CN104263384A - Polymer stabilized blue phase liquid crystal composition as well as preparation method and application of liquid crystal composition - Google Patents
Polymer stabilized blue phase liquid crystal composition as well as preparation method and application of liquid crystal composition Download PDFInfo
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Abstract
The invention discloses a polymer stabilized blue phase liquid crystal composition as well as a preparation method and application of the liquid crystal composition. The liquid crystal composition comprises a component I, a component II and a component III, wherein the component I is a nematic phase liquid crystal which meets the following conditions: delta n is 0.13-0.2, and delta epsilon is 25-50; the component II is a chiral compound; the component III is a product which is prepared from a monomer in a photopolymerization manner. According to the liquid crystal composition disclosed by the invention, photopolymerization is initiated from a polymer monomer compound III by using a photoinitiator so as to form stable combination of the polymer, the chiral compound and a liquid crystal main body, so that the blue phase liquid crystal material is formed, the blue phase width of the blue phase liquid crystal material is effectively widened, for example, greater than 100 DEG C, and the blue phase temperature area of the blue phase liquid crystal material is widened to be extreme low temperature, such as at least -30 DEG C, so that the application range of the blue phase liquid crystal material is widened.
Description
Technical field
The invention belongs to Material Field, relate to a kind of polymer stabilizing blue-phase liquid crystal composition and preparation method thereof and application.
Background technology
Blue phase liquid crystal technique of display (Blue Phase Liquid Crystal is hereinafter referred to as BPLC), its distinctive photoelectric response pattern and photoelectric response speed make it have wide development space in flat display field.Compared to available liquid crystal material, blue phase liquid crystal has the following advantages: (1) has the time of response of sub-millisecond; (2) do not need oriented layer, can greatly simplify tube-making process process; (3) without being optical isotropy under electric field, therefore there is broad visual angle of cutting symmetry; (4) insensitive to the thickness of liquid crystal cell, be suitable for making large size display screen.But because indigo plant generally occurs and narrow temperature between cholesteryl phase and isotropic phase mutually, and this temperature is higher, hinders the application of blue phase liquid crystal.The existing method widening blue phase temperature range has nanoparticle doped method, banana liquid crystal doping method, polymer stabilizing method and itself has the method for the blue phase of wide temperature.
Although nanoparticle doped can widen the interval of blue phase with banana molecular dopant, be but difficult to indigo plant to be stabilized in room temperature range mutually, be therefore unfavorable for the practicality of blue phase liquid crystal.Although the liquid crystal itself with the blue phase of wide temperature has the interval of 44 DEG C at normal temperatures, the condition forming this blue phase is harsh, is also unfavorable for its practical application.Polymer stabilizing method has the potentiality obtaining the blue phase scope of ultra-wide, and by the regulation and control of liquid crystal and polymkeric substance, can adjusting function easily, is expected to the main force becoming liquid-crystal display of future generation.
Polymer stabilizing blue phase liquid crystal material is made up of liquid crystal material, chiral material, polymer materials three part.Will meet specific inductivity respectively large, viscosity is low, good stability; Helical twisting power is large, and pitch is good with temperature dependency; Fixed action is had to blue phase lattice after polymerization.Present stage polymer stabilizing blue phase liquid crystal material also exist some problems to be improved as: driving voltage is higher; Viscosity of material is comparatively large, is unfavorable for processing; There is hysteresis phenomenon; Polymer network is aging.
Summary of the invention
The object of this invention is to provide a kind of polymer stabilizing blue-phase liquid crystal composition and preparation method thereof and application.
Liquid-crystal composition provided by the invention, comprises component I, component I I and component III;
Wherein, described component I is the nematic liquid crystal of satisfied following condition: △ n is 0.13 ~ 0.2; △ ε is 25 ~ 50;
Described component I is specially that △ n is 0.156, △ ε is the nematic liquid crystal of 33.6, and production code member is P70-003 mixed crystal, can purchased from Shijiazhuang Chengzhi Yonghua Display Materials Co., Ltd.;
Component I I is selected from least one in following chipal compounds:
Shown in above-mentioned, compound is chipal compounds, and for the chipal compounds of often kind of structure, its chiral centre can be S type also can be R type, and two kinds of configurations all can use respectively, but can not by used in combination for the homostructural chipal compounds of R, S configuration.
