CN103275736A - Preparation method of polymer-stabilized liquid crystal thin film material with wide wave reflection - Google Patents
Preparation method of polymer-stabilized liquid crystal thin film material with wide wave reflection Download PDFInfo
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Abstract
The invention relates to a preparation method of a polymer-stabilized liquid crystal thin film material with wide wave reflection. The preparation method belongs to the technical field of optical thin film materials. In order to solve the problem that a present technological process is complex, is not easy to control and has a disadvantage of narrow reflected wave, the invention provides the preparation method of the polymer-stabilized liquid crystal thin film material with wide wave reflection. The preparation method comprises the following steps: mixing 5wt%-85wt% of a nematic phase liquid crystal, 5.0wt%-15wt% of a chiral compound and 8.0wt%-20wt% of a liquid crystal polymerizable monomer, adding 0.2wt%-1.5wt% of an azo chiral compound and 0.01wt%-10wt% of a photoinitiator so as to obtain a mixed liquid crystal system; injecting into a liquid crystal cell which has undergone plane orientation in advance so as to obtain a thin film sample; and carrying out UV-light irradiation within the cholesteric phase temperature so as to obtain the liquid crystal thin film material. The preparation method provided by the invention has advantages of simple process, wide temperature range of the cholesteric phase and wide wave reflection, and is easy to operate.
Description
Technical field
The present invention relates to a kind of preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection, belong to optically thin technology field of membrane materials.
Background technology
Liquid crystal has obtained vigorous growth over nearly 20 years since finding in 1888.From the Die elektrische Zeituhr that comes into vogue, to LCD TV, mobile phone, Electronic Paper till now, e-book again, the application of liquid crystal is more and more widely in people's daily life.When lcd technology maked rapid progress, energy-conserving and environment-protective became the new problem that we will face again.
As everyone knows, most liquid crystal self can be not luminous, need have back light source system that light source is provided, and the brightness of liquid-crystal display affects the quality of image to a certain extent.Because it is very high that back light source system accounts for the power consumption proportion of whole main frame, therefore increase the non-wise move of brightness of backlight itself.Use light brightness enhancement film can significantly increase light utilization efficiency and the brightness of liquid crystal display, thereby reduce the current consumption of the backlight lighting tube of liquid crystal display.In addition, portable liquid crystal display such as notebook computer, mobile phone etc., energy-conservation is its important need, use light brightness enhancement film not only can promote display brightness but also can increase standby time, the energy-saving effect excellence, this light brightness enhancement film can prepare by having the wide wave reflection characteristics cholesteric liquid crystal.
The helicoidal structure of cholesteric liquid crystal molecule uniqueness has determined the optical characteristics that it is special, character such as selective reflection, circular dichroism, opticity for example, cholesteric liquid crystal is had a wide range of applications at numerous areas, usually be used to prepare the optics with energy-saving environmental-protection function.In the cholesteric liquid crystal, the major axis of liquid crystal molecule revolve three-sixth turn the distance of process be called as pitch P, the helically twisted power of chipal compounds is inversely proportional in the size of P and the liquid crystal.Cholesteric liquid crystal is owing to this special spirane structure has selectivity Prague reflective optical characteristic.The wide △ λ of the reflection wave that the cholesteric liquid crystal of single pitch can reflect the incident light=△ nP, wherein △ n is the degree of birefringence of liquid crystal.Because (generally the pitch of cholesteric liquid crystal generally is to be lower than 1 μ m to the pitch stability of cholesteric liquid crystal, and maximum is no more than 2 μ m) and the restriction of common liquid crystals mean refractive index (mean refractive index of common liquid crystals is about 1.5), make the wide and reflection wave position of the reflection wave of cholesteric liquid crystal all be subjected to restriction to a certain degree.In visible-range, the reflection wave of the cholesteric liquid crystal of single pitch is wide usually below 150nm, there is the narrower defective of reflection wave, and the liquid-crystal film material with wide wave reflection characteristics has widely and to use, and normally the pitch gradient by forming cholesteryl phase or pitch uneven distribution obtain.1996, the people such as D.J.Broer of Holland Philips company utilize chirality polymerisable monomer gradient diffusion principle to prepare the individual layer cholesteryl phase liquid crystal polymer film that reflects whole visible region, and it is applied on the liquid-crystal display light brightness enhancement film, this method, though increased the scope of reflection to a certain extent, but but can only reflect whole light light wavelength scope, and this method mixed liquid crystal is quite strict to the requirement of ultraviolet ray intensity gradient, is unfavorable for actually operating control.
