CN116120942B - Fast response liquid crystal composition for AR display and preparation method thereof - Google Patents
Fast response liquid crystal composition for AR display and preparation method thereof Download PDFInfo
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- CN116120942B CN116120942B CN202310195478.3A CN202310195478A CN116120942B CN 116120942 B CN116120942 B CN 116120942B CN 202310195478 A CN202310195478 A CN 202310195478A CN 116120942 B CN116120942 B CN 116120942B
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- 239000004973 liquid crystal related substance Substances 0.000 title claims abstract description 101
- 239000000203 mixture Substances 0.000 title claims abstract description 79
- 230000004044 response Effects 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 108
- 239000000126 substance Substances 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 3
- 230000000630 rising effect Effects 0.000 description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 210000002858 crystal cell Anatomy 0.000 description 6
- 238000012360 testing method Methods 0.000 description 4
- 239000005388 borosilicate glass Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 125000001810 isothiocyanato group Chemical group *N=C=S 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000003190 augmentative effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
- C09K19/04—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit
- C09K19/06—Non-steroidal liquid crystal compounds
- C09K19/08—Non-steroidal liquid crystal compounds containing at least two non-condensed rings
- C09K19/10—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing at least two benzene rings
- C09K19/14—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing at least two benzene rings linked by a carbon chain
- C09K19/18—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing at least two benzene rings linked by a carbon chain the chain containing carbon-to-carbon triple bonds, e.g. tolans
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
- C09K19/04—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit
- C09K19/06—Non-steroidal liquid crystal compounds
- C09K19/08—Non-steroidal liquid crystal compounds containing at least two non-condensed rings
- C09K19/10—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing at least two benzene rings
- C09K19/14—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing at least two benzene rings linked by a carbon chain
- C09K19/18—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing at least two benzene rings linked by a carbon chain the chain containing carbon-to-carbon triple bonds, e.g. tolans
- C09K2019/181—Ph-C≡C-Ph
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Abstract
The application discloses a fast response liquid crystal composition for AR display and a preparation method thereof, and belongs to the technical field of liquid crystal materials. The liquid crystal composition comprises a compound T 1, a compound T 2, a compound T 3 and a compound T 4, wherein: compound T 1 has a chemical structure represented by formula (1): compound T 2 has a chemical structure represented by formula (2): Compound T 3 has a chemical structure represented by formula (3): Compound T 4 has a chemical structure represented by formula (4): The liquid crystal composition has the performances of high birefringence, large dielectric anisotropy, low viscoelasticity constant and the like, the response time of 2 pi phase modulation quantity under the drive of 5V voltage is 1.26-1.62ms, the specific resistance requirement required by AR display can be met, and the actual experience of AR display can be improved.
Description
Technical Field
The application belongs to the technical field of liquid crystal materials, and particularly relates to a fast response liquid crystal composition for AR display and a preparation method thereof.
Background
The liquid crystal on silicon micro device has functions of enlarging a field of view, suppressing chromatic aberration, and improving a frame rate, and can be used for Augmented Reality (AR) display. However, since it is generally difficult to satisfy the millisecond-level response speed with the liquid crystal material for the liquid crystal on silicon device, problems such as focus-convergence conflict, image motion blur and the like are easily generated in the AR display, resulting in generally poor actual effects and experiences of the AR display. Therefore, it is necessary to develop a millisecond-order response liquid crystal that satisfies AR display.
In the related art Wu Shicong et al disclose a nematic composition liquid crystal which is capable of achieving 2 pi phase modulation and response speed of 2.08ms under the drive of a temperature of 40 ℃ and an operating voltage of 5.38V, but which cannot meet the speed requirement of millisecond response and cannot meet the maximum drive voltage of a high resolution liquid crystal on silicon device; huang-MING PHILIP CHEN et al discloses a liquid crystal with high birefringence containing isothiocyanato, which can realize 2 pi phase modulation of sub-millisecond response under 5V driving voltage. However, since the resistivity of the isothiocyanato-containing high-birefringent liquid crystal is less than 10 11 Ω·cm, the requirements of the AR display for resistivity (> 10 12 Ω·cm) cannot be satisfied, and practical application of the isothiocyanato-containing high-birefringent liquid crystal in AR display is hindered.
Thus, the prior art does not achieve 2pi phase modulation of millisecond response at 5V drive voltages.