Wherein,
be numbered R5011;
Described component III is carry out by component A and B component the product that photopolymerization obtains; The mass ratio of described component A and B component is 1:4-4:1, is specially 3:4,4:4,1:4,1-3:4,3-4:4 or 1-4:4;
Wherein, described component A is selected from least one in following compound:
Described B component is selected from least one in compound shown in compound and C6M shown in RM257:
In above-mentioned liquid-crystal composition, described component III accounts for 5% ~ 12% of described liquid-crystal composition gross weight, is specially 5%, 7% or 5-7%;
The mass ratio of described component I and component I I is 50 ~ 99:2 ~ 30, is specially 93:41.6,95:35.5,93:45,93-95:35.5-45.
Described liquid-crystal composition also comprises light trigger;
Described light trigger is specially ultraviolet initiator;
Described ultraviolet initiator is more specifically following compound:
IGRACURE184、
Described light trigger accounts for 0.01 ~ 0.08% of described liquid-crystal composition gross weight, is specially 0.03-0.08%, is specially 0.047% or 0.03% or 0.03%-0.047%.
The temperature range that the indigo plant of described liquid-crystal composition exists mutually is greater than 100 DEG C; Wherein, the implication of the blue temperature range existed mutually is as follows: liquid crystal watch reveals the temperature range of the character of blue phase phase;
The lowest temperature value of the blue phase warm area of described liquid-crystal composition at least reaches subzero 30 DEG C.
The method of the described liquid-crystal composition of preparation provided by the invention, after comprising the steps: that aforementioned each component is mixed and heated to isotropy according to proportioning, at the uniform velocity cools, then carries out the irradiation of ultraviolet constant temperature, obtain described liquid-crystal composition.
In aforesaid method, be heated in isotropy step, the final temperature of heating needs by being with the polarizing microscope of thermal station to confirm in advance, to be heated on clearing point 1 ~ 2 DEG C.
In described at the uniform velocity cooling step, rate of cooling is 5-0.2 DEG C/min, is specially 1 DEG C/min;
In described ultraviolet constant temperature irradiating step, temperature is in blue phase warm area scope or on blue phase warm area higher limit 5 DEG C; Time is 10 ~ 60 minutes; Energy is 0.2 ~ 10 milliwatt/square centimeter.
In addition, the application of the liquid-crystal composition that the invention described above provides in preparation blue phase liquid crystal material, also belongs to protection scope of the present invention.
Liquid-crystal composition provided by the invention polymer monomer composition I II is formed stabilization of polymer and chiral agent and liquid crystal host via light trigger initiation photopolymerization be compounded to form blue phase liquid crystal material, effectively widen that the indigo plant of blue phase liquid crystal material is mutually warm is widely such as greater than 100 DEG C, and the blue phase warm area of blue phase liquid crystal material is widened to extreme low temperature such as at least subzero 30 DEG C, widen the range of application of blue phase liquid crystal material.
Accompanying drawing explanation
Fig. 1 is the photoelectric curve of embodiment 1 gained liquid-crystal composition.
Fig. 2 is the photoelectric curve of embodiment 2 gained liquid-crystal composition.
Fig. 3 is the photoelectric curve of embodiment 3 gained liquid-crystal composition.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Described method is ordinary method if no special instructions.Described starting material all can obtain from open commercial sources if no special instructions.
The method preparing liquid-crystal composition provided by the invention, comprises the steps:
First, each component can be placed in container and adopt magnetic stirring apparatus via heated and stirred Homogeneous phase mixing, thus obtained mixture.
Secondly, heated mixt is to isotropy.Mixture is poured in liquid crystal cell, liquid crystal cell is placed on cold and hot platform and is heated to isotropy, with obtained isotropic mixture.