Summary of the invention
The present invention is directed to above problems of the prior art, a kind of preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection is provided, it is simple to have technology, and easy handling and the thin-film material that obtains can be realized the effect of wide wave reflection.
The objective of the invention is to be achieved by the following technical programs, a kind of preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection, this method may further comprise the steps:
A, be that the nematic liquid crystal of 65wt%～85wt%, the chipal compounds that mass percent is 5.0wt%～15wt%, the liquid crystal polymerisable monomer that mass percent is 8.0wt%～20wt% are mixed evenly with mass percent, then, the azo chipal compounds and the mass percent that add mass percent again and be 0.2wt%～1.5wt% are the light trigger of 0.01wt%～10wt%, be mixed, obtain the mixed liquid crystal system;
B, the above-mentioned mixed liquid crystal system that obtains is injected the liquid crystal cell that passes through planar orientation in advance, obtain corresponding film sample;
C, the film sample that step B is obtained carry out ultraviolet light irradiation in the cholesteryl phase temperature range, make the polymerization of mixed liquid crystal system form macromolecule network, obtain having the polymer stabilizing liquid-crystal film material of wide wave reflection.
The present invention is by being mixed nematic liquid crystal, chipal compounds and liquid crystal polymerisable monomer evenly, make the liquid crystal that is mixed that obtains have very wide N* phase temperature range, N* phase temperature range of the present invention can reach 0 ℃～85 ℃, has very wide temperature range, thereby the entire operation process is carried out in wide temperature range, need not painstakingly go to control temperature, as long as guarantee in N* phase temperature range, be easier to working control, simplified production technique.Simultaneously, the present invention is by the effect of combining with ultraviolet radiation of adding azo chipal compounds, thereby the thin-film material that realization obtains has the effect of wide wave reflection.Further say, the helically twisted power of the azo chipal compounds that adds reduces along with the increase of irradiation ultraviolet ray intensity, and when the ultraviolet light irradiation in the ultraviolet ray intensity gradient that forms up and down of liquid-crystal film material, make in the liquid-crystal film material system the helically twisted power difference of azo chipal compounds from top to bottom, thereby in the liquid-crystal film material system, formed the pitch gradient of the pitch variation that reduces successively from top to bottom, make wide the widening of reflection wave of liquid crystal film, make the film that obtains to realize having the effect of wide wave reflection.
In the preparation method of the above-mentioned polymer stabilizing liquid-crystal film material with wide wave reflection, as preferably, the mass percent of the raw material described in the steps A is:
Nematic liquid crystal: 70wt%～75wt%; Chipal compounds: 8.0wt%～12wt%;
Liquid crystal polymerisable monomer: 12wt%～16wt%; Azo chipal compounds: 0.5wt%～1.0wt%; Light trigger: 0.2wt%～4.8wt%.
In the preparation method of the above-mentioned polymer stabilizing liquid-crystal film material with wide wave reflection, as further preferred, the mass percent of the raw material described in the steps A is:
Nematic liquid crystal: 75wt%; Chipal compounds: 10wt%; Liquid crystal polymerisable monomer: 14wt%; Azo chipal compounds: 0.4wt%; Light trigger: 0.6wt%.
In the preparation method of the above-mentioned polymer stabilizing liquid-crystal film material with wide wave reflection, the helically twisted power of the chirality azo-compound described in the steps A reduces along with the increase of ultraviolet ray intensity.As preferably, the chirality azo-compound described in the steps A is selected from one or more in the following compound:
N is selected from 2,4,6,8,10 or 12 described in the formula I;
N is selected from 2,4,6,8,10 or 12 described in the formula II;
N is selected from 2,4,6,8,10 or 12 described in the formula III.Adopting and not holding carbochain is even number, is in order to make the azo chipal compounds improve the solvability of azo chipal compounds in nematic liquid crystal better with the nematic liquid crystal dissolving.
