CN109856886A - A kind of flexibility holographic polymer dispersed liquid crystal grating and preparation method thereof - Google Patents
A kind of flexibility holographic polymer dispersed liquid crystal grating and preparation method thereof Download PDFInfo
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- CN109856886A CN109856886A CN201910245953.7A CN201910245953A CN109856886A CN 109856886 A CN109856886 A CN 109856886A CN 201910245953 A CN201910245953 A CN 201910245953A CN 109856886 A CN109856886 A CN 109856886A
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Abstract
The invention discloses a kind of flexible holographic polymer dispersed liquid crystal gratings and preparation method thereof, comprising the following steps: (1) is uniformly mixed acrylate monomer, photoinitiator, plasticizer and liquid crystal, obtains dispersed liquid crystal liquid；(2) introns are dispersed in two panels flexible substrates, then two panels flexible substrates is stacked, with solidification adhesive edge, liquid crystal cell is made；(3) the dispersed liquid crystal liquid is injected in the liquid crystal cell, liquid crystal cell is exposed using two beam coherent lasers, form interference figure, solidification obtains flexible holographic polymer dispersed liquid crystal grating after.The bent deformation of flexibility holographic polymer dispersed liquid crystal grating can be applied to 3D body and show and wearable display equipment.
Description
Technical field
The present invention relates to functional composite material application field more particularly to a kind of flexible holographic polymer dispersed liquid crystal gratings
And preparation method thereof.
Background technique
Currently, liquid crystal material has been widely applied in conventional display device field, with the development of science and technology and people
Improvement of living standard, 3D body is shown and the wearable popular direction shown as display device.
Holographic polymer dispersed liquid crystal (HPDLC) grating has high efficiency, changeable, excellent processing performance and optics special
Property, it is widely used in 3D display, biosensor, data storage and safe-guarding and anti-counterfeiting grade height Environment Science field.
By control polymerization reaction and preferred liquid crystal material, the holographic polymerization of high-diffraction efficiency and fast-response time can get
Object dispersed LCD grating.For example, the Chinese patent literature of Publication No. CN106950744A discloses a kind of holographic polymer point
Liquid crystal grating is dissipated, is obtained after holographic recording is handled by the mixture including compounding liquid crystal and photopolymerizable monomer
's；Compounding liquid crystal includes first kind liquid-crystal compounds and the second class liquid-crystal compounds；Wherein, first kind liquid-crystal compounds is
Biphenyl cyanogen class liquid-crystal compounds；It compounds in liquid crystal, the mass ratio of both first kind liquid-crystal compounds and second class liquid-crystal compounds
It is 3/26~15/10；The mass ratio for compounding both liquid crystal and photopolymerizable monomer is 25/50~50/30.By to crucial holographic
Structure, composition and the corresponding preparation method of polymer dispersed liquid crystals grating improve, and provide a kind of holographic polymerization of improvement
The new way that object dispersed LCD diffraction efficiency of grating and driving voltage require.Also have document (J.Am.Chem.Soc., 2014,
136,8855-8858.) the holographic polymer dispersed liquid crystal light that similar approach obtains high-diffraction efficiency and fast-response time is disclosed
Grid.
But these gratings are all based on made of the hard substrate fabrication such as glass, 3D body show and wearable display in
Application scenarios are limited to.Such as curved-surface display --- according to the liquid crystal cell of bend glass preparation, laser can not pass through holography
Expose the uniform grating of manufacturing cycle.
Summary of the invention
The present invention provides a kind of flexible holographic polymer dispersed liquid crystal grating and preparation method thereof, the holographic polymerizations of the flexibility
The bent deformation of object dispersed LCD grating can be applied to 3D body and show and wearable display equipment.
Specific technical solution is as follows:
A kind of preparation method of flexibility holographic polymer dispersed liquid crystal grating, comprising the following steps:
(1) acrylate monomer, photoinitiator, plasticizer and liquid crystal are uniformly mixed, obtain dispersed liquid crystal liquid；
(2) introns are dispersed in two panels flexible substrates, then two panels flexible substrates is stacked, sealed with solidification glue
Liquid crystal cell is made in side；
(3) the dispersed liquid crystal liquid is injected in the liquid crystal cell, liquid crystal cell is exposed using two beam coherent lasers
Light forms interference figure, and solidification obtains flexible holographic polymer dispersed liquid crystal grating after.
The degree of functionality of the acrylate monomer is 3~8.Grating diffration effect can be improved using high functionality monomer
Rate.
It is further preferred that the acrylate monomer is pentaerythritol triacrylate (PETA), pentaerythrite four
Acrylate (PETTA), dipentaerythritol be amyl-/hex- acrylic acid (DPHA) and the hyperbranched monomer ETERCURE of eight degrees of functionality
At least one of 6361-100.