Afterwards, isotropic mixture is at the uniform velocity cooled.The liquid crystal cell containing isotropic mixture is continued to be placed on cold and hot platform, with cold and hot controlled cooling model speed, isotropic mixture is at the uniform velocity cooled to the lowest temperature value that blue phase warm area T1 ~ T2, T1 are this blue phase warm areas, T2 is the temperature upper limit of this blue phase warm area.
Then, cooled mixture is carried out the irradiation of ultraviolet constant temperature between 5 DEG C on blue phase temperature range lower value to blue phase temperature range higher limit, thus obtained blue phase liquid crystal material.That is, ultraviolet constant temperature irradiates the uv irradiating temperature T of cooled mixture
uVbe selected from blue phase warm area and 5 DEG C of contiguous isotropy warm areas thereof.In other words, uv irradiating temperature T
uVbetween lowest temperature value T1 and temperature upper limit T2+5 DEG C.It is preferred that uv irradiating temperature T
uVlower than temperature upper limit T2 about 1 ~ 2 DEG C.In addition, the time of ultraviolet irradiation that ultraviolet constant temperature irradiates cooled mixture is 10 ~ 60 minutes (min), and uv irradiating energy is 0.2 ~ 10 milliwatt/square centimeter (mw/cm2).Constant temperature via UV-light irradiates, and due to the effect of light trigger, polymer monomer mixture generation photopolymerization reaction, forms stabilization of polymer, and be compounded to form blue phase liquid crystal material with liquid crystal host and chiral reagent.
Blue phase warm area T1 ~ T2, the T1 of the blue phase liquid crystal material obtained by aforesaid method are the lowest temperature values of this blue phase warm area, and T2 is the temperature upper limit of this blue phase warm area.The indigo plant mutually warm wide (T2-T1) of the blue phase liquid crystal material obtained by aforesaid method is greater than 100 DEG C, and the mutually warm wide lowest temperature value T1 of indigo plant of blue phase liquid crystal material obtained by aforesaid method at least can reach subzero 30 DEG C, minimum can to subzero 196 DEG C.Therefore, the temperature of obtained blue phase liquid crystal material is wide extremely wide.
Embodiment 1
1) take the 400mg of compound shown in B component RM257 and component A TMPEOTA400mg in component III respectively and be placed in container such as penicillin bottle, put into little stirrer, on magnetic stirring apparatus, heated and stirred is even, make polymer monomer mixture stand-by, this monomer mixture after follow-up generation photopolymerization using as the component III in blue-phase liquid crystal composition.
2) the 930mg △ n taken respectively as component I is 0.156, △ ε be 33.6 nematic liquid crystal (production code member is P70-003, purchased from Shijiazhuang Chengzhi Yonghua Display Materials Co., Ltd.) and 70mg step 1) resulting polymers monomer mixture is placed in container such as penicillin bottle, and continues to take the chiral agent R5011 as component I I
41.6mg and ultraviolet initiator IGRACURE1840.5mg adds in penicillin bottle, adds stirrer in the vial, and on magnetic stirring apparatus, heated and stirred is even, forms mixing solutions.Afterwards, pour in liquid crystal cell by mixed uniformly mixing solutions, be placed on cold and hot platform by liquid crystal cell, be heated to isotropy, the final temperature of heating is confirmed in advance by the polarizing microscope of band thermal station, to be heated on clearing point 1 DEG C, with obtained isotropic mixture.Then, controlled with the speed slow cooling of 1 DEG C/min by cold and hot, so that isotropic mixture is at the uniform velocity cooled.After cooling, the blue phase warm area T1 ~ T2 of gained mixture is 54 ~ 61 DEG C.Then, the irradiation of UV-light constant temperature is carried out, uv irradiating temperature T
uVbe 58 DEG C, uv irradiating energy is 0.2mw/cm
2, time of ultraviolet irradiation is 60min, obtains blue-phase liquid crystal composition provided by the invention.
Afterwards, the blue phase warm area T1 ~ T2 measuring this blue-phase liquid crystal composition is-196 DEG C ~ 83 DEG C, and also namely the indigo plant of this blue-phase liquid crystal composition mutually warm wide (T2-T1) is 282 DEG C.
