid crystal material dispersion of energy.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of polymer dispersion bistable state smectic C liquid crystal film, should
The film of method preparation is provided simultaneously with that excellent in stability, response modes are simple, the higher advantage of contrast, is a kind of good section
Energy environment-friendly materials, have broad application prospects in terms of building with automobile door and window, flexible electronic paper.
In order to achieve the above objectives, present invention employs the following technical solutions:
A kind of preparation method of polymer dispersion bistable state smectic C liquid crystal film, the described method comprises the following steps:
Smectic C liquid crystal, ionic liquid, photoinitiator, the glass that ultraviolet light polymerisable monomer, dielectric anisotropy are positive
Glass microballon mixes according to the ratio to be placed on two panels and is coated between indium tin oxide films, is squeezed into film, ultraviolet light polymerize to obtain
Polymer disperses bistable state smectic C liquid crystal film.
Further, ultraviolet light polymerisable monomer mass ratio is 10%-50%, the smectic C that dielectric anisotropy is positive
Liquid crystal mass ratio is 50%-90%;
Ionic liquid additive amount is ultraviolet light polymerisable monomer and the smectic C liquid crystal gross mass that dielectric anisotropy is positive
0.05%-5%, the additive amount of photoinitiator is ultraviolet light polymerisable monomer and the smectic C liquid that dielectric anisotropy is positive
The 0.1%-10% of brilliant gross mass, the additive amount of glass microballoon are positive for ultraviolet light polymerisable monomer with dielectric anisotropy close
The 0.1%-10% of brilliant A phase liquid crystal gross mass.
In the above method, be squeezed into film with a thickness of 0.5-40 μm.
Ultraviolet light, ultraviolet light intensity 1-20mw/cm are carried out at 0 DEG C -100 DEG C2, irradiation time is 1-30 minutes.
Preferably, the ultraviolet polymerisable monomer includes the ultraviolet polymerisable monomer of unsaturated polyester (UP) class, epoxy acrylate
The ultraviolet polymerisable monomer of class, the ultraviolet polymerisable monomer of polyurethane acrylates, the ultraviolet polymerisable monomer of polyester acrylates,
The ultraviolet polymerisable monomer of Epoxy Acrylates, the ultraviolet polymerisable monomer of polyenoid thiol, polyoxyalkylene acrylate esters are ultraviolet can
One of polymerized monomer, the ultraviolet polymerisable monomer of water soluble acrylic acid esters, the ultraviolet polymerisable monomer of vinyl ethers are a variety of.
It is highly preferred that the esters of acrylic acid ultraviolet light polymerisable monomer is acrylic acid -3,5, the own ester of 5- trimethyl, methyl
One of the different ice ester of acrylic acid, polyethyleneglycol diacrylate 600 are a variety of.
Preferably, the photoinitiator is selected from one or more of following compounds: benzophenone, benzoin dimethylether
(Irgacure 651), 2- chloro thioxanthone (CTX), 2,4- diethyl thioxanthone (DETX), isopropyl thioxanthone
(ITX), 2- hydroxyl-2,2- methyl-1-phenylacetone (UV1173), 1- hydroxy cyclohexyl phenylketone (UV184), 2- methyl-1-
[4- (methyl mercapto) phenyl] -2- morpholinyl -1- acetone (907), 2- phenyl -2-N- dimethylamino -1- (4- morpholinyl phenyl)-butanone
(369), 2,4,6- trimethylbenzoy-dipheny phosphine oxides (TPO).
Preferably, the smectic C liquid crystal that dielectric anisotropy is positive is the smectic A that biphenyl cyanogen class dielectric anisotropy is positive
The smectic C liquid crystal that phase liquid crystal or type siloxane dielectric anisotropy are positive.
It is highly preferred that the smectic C liquid crystal that is positive of biphenyl cyanogen class dielectric anisotropy is 8CB, 10CB, 12CB, wherein
The mass ratio of 8CB:10CB:12CB is 49:21:30.
