CN101825801B - High-efficiency polymer-liquid crystal composite optical grating and preparation method thereof - Google Patents
High-efficiency polymer-liquid crystal composite optical grating and preparation method thereof Download PDFInfo
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- CN101825801B CN101825801B CN200910047119.3A CN200910047119A CN101825801B CN 101825801 B CN101825801 B CN 101825801B CN 200910047119 A CN200910047119 A CN 200910047119A CN 101825801 B CN101825801 B CN 101825801B
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Abstract
The invention belongs to the field of preparation of electro-optical functional materials, and relates to a high-efficiency polymer-liquid crystal composite optical grating and a preparation method thereof. The polymer-liquid crystal composite optical grating with high diffraction efficiency, quick driving response and low drive voltage is prepared from a mixed emulsion consisting of multi-functional group acrylate monomers, a cross-linking agent, an initiator and a co-initiator, and nematic liquid crystals serving as preparation materials by the following steps of: firstly, coating the mixed emulsion on two pieces of conductive glass respectively; secondly, putting the two pieces of conductive glass in an interference optical field of a green laser for holographic exposure, and removing unreacted monomers in an organic solvent and dissolving the unreacted monomers; thirdly, uniformly exposing the dissolved monomers with ultraviolet light, dripping the liquid crystals on one piece of conductive glass on a heating stage, and adding an interval on the piece of conductive glass; and finally, covering the other piece of conductive glass on the conductive glass and sealing into a box.
Description
Technical field
The invention belongs to electric light functional material preparation field, be specifically related to a kind of high-efficiency polymer-liquid crystal composite optical grating and preparation method thereof.
Background technology
Known in this field, the Bragg body grating that specific inductive capacity has sinusoidal pattern modulation has very high diffraction efficiency, diffraction efficiency and incident wavelength, and incident angle, body Refractive Index of Material depth of modulation is (Δ n), and the relating to parameters such as the thickness of body grating.The incident ray that meets Bragg condition in theory diffraction efficiency can reach 100%.
Polymer-liquid crystal compound substance is as a kind of electric light functional material, due to its can be automatically controlled optical property, be applied to preparing in the research of Bragg body grating, but its general effect is still undesirable.Be mainly manifested in diffraction efficiency not high, be less than 85%. scattering losses large etc., and driving voltage be high, exceedes 18V/ μ m etc.
The main cause one that the problems referred to above exist is good not to grating formation process parameter control in common holographic preparation method, as exposure intensity and time shutter.Thereby easily form larger liquid crystal droplet.In addition, driving voltage is too high, is commonly referred to be being separated of liquid crystal and polymkeric substance bad, and the liquid crystal area in the optical grating construction forming exists polymkeric substance and remaining monomer.The diffraction efficiency of the transmission-type grating of the reports such as Caputo reaches 98%, photoswitch control voltage is 5V/ μ m[], wherein, make above holographic exposure by material being heated to liquid crystal cleaning point, to form so-called polymer-liquid crystal stratiform new construction (POLYCRYPS), realize being preferably separated of liquid crystal and polymkeric substance.
According to the one dimension reaction-diffusion theory [Zhao] of at present current photopolymerization, the reaction of monomer and diffusivity all can be index decreased along with the increase of polymer concentration in reaction. the monomer [maji] that therefore can contain unreacted in the dark space of holographic exposure process (being rich solution crystalline region) and fully not spread.Visible this traditional holographic exposure (so-called single stage method onestep) is at present realized the optical grating construction that liquid crystal-polymerization is separated, even if there is Mr.'s deficiency of the imperfection of monomer reaction and diffusion. adopt the time shutter of 1000 seconds of Caputo, can not say that the monomer in dark space has not just existed.So conventionally also will carry out UV uniform exposure (flood) to sample after holographic exposure, to eliminate monomer remaining in grating.In this process, diffraction efficiency has decline to a certain degree conventionally. and the monomer that shows these remaining (mainly in liquid crystal areas) is now able to polymerization; consequently can change both structures of the established polymer-liquid crystal grating with high-diffraction efficiency on the one hand; in addition also in the mixed network structure of some unsound polymer-liquid crystals of rich solution crystal zone formation, thereby increase the anchoring strength to liquid crystal.