In the preparation method of the above-mentioned polymer stabilizing liquid-crystal film material with wide wave reflection, as preferably, the described chipal compounds of steps A is selected from chiral compound S 811, chipal compounds R811, chipal compounds R1011(ZLI-4572), chipal compounds CB15 and chiral compound S 1011(ZLI-4571) in one or more.As further preferred, described chipal compounds is chiral compound S 811, and the molecular structural formula of described chiral compound S 811 is as follows:
In the preparation method of the above-mentioned polymer stabilizing liquid-crystal film material with wide wave reflection, the corresponding construction formula of described chipal compounds is as follows:
In the preparation method of the above-mentioned polymer stabilizing liquid-crystal film material with wide wave reflection, as preferably, described liquid crystal polymerisable monomer is selected from chirality or achirality liquid crystal liquid crystal property monomer.The pitch gradient that can polymerization forms the polymer network fixed film.As further preferred, described liquid crystal polymerisable monomer is selected from one or more in the following compound, but is not limited to following compound:
Among the preparation method of the above-mentioned polymer stabilizing liquid-crystal film material with wide wave reflection, as preferably, described light trigger is selected from one or both in benzoin isopropyl ether (light trigger 651) and the benzophenone.Can play the effect of initiated polymerization thing monomer polymerization.
Among the preparation method of the above-mentioned polymer stabilizing liquid-crystal film material with wide wave reflection, as preferably, described nematic liquid crystal is selected from nematic liquid crystal SLC1717.
In the preparation method of the above-mentioned polymer stabilizing liquid-crystal film material with wide wave reflection, step B can adopt following method to replace:
With the plastics film that is orientated through surperficial parallel friction in advance the liquid crystal compound system that is mixed that above-mentioned steps A obtains is pressed into film, with the thickness of separation pad or glass microballon control liquid crystal layer, prepares corresponding film sample again.
Among the preparation method of the above-mentioned polymer stabilizing liquid-crystal film material with wide wave reflection, as preferably, the ultraviolet light wavelength described in the step C is 365nm, and ultraviolet ray intensity is 1 μ W/cm
2～5mW/cm
2, the ultraviolet light irradiation time is 1 minute～1 hour.As further preferred, described ultraviolet ray intensity is 1mW/cm
2～3mW/cm
2, the ultraviolet light irradiation time is 30min～40min.
Among the preparation method of the above-mentioned polymer stabilizing liquid-crystal film material with wide wave reflection, as preferably, the temperature of the ultraviolet light irradiation described in the step C is 0 ℃～85 ℃.The temperature of ultraviolet light irradiation is selected for use in the cholesteryl phase temperature range, and cholesteryl phase temperature range of the present invention is wide, therefore, more is conducive to operation.Described cholesteryl phase temperature also can be described as hand and levies the nematic phase temperature.Further preferred, the temperature of the ultraviolet light irradiation described in the step C is 35 ℃～45 ℃.
In the preparation method of the above-mentioned polymer stabilizing liquid-crystal film material with wide wave reflection, as preferably, the thickness of described liquid-crystal film material is 10 μ m～300 μ m.
The liquid-crystal film material that preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection of the present invention obtains can be applied to liquid-crystal display, intelligent glass and association area thereof, is with a wide range of applications.
In sum, the present invention compared with prior art has the following advantages:
1. the preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection of the present invention, the characteristics that reduce with increasing to of irradiation ultraviolet ray intensity by the helically twisted power of utilizing the azo chipal compounds, during by ultraviolet light irradiation in the ultraviolet ray intensity gradient that forms up and down of liquid crystal film sample, the helically twisted power difference of the chipal compounds about making in the brilliant film sample system of liquid crystal, thereby in the sample system, formed the pitch gradient of the pitch variation that reduces successively from top to bottom, make the reflection wave of the liquid-crystal film material that obtains wide and widen, make wide the widening of reflection wave of liquid-crystal film material, realize having the effect of wide wave reflection.
2. the preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection of the present invention, used material source is extensive, technology is simple, with low cost, processes easyly, is conducive to big area production.
3. the preparation method with polymer stabilizing liquid-crystal film material of wave reflection of the present invention, the ratio of consumption by control nematic liquid crystal, chipal compounds and liquid crystal polymerisable monomer, make mixed crystal of the present invention have very wide N* phase temperature range, thereby make operational temperature conditions be easier to control, easy handling, simple production technology.
Description of drawings
Fig. 1 is the change curve of the helically twisted power of azo chipal compounds 2C of the present invention with the ultraviolet light irradiation time.
Fig. 2 is the reflection wave spectrogram of the liquid-crystal film material of the embodiment of the invention 1 preparation.
Fig. 3 is the reflection wave spectrogram of the liquid-crystal film material of the embodiment of the invention 2 preparations.