The present invention also provides gather prepared by the preparation method of above-mentioned polymer dispersion bistable state smectic C liquid crystal film
It closes object and disperses bistable state smectic C liquid crystal film.
The present invention obtains the film for having bistable behaviour using the method for polymer dispersion SmA phase liquid crystal.Bistable state refers to
Two kinds of transparent state, scattering states stable states can be kept under null field.Two kinds of stable states are switched over by applying disposable voltage, i.e., when pair
When film applies high-frequency electric field, liquid crystal molecule becomes vertically oriented molecules align state from conical texture, and film is scattered from light
State becomes pellucidity, and after electric field is closed, which, which can stablize, remains behind (10 days or more);Apply when to film
When low frequency electric field, liquid crystal molecule becomes the molecules align state of conical texture from vertical orientation, and film becomes light from pellucidity
Scattering state, after electric field is closed, which, which can stablize, remains behind (10 days or more).
Smectic C liquid crystal in the present invention is nCB, chemical structure such as following formula:
Wherein, n=8,10,12;
Ultraviolet polymerisable monomer chemical structure in the present invention is shown below:
The own ester of acrylic acid -3,5,5- trimethyl (TMHA):
The different ice ester (IBMA) of methacrylic acid:
Polyethyleneglycol diacrylate 600 (PEGDA600):n≈14。
Ionic liquid in the present invention is cetyl -3- methylimidazole bromide:
Photoinitiator in the present invention: benzoin dimethylether (Irgacure 651):
It is wound, the mobile destruction of ion in the present invention since SmA phase viscosity is larger, molecular end chain is longer
The orientation of liquid crystal molecule, causes the positivity SmA phase dynamic scattering can occur.
Detailed description of the invention
Fig. 1 and Fig. 2 is the electro-optical curve figure of polymer dispersion bistable state SmA phase liquid crystal film prepared by embodiment 1;
Fig. 3 is the scanning electron microscope (SEM) photograph of polymer dispersion bistable state SmA phase liquid crystal film prepared by embodiment 1;
Fig. 4 and Fig. 5 is the electro-optical curve figure of polymer dispersion bistable state SmA phase liquid crystal film prepared by embodiment 2;
Fig. 6 and Fig. 7 is the electro-optical curve figure of polymer dispersion bistable state SmA phase liquid crystal film prepared by embodiment 3.
Specific embodiment
With the drawings and specific embodiments, the present invention is described in further detail below.
Embodiment 1
According to sample ratio sample in table 1, limpid, taking-up mixing is heated in 80 DEG C of baking ovens, instillation two panels plating is aerobic
Change between indium tin thin film, roller bearing is pressed into 40 μm of film.It is 3.0mW/cm in ultraviolet light (365nm) intensity2It is irradiated under light intensity
10 minutes, temperature was 30 DEG C.It obtains sample and carries out electro-optical properties test, test method is to utilize ultraviolet-visible-near-infrared point
Light photometer, tests the light transmission rate of sample under 632nm wavelength, and reference is empty liquid crystal cell.It is through state test transmitance method,
Successively apply 5KHz, 20V to 160V voltage by step-length of 20V, is both needed to apply 0.01Hz every time after test, 160V voltage keeps its extensive
It is again scattering states;It is successively to apply 0.01Hz, 20V to 160V voltage by step-length of 20V, often that scattering states, which test transmitance method,
Apply 5KHz after secondary test, 160V voltage makes it revert to transparent state.It is as depicted in figs. 1 and 2 to obtain electro-optical curve figure, from figure
1 and Fig. 2, which can be seen that sample transmitance, can occur transformation between transparent state and scattering states by applying voltage, realize
Bistable behaviour.It was the steady-state performance of period measuring sample with 30 days, 30 can be kept by obtaining the bistable two kinds of stable states of sample
It.Sample after test is placed in cyclohexane solvent, after bubble removes liquid crystal, gained network sample scanning electron microscopic observation, such as Fig. 3,
From figure 3, it can be seen that foring the polymer scatternet that can play the role of mechanically stable liquid crystal in sample.
