CN109828401A - Quick response polymer stabilized cholesteric phase liquid crystal light valve based on hyperbranched monomer and preparation method thereof - Google Patents
Quick response polymer stabilized cholesteric phase liquid crystal light valve based on hyperbranched monomer and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of quick response polymer stabilized cholesteric phase liquid crystal light valve based on hyperbranched monomer, includes liquid crystal compound, is calculated in mass percent, contain in liquid crystal compound precursor: hyperbranched monomer 0.1~1%;Liquid crystal monomer 4~4.9%;Photoinitiator 0.2~0.4%;Chiral agent 0.1~10%;Liquid crystal 85~95%.The invention also discloses the preparation methods of the quick response polymer stabilized cholesteric phase liquid crystal light valve.The present invention, which introduces hyperbranched monomer into liquid crystal compound precursor, can be effectively reduced the response time of liquid crystal light valve, and can weaken the granular sensation phenomenon that liquid crystal light valve occurs in imaging process.
Description
Technical field
The present invention relates to liquid crystal material technical field more particularly to a kind of quick response polymer based on hyperbranched monomer
Stabilized cholesteric phase liquid crystal light valve and preparation method thereof.
Background technique
Currently, liquid crystal material has been widely applied in conventional display device field.With the development of science and technology and people
Improvement of living standard, said three-dimensional body is shown and the wearable popular direction shown as display device.
The display body of said three-dimensional body display system is made of multilayer liquid crystal light valve, by circuit drives liquid crystal light valve is existed
It is switched fast between scattering states and transparent state, it is steady that the refresh rate of light valve need to reach the picture that at least 48Hz or more could make
Determine flicker free;Further, since image need to pass through multilayer liquid crystal light valve, therefore light loss is very serious, and brightness reduction then will lead to figure
As smudgy clear;Therefore, said three-dimensional body display system needs the light valve of a kind of high transmittance and quick response.
And polymer stabilizing cholesteric phase (Polymer-stabilized Cholesteric Texture, PSCT) liquid crystal light
There is valve relatively high transmitance, biggish visual angle, faster response speed can realize that said three-dimensional body is shown.
The response time of PSCT liquid crystal light valve significantly affects the image quality that body is shown.It is not powered on PSCT liquid crystal
Light valve is in Focal conic state, then causes nematic state in field after power-up, the twisting resistance that the chiral agent in liquid crystal compound generates with polymerize
The anchoring dynamic balance that object network generates makes PSCT liquid crystal light valve be in stable Focal conic state, PSCT liquid crystal light valve rise time master
Electric field strength is depended on, and fall time then depends on chiral agent and is anchored to the twisting resistance and polymer grid of liquid crystal to liquid crystal
Relationship of vying each other between power, polymer network anchorage force have very important influence to the PSCT liquid crystal light valve response time.
But have the research to the PSCT liquid crystal light valve response time, focus mostly in by change polymer monomer type,
The monomer cure temperature and intensity of ultraviolet light carrys out the optimizer response time when solidifying.For example, bibliography (quick response light valve
In preparation and the application in real tri-dimension is shown, photoelectric project, in August, 2018 the 8th phase of volume 39) by adding in liquid crystal
A small amount of polymer and chiral object additive is added to prepare the polymer stabilized cholesteric phase liquid crystal light valve of quick response, ON state penetrates
Rate reaches 88%, and the response time is less than 3ms.It is applied to real tri-dimension display system, display picture is steady and audible, no sudden strain of a muscle
It is bright.
PSCT liquid crystal light valve is expected to due to transparent state transmitance with higher and faster response time wearable aobvious
Show that field is exhibited one's skill to the full.On the other hand, from after Googleglass and Microsoft Hololens publication, augmented reality (AR) becomes aobvious
The popular direction shown, and existing PSCT liquid crystal light valve is uneven since liquid crystal farmland size distribution unevenness will lead to scatter distributions,
Due to the limitation in terms of the AR special optical path shown and small size, need on PSCT liquid crystal light valve imaging amplify
(can be amplified 4~10 times), this leads to occur defect in imaging process, seriously affects imaging effect.