Fig. 4 is the reflection wave spectrogram of the liquid-crystal film material of reference examples 1 preparation of the present invention.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail, but the present invention is not limited to these embodiment.
Embodiment 1
At first ito glass is cleaned up, the thickness of making the parallel friction orientation processing of internal surface process is the liquid crystal cell of 10 μ m, and is standby;
According to mass percent the compound system of liquid crystal liquid crystal property polymerisable monomer C6M/ chiral compound S 811/ small molecules nematic liquid crystal SLC1717/ light trigger 651/ azo chipal compounds 2C is carried out blend according to mass ratio 15.00wt%/9.20wt%/75.00wt%/0.40wt%/0.40wt%, obtain having the liquid crystal compound system of very wide N* phase temperature range, earlier the liquid crystal compound system is poured under 100 ℃ of conditions in the above-mentioned liquid crystal cell that passes through surperficial parallel friction orientation in advance, obtain corresponding thin-film material sample, (the ultraviolet light intensity is 1mw/cm to use UV-light then under 40 ℃ condition
2, the ultraviolet light wavelength is 365nm) and irradiation is after 30 minutes, makes the polymerization of mixed liquid crystal system form macromolecule network, obtains having the liquid-crystal film material of wide wave reflection.The liquid-crystal film material that obtains is tested, and experimental result shows: the reflected range of the covered 1000nm～1600nm of the liquid-crystal film material with wide wave reflection that makes, specifically as shown in Figure 2.
In this reference examples used nematic liquid crystal (Nematic LC) SLC1717 buy from Shijiazhuang Yongshenghuaqing Liquid Crystal Co., Ltd (Yongsheng Huatsing Liquid Crystal Co., Ltd), the n of described SLC1717
o=1.519, n
e=1.720,
The structural formula of the chiral compound S 811 described in the present embodiment is as follows:
The structural formula of liquid crystal liquid crystal property polymerisable monomer C6M described in the present embodiment is as follows:
The structural formula of the light trigger 651 described in the present embodiment is as follows:
The structural formula of azo chipal compounds 2C described in the present embodiment is as follows:
Embodiment 2
At first ito glass is cleaned up, the thickness of making the parallel friction orientation processing of internal surface process is the liquid crystal cell of 10 μ m, and is standby;
According to mass percent, the compound system of stock liquid crystallinity polymerisable monomer C6M/ chiral compound S 811/ small molecules nematic liquid crystal SLC1717/ light trigger 651/ azo chipal compounds 2C is carried out blend according to mass ratio 15.00wt%/9.00wt%/75.00wt%/0.40wt%/0.60wt%, obtain having the liquid crystal compound system of very wide N* phase temperature range, earlier the liquid crystal compound system is poured under 100 ℃ of conditions in the above-mentioned liquid crystal cell that passes through surperficial parallel friction orientation in advance, obtain corresponding thin-film material sample, (described ultraviolet light intensity is 3mw/cm to use UV-light then under 40 ℃ condition
2, described ultraviolet light wavelength is 365nm) and irradiation is after 30 minutes, makes the polymerization of mixed liquid crystal system form macromolecule network, obtains having the liquid-crystal film material of wide wave reflection.The liquid-crystal film material that obtains is tested, and experimental result shows: make the reflected range of the covered 900nm～2400nm of liquid crystal film sample, specifically as shown in Figure 3.
Embodiment 3
At first ito glass is cleaned up, the thickness of making the parallel friction orientation processing of internal surface process is the liquid crystal cell of 10 μ m, and is standby;
Liquid crystal liquid crystal property polymerisable monomer, the azo chipal compounds of 1.5wt% and the light trigger benzophenone of 0.5wt% of chipal compounds R811,8.0wt% that takes by weighing nematic liquid crystal SLC1717, the 5.0wt% of raw material 85wt% according to mass percent carried out blend, obtain having the liquid crystal compound system of very wide N* phase temperature range, earlier the liquid crystal compound system is poured under 100 ℃ of conditions in the above-mentioned liquid crystal cell that passes through surperficial parallel friction orientation in advance, obtain corresponding thin-film material sample, (described ultraviolet light intensity is 1 μ w/cm to use UV-light then under 45 ℃ condition
2, described ultraviolet light wavelength is 365nm) and irradiation is after 1 hour, makes the polymerization of mixed liquid crystal system form macromolecule network, obtains liquid-crystal film material.Experimental result shows that the liquid-crystal film material with wide wave reflection that makes can cover the reflected range of 1000nm～1800nm.