Sample ratio in 1 embodiment 1 of table
Embodiment 2
According to sample ratio sample in table 2, limpid, taking-up mixing is heated in 80 DEG C of baking ovens, instillation two panels plating is aerobic
Change between indium tin thin film, roller bearing is pressed into 20 μm of film.It is 20mW/cm in ultraviolet light (365nm) intensity21 is irradiated under light intensity
Minute, temperature is 100 DEG C.It obtains sample and carries out electro-optical properties test, test method is to be divided using ultraviolet-visible-near-infrared
Photometer, tests the light transmission rate of sample under 632nm wavelength, and reference is empty liquid crystal cell.It is through state test transmitance method, with
20V is that step-length successively applies 5KHz, 20V to 160V voltage, is both needed to apply 0.01Hz every time after test, 160V voltage makes its recovery
For scattering states;It is successively to apply 0.01Hz, 20V to 160V voltage by step-length of 20V, every time that scattering states, which test transmitance method,
Apply 5KHz after test, 160V voltage makes it revert to transparent state.It is as shown in Figure 4 and Figure 5 to obtain electro-optical curve figure, from Fig. 4
And Fig. 5, as can be seen that by applying voltage the transformation between transparent state and scattering states can occur for sample transmitance, realization is double
Steady-state performance.And with 30 days steady-state performances for period measuring sample, 30 can be kept by obtaining the bistable two kinds of stable states of sample
It.
Sample ratio in 2 embodiment 2 of table
Embodiment 3
According to sample ratio sample in table 3, limpid, taking-up mixing is heated in 80 DEG C of baking ovens, instillation two panels plating is aerobic
Change between indium tin thin film, roller bearing is pressed into 0.5 μm of film.It is 1mW/cm in ultraviolet light (365nm) intensity230 are irradiated under light intensity
Minute, temperature is 0 DEG C.It obtains sample and carries out electro-optical properties test, test method is to be divided light using ultraviolet-visible-near-infrared
Degree meter, tests the light transmission rate of sample under 632nm wavelength, and reference is empty liquid crystal cell.It is through state test transmitance method, with
20V is that step-length successively applies 5KHz, 20V to 160V voltage, and being both needed to application 0.01Hz, 160V voltage after test every time makes its recovery
For scattering states;It is successively to apply 0.01Hz, 20V to 160V voltage by step-length of 20V, every time that scattering states, which test transmitance method,
Applying 5KHz, 160V voltage after test makes it revert to transparent state.It is as shown in Figure 6 and Figure 7 to obtain electro-optical curve figure, from Fig. 6
And Fig. 7, as can be seen that by applying voltage the transformation between transparent state and scattering states can occur for sample transmitance, realization is double
Steady-state performance.And with 30 days steady-state performances for period measuring sample, 30 can be kept by obtaining the bistable two kinds of stable states of sample
It.
Sample ratio in 3 embodiment 3 of table
It should be noted last that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting.Although ginseng
It is described the invention in detail according to embodiment, it will be apparent to an ordinarily skilled person in the art that technical side of the invention
Case is modified or replaced equivalently, and without departure from the spirit and scope of technical solution of the present invention, should all be covered in the present invention
Scope of the claims in.
Claims (8)
1. a kind of preparation method of polymer dispersion bistable state smectic C liquid crystal film, the described method comprises the following steps:
Smectic C liquid crystal, ionic liquid, photoinitiator, the glass that ultraviolet light polymerisable monomer, dielectric anisotropy are positive are micro-
Pearl mixes according to the ratio to be placed on two panels and is coated between the film of tin indium oxide, is squeezed into film, ultraviolet light, which polymerize, is gathered
It closes object and disperses bistable state smectic C liquid crystal film;
Ultraviolet light polymerisable monomer mass ratio is 10%-50%, and the smectic C liquid crystal mass ratio that dielectric anisotropy is positive is
50%-90%;
Ionic liquid additive amount is ultraviolet light polymerisable monomer and the smectic C liquid crystal gross mass that dielectric anisotropy is positive
0.05%-5%, the additive amount of photoinitiator are ultraviolet light polymerisable monomer and the smectic C liquid crystal that dielectric anisotropy is positive
The 0.1%-10% of gross mass, the additive amount of glass microballoon are ultraviolet light polymerisable monomer and the smectic that dielectric anisotropy is positive
The 0.1%-10% of A phase liquid crystal gross mass.