Summary of the invention
Quick response polymer stabilizing cholesteric phase (PSCT) liquid crystal light based on hyperbranched monomer that the present invention provides a kind of
Valve improves the response speed of PSCT liquid crystal light valve by introducing hyperbranched monomer in its liquid crystal compound precursor, weaken its
The granular sensation phenomenon occurred in imaging process.
Specific technical solution is as follows:
A kind of quick response polymer stabilized cholesteric phase liquid crystal light valve based on hyperbranched monomer includes liquid crystal mixing
Object is calculated in mass percent, and is contained in liquid crystal compound precursor:
Liquid crystal compound precursor forms liquid crystal compound after photocuring.In Light Curing, acted in particular light
Under, photoinitiator causes hyperbranched monomer and liquid crystal monomer polymerization, forms polymer, liquid crystal and chiral agent are anchored at polymer
Grid in.
The liquid crystal monomer be 4- (3- acryloxy propoxyl group) benzoic acid 2- methyl-1,4- phenyl ester (RM257), 1,
Bis- [4- (6- acryloxy hexyloxy) the benzoyloxy] -2- methylbenzenes (RM82) of 4-.
The hyperbranched monomer is the acrylic ester monomer of 3~8 functional groups.
The liquid crystal monomer polymerization that is introduced as of the hyperbranched monomer provides node, so that polymer network is more equal
Even, grid defect is reduced, and uniform polymer grid reduces its anchoring to liquid crystal so that PSCT remove electricity after liquid crystal in chirality
Faster restore from vertical TEXTURE STATE (H state) to conical texture state (FC state), and uniform polymeric web under agent effect
Lattice can make PSCT scattering states multidomain structure more uniform, and scattering imperfection reduces, and effectively weaken imaging particle sense problem.
Preferably, in the liquid crystal compound precursor, the gross mass percentage of hyperbranched monomer and liquid crystal monomer is 4.5
~6%.If monomer total amount is excessively high, monomer polymerization formation polymer network anchorage force is too strong, and liquid crystal cannot restore from H state to FC
State;If monomer total amount is too low, monomer polymerization forms polymer and has just fallen anchorage force deficiency, and liquid crystal is in chiral power and polymer grid anchor
Determine to be difficult to maintain FC state under the competitive relation of power, PSCT scattering strength is greatly reduced.
Further, in the liquid crystal compound precursor, hyperbranched monomer mass percentage is 0.2~0.6%, over-expense
It is too low to change content of monomer, it is difficult to play the role of regulating and controlling polymer network, hyperbranched content of monomer is excessively high, then monomer polymerization polymerize
Degree reduces, and formation polymer network aperture is excessive, causes the reduction of PSCT scattering strength.
It is further preferred that the hyperbranched monomer is that (manufacturer is the special material in Changxing to ETERCURE 6361-100
Expect Co., Ltd, product grade is ETERCURE 6361-100), pentaerythritol triacrylate (PETA), dipentaerythritol
Amyl-/at least one of hex- acrylic acid (DPHA) and pentaerythritol tetraacrylate (PETTA).
The liquid crystal monomer be 4- (3- acryloxy propoxyl group) benzoic acid 2- methyl-1,4- phenyl ester (RM257) and/
Or bis- [4- (6- acryloxy hexyloxy) the benzoyloxy] -2- methylbenzenes (RM82) of Isosorbide-5-Nitrae -.
Preferably, chiral agent distortion force constant (HTP value) is 30~120.Since liquid crystal screw pitch has been set, HTP
It is worth higher, then the chiral agent content of required addition is lower in liquid crystal compound, and liquid crystal compound physical property is (viscosity, limpid
Point transition temperature etc.) it is smaller by being influenced.