The structural formula of the liquid crystal liquid crystal property polymerisable monomer described in the present embodiment is as follows:
The structural formula of the azo chipal compounds described in the present embodiment is as follows:
Embodiment 4
At first ito glass is cleaned up, the thickness of making the parallel friction orientation processing of internal surface process is the liquid crystal cell of 10 μ m, and is standby;
Liquid crystal liquid crystal property polymerisable monomer, the azo chipal compounds of 0.2wt% and the light trigger benzophenone of 4.8wt% of chipal compounds R1011,20wt% that takes by weighing nematic liquid crystal SLC1717, the 10.0wt% of raw material 65wt% according to mass percent carried out blend, obtain having the liquid crystal compound system of very wide N* phase temperature range, earlier the liquid crystal compound system is poured under 100 ℃ of conditions in the above-mentioned liquid crystal cell that passes through surperficial parallel friction orientation in advance, obtain corresponding thin-film material sample, (described ultraviolet light intensity is 5mw/cm to use UV-light then under 35 ℃ condition
2, described ultraviolet light wavelength is 365nm) and irradiation is after 40 minutes, makes the polymerization of mixed liquid crystal system form macromolecule network, obtains having the liquid-crystal film material of wide wave reflection.Experimental result shows that the liquid-crystal film material with wide wave reflection that makes can cover the reflected range of 1000nm～2200nm.
The structural formula of the liquid crystal liquid crystal property polymerisable monomer described in the present embodiment is as follows:
The structural formula of the azo chipal compounds described in the present embodiment is as follows:
Embodiment 5
The preparation method of the liquid-crystal film material with wide wave reflection of present embodiment repeats no more here with embodiment 4, and difference only is that described azo chipal compounds adopts the azo chipal compounds of following structural formula to replace.Experimental result shows, the reflected range of the covered 1000nm～1800nm of the liquid-crystal film material with wide wave reflection that makes.
The structural formula of described azo chipal compounds is as follows:
Embodiment 6
At first ito glass is cleaned up, the thickness of making the parallel friction orientation processing of internal surface process is the liquid crystal cell of 10 μ m, and is standby;
Liquid crystal liquid crystal property polymerisable monomer, the azo chipal compounds of 1.0wt% and the light trigger benzoin isopropyl ether of 2.0wt% of chipal compounds CB11,12wt% that takes by weighing nematic liquid crystal SLC1717, the 15wt% of raw material 70wt% according to mass percent carries out blend, obtain having the liquid crystal compound system of very wide N* phase temperature range, earlier the liquid crystal compound system is poured under 90 ℃ of conditions in the above-mentioned liquid crystal cell that passes through surperficial parallel friction orientation in advance, obtain corresponding thin-film material sample, (described ultraviolet light intensity is 2mw/cm to use UV-light then under 85 ℃ condition
2, described ultraviolet light wavelength is 365nm) and irradiation is after 1 minute, makes the polymerization of mixed liquid crystal system form macromolecule network, obtains having the liquid-crystal film material of wide wave reflection.Experimental result shows, the reflected range of the covered 1000nm～2000nm of the liquid-crystal film material with wide wave reflection that makes.
The structural formula of the liquid crystal liquid crystal property polymerisable monomer described in the present embodiment is as follows:
The structural formula of the azo chipal compounds described in the present embodiment is as follows:
Embodiment 7
The preparation method of the liquid-crystal film material with wide wave reflection of present embodiment is with embodiment 6, here repeat no more, difference only is that described azo chipal compounds and liquid crystal liquid crystal property polymerisable monomer adopt the azo chipal compounds of following structural formula and liquid crystal liquid crystal property polymerisable monomer to replace.Experimental result shows, the reflected range of the covered 1000nm～1700nm of the liquid-crystal film material with wide wave reflection that makes.
