CN102604649B - Fast response liquid crystal material for liquid crystal wave-front corrector and preparation method thereof - Google Patents
Fast response liquid crystal material for liquid crystal wave-front corrector and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of liquid crystal material preparation and relates to a fast response liquid crystal material for a liquid crystal wave-front corrector and a preparation method. The preparation method is characterized in that eight compounds such as alkyl biphenyl isothiocyanate, alkyl triple phenyl isothiocyanate, alkyl diphenyl acetylenyl isothiocyanate and alkyl phenyl diphenyl acetylenyl isothiocyanate are mixed in percentage by weight, and the mixture is heated and uniformly blended to obtain a wide-temperature nematic liquid crystal with a delta n value of 0.30-0.45 and low viscosity; the obtained liquid crystal material is manufactured into a reflection-type parallel arrangement liquid crystal box which is equivalent to a single pixel liquid crystal wave-front corrector; the thickness of a liquid crystal layer is controlled to be 1.6mum-2.0mum; the modulated quantity of a phase is ensured to be greater than one 785nm-wavelength; and the response time of the modulated quantity of a wavelength phase is 2.4ms-2.5ms under the driving of a 5V-voltage.
Description
Technical field
The invention belongs to the liquid crystal material preparing technical field, relate to the liquid crystal material in liquid crystal wavefront corrector, is a kind of fast response liquid crystal material and preparation method, specifically for fast response liquid crystal material and the preparation method of liquid crystal wavefront corrector.
Background technology
The function of adaptively correcting system is that distorted wavefront to incident light carries out the real-Time Compensation correction before light wave, obtains desirable optical imagery.
Based on the liquid crystal wavefront corrector of nematic liquid crystal material, adopt ripe microelectronics preparation technology, have the characteristics of high pixel density, not only correction accuracy is high, and can utilize kinoform correction of typist's errors wavefront, and only need the absolute position phase modulation voltage of 1 λ (λ is modulated light wavelength), can correction depth be just distorted wavefront [the Cao Z. of 10 λ, Xuan L., Hu L., Liu Y., and Mu Q., Opt.Express 13,5186 (2005)].Therefore use the ADAPTIVE OPTICS SYSTEMS of liquid crystal wavefront corrector to have very large application potential in heavy caliber visual telescope imaging field.But the response speed of nematic liquid crystal device is usually slower, when especially position phase modulation voltage reached 785nm, the time of response was longer than 6ms, but the atmosphere adaptive optics requires the speed of wave-front corrector to want 10～20 times to the change frequency of atmospheric turbulence, and the change frequency of atmospheric turbulence is mainly between 30Hz～60Hz, thus the time of response of liquid crystal device must be shorter than 2.5ms.If response device speed is faster, the light wave front-distortion residual volume after adaptively correcting will be less, can be better through the optical system imaging effect of adaptively correcting.
The principle of work of liquid crystal wavefront corrector is: modulated polarized light impinges perpendicularly on liquid crystal device, and polarization electric vector direction is parallel with the orientation of liquid crystal molecule, when liquid crystal device is applied to driving voltage from low to high, liquid crystal molecule can occur from parallel to the rotation perpendicular to substrate, thereby show different specific refractory poweres, (Δ n is the anisotropic refraction rate variance of liquid crystal material maximum namely can to obtain relative path difference from 0 to Δ nd, d is thickness of liquid crystal layer), make accordingly liquid crystal wavefront corrector, its dominant bit phase modulation voltage is Δ nd.Liquid crystal molecule rearranges under different voltage time is called the time of response.When voltage raise, liquid crystal molecule trended towards vertical substrate and arranges under electric field driven; When loss of voltage, liquid crystal molecule relies on the elastic force of self to arrange and transfer the arrangement of trend parallel substrate to perpendicular to substrate from trend; Usually the elastic force of liquid crystal is less than the reactive force of electric field, therefore the time of response of rear process is generally long than front process, so the time of response of liquid crystal wavefront corrector is defined as, remove elastic force that liquid crystal molecule after highfield relies on self from perpendicular to substrate, arranging and turn to parallel substrate to arrange, the time of having experienced when Δ nd has changed a wavelength is the time of response of liquid crystal wavefront corrector.The character of the time of response of liquid crystal wavefront corrector by liquid crystal material is determined.So people should adopt the liquid crystal material of quick response when preparing liquid crystal wavefront corrector.