Further, the chiral agent is bis- [4- (trans- -4- pentylcyclohexyl) benzoic acid] (R) -1- phenyl -1,2-
Ethyl (R1011), (13BR) -5,6- dihydro -5- (trans- -4- propylcyclohexyl) -4H- dinaphtho [- H of 2,1-F:1 ', 2 ']
At least one of [1,5] dioxane nonyl tetraene (S5011) and TADDOL class chiral agent.
The present invention also provides the described quick response polymer stabilized cholesteric phase liquid crystal light valve based on hyperbranched monomer
Preparation method, comprising the following steps:
(1) the liquid crystal compound precursor is prepared;
(2) the liquid crystal compound precursor is poured into liquid crystal cell;
(3) apply alternating current to liquid crystal cell, while carrying out ultraviolet light solidification.
The excessively high liquid crystal that will cause of the ac frequency is difficult to respond, and ac frequency is too low, will cause liquid crystal list
Body vibration causes monomer polymerization to form defect and increases.
The excessively weak monomer that will cause of the ultraviolet light intensity combines not exclusively, and ultraviolet light intensity is too strong that it will cause liquid crystal and monomer
Mutually separation is excessively violent, causes the generation of monomer polymerization defect.
Preferably, the frequency of the alternating current is 1000~25000Hz, and voltage is 80~120V;The light of the ultraviolet light
It is by force 0.2~1mW/cm2。
Compared with prior art, the invention has the benefit that
The present invention, which introduces hyperbranched monomer into liquid crystal compound precursor, can be effectively reduced the response time of liquid crystal light valve,
And the granular sensation phenomenon that liquid crystal light valve occurs in imaging process can be weakened.
Detailed description of the invention
Fig. 1 is the AR light path schematic diagram for testing liquid crystal light valve imaging effect.
Fig. 2 is liquid crystal light valve voltage-transmittance curve figure made from Examples 1 to 3 and comparative example 1;
Fig. 3 is liquid crystal light valve response time-voltage curve made from Examples 1 to 3 and comparative example 1;
Fig. 4 is imaging effect figure of the liquid crystal light valve in AR optical path made from embodiment 3 and comparative example 1, wherein (a) is real
Example 3 is applied, (b) is comparative example 1;
Fig. 5 is liquid crystal light valve voltage-transmittance curve figure made from embodiment 4~6 and comparative example 2;
Fig. 6 is liquid crystal light valve response time-voltage curve made from embodiment 4~6 and comparative example 2;
Fig. 7 is liquid crystal light valve rise time-voltage curve made from embodiment 4~6 and comparative example 2;
Fig. 8 is liquid crystal light valve recovery time-voltage curve made from embodiment 4~6 and comparative example 2;
Fig. 9 is imaging effect figure of the liquid crystal light valve in AR optical path made from embodiment 6;
Figure 10 is liquid crystal light valve response time-voltage curve made from embodiment 7 and comparative example 1;
Figure 11 is liquid crystal light valve response time-voltage curve made from embodiment 8 and comparative example 1.