Wherein, the manufacturer of the hyperbranched monomer ETERCURE 6361-100 of eight degrees of functionality is Changxing material supplier
Industry limited liability company, product grade are ETERCURE 6361-100.
The selection of photoinitiator directly affects the performance of HPDLC, it is preferred that the photoinitiator is Irgacure
784, the red Y of Bengal rose red, potato, methylene blue, rhodamine 6G, diiodofluorescein, michaelis ketone or 3, the bis- (7- bis- of 3 '-carbonyls
Ethylaminocoumarin).
The efficiency of initiation of above-mentioned photoinitiator is higher；And can by visible light-initiated, due to it is visible light-initiated when it is required
Exposure sources it is simple, cost of manufacture is lower；In addition, expose cause after, above-mentioned photoinitiator can by ultraviolet light or
Radiation of visible light bleaching, makes finally obtained grating transmitance higher.
Preferably, the photoinitiator is Irgacure 784, Bengal rose red, the red Y of potato, methylene blue, Luo Dan
Bright 6G or diiodofluorescein.
When using above-mentioned photoinitiator, the laser that 532nm can be used is exposed initiation, again through ultraviolet and can after exposure
After light-exposed bleaching, obtained grating transmitance and absolute diffraction efficiency is all higher.
Most preferably, the photoinitiator is diiodofluorescein.After being exposed using the laser of 532nm, then through purple
After outer and visible photobleaching, obtained grating transmitance is up to 95%, and absolute diffraction efficiency is up to 85%.
Preferably, the photoinitiator is michaelis ketone or 3, and 3 '-carbonyls are bis- (7- lignocaine cumarin).
When using above-mentioned photoinitiator, the laser that 460nm can be used is exposed initiation, again through ultraviolet and can after exposure
After light-exposed bleaching, obtained grating transmitance and absolute diffraction efficiency is all higher.After being exposed using the laser of 460nm, then
After Uv and visible light is bleached, obtained grating transmitance is up to 90%, and absolute diffraction efficiency is up to 80%.
The plasticizer be n-vinyl pyrrolidone, dibutyl phthalate, dicyclohexyl phthalate and
At least one of diisobutyl phthalate.
The liquid crystal is E7.
Preferably, it in the dispersed liquid crystal liquid, is calculated in mass percent, includes:
Based on above-mentioned dispersed liquid crystal liquid, in step (3), liquid crystal cell is exposed using visible light lasers, forms interference
Pattern is solidified after being carried out again using ultraviolet or visible light later.
Visible light lasers by polarisation, expand after using spectroscope, obtain two beam coherent lights, two beam coherent lights are in liquid crystal
Box surface forms light and dark striped.Acrylate monomer is initiated polymerization in clear zone and forms polymer, and liquid crystal is then converged
Gather in dark space, since polymer and liquid-crystal refractive-index have differences and forms grating.Later, it is carried out by ultraviolet or visible light
After solidify, photoinitiator therein is bleached, the transmitance of the grating made is higher.
Further, the wavelength of the visible light lasers is 450~550nm, and exposure light intensity is 1~15mW/cm2。
The material of the flexible substrates is polyethylene terephthalate (PET) or polyethylene naphthalate
(PEN)。
Further, the flexible substrates surface is coated with tin indium oxide (ITO) or fluorine-doped tin dioxide (FTO) is conductive
Layer.
Using flexibility holographic polymer dispersed liquid crystal grating made from conductive flexible substrate, liquid crystal is driven by electric field after power-up
Dynamic, liquid-crystal refractive-index reduces, at this time the refractive index close of polymer and liquid crystal, even disappears so that optical grating diffraction weakens, so
Its light can be adjusted by powered or non-powered using flexibility holographic polymer dispersed liquid crystal grating made from conductive flexible substrate
Grid diffraction situation.
Flexible holographic polymer dispersed liquid crystal grating is sandwich structure: upper layer and lower layer flexible substrates pass through intermediate interval
Son separates, and centre forms cavity, so that intermediate polymer liquid crystal mixture be made to have certain thickness, this thickness is known as box
It is thick.
The size and uniformity of box thickness determine by introns, thus the dispersing method of introns to the control of box thickness especially
It is important.For the HPDLC grating of the hard substrates such as glass, introns can be divided introns solution by modes such as spin coating or drop coatings
It is dispersed in substrate surface.However, these methods are not suitable for the production of flexible substrates HPDLC grating.
It is preferably, in step (2), introns are evenly dispersed on a flexible substrate, comprising:
(i) introns are distributed in easy volatile solvent, obtain introns dispersion liquid；
(ii) flexible substrates are immersed in the introns dispersion liquid, soaking time is 2~5min；
(iii) flexible substrates are taken out, it is dry.