In the world, people once proposed to utilize ferroelectric liquid crystal material and dual-frequency liquid crystal material to realize the high speed wavefront correction.But ferroelectric liquid crystals position phase modulation voltage is little, can't meet the requirement of correcting value; There is the problem that driving voltage is high, surpass large-scale integrated circuit load in dual-frequency liquid crystal, makes device resolving power be difficult to do height.Therefore, they all are not suitable for liquid crystal wavefront corrector.
In liquid crystal display applications, people once proposed Liquid Crystal structure and the mixing formula [Lei Yanrong, Zhu Xia, Zhang Hongwei etc., TN type fast response liquid crystal composition, Chinese patent, publication number: CN101928568A] of multiple quick response.But these demonstrations are not suitable for preparing liquid crystal wavefront corrector with the fast LC material, the liquid crystal material of use needs wide visual angle because show, so Δ n<0.1, and wave-front corrector must have the modulation voltage of 1 λ (λ is modulated light wavelength), common modulated light is the near infrared light wave band, here λ～the 785nm of take is example, adopt reflective devices, namely want 2 Δ nd>785nm, if Δ n<0.1, the thickness d of liquid crystal layer>3.9 μ m, and time of response and d
2Be directly proportional [Wang Xinjiu, liquid crystal optics and liquid-crystal display, Science Press, first version in 2006], d>3 μ m devices will lose the fast-response energy usually.Therefore, for the liquid crystal material of liquid crystal wavefront corrector, usually want Δ n>0.3.
Commercial high Δ n liquid crystal material has itrile group biphenyl, the itrile group terphenyl, and the compound of phenylbenzene alkynes structure, the rotary viscosity of these liquid crystal materials is larger, and the time of response generally, more than 10ms, even is longer than 30ms, does not also meet the requirement of liquid crystal wavefront corrector.Therefore, the liquid crystal material in liquid crystal wavefront corrector must have high Δ n and low viscosity two specific characters simultaneously.
In the proposition liquid crystal molecules such as the Wu S of the U.S., contain dibenzenyl and the lsothiocyanates group can obtain high Δ n and low viscosity, and provided basic chemical structure [the Gauza S. of some liquid crystal materials, Wen C., Wu B., Wu S.et al.Liquid Crystals, 2006,33 (6): 705-710; Wu S., Chai Z., USPatent, 6,838,017], but in these papers and patent, do not provide composition and the proportioning of liquid crystal compound, also not mentioned this material is the time of response under the phase modulation voltage of 785nm position at 1 λ, the parameter estimation of announcing in the literature according to them, this liquid crystal material is for the reflection type liquid crystal wave-front corrector, and (time of response under the position phase modulation voltage of λ=785nm) should be slightly larger than 3ms to 1 λ, can't meet the requirement of liquid crystal wavefront corrector.
Summary of the invention
The present invention is in order to overcome the deficiency of available liquid crystal material, realize that the reflection type liquid crystal wave-front corrector is in 1 λ (the quick response under the phase modulation voltage of the position of λ=785nm), proposed the composition and ratio of a kind of high Δ n and low viscosity liquid crystal material, purpose is to provide a kind of fast response liquid crystal material for liquid crystal wavefront corrector and preparation method.
In dispensing liquid crystal of the present invention, contain a kind of alkyl biphenyl base lsothiocyanates, two kinds of alkyl terphenyl lsothiocyanates, three kinds of alkyl diphenyl ethynyl lsothiocyanates, two kinds of alkyl phenyl tolane base lsothiocyanates, totally eight kinds of liquid crystalline cpds.The molecular formula of these eight kinds of compounds is:
Above-mentioned 8 kinds of compound purities are greater than 99.5%, by following mass percent, mix: (a) 3%～8%, (b) 6%～10%, (c) 5%～9%, (d) 10%～15%, (e) 31%～36%, (f) 20%～25%, (g) 5%～10%, (h) 5%～10%; Mixture is put into to the borosilicate glass vessel, be placed in the water-bath heating slot of induction stirring, 50 ℃～70 ℃ constant temperature stirred 1 hour～1.5 hours, until all solidss dissolve fully, formed the liquid crystal compound of homogeneous.
According to the liquid crystal compound that above-mentioned preparation method forms, 0 ℃～70 ℃ temperature ranges, be nematic liquid crystal at least, Δ n value is 0.30～0.45.