Specific embodiment
Examples 1 to 3
The preparation method of quick response polymer stabilizing cholesteric phase (PSCT) liquid crystal light valve based on hyperbranched monomer includes:
(1) by the hyperbranched monomer ETERCURE 6361-100 of eight functional groups, (manufacturer is the limited public affairs of Changxing special material
Department, product grade are ETERCURE 6361-100) with being sealed after methylene chloride 1:2000 in mass ratio dispersion, it is stirred using magnetic force
It mixes to obtain uniform dispersion liquid;
(2) by liquid crystal monomer 4- (3- acryloxy propoxyl group) benzoic acid 2- methyl-1,4- phenyl ester (RM257) uses dichloro
It is sealed after methane 1:1000 in mass ratio dispersion, obtains uniform dispersion liquid using magnetic agitation;
(3) by high twist force constant (HTP) chiral agent S5011 ((13BR) -5,6- dihydro -5- (trans- -4- cyclohexyl
Base) -4H- dinaphtho [- the H of 2,1-F:1 ', 2 '] [1,5] dioxane nonyl tetraene) dispersed with methylene chloride in mass ratio 1: 1000
After seal, obtain uniform dispersion liquid using magnetic agitation;
(4) hyperbranched monomer dispersion liquid, liquid crystal monomer dispersion liquid, chiral agent dispersing liquid are added to nematic liquid crystal (E7)
Liquid crystal compound is obtained, then is protected from light after photoinitiator 2- methoxyl group -1,2- diphenylethan (BME) is added to liquid crystal compound kind
Magnetic agitation, the methylene chloride dispersion liquid in removal system are used while system is heated to 65 DEG C;
(5) PSCT screw pitch is set as 600nm, and liquid crystal compound mass fraction shared by corresponding S5011 is 1.515%, liquid crystal
It is 0.2%, RM257 and hyperbranched monomer 6361-100 total amount that E7 proportion, which is 93.285%, BME proportion, in mixture
Remain 5% constant, in Examples 1 to 3, the mass fraction of hyperbranched monomer 6361-100 is respectively 0.2%, 0.4%, 0.6%;
(6) liquid crystal compound for obtaining step 4 pours into 10 μm of empty liquid crystal cells after being heated to clearing point (65 DEG C);
(7) applying frequency to liquid crystal cell both sides when solidifying is 1000Hz, the square wave alternating-current electricity that voltage is 100V;
(8) ultraviolet (UV) is selected to solidify PSCT, ultra-violet curing light intensity is all 0.5mW/cm2。
Comparative example 1
Difference from example 1 is that hyperbranched monomer is not added in liquid crystal compound, in liquid crystal compound
The mass fraction of RM257 is 5%.
Fig. 2 is voltage-transmittance curve figure of liquid crystal light valve made from Examples 1 to 3 and comparative example 1, it can be seen that
As hyperbranched content of monomer rises, larger amplitude variation does not occur for PSCT driving voltage.
Fig. 3 is the response time-voltage curve of liquid crystal light valve made from Examples 1 to 3 and comparative example 1, Ke Yiming
Aobvious to find out, with the rising of hyperbranched content of monomer, the PSCT response time is reduced.
Over-expense (is not added using optical test path embodiment 3 (hyperbranched content of monomer 0.6%) shown in FIG. 1 and comparative example 1
Change monomer) made from liquid crystal light valve imaging effect, as a result as shown in figure 4, wherein (a) be embodiment 3, (b) be comparative example 1.
By PSCT liquid crystal light valve obtained by the present invention at image by the way that 4~10 can be amplified after the AR optical path of Fig. 1
Times, this meeting is so that imaged particles sense caused by the intrinsic scattering imperfection of PSCT liquid crystal light valve is arrived by eye-observation.It can from Fig. 4
The PSCT imaging that hyperbranched monomer is added out is finer and smoother, and imaging particle sense reduces.