It is worth mentioning that, in view of the restriction of existing experimental installation, when experiment has measured subzero 30 DEG C, blue phase liquid crystal material all also has indigo plant to exist mutually, the existing equipment of temperature low again cannot complete, but is placed among liquid nitrogen by the blue phase liquid crystal material after polymerization, takes out and still have indigo plant to exist mutually after immersion, therefore the lowest temperature value T1 of the blue phase warm area T1 ~ T2 of blue phase liquid crystal material is at least subzero-196 DEG C, and indigo plant mutually warm wide (T2-T1) is greater than 282 DEG C.
The photoelectric curve of gained blue-phase liquid crystal composition as shown in Figure 1.
As shown in the figure, saturation voltage 58V, threshold voltage 23V.The liquid crystal comprehensive parameter tester that used test instrument is Changchun ray machine.
Embodiment 2
According to the step of embodiment 1, only the consumption of component A TMPEOTA is replaced with 100mg by 400mg, production code member is that the consumption that P70-003 △ n is 0.156, △ ε is the nematic liquid crystal of 33.6 replaces with 950mg by 930mg, the consumption of polymer monomer mixture replaces with 50mg by 70mg, the consumption of chiral agent R5011 replaces with 35.5mg by 41.6mg, the consumption of ultraviolet initiator IGRACURE184 replaces with 0.3mg by 0.5mg, and after cooling, the blue phase warm area T1 ~ T2 of gained mixture is 57 ~ 66 DEG C.Then, the irradiation of UV-light constant temperature is carried out, uv irradiating temperature T
uVbe 59 DEG C, uv irradiating energy is 0.2mw/cm
2, time of ultraviolet irradiation is 30min, obtains blue-phase liquid crystal composition provided by the invention.
Afterwards, the blue phase warm area T1 ~ T2 measuring this blue-phase liquid crystal composition is-196 DEG C ~ 88 DEG C, and also namely the indigo plant of this blue-phase liquid crystal composition mutually warm wide (T2-T1) is 290 DEG C.
It is worth mentioning that, in view of the restriction of existing experimental installation, when experiment has measured subzero 30 DEG C, blue phase liquid crystal material all also has indigo plant to exist mutually, the existing equipment of temperature low again cannot complete, but is placed among liquid nitrogen by the blue phase liquid crystal material after polymerization, takes out and still have indigo plant to exist mutually after immersion, therefore the lowest temperature value T1 of the blue phase warm area T1 ~ T2 of blue phase liquid crystal material is at least subzero-196 DEG C, and indigo plant mutually warm wide (T2-T1) is greater than 290 DEG C.
The photoelectric curve of gained blue phase liquid crystal is as shown in Figure 2:
As shown in the figure, saturation voltage 70V, threshold voltage 27V.The liquid crystal comprehensive parameter tester that used test instrument is Changchun ray machine.
Embodiment 3
According to the step of embodiment 1, only the consumption of component A TMPEOTA is replaced with 300mg by 400mg, the consumption of chiral agent R5011 replaces with 45mg by 41.6mg, and after cooling, the blue phase warm area T1 ~ T2 of gained mixture is 54 ~ 61 DEG C.Then, the irradiation of UV-light constant temperature is carried out, uv irradiating temperature T
uVbe 63 DEG C, uv irradiating energy is 0.2mw/cm2, and time of ultraviolet irradiation is 60min, obtains blue-phase liquid crystal composition provided by the invention.
Afterwards, the blue phase warm area T1 ~ T2 measuring this blue-phase liquid crystal composition is-30 DEG C ~ 83 DEG C, and also namely the indigo plant of this blue-phase liquid crystal composition mutually warm wide (T2-T1) is 113 DEG C.
Therefore, on the mutually interval ceiling temperature of indigo plant certain temperature interval in ultra-violet curing still can obtain the blue phase of polymer stabilizing.
The photoelectric curve of gained blue-phase liquid crystal composition as shown in Figure 3.
As shown in the figure, saturation voltage 80V, threshold voltage 36V.The liquid crystal comprehensive parameter tester that used test instrument is Changchun ray machine.