In view of the above problems, eliminate remaining monomer in liquid crystal area, will become stabilizing device performance and reduce the key of driving voltage with the hybrid structures of avoiding forming Polymer Dispersed Liquid Crystal.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, the polymer-liquid crystal composite grating structure of the low driving fast-response of a kind of high-level efficiency is provided.Its grating vector direction keeps the modulation of (closely) sinusoidal pattern specific inductive capacity, and to realize in liquid crystal layer containing the pure phase structure of the monomer of polyreaction not. this optical grating construction can make diffraction effectively concentrate on single order and eliminate high-order loss. and the pure phase structure of liquid crystal layer can make liquid crystal tie up to strain flexibly under outer field action simultaneously, reach the effect that reduces grappling, thereby reduce driving voltage. and by controlling suitable grating thickness to reach corresponding response speed.
High-efficiency polymer-liquid crystal composite optical grating of the present invention is prepared by following method and step,
Adopt by multi-functional acrylate monomer, glue crosslinking agent, initiating agent, the mixed emulsion of association's initiating agent composition and nematic liquid crystal are for preparing material.First respectively two above-mentioned photopolymerizable mixed emulsions of conductive glass surface coating, then be placed on respectively in the interference optical field of green laser and carry out holographic exposure, accurately control exposure strong, degree and time, then two electro-conductive glass are dipped in suitable organic solvent in darkroom, leave standstill 10-20 minute. unreacted monomer is dissolved and removed, and then it is carried out to the uniform exposure of appropriate time with the ultraviolet light of suitable intensity, again on warm table to liquid crystal drip-injection on an electro-conductive glass, on this electro-conductive glass, add interval again, thereon by another piece electro-conductive glass lid finally, and Feng Kuangcheng box, the thick 25 μ m of box, prepared polymer-liquid crystal composite grating there is high-diffraction efficiency, fast driving response, with low driving voltage.
Of the present invention preparation in material, the percentage by weight of mentioned component content is as following:
Described multi-functional acrylate monomer adopts the acrylate monomer trimethylolpropane triacrylate (TMPTA) of trifunctional. and its component content is 50%-80%,
It is 20%-30% that described glue crosslinking agent adopts its component content of NVP N-vinylpyrrollidone (NVP),
Described initiating agent adopts tetrachlorotetraiodofluorescein sodium Rose Bengal (RB), and its component content is 0.4%-0.6%,
Described association's initiating agent adopts N-phenylglycine N-phenylglycine (NPG), and its component content is 0.5%-1%,
Described nematic liquid crystal adopts RO-TN-570, or E7 and with similarly mixed liquid crystal of E7.
In preparation method of the present invention, the time shutter is controlled at 5-20 second;
In preparation method of the present invention, described organic solvent is ethanol or acetone;
In preparation method of the present invention, on described warm table, electro-conductive glass is heated on liquid crystal clearing point temperature, is generally 50-70 DEG C, carries out liquid crystal drip-injection;
In preparation method of the present invention, described on electro-conductive glass, add be spaced apart plastics or glass liner, particle diameter 10-30 μ m.
In preparation method of the present invention, the rectify thick 25 μ m of box of box of described envelope.
Preparation method of the present invention is applicable to planar technology, and especially plane spin coating proceeding can carry out large-scale production.
For the ease of understanding, below will be described in detail the present invention by specific embodiment.It needs to be noted, these descriptions are only exemplary descriptions, do not form limitation of the scope of the invention.