Embodiment 4~6
The preparation method of quick response polymer stabilizing cholesteric phase (PSCT) liquid crystal light valve based on hyperbranched monomer includes:
(1) by the hyperbranched monomer of eight functional groups (ETERCURE 6361-100) with 1: 2000 point in mass ratio of methylene chloride
It is sealed after dissipating, obtains uniform dispersion liquid using magnetic agitation;
(2) by liquid crystal monomer 4- (3- acryloxy propoxyl group) benzoic acid 2- methyl-1,4- phenyl ester (RM257) uses dichloro
Methane in mass ratio 1: 1000 seals after dispersing, and obtains uniform dispersion liquid using magnetic agitation;
(3) close after dispersing high twist force constant (HTP) chiral agent (S5011) with methylene chloride in mass ratio 1: 1000
Envelope, obtains uniform dispersion liquid using magnetic agitation;
(4) hyperbranched monomer dispersion liquid, liquid crystal monomer dispersion liquid, chiral agent dispersing liquid are added to nematic liquid crystal (E7)
It obtains liquid crystal compound, then is added after photoinitiator (BME) to liquid crystal compound kind and to be protected from light while system is heated to 65 DEG C
Methylene chloride dispersion liquid using magnetic agitation, in removal system;
(5) PSCT screw pitch is set as 600nm, and liquid crystal compound mass fraction shared by corresponding S5011 is 1.515%, liquid crystal
It is 0.2%, RM257 and hyperbranched monomer 6361-100 total amount that E7 proportion, which is 93.285%, BME proportion, in mixture
Remain 5% constant, in embodiment 4~6, the mass fraction of hyperbranched monomer 6361-100 is respectively 0.2%, 0.4%, 0.6%;
(6) liquid crystal compound for obtaining step 4 pours into 10 μm of empty liquid crystal cells after being heated to clearing point (65 DEG C);
(7) applying frequency to liquid crystal cell both sides when solidifying is 10000Hz, the square wave alternating-current electricity that voltage is 100V;
(8) ultraviolet (UV) is selected to solidify PSCT, ultra-violet curing light intensity is all 0.5mW/cm2。
Comparative example 2
The difference is that, hyperbranched monomer is not added in liquid crystal compound with embodiment 4, in liquid crystal compound
The mass fraction of RM257 is 5%.
Fig. 5 is voltage-transmittance curve figure of liquid crystal light valve made from embodiment 4~6 and comparative example 2, it can be seen that
As hyperbranched content of monomer rises, larger amplitude variation does not occur for PSCT driving voltage.
Fig. 6 is the response time-voltage curve of liquid crystal light valve made from embodiment 4~6 and comparative example 2, Ke Yiming
Aobvious to find out, with the rising of hyperbranched content of monomer, the PSCT response time is reduced.
Fig. 7 is the rise time-voltage curve of liquid crystal light valve made from embodiment 4~6 and comparative example 2, can be seen
The rise time does not rise with the content of monomer hyperbranched in liquid crystal compound and is changed out.
Fig. 8 is the recovery time-voltage curve of liquid crystal light valve made from embodiment 4~6 and comparative example 2, can be seen
Out with the rising of content of monomer hyperbranched in liquid crystal compound, PSCT recovery time is reduced.
Fig. 9 is imaging effect figure of the liquid crystal light valve in AR optical path (Fig. 1) made from embodiment 6, it can be seen that liquid crystal light
Valve imaging image quality is clear, and picture is uniformly without obvious image defects.
Embodiment 7
The preparation method of quick response polymer stabilizing cholesteric phase (PSCT) liquid crystal light valve based on hyperbranched monomer includes:
(1) after hyperbranched monomer pentaerythritol triacrylate (PETA) being dispersed with methylene chloride in mass ratio 1: 2000
Sealing, obtains uniform dispersion liquid using magnetic agitation;
(2) by liquid crystal monomer 4- (3- acryloxy propoxyl group) benzoic acid 2- methyl-1,4- phenyl ester (RM257) uses dichloro
Methane in mass ratio 1: 1000 seals after dispersing, and obtains uniform dispersion liquid using magnetic agitation;
(3) close after dispersing high twist force constant (HTP) chiral agent (S5011) with methylene chloride in mass ratio 1: 1000
Envelope, obtains uniform dispersion liquid using magnetic agitation;
(4) hyperbranched monomer dispersion liquid, liquid crystal monomer dispersion liquid, chiral agent dispersing liquid are added to nematic liquid crystal (E7)
It obtains liquid crystal compound, then is added after photoinitiator (BME) to liquid crystal compound kind and to be protected from light while system is heated to 65 DEG C
Methylene chloride dispersion liquid using magnetic agitation, in removal system;
(5) PSCT screw pitch is set as 600nm, and liquid crystal compound mass fraction shared by corresponding S5011 is 1.515%, liquid crystal
It is 0.2%, RM257 proportion is shared by 4.4%, PETA that E7 proportion, which is 93.285%, BME proportion, in mixture
Ratio is 0.6%;
(6) liquid crystal compound for obtaining step 4 pours into 10 μm of empty liquid crystal cells after being heated to clearing point (65 DEG C);
(7) applying frequency to liquid crystal cell both sides when solidifying is 1000Hz, the square wave alternating-current electricity that voltage is 100V;
(8) ultraviolet (UV) is selected to solidify PSCT, ultra-violet curing light intensity is all 0.5mW/cm2。
Figure 10 is the response time-voltage curve of liquid crystal light valve made from embodiment 7 and comparative example 1, it can be seen that
After PETA is added, there is apparent reduction in the response time of PSCT.