Embodiment 4
According to the step of embodiment 1, only the consumption of component A TMPEOTA is replaced with 300mg by 400mg, after cooling, the blue phase warm area T1 ~ T2 of gained mixture is 54 ~ 61 DEG C.Then, the irradiation of UV-light constant temperature is carried out, uv irradiating temperature T
uVbe 58 DEG C, uv irradiating energy is 10mw/cm
2, time of ultraviolet irradiation is 60min, obtains blue-phase liquid crystal composition provided by the invention.
Afterwards, the blue phase warm area T1 ~ T2 measuring this blue-phase liquid crystal composition is-30 DEG C ~ 83 DEG C, and also namely the indigo plant of this blue-phase liquid crystal composition mutually warm wide (T2-T1) is 113 DEG C.Therefore, the stronger ultra-violet curing of energy is used still can to obtain the blue phase of polymer stabilizing.
Embodiment 5
According to the step of embodiment 1, only compound shown in B component RM257 is replaced with 200mg by 400mg, component A TMPEOTA 400mg replaces with vinylformic acid trifluoro ethyl ester 150mg, the consumption of chiral agent R5011 replaces with 41.7mg by 41.6mg, and after cooling, the blue phase warm area T1 ~ T2 of gained mixture is 56 ~ 63 DEG C.Then, the irradiation of UV-light constant temperature is carried out, uv irradiating temperature T
uVbe 60 DEG C, uv irradiating energy is 0.2mw/cm
2, time of ultraviolet irradiation is 60min, obtains blue-phase liquid crystal composition provided by the invention.
Afterwards, the blue phase warm area T1 ~ T2 measuring this blue-phase liquid crystal composition is-30 DEG C ~ 82 DEG C, and also namely the indigo plant of this blue-phase liquid crystal composition mutually warm wide (T2-T1) is 112 DEG C.Prove that fluorine-containing polymer monomer still may be used for the blue phase of polymer stabilizing.
Embodiment 6
According to the step of embodiment 1, only compound shown in B component RM257 is replaced with 200mg by 400mg, component A TMPEOTA 400mg replaces with lauryl acrylate 150mg, the consumption of chiral agent R5011 replaces with 41.7mg by 41.6mg, and after cooling, the blue phase warm area T1 ~ T2 of gained mixture is 55 ~ 62 DEG C.Then, the irradiation of UV-light constant temperature is carried out, uv irradiating temperature T
uVbe 60 DEG C, uv irradiating energy is 0.2mw/cm
2, time of ultraviolet irradiation is 60min, obtains blue-phase liquid crystal composition provided by the invention.
Afterwards, the blue phase warm area T1 ~ T2 measuring this blue-phase liquid crystal composition is-30 DEG C ~ 83 DEG C, and also namely the indigo plant of this blue-phase liquid crystal composition mutually warm wide (T2-T1) is 113 DEG C.
Embodiment 7
According to the step of embodiment 1, only compound shown in B component RM257 is replaced with 200mg by 400mg, component A TMPEOTA 400mg replaces with Ethyl acrylate 150mg, the consumption of chiral agent R5011 replaces with 41.7mg by 41.6mg, and after cooling, the blue phase warm area T1 ~ T2 of gained mixture is 55 ~ 63 DEG C.Then, the irradiation of UV-light constant temperature is carried out, uv irradiating temperature T
uVbe 60 DEG C, uv irradiating energy is 0.2mw/cm
2, time of ultraviolet irradiation is 60min, obtains blue-phase liquid crystal composition provided by the invention.
Afterwards, the blue phase warm area T1 ~ T2 measuring this blue-phase liquid crystal composition is-30 DEG C ~ 84 DEG C, and also namely the indigo plant of this blue-phase liquid crystal composition mutually warm wide (T2-T1) is 114 DEG C.