The concentration of introns has significant impact to its dispersion effect in introns dispersion liquid.Introns concentration is smaller
When, the introns distribution after dispersion in flexible substrates is sparse, and flexible substrates are easy to collapse；When introns concentration is larger, dispersion
Introns distribution afterwards in flexible substrates is overstocked, and introns adhesion is serious, so that box thickness ununiformity one.
Preferably, in introns dispersion liquid, introns concentration is 0.1~2mg/mL.After dispersion, introns in flexible substrates
Tamped density in 20~200/mm2Left and right, introns distribution situation are normal.
It is further preferred that introns concentration is 0.5~1mg/mL in introns dispersion liquid.After dispersion, in flexible substrates
The tamped density of introns is in 50~90/mm2Left and right, introns distribution situation is good, and flexible substrates were under external force both
It will not collapse, the distribution of box thickness is also more uniform.
The introns are SiO2Microballoon or polystyrene microsphere, a diameter of 3~100 μm.The diameter of introns can
Select according to box thickness.
The easy volatile solvent is ethyl alcohol, acetone, ether, ethyl acetate or isopropanol.
Compared with prior art, the invention has the benefit that
(1) the bent deformation of flexible holographic polymer dispersed liquid crystal grating prepared by the present invention, can be applied to 3D body and shows
And wearable display equipment, and diffraction efficiency with higher and shorter electric drive response time；
(2) preparation process of the invention is simple, is suitable for industrialized production.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of flexible holographic polymer dispersed liquid crystal grating；
Fig. 2 is the dispersion figure of introns on a flexible substrate in embodiment 4；
Fig. 3 is the dispersion figure of introns on a flexible substrate in embodiment 6；
Fig. 4 is flexible liquid crystal box exposure light path schematic diagram；
Fig. 5 is the flexible holographic polymer dispersed liquid crystal grating diffration efficiency chart that embodiment 7 obtains；
Fig. 6 is the response speed figure for the flexible holographic polymer dispersed liquid crystal grating that embodiment 7 obtains；
Fig. 7 is the stereoscan photograph for the flexible holographic polymer dispersed liquid crystal grating that embodiment 7 obtains.
Specific embodiment
As shown in Figure 1, flexibility HPDLC grating is sandwich structure: the polymer of upper layer and lower layer flexible substrates and centre
Liquid crystal compound.Upper layer and lower layer flexible substrates are separated by intermediate introns, to allow intermediate polymer liquid crystal mixture
With certain thickness, this thickness is commonly referred to as box thickness.The size and uniformity of box thickness are determined by introns, therefore introns
Dispersing method it is particularly important to the control of box thickness.
For the HPDLC grating of the hard substrates such as glass, introns can be molten by introns by modes such as spin coating or drop coatings
Liquid is dispersed in substrate surface.However, these methods are not suitable for the production of flexible substrates HPDLC grating.
Examples 1 to 6
Introns dispersing method:
Examples 1 to 6 is dispersed introns on a flexible substrate using czochralski method, comprising:
(1) introns (SiO for being 10 μm by diameter2Microballoon) ultrasonic disperse is in the volatile solvent such as isopropanol；It is real
It applies in example 1~6, introns concentration is respectively 0.1,0.2,0.5,1.0,1.5,2.0mg/mL in introns dispersion liquid:
(2) flexible substrates are vertically immersed in introns dispersion liquid, 2~5min of soaking time；
(3) flexible substrates are taken out, it is dry under room temperature.
After drying, the dispersion of introns is as shown in table 1 in Examples 1 to 6.
The dispersion of introns in 1 Examples 1 to 6 of table
In embodiment 4, when introns concentration is 1.0mg/mL in introns dispersion liquid, after dry, in flexible substrates between
Normal every sub- distribution situation, Fig. 2 is its microscope photo.
In embodiment 6, when introns concentration is 2.0mg/mL in introns dispersion liquid, after dry, in flexible substrates between
Serious every sub- adhesion, Fig. 3 is its microscope photo.
Embodiment 7
(1) by 50wt.% acrylate monomer (one of ETERCURE 6361-100, PETA, PETTA and DPHA or
It is a variety of), 10wt.% plasticizer (n-vinyl pyrrolidone etc.), 2.5wt.% photoinitiator, 37.5wt.% liquid crystal E7 difference
It is added in brown sample bottle, stirs to uniformly mixed；
(2) the PET-ITO substrate liquid crystal cell of the conductive coating containing ITO is prepared, wherein a piece of PET-ITO uses 3 side of embodiment
The SiO that 60 microns of method dispersion diameter2Introns, liquid crystal cell box thickness are 60 microns；
(3) liquid crystal compound in step (1) is poured into the liquid crystal cell of step (2)；
(4) liquid crystal cell of step (3) is placed in optical path as shown in Figure 4, by the laser of a branch of 532nm by inclined
Light is divided into two beam coherent lights after expanding, sample cell surface, control exposure light intensity, time for exposure 1min are converged in after reflection；
(5) after end exposure, sample liquid crystal cell is placed in ultraviolet light solidification case after carrying out and is solidified, time 2min is obtained
Flexible holographic polymer dispersed liquid crystal grating, the results are shown in Table 2.