With liquid crystal material of the present invention, make the reflective liquid crystal cell be arranged in parallel, be equivalent to the single-pixel liquid crystal wave-front corrector; Wherein thickness of liquid crystal layer is controlled at 1.6 μ m～2.0 μ m, guarantees that position phase modulation voltage is greater than 785nm; The liquid crystal cell driven saturated voltage that made can be detected is less than 5V; Under the driving of 5V voltage, the time of response of 1 λ position phase modulation voltage is 2.4ms～2.5ms.
The accompanying drawing explanation
Fig. 1 is the optical system for testing figure of liquid crystal response time.Wherein 1 is laser apparatus, and 2 is the polarizer, and 3 is liquid crystal cell, and 4 is speculum, and 5 is analyzer, and 6 is photo-detector.
Fig. 2 is response curve and the intercept method of 1 λ position phase lower time of response of modulation voltage of liquid crystal S1 of the present invention.
Embodiment
For clearer, understand the present invention, below in conjunction with embodiment, this fast response liquid crystal material for liquid crystal wavefront corrector and preparation method are elaborated.
Synthetic above-mentioned eight kinds of compounds (a), (b), (c), (d), (e), (f), (g), (h) each 10g, all be greater than 99.5% by the purity of every kind of compound of high performance liquid chromatography (HPLC) mensuration respectively.
Weight percent according to mixture: (a) 5%, (b) 8%, (c) 7%, (d) 11%, (e) 33%, (f) 22%, (g) 7%, (h) 7%, with analytical balance from synthetic (a) compound, taking in 0.0500g, (b) compound and take in 0.0800g, (c) compound and take in 0.0700g, (d) compound and take in 0.1100g, (e) compound and take in 0.3300g, (f) compound and take in 0.2200g, (g) compound and take in 0.0700g, (h) compound and take 0.0700g.Eight kinds of compounds that take are put into to the borosilicate glass reagent bottle of a volume 5mL, added the tetrafluoroethylene stirrer of length 5mm, build the bottle cap with pad in teflon seal; Reagent bottle is placed in to 60 ℃ of water-baths, induction stirring 1 hour, all solidss all dissolve, and have obtained the Object LC material, are called liquid crystal S1.
Detect the physical property of liquid crystal S1:
(1) nematic temperature range
The employing differential thermal analyzer detects: with syringe, get 3.0mg liquid crystal S1, inject the sample crucible of differential thermal analyzer, this sample is carried out to the differential scanning between-10 ℃～250 ℃, 10 ℃/min of temperature rise rate.In the collection of illustrative plates obtained, can see two obvious endotherm(ic)peaks, should be respectively fusing point and the clearing point of liquid crystal S1, by instrument software, provide the temperature at each peak, be respectively-5.0 ℃ and 110.5 ℃.On clean slide, drip the brilliant S1 of a dropping liquid, room temperature is watched texture under polarizing microscope again, sees typical four brush texture, and explanation is nematic phase, thereby concludes that the nematic temperature range of liquid crystal S1 is-5 ℃～110 ℃.
(2) measuring result of Δ n
Get the ito glass substrate of two clean 25mm * 20mm * 1.1mm, ITO face side coating polyimide PI (RN-1199, Nissan company) alignment films [be shown in by the coating method of alignment films, Gao Hongjin, Dong Youmei, liquid crystal and flat panel display, press of Beijing University of Post & Telecommunication, in May, 2008 second edition]; Two substrates with the PI film are done to the antiparallel friction orientation and process, make the sylphon that can make liquid crystal S1 parallel-oriented, the two substrates gap is 1.9 μ m; At room temperature to sylphon, inject liquid crystal S1, form and have a single-pixel liquid crystal box of phase electrical modulation ability.This liquid crystal cell is placed on the elliptic polarization spectrometer of French JY company, 35 ℃ of envrionment temperatures, the Δ n that measures liquid crystal S1 is 0.34.