Embodiment
Embodiment 1
Adopting the acrylate monomer (TMPTA) of the trifunctional of following content percentage by weight. its content is 50%, glue crosslinking agent NVP (NVP) 20%, initiating agent tetrachlorotetraiodofluorescein sodium (RB) 0.4%, association's initiating agent N-phenylglycine (NPG) 0.5%, the mixed emulsion of composition, first respectively plane spin application is on two conductive glass surfaces, then be placed on respectively in the interference optical field of green laser and carry out holographic exposure, controlling exposure intensity and time shutter is 5-20 second, then two electro-conductive glass are dipped in organic solvent ethanol or acetone in darkroom, leave standstill 10-20 minute. unreacted monomer is dissolved and removed, and then it is carried out to the uniform exposure of appropriate time with the ultraviolet light of suitable intensity, again on warm table to liquid crystal drip-injection on an electro-conductive glass, described liquid crystal adopts RO-TN-570, or E7 and with similarly mixed liquid crystal of E7, electro-conductive glass is heated on liquid crystal clearing point temperature, temperature is 50-70 DEG C, on this electro-conductive glass, add again plastics or the glass liner interval of particle diameter 10-30 μ m, thereon by another piece electro-conductive glass lid finally, and the box of the thick 25 μ m of Feng Kuangcheng, prepared polymer-liquid crystal composite grating there is high-diffraction efficiency, fast driving response, and low driving voltage.
Embodiment 2
Adopting the acrylate monomer (TMPTA) of the trifunctional of following content percentage by weight. its content is 80%, glue crosslinking agent NVP (NVP) 30%, initiating agent tetrachlorotetraiodofluorescein sodium (RB) 0.6%, association's initiating agent N-phenylglycine (NPG) 1%, the mixed emulsion of composition, first respectively plane spin application is on two conductive glass surfaces, then be placed on respectively in the interference optical field of green laser and carry out holographic exposure, controlling exposure intensity and time shutter is 5-20 second, then two electro-conductive glass are dipped in organic solvent ethanol or acetone in darkroom, leave standstill 10-20 minute. unreacted monomer is dissolved and removed, and then it is carried out to the uniform exposure of appropriate time with the ultraviolet light of suitable intensity, again on warm table to liquid crystal drip-injection on an electro-conductive glass, described liquid crystal adopts RO-TN-570, or E7 and with similarly mixed liquid crystal of E7, electro-conductive glass is heated on liquid crystal clearing point temperature, temperature is 50-70 DEG C, on this electro-conductive glass, add again plastics or the glass liner interval of particle diameter 10-30 μ m, thereon by another piece electro-conductive glass lid finally, and the box of the thick 25 μ m of Feng Kuangcheng, prepared polymer-liquid crystal composite grating there is high-diffraction efficiency, fast driving response, and low driving voltage.
Embodiment 3
Adopting the acrylate monomer (TMPTA) of the trifunctional of following content percentage by weight. its content is 70%, glue crosslinking agent NVP (NVP) 28.4%, initiating agent tetrachlorotetraiodofluorescein sodium (RB) 0.6%, association's initiating agent N-phenylglycine (NPG) 1%, the mixed emulsion of composition, first respectively plane spin application is on two conductive glass surfaces, then be placed on respectively in the interference optical field of green laser and carry out holographic exposure, controlling exposure intensity and time shutter is 5-20 second, then two electro-conductive glass are dipped in organic solvent ethanol or acetone in darkroom, leave standstill 10-20 minute. unreacted monomer is dissolved and removed, and then it is carried out to the uniform exposure of appropriate time with the ultraviolet light of suitable intensity, again on warm table to liquid crystal drip-injection on an electro-conductive glass, described liquid crystal adopts RO-TN-570, or E7 and with similarly mixed liquid crystal of E7, electro-conductive glass is heated on liquid crystal clearing point temperature, temperature is 50-70 DEG C, on this electro-conductive glass, add again plastics or the glass liner interval of particle diameter 10-30 μ m, thereon by another piece electro-conductive glass lid finally, and the box of the thick 25 μ m of Feng Kuangcheng, prepared polymer-liquid crystal composite grating there is high-diffraction efficiency, fast driving response, and low driving voltage.