The condition and result of 2 embodiment 7~12 of table
Note: absolute diffraction efficiency=diffraction intensity/incident intensity.
The transmitance of flexibility holographic polymer dispersed liquid crystal grating made from embodiment 7 is 80% (as shown in Figure 5), absolutely
Diffraction efficiency is 65%, opening time 1.5ms, and the shut-in time is 2.5ms (as shown in Figure 6).
Due in PET-ITO and liquid crystal cell polymer and liquid crystal be flexible material, apply perpendicular to sample surface power
Can make its bending, after bending grating there is also and can restore.
The bending curvature of flexibility holographic polymer dispersed liquid crystal grating made from embodiment 7~12 is 30m-1, screen periods
For 750nm (as shown in Figure 7).
Technical solution of the present invention and beneficial effect is described in detail in embodiment described above, it should be understood that
Above is only a specific embodiment of the present invention, it is not intended to restrict the invention, it is all to be done in spirit of the invention
Any modification, supplementary, and equivalent replacement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of flexibility holographic polymer dispersed liquid crystal grating, which comprises the following steps:
(1) acrylate monomer, photoinitiator, plasticizer and liquid crystal are uniformly mixed, obtain dispersed liquid crystal liquid；
(2) introns are dispersed in two panels flexible substrates, then two panels flexible substrates is stacked, with solidification adhesive edge, system
At liquid crystal cell；
(3) the dispersed liquid crystal liquid is injected in the liquid crystal cell, liquid crystal cell is exposed using two beam coherent lasers, shape
At interference figure, solidification obtains flexible holographic polymer dispersed liquid crystal grating after.
2. the preparation method of flexibility holographic polymer dispersed liquid crystal grating according to claim 1, which is characterized in that described
Acrylate monomer degree of functionality be 3~8.
3. the preparation method of flexibility holographic polymer dispersed liquid crystal grating according to claim 2, which is characterized in that described
Acrylate monomer be pentaerythritol triacrylate, pentaerythritol tetraacrylate, dipentaerythritol it is amyl-/hex- acrylic acid
At least one of with the hyperbranched monomer ETERCURE 6361-100 of eight degrees of functionality.
4. the preparation method of flexibility holographic polymer dispersed liquid crystal grating according to claim 1, which is characterized in that described
Photoinitiator be Irgacure 784, Bengal rose red, the red Y of potato, methylene blue, rhodamine 6G, diiodofluorescein, Michaelis
Ketone or 3,3'- carbonyl are bis- (7- lignocaine cumarin).
5. the preparation method of flexibility holographic polymer dispersed liquid crystal grating according to any one of claims 1 to 4, feature
It is, in the dispersed liquid crystal liquid, is calculated in mass percent, includes:
6. according to right want 1 described in flexible holographic polymer dispersed liquid crystal grating preparation method, which is characterized in that step
It is (2) in, introns are evenly dispersed on a flexible substrate, comprising:
Introns are distributed in easy volatile solvent by (I), obtain introns dispersion liquid；
Flexible substrates are immersed in the introns dispersion liquid by (II), and soaking time is 2~5min；
(III) takes out flexible substrates, dry.
7. according to right want 6 described in flexible holographic polymer dispersed liquid crystal grating preparation method, which is characterized in that introns
In dispersion liquid, introns concentration is 0.1~2mg/mL.
8. the preparation method of flexibility holographic polymer dispersed liquid crystal grating according to any one of claims 1 to 4, feature
It is, in step (3), liquid crystal cell is exposed using visible light lasers, form interference figure, later again using ultraviolet or can
Solidify after light-exposed progress.
9. according to right want 8 described in flexible holographic polymer dispersed liquid crystal grating preparation method, which is characterized in that it is described can
The wavelength of light-exposed laser is 450~550nm, and exposure light intensity is 1~15mW/cm2。
10. a kind of flexibility holographic polymer dispersed liquid crystal grating, which is characterized in that use 1~9 described in any item preparation methods
It is made.
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| CN115820267A (en) * | 2023-02-23 | 2023-03-21 | 北京灵犀微光科技有限公司 | Holographic polymer dispersed liquid crystal material and application thereof |
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