(3) time of response
Optical system for testing such as Fig. 1, wherein 1 is the laser apparatus of wavelength 785nm, and 2 is the polarizer of light transmission shaft perpendicular to paper, and 3 is the liquid crystal cell described in " (2) ", and 4 is plane mirror, and 5 for light transmission shaft is parallel to the analyzer of paper, and 6 is photo-detector.Photo-detector 6 is connected with oscilloscope, and liquid crystal cell 3 is connected with signal generator.From the laser sent laser apparatus 1, pass through the polarizer 2, make the laser polarization direction seen through also perpendicular to paper, then near normal incident liquid crystal cell 3, the frictional direction of liquid crystal cell 3 is that liquid crystal S1 differently-oriented directivity becomes miter angle with the light transmission shaft of the polarizer 2, make incident laser in liquid crystal cell 3, produce equicohesive o light and e light, fall behind mutually o light 1.9 μ m * 0.34=646nm by the rear e light of liquid crystal cell 3 position; The rear 5cm of liquid crystal cell 3 place holding plane speculum 4, make reflection ray again by liquid crystal cell 3, makes that incident and reflected light angle are 3 to spend, and angular bisector is the normal of speculum 4; Liquid crystal cell 3 is combined and is equivalent to reflective liquid crystal on silicon with plane mirror 4, and the phasic difference of e light and o light is doubled, and is 646nm * 2=1292nm, the position phase modulation voltage of corresponding 1.6 λ; Reflected beam forms the elliptical light of major axis on specific direction by the rear phasic difference according to e light and o light of liquid crystal cell 3, produces corresponding light intensity by analyzer 5, arrives photo-detector 6.
During detection, liquid crystal cell 3 is applied ± square-wave voltage of 5V, 1000Hz, make liquid crystal molecule from parallel substrate, arrange to turn to perpendicular to substrate under this highfield drives and arrange, now the light by liquid crystal layer only has o light; Then remove voltage, liquid crystal molecule relies on the elastic force of self again from perpendicular to substrate, arranging and turn to parallel substrate to arrange, and in process, the e light intensity increases sharply, and the phasic difference of e light and o light continues to increase, and output intensity is temporal evolution also; Oscilloscope has recorded the time dependent curve of light intensity by photo-detector 5, it is the response curve of liquid crystal S1, as shown in Figure 2, from the starting point of response curve, it is the straight line that flex point is drawn a parallel axis of abscissa, this straight line intersects with response curve for twice in succession, to second intersection point response curve, just in time complete a sinusoidal wave, intercept the time of response that the corresponding time of this sinusoidal wave is 1 λ position phase modulation voltage.Result shows, the time of response of liquid crystal S1 1 λ position phase modulation voltage in 1.9 μ m liquid crystal cells is 2.4ms.
Weight percent according to mixture: (a) 3%, (b) 7%, (c) 6%, (d) 11%, (e) 33%, (f) 22%, (g) 9%, (h) 9%, with analytical balance from synthetic (a) compound, taking in 0.0300g, (b) compound and take in 0.0700g, (c) compound and take in 0.0600g, (d) compound and take in 0.1100g, (e) compound and take in 0.2200g, (f) compound and take in 0.3300g, (g) compound and take in 0.0900g, (h) compound and take 0.0900g.Eight kinds of compounds that take are put into to the borosilicate glass reagent bottle of a volume 5mL, added the tetrafluoroethylene stirrer of length 5mm, build the bottle cap with pad in teflon seal; Reagent bottle is placed in to 60 ℃ of water-baths, induction stirring 1 hour, all solidss all dissolve, and have obtained the Object LC material, are called liquid crystal S2.
Detect the physical property of liquid crystal S2:
(1) nematic temperature range
According to the testing method of embodiment 1, the nematic temperature range that records liquid crystal S2 is 0 ℃～120 ℃.
(2) measuring result of Δ n
According to the testing method of embodiment 1, the Δ n that records liquid crystal S2 is 0.35.
(3) time of response
According to the testing method of embodiment 1, make the liquid crystal cell that the liquid crystal bed thickness is 1.8 μ m, position phase modulation voltage is 1.8 μ m * 0.35 * 2=1260nm, corresponding 1.6 λ; The time of response that records liquid crystal S2 1 λ position phase modulation voltage in 1.8 μ m liquid crystal cells is 2.4ms.
Embodiment 3
Weight percent according to mixture: (a) 6%, (b) 8%, (c) 7%, (d) 12%, (e) 34%, (f) 23%, (g) 5%, (h) 5%, with analytical balance from synthetic (a) compound, taking in 0.0600g, (b) compound and take in 0.0800g, (c) compound and take in 0.0700g, (d) compound and take in 0.1200g, (e) compound and take in 0.3400g, (f) compound and take in 0.2300g, (g) compound and take in 0.0500g, (h) compound and take 0.0500g.Eight kinds of compounds that take are put into to the borosilicate glass reagent bottle of a volume 5mL, added the tetrafluoroethylene stirrer of length 5mm, build the bottle cap with pad in teflon seal; Reagent bottle is placed in to 60 ℃ of water-baths, induction stirring 1 hour, all solidss all dissolve, and have obtained the Object LC material, are called liquid crystal S3.