Claims (6)
1. a high-efficiency polymer-liquid crystal composite optical grating, it is characterized in that, prepare by following method and step: adopt the acrylate monomer by trifunctional, glue crosslinking agent, initiating agent, the mixed emulsion of association's initiating agent composition and nematic liquid crystal are for preparing material, first respectively two above-mentioned mixed emulsions of conductive glass surface coating, then be placed on respectively in the interference optical field of green laser and carry out holographic exposure, then two electro-conductive glass are dipped in organic solvent in darkroom, leave standstill 10-20 minute, remove unreacted monomer, and then it is carried out to uniform exposure with ultraviolet light, on warm table to dispenser method on an electro-conductive glass, on this electro-conductive glass, add interval, thereon by another piece electro-conductive glass lid finally, Feng Kuangcheng box, make high-efficiency polymer-liquid crystal composite optical grating,
The acrylate monomer of described trifunctional, its percentage by weight is 70%;
Described to prepare glue crosslinking agent in material be NVP, and its percentage by weight is 28.4%;
Described to prepare initiating agent in material be tetrachlorotetraiodofluorescein sodium, and its percentage by weight is 0.6%;
Described prepare that in material, to assist initiating agent be N-phenylglycine, its percentage by weight is 1%.
2. by high-efficiency polymer-liquid crystal composite optical grating claimed in claim 1, it is characterized in that the described nematic liquid crystal in material of preparing is selected from RO-TN-570 or E7 or similarly mixes liquid crystal with E7.
3. by high-efficiency polymer-liquid crystal composite optical grating claimed in claim 1, it is characterized in that the described control holographic exposure time is 5-20 second.
4. by high-efficiency polymer-liquid crystal composite optical grating claimed in claim 1, it is characterized in that described organic solvent is ethanol or acetone.
5. by high-efficiency polymer-liquid crystal composite optical grating claimed in claim 1, it is characterized in that described electro-conductive glass heating-up temperature is 50-70 DEG C.
6. by high-efficiency polymer-liquid crystal composite optical grating claimed in claim 1, it is characterized in that described plastics or glass liner, the particle diameter 10-30 μ m of being spaced apart.
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| CN102279557B (en) * | 2011-07-26 | 2013-10-30 | 华中科技大学 | Method for preparing colour three-dimensional hologram based on holographic polymer dispersed liquid crystal grating |
| CN110596944B (en) * | 2019-09-19 | 2022-11-04 | 京东方科技集团股份有限公司 | Display device and manufacturing method thereof |
| CN113625380A (en) * | 2021-05-27 | 2021-11-09 | 邓景月 | Grating preparation method and ARPDLC holographic polymer liquid crystal grating |
Citations (2)
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| CA2479467A1 (en) * | 2002-03-15 | 2003-09-25 | Pd-Ld, Inc. | Fiber optic devices having volume bragg grating elements |
| US7198737B2 (en) * | 1998-07-29 | 2007-04-03 | Science Applications International Corporation | Electrically switchable polymer-dispersed liquid crystal materials including switchable optical couplers and reconfigurable optical interconnects |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7198737B2 (en) * | 1998-07-29 | 2007-04-03 | Science Applications International Corporation | Electrically switchable polymer-dispersed liquid crystal materials including switchable optical couplers and reconfigurable optical interconnects |
| CA2479467A1 (en) * | 2002-03-15 | 2003-09-25 | Pd-Ld, Inc. | Fiber optic devices having volume bragg grating elements |
Non-Patent Citations (3)
| Title |
|---|
| 尹德金.高效全息聚合物分散液晶Bragg光栅制备研究.《复旦大学硕士学位论文》.复旦大学,2009,全文. * |
| 曹良才等.基于多重体全息光栅的光谱器件的研究.《光电子.激光》.2003,第14卷(第02期),全文. * |
| 郑致刚等.双重复合式液晶/聚合物电调谐光栅的制备.《物理学报》.2008,第57卷(第11期),全文. * |
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