The structural formula of used azo chipal compounds is as follows in the present embodiment:
The structural formula of used liquid crystal liquid crystal property polymerisable monomer is as follows in the present embodiment:
Embodiment 8
At first ito glass is cleaned up, the thickness of making the parallel friction orientation processing of internal surface process is the liquid crystal cell of 10 μ m, and is standby;
Take by weighing the nematic liquid crystal SLC1717 of raw material 71.3wt% according to mass percent, the chiral compound S 1011 of 12wt%, the liquid crystal liquid crystal property polymerisable monomer of 16wt%, the azo chipal compounds of 0.5wt% and the light trigger benzoin isopropyl ether of 0.2wt% carry out blend, obtain having the liquid crystal compound system of very wide N* phase temperature range, earlier the liquid crystal compound system is poured under 100 ℃ of conditions in the above-mentioned liquid crystal cell that passes through surperficial parallel friction orientation in advance, obtain corresponding thin-film material sample, (described ultraviolet light intensity is 3mw/cm to use UV-light then under 50 ℃ condition
2, described ultraviolet light wavelength is 365nm) and irradiation is after 20 minutes, makes the polymerization of mixed liquid crystal system form macromolecule network, obtains having the liquid-crystal film material of wide wave reflection.Experimental result shows, the reflected range of the covered 1000nm～2000nm of the liquid-crystal film material with wide wave reflection that makes.The structural formula of the liquid crystal liquid crystal property polymerisable monomer described in the present embodiment is as follows:
The structural formula of the azo chipal compounds described in the present embodiment is as follows:
Embodiment 9
At first ito glass is cleaned up, the thickness of making the parallel friction orientation processing of internal surface process is the liquid crystal cell of 10 μ m, and is standby;
Take by weighing the nematic liquid crystal SLC1717 of raw material 71.2wt% according to mass percent, the chiral compound S 1011 of 8.0wt%, the liquid crystal liquid crystal property polymerisable monomer of 10wt%, the azo chipal compounds of 0.8wt%, the light trigger benzophenone of 5.0wt% and the light trigger benzoin isopropyl ether of 5.0wt% carry out blend, obtain having the liquid crystal compound system of very wide N* phase temperature range, earlier the liquid crystal compound system is poured under 100 ℃ of conditions in the above-mentioned liquid crystal cell that passes through surperficial parallel friction orientation in advance, obtain corresponding thin-film material sample, (described ultraviolet light intensity is 3mw/cm to use UV-light then under 20 ℃ condition
2, described ultraviolet light wavelength is 365nm) and irradiation is after 40 minutes, makes the polymerization of mixed liquid crystal system form macromolecule network, obtains having the liquid-crystal film material of wide wave reflection.Experimental result shows, the reflected range of the covered 1000nm～2200nm of the liquid-crystal film material with wide wave reflection that makes.
The structural formula of the liquid crystal liquid crystal property polymerisable monomer described in the present embodiment is as follows:
The structural formula of the azo chipal compounds described in the present embodiment is as follows:
At first ito glass is cleaned up, the thickness of making the parallel friction orientation processing of internal surface process is the liquid crystal cell of 10 μ m, and is standby;
Take by weighing the nematic liquid crystal SLC1717 of raw material 70wt% according to mass percent, the chipal compounds CB15 of 12wt%, the liquid crystal liquid crystal property polymerisable monomer of 14wt%, the azo chipal compounds of 1.2wt%, the light trigger benzophenone of 0.8wt% and the light trigger benzoin isopropyl ether of 2.0wt% (light trigger 651) carry out blend, obtain having the liquid crystal compound system of very wide N* phase temperature range, earlier the liquid crystal compound system is poured under 100 ℃ of conditions in the above-mentioned liquid crystal cell that passes through surperficial parallel friction orientation in advance, obtain corresponding thin-film material sample, (described ultraviolet light intensity is 4mw/cm to use UV-light then under 25 ℃ condition
2, described ultraviolet light wavelength is 365nm) and irradiation is after 40 minutes, makes the polymerization of mixed liquid crystal system form macromolecule network, obtains having the liquid-crystal film material of wide wave reflection.Experimental result shows, the reflected range of the covered 1000nm～2000nm of the liquid-crystal film material with wide wave reflection that makes.
The structural formula of the liquid crystal liquid crystal property polymerisable monomer described in the present embodiment is as follows:
The structural formula of the azo chipal compounds described in the present embodiment is as follows:
Embodiment 11
Take by weighing the nematic liquid crystal SLC1717 of raw material 75wt% according to mass percent, the chipal compounds CB15 of 9.0wt%, the liquid crystal liquid crystal property polymerisable monomer of 15wt%, the azo chipal compounds of 0.4wt%, the light trigger benzoin isopropyl ether of 0.6wt% (light trigger 651) carries out blend, obtain having the liquid crystal compound system of very wide N* phase temperature range, with the plastics film that passes through surperficial parallel friction orientation in advance the above-mentioned liquid crystal compound system that is mixed that obtains is pressed into film, adopt the thickness of separation pad or glass microballon control liquid crystal layer again in the scope of 10 μ m～300 μ m, prepare corresponding film sample, (described ultraviolet light intensity is 1mw/cm to use UV-light then under 45 ℃ condition
2, described ultraviolet light wavelength is 365nm) and irradiation is after 30 minutes, makes the polymerization of mixed liquid crystal system form macromolecule network, obtains having the liquid-crystal film material of wide wave reflection.Experimental result shows, the reflected range of the covered 1000nm～1800nm of the liquid-crystal film material with wide wave reflection that makes.