Detect the physical property of liquid crystal S3:
(1) nematic temperature range
According to the testing method of embodiment 1, the nematic temperature range that records liquid crystal S3 is-10 ℃～107 ℃.
(2) measuring result of Δ n
According to the testing method of embodiment 1, the Δ n that records liquid crystal S3 is 0.33.
(3) time of response
According to the testing method of embodiment 1, make the liquid crystal cell that the liquid crystal bed thickness is 2.0 μ m, position phase modulation voltage is 2.0 μ m * 0.33 * 2=1320nm, corresponding 1.7 λ; The time of response that records liquid crystal S3 1 λ position phase modulation voltage in 2.0 μ m liquid crystal cells is 2.5ms.
Claims (3)
1. fast response liquid crystal material for liquid crystal wavefront corrector, it is characterized by fast response liquid crystal material and comprise (a), (b), (c), (d), (e), (f), (g), (h) eight kinds of compounds, molecular formula is respectively:
The weight percent of above-mentioned (a), (b), (c), (d), (e), (f), (g), (h) eight kinds of compounds is: (a) 3%～8%, (b) 6%～10%, (c) 5%～9%, (d) 10%～15%, (e) 31%～36%, (f) 20%～25%, (g) 5%～10%, (h) 5%～10%;
The Δ n of above-mentioned liquid crystal material is 0.30～0.45, and the temperature range of its nematic liquid crystal is at least 0 ℃～70 ℃; With above-mentioned liquid crystal material, make the reflective liquid crystal cell be arranged in parallel, when wherein thickness of liquid crystal layer is controlled at 1.6 μ m～2.0 μ m, position phase modulation voltage can be greater than a wavelength X=785nm, and under 5V voltage drove, the time of response of 1 λ position phase modulation voltage was 2.4ms～2.5ms.
2. the fast response liquid crystal material for liquid crystal wavefront corrector according to claim 1, the weight percent that it is characterized by above-mentioned eight kinds of compound formulas is:
(a) 5%, (b) 8%, (c) 7%, (d) 11%, (e) 33%, (f) 22%, (g) 7%, (h) 7%; By the liquid crystal material that this mixing formula obtains, its Δ n is 0.34, nematic temperature range is-5 ℃～110 ℃;
Make the parallel-oriented reflection type liquid crystal box of liquid crystal, liquid crystal bed thickness 1.9 μ m; When lambda1-wavelength was 785nm, the driving of 5V voltage, the time of response of 1 λ position phase modulation voltage was 2.4ms.
3. the preparation method of a kind of fast response liquid crystal material for liquid crystal wavefront corrector according to claim 1, is characterized in that: by following eight kinds of compounds
Mix, 50 ℃～70 ℃ lower heated and stirred, until form the liquid crystal compound of homogeneous.
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| CN103725294B (en) * | 2013-12-19 | 2015-02-18 | 中国科学院长春光学精密机械与物理研究所 | Molecular design and mixing formula of quick liquid crystal material for liquid crystal wavefront corrector |
| EP2982730B1 (en) | 2014-08-08 | 2019-10-16 | Merck Patent GmbH | Liquid-crystalline medium and high-frequency components comprising same |
| CN106978192B (en) * | 2017-04-18 | 2019-02-12 | 西安近代化学研究所 | A kind of high birefringence rate liquid crystal compound and preparation method thereof with and combinations thereof |
| CN107474856B (en) * | 2017-09-21 | 2019-11-12 | 中国科学院长春光学精密机械与物理研究所 | A kind of mixing formula of Millisecond fast response liquid crystal material |
| CN108865180B (en) * | 2018-08-17 | 2021-10-01 | 西安近代化学研究所 | Liquid crystal composition and high-frequency assembly comprising same |
| CN110938439B (en) * | 2019-11-14 | 2021-03-19 | 清华大学 | High-polarity large-optical birefringence liquid crystal composition |
| CN115895677B (en) * | 2022-10-14 | 2024-05-17 | 中国科学院长春光学精密机械与物理研究所 | High-birefringence liquid crystal material with wide nematic phase temperature and preparation method and application thereof |
| CN118085885B (en) * | 2024-02-26 | 2024-09-20 | 华南理工大学 | Novel nematic liquid crystal material with high dielectric and high polarity and preparation method thereof |
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