2. the preparation method of polymer dispersion bistable state smectic C liquid crystal film according to claim 1, feature exist
In, be squeezed into film with a thickness of 0.5-40 μm.
3. the preparation method of polymer dispersion bistable state smectic C liquid crystal film according to claim 1, feature exist
In carrying out ultraviolet light, ultraviolet light intensity 1-20mw/cm at 0 DEG C -100 DEG C2, irradiation time is 1-30 minutes.
4. the preparation method of polymer dispersion bistable state smectic C liquid crystal film according to claim 1, feature exist
It include that the ultraviolet polymerisable monomer of unsaturated polyester (UP) class, Epoxy Acrylates are ultraviolet polymerizable in, the ultraviolet polymerisable monomer
The ultraviolet polymerisable monomer of monomer, polyurethane acrylates, the ultraviolet polymerisable monomer of polyester acrylates, polyenoid thiol
Ultraviolet polymerisable monomer, the ultraviolet polymerisable monomer of polyoxyalkylene acrylate esters, the ultraviolet polymerisable monomer of water soluble acrylic acid esters, ethylene
One of ultraviolet polymerisable monomer of base ethers is a variety of.
5. the preparation method of polymer dispersion bistable state smectic C liquid crystal film according to claim 1, feature exist
In the ultraviolet light polymerisable monomer is acrylic acid -3,5, the different ice ester of the own ester of 5- trimethyl, methacrylic acid, polyethylene glycol two
One of acrylate 600 is a variety of.
6. the preparation method of polymer dispersion bistable state smectic C liquid crystal film according to claim 1, feature exist
In the smectic C liquid crystal that dielectric anisotropy is positive is the smectic C liquid crystal or silicon oxygen that biphenyl cyanogen class dielectric anisotropy is positive
The smectic C liquid crystal that alkanes dielectric anisotropy is positive.
7. the preparation method of polymer dispersion bistable state smectic C liquid crystal film according to claim 6, feature exist
In, the smectic C liquid crystal that biphenyl cyanogen class dielectric anisotropy is positive be 8CB, 10CB, 12CB, the wherein matter of 8CB:10CB:12CB
Amount is than being 49:21:30.
8. prepared by the preparation method of any one of the claim 1-7 polymer dispersion bistable state smectic C liquid crystal film
Polymer disperses bistable state smectic C liquid crystal film.
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CN110862829B (en) * | 2019-11-19 | 2021-11-05 | 北京大学 | Low-driving-voltage liquid crystal composition for PDLC (polymer dispersed liquid crystal) and preparation method thereof |
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CN114889276B (en) * | 2022-04-24 | 2023-02-24 | 东华大学 | Flexible bistable film mechanism based on photoresponse and preparation method and application thereof |
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CN101542373A (en) * | 2006-11-24 | 2009-09-23 | 大日本印刷株式会社 | Liquid crystal display element |
CN102585168B (en) * | 2012-03-07 | 2014-01-01 | 北京科技大学 | Preparation method of polymer dispersed liquid crystal film |
CN104570434A (en) * | 2013-10-23 | 2015-04-29 | 久正光电股份有限公司 | Double-frequency bi-stable liquid crystal display and double-frequency bi-stable liquid crystal composition |
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CN101542373A (en) * | 2006-11-24 | 2009-09-23 | 大日本印刷株式会社 | Liquid crystal display element |
CN102585168B (en) * | 2012-03-07 | 2014-01-01 | 北京科技大学 | Preparation method of polymer dispersed liquid crystal film |
CN104570434A (en) * | 2013-10-23 | 2015-04-29 | 久正光电股份有限公司 | Double-frequency bi-stable liquid crystal display and double-frequency bi-stable liquid crystal composition |
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