The structural formula of the liquid crystal liquid crystal property polymerisable monomer described in the present embodiment is as follows:
The structural formula of the azo chipal compounds described in the present embodiment is as follows:
Embodiment 12
Take by weighing the nematic liquid crystal SLC1717 of raw material 70wt% according to mass percent, the chipal compounds CB15 of 15wt%, the liquid crystal liquid crystal property polymerisable monomer of 12wt%, the azo chipal compounds of 1.0wt%, the light trigger benzoin isopropyl ether of 2.0wt% (light trigger 651) carries out blend, obtain having the liquid crystal compound system of very wide N* phase temperature range, with the plastics film that passes through surperficial parallel friction orientation in advance the above-mentioned liquid crystal compound system that is mixed that obtains is pressed into film, adopt the thickness of separation pad or glass microballon control liquid crystal layer again in the scope of 10 μ m～300 μ m, prepare corresponding film sample, (described ultraviolet light intensity is 1mw/cm to use UV-light then under 45 ℃ condition
2, described ultraviolet light wavelength is 365nm) and irradiation is after 30 minutes, makes the polymerization of mixed liquid crystal system form macromolecule network, obtains having the liquid-crystal film material of wide wave reflection.Experimental result shows, the reflected range of the covered 1000nm～1700nm of the liquid-crystal film material with wide wave reflection that makes.
The structural formula of the liquid crystal liquid crystal property polymerisable monomer described in the present embodiment is as follows:
The structural formula of the azo chipal compounds described in the present embodiment is as follows:
Embodiment 13
At first ito glass is cleaned up, the thickness of making the parallel friction orientation processing of internal surface process is the liquid crystal cell of 10 μ m～300 μ m, and is standby;
Take by weighing the nematic liquid crystal SLC1717 of raw material 75wt% according to mass percent, the chipal compounds R1011 of 5.0wt%, the liquid crystal liquid crystal property polymerisable monomer of 18wt%, the azo chipal compounds of 1.4wt% and the light trigger benzophenone of 0.6wt% are carried out blend, obtain having the liquid crystal compound system of very wide N* phase temperature range, earlier the liquid crystal compound system is poured under 100 ℃ of conditions in the above-mentioned liquid crystal cell that passes through surperficial parallel friction orientation in advance, obtain corresponding thin-film material sample, (described ultraviolet light intensity is 2.0mw/cm to use UV-light then under 40 ℃ condition
2, described ultraviolet light wavelength is 365nm) and irradiation is after 30 minutes, makes the polymerization of mixed liquid crystal system form macromolecule network, obtains having the liquid-crystal film material of wide wave reflection.Experimental result shows, the reflected range of the covered 1000nm～1900nm of the liquid-crystal film material with wide wave reflection that makes.
The structural formula of the liquid crystal liquid crystal property polymerisable monomer described in the present embodiment is as follows:
The structural formula of the azo chipal compounds described in the present embodiment is as follows:
Reference examples 1
At first ito glass is cleaned up, the thickness of making the parallel friction orientation processing of internal surface process is the liquid crystal cell of 10 μ m, and is standby;
Be that the ratio of 15.00wt%:9.60wt%:75.00wt%:0.40wt% carry out blend with the compound system of stock liquid crystallinity polymerisable monomer C6M, chiral compound S 811, small molecules nematic liquid crystal SLC1717 and light trigger 651 according to mass ratio according to mass percent, obtain having the liquid crystal compound system of very wide N* phase temperature range; Earlier the liquid crystal compound system is poured under 100 ℃ of conditions in the above-mentioned liquid crystal cell that passes through surperficial parallel friction orientation in advance, obtain corresponding thin-film material sample, control temperature then and under 40 ℃ condition, use UV-light (described ultraviolet light intensity is 3mw/cm
2, described ultraviolet light wavelength is 365nm) and carry out irradiation after 30 minutes, make the polymerization of mixed liquid crystal system form macromolecule network, obtain liquid-crystal film material.The liquid-crystal film material that obtains is tested, and experimental result shows: the reflection wave that makes liquid-crystal film material is positioned at about 1300nm, and reflection wave wide very narrow (about 130nm), specifically as shown in Figure 4.