Embodiment 8
With embodiment 7 the difference is that, by the hyperbranched monomer pentaerythritol triacrylate in liquid crystal compound
(PETA) replace with hyperbranched monomer dipentaerythritol it is amyl-/hex- acrylic acid (DPHA), dosage and the same embodiment of other parameters
7。
Figure 11 is the response time-voltage curve of liquid crystal light valve made from embodiment 8 and comparative example 1, it can be seen that
After DPHA is added, there is apparent reduction in the response time of PSCT.
Technical solution of the present invention and beneficial effect is described in detail in embodiment described above, it should be understood that
Above is only a specific embodiment of the present invention, it is not intended to restrict the invention, it is all to be done in spirit of the invention
Any modification, supplementary, and equivalent replacement etc., should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of quick response polymer stabilized cholesteric phase liquid crystal light valve based on hyperbranched monomer, includes liquid crystal compound,
It is characterized in that, being calculated in mass percent, contain in liquid crystal compound precursor:
2. the quick response polymer stabilized cholesteric phase liquid crystal light valve according to claim 1 based on hyperbranched monomer,
It is characterized in that, the hyperbranched monomer is the acrylic ester monomer of 3~8 functional groups.
3. according to right want 2 described in the quick response polymer stabilized cholesteric phase liquid crystal light valve based on hyperbranched monomer, it is special
Sign is, the hyperbranched monomer is ETERCURE 6361-100, pentaerythritol triacrylate, dipentaerythritol it is amyl-/
At least one of hex- acrylic acid and pentaerythritol tetraacrylate.
4. the quick response polymer stabilized cholesteric phase liquid crystal light valve according to claim 1 based on hyperbranched monomer,
It is characterized in that, in the liquid crystal compound precursor, the gross mass percentage of hyperbranched monomer and liquid crystal monomer is 4.5~6%.
5. the quick response polymer stabilized cholesteric phase liquid crystal light valve according to claim 1 or 4 based on hyperbranched monomer,
It is characterized in that, hyperbranched monomer mass percentage is 0.2~0.6% in the liquid crystal compound precursor.
6. the quick response polymer stabilized cholesteric phase liquid crystal light valve according to claim 1 based on hyperbranched monomer,
It is characterized in that, the liquid crystal monomer is 4- (3- acryloxy propoxyl group) benzoic acid 2- methyl-1,4- phenyl ester and/or Isosorbide-5-Nitrae-
Bis- [4- (6- acryloxy hexyloxy) benzoyloxy] -2- methylbenzenes.
7. a kind of quick response polymer stabilizing cholesteric phase as described in any one of claims 1 to 6 based on hyperbranched monomer
The preparation method of liquid crystal light valve, which comprises the following steps:
(1) the liquid crystal compound precursor is prepared;
(2) the liquid crystal compound precursor is poured into liquid crystal cell;
(3) apply alternating current to liquid crystal cell, while carrying out ultraviolet light solidification.
8. the preparation of the quick response polymer stabilized cholesteric phase liquid crystal light valve according to claim 7 based on hyperbranched monomer
Method, which is characterized in that the frequency of the alternating current is 1000~25000Hz, and voltage is 80~120V;The light of the ultraviolet light
It is by force 0.2~1mW/cm2。
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