Embodiment 8
According to the step of embodiment 1, only the 400mg of compound shown in B component RM257 is replaced with the 200mg of compound shown in C6M, component A TMPEOTA replaces with 150mg by 400mg, the consumption of chiral agent R5011 replaces with 41.7mg by 41.6mg, and after cooling, the blue phase warm area T1 ~ T2 of gained mixture is 56 ~ 65 DEG C.Then, the irradiation of UV-light constant temperature is carried out, uv irradiating temperature T
uVbe 63 DEG C, uv irradiating energy is 0.2mw/cm
2, time of ultraviolet irradiation is 60min, obtains blue-phase liquid crystal composition provided by the invention.
Afterwards, the blue phase warm area T1 ~ T2 measuring this blue-phase liquid crystal composition is-30 DEG C ~ 82 DEG C, and also namely the indigo plant of this blue-phase liquid crystal composition mutually warm wide (T2-T1) is 112 DEG C, proves that two kinds of polymer monomer B component all have the effect of stable blue phase.
In sum, in blue-phase liquid crystal composition provided by the invention, component III causes photopolymerization by light trigger and forms stabilization of polymer and be combined into blue phase liquid crystal material with liquid crystal host and chiral reagent, widely 100 DEG C are such as greater than so that the indigo plant effectively widening blue phase liquid crystal material is mutually warm, and the blue phase warm area of blue phase liquid crystal material is widened at most can to extreme low temperature such as at least subzero 196 DEG C, thus realize the application of blue phase liquid crystal under extreme low temperature condition, to increase the range of application of blue phase liquid crystal material.
Above blue phase liquid crystal material provided by the present invention is filled a prescription, and adopt this blue phase liquid crystal material made by blue phase liquid crystal material formula and preparation method thereof to be described in detail, apply specific case herein to set forth principle of the present invention and embodiment, the explanation of above embodiment just understands method of the present invention and core concept thereof for helping; Meanwhile, for one of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, in sum, this description should not be construed as limitation of the present invention.
Claims (7)
1. a liquid-crystal composition, comprises component I, component I I and component III;
Wherein, described component I is the nematic liquid crystal of satisfied following condition: △ n is 0.13 ~ 0.2; △ ε is 25 ~ 50; Component I I is selected from least one in following chipal compounds:
Described component III is carry out by component A and B component the product that photopolymerization obtains;
Wherein, described component A is selected from least one in following compound:
Described B component is selected from least one in compound shown in compound and C6M shown in RM257:
2. composition according to claim 1, is characterized in that: in described component III, and the mass ratio of component A and B component is 1:4 ~ 4:1, is specially 3:4;
Described component III accounts for 5% ~ 12% of described liquid-crystal composition gross weight;
The mass ratio of described component I and component I I is 50 ~ 99:2 ~ 30.
3. composition according to claim 1 and 2, is characterized in that: described liquid-crystal composition also comprises light trigger; Described light trigger is specially ultraviolet initiator; Described ultraviolet initiator is more specifically following compound:
IGRACURE184 or
Described light trigger accounts for 0.01 ~ 0.08% of described liquid-crystal composition gross weight, is specially 0.03-0.08%.
4., according to the arbitrary described composition of claim 1-3, it is characterized in that: the temperature range that the indigo plant of described liquid-crystal composition exists mutually is greater than 100 DEG C;
The lowest temperature value of the blue phase warm area of described liquid-crystal composition at least reaches subzero 30 DEG C.
5. prepare the method for the arbitrary described liquid-crystal composition of claim 1-4 for one kind, after comprising the steps: that arbitrary for claim 1-4 described each component is mixed and heated to isotropy according to proportioning, at the uniform velocity cool, then carry out the irradiation of ultraviolet constant temperature, obtain described liquid-crystal composition.
6. method according to claim 5, is characterized in that: described in be heated in isotropy step, the final temperature of heating is on clearing point 1 ~ 2 DEG C
In described at the uniform velocity cooling step, rate of cooling is 5-0.2 DEG C/min, is specially 1 DEG C/min;
In described ultraviolet constant temperature irradiating step, temperature is in blue phase warm area scope or on blue phase warm area higher limit 5 DEG C; Time is 10 ~ 60 minutes; Energy is 0.2 ~ 10 milliwatt/square centimeter.
7. the application of the arbitrary described liquid-crystal composition of claim 1-5 in preparation blue phase liquid crystal material.
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