In this reference examples used nematic liquid crystal (Nematic LC) SLC-1717 buy from Shijiazhuang Yongshenghuaqing Liquid Crystal Co., Ltd (Yongsheng Huatsing Liquid Crystal Co., Ltd), the n of described SLC-1717
o=1.519, n
e=1.720,
The structural formula of the chiral compound S 811 described in this reference examples is as follows:
The structural formula of liquid crystal liquid crystal property polymerisable monomer C6M described in this reference examples is as follows:
The structural formula of the light trigger 651 described in the present embodiment is as follows:
As can be seen from Figure 1, the variation diagram that reduces along with the prolongation of ultraviolet light irradiation time (irradiation time) of the helically twisted power of azo chipal compounds 2C of the present invention (Helical Twisting Powers).
Specific embodiment described in the present invention only is that the present invention's spirit is illustrated.Those skilled in the art can make various modifications or replenish or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.
Although the present invention has been made detailed explanation and has quoted some specific embodiments as proof, to those skilled in the art, only otherwise leave that the spirit and scope of the present invention can be done various variations or correction is obvious.
Claims (10)
1. preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection is characterized in that this method may further comprise the steps:
A, be that the nematic liquid crystal of 65wt%～85wt%, the chipal compounds that mass percent is 5.0wt%～15wt%, the liquid crystal liquid crystal property polymerisable monomer that mass percent is 8.0wt%～20wt% are mixed evenly with mass percent, then, the azo chipal compounds and the mass percent that add mass percent again and be 0.2wt%～1.5wt% are the light trigger of 0.01wt%～10wt%, be mixed, obtain the mixed liquid crystal system;
B, the above-mentioned mixed liquid crystal system that obtains is injected the liquid crystal cell that passes through surperficial parallel friction orientation in advance, prepare corresponding film sample;
C, the film sample that step B is obtained carry out ultraviolet light irradiation in the cholesteryl phase temperature range, make the polymerization of mixed liquid crystal system form macromolecule network, obtain having the polymer stabilizing liquid-crystal film material of wide wave reflection.
2. according to the described preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection of claim 1, it is characterized in that the chirality azo-compound described in the steps A is selected from one or more in the following compound:
N is selected from 2,4,6,8,10 or 12 described in the formula I;
N is selected from 2,4,6,8,10 or 12 described in the formula II;
N is selected from 2,4,6,8,10 or 12 described in the formula III.
3. the preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection according to claim 2, it is characterized in that the described chipal compounds of steps A is selected from one or more in chiral compound S 811, chipal compounds R811, chipal compounds R1011, chipal compounds CB15 and the chiral compound S 1011.
4. according to the described preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection of claim 2, it is characterized in that described liquid crystal liquid crystal property polymerisable monomer is selected from one or more in the following compound:
5. according to the described preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection of claim 2, it is characterized in that described light trigger is selected from one or both in benzoin isopropyl ether and the benzophenone.
6. according to the described preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection of claim 2, it is characterized in that described nematic liquid crystal is selected from nematic liquid crystal SLC1717.
7. according to any described preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection of claim 1-6, it is characterized in that step B adopts following method to replace:
With the plastics film that passes through surperficial parallel friction orientation in advance the liquid crystal compound system that is mixed that above-mentioned steps A obtains is pressed into film, with the thickness of separation pad or glass microballon control liquid crystal layer, prepares corresponding film sample again.
8. according to any described preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection of claim 1-6, it is characterized in that the ultraviolet light wavelength described in the step C is 365nm, ultraviolet ray intensity is 1 μ W/cm
2～5mW/cm
2, the ultraviolet light irradiation time is 1 minute～1 hour.
9. according to any described preparation method with polymkeric substance thing steady liquid-crystal film material of wide wave reflection of claim 1-6, it is characterized in that the temperature of the ultraviolet light irradiation described in the step C is 35 ℃～45 ℃.
10. according to any described preparation method with polymer stabilizing liquid-crystal film material of wide wave reflection of claim 1-6, it is characterized in that the thickness of described liquid-crystal film material is 10 μ m～300 μ m.
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