Disclosure of Invention
The application aims to provide a fast response liquid crystal composition for AR display and a preparation method thereof, and aims to solve the technical problem that the response speed of the existing liquid crystal for AR display is low.
In order to achieve the above object, the technical scheme of the present application is as follows:
The first aspect of the present application provides a fast response liquid crystal composition for AR display. The fast response liquid crystal composition for AR display comprises a compound T 1, a compound T 2, a compound T 3 and a compound T 4, wherein:
compound T 1 has a chemical structure represented by formula (1):
compound T 2 has a chemical structure represented by formula (2):
Compound T 3 has a chemical structure represented by formula (3):
Compound T 4 has a chemical structure represented by formula (4):
In an alternative implementation manner of the first aspect, the fast response liquid crystal composition for AR display is prepared by mixing a compound T 1, a compound T 2, a compound T 3 and a compound T 4.
In an alternative implementation of the first aspect, the mass ratio of compound T 1, compound T 2, compound T 3, and compound T 4 is 1:1:1:1-3.
In an alternative implementation manner of the first aspect, the raw material components include, based on 100% of the total mass of the liquid crystal composition:
15-25% of compound T 1; 15-25% of compound T 2;
15-25% of compound T 3; 25-50% of compound T 4.
In an alternative implementation manner of the first aspect, the raw material components include, based on 100% of the total mass of the liquid crystal composition:
25% of compound T 1; 25% of compound T 2;
25% of compound T 3; 25% of compound T 4.
The fast response liquid crystal composition for AR display provided by the application is composed of a wide-temperature-range liquid crystal component, a high-birefringence component, a large dielectric anisotropy component and a liquid crystal diluent component. Wherein, the compound T 3 is used as a liquid crystal component in a wide temperature zone, the melting point is 55.39 ℃, the clearing point is 103.51 ℃, and the nematic phase temperature zone is 48.12 ℃; compound T 2 as a high-birefringence component, whose birefringence was 0.285; compound T 4 as a component of large dielectric anisotropy, whose dielectric anisotropy is 13.16; compound T 1 is used as a liquid crystal diluent component, mainly for adjusting the melting point and viscosity of the mixed liquid crystal. The four compounds have the same molecular skeleton, exhibit the characteristics of high birefringence and low viscosity, can keep the advantages of high birefringence and low viscosity by mixing according to any proportion, are beneficial to realizing the fast response speed, can regulate and control the dielectric anisotropy and the working temperature range of the mixed liquid crystal according to the device performance requirement, and can easily realize the mixed liquid crystal with low driving voltage, 2 pi phase modulation and fast response speed.
In an alternative implementation of the first aspect, the gas chromatographic purities of compound T 1, compound T 2, compound T 3 and compound T 4 are all greater than 99.5% and the resistivities are all greater than 10 13 Ω cm.
A second aspect of the present application provides a method for preparing the fast response liquid crystal composition for AR display according to the first aspect, comprising the steps of:
And mixing the compound T 1, the compound T 2, the compound T 3 and the compound T 4, stirring at constant temperature until the four compounds are completely dissolved, and slowly cooling under full mixing to obtain the fast response liquid crystal composition for AR display.
In an alternative implementation of the second aspect, the temperature of the constant temperature stirring is 50-60 ℃ for 1h.
A third aspect of the present application provides the use of the fast response liquid crystal composition for AR display of the first aspect in AR display.
Compared with the prior art, the application has the advantages or beneficial effects that at least comprises:
According to the fast response liquid crystal composition for AR display provided by the first aspect of the application, through the compounding of the compound T 1, the compound T 2, the compound T 3 and the compound T 4, the liquid crystal composition has the performances of high double refraction index, large dielectric anisotropy, low viscoelasticity constant and the like, on one hand, the maximum working voltage of the 2 pi phase modulation quantity can be smaller than 5V, and the response time of the 2 pi phase modulation quantity under the driving of the voltage of 5V is 1.26-1.62ms; on the other hand, the operating temperature range (35-50 ℃) of the AR display device applied indoors can be met; the third aspect can meet the resistivity requirement required for AR display, and thus is expected to be applied to a liquid crystal on silicon device in AR display to improve display experience and effect.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the description of the embodiments will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained from these drawings without inventive effort for a person of ordinary skill in the art.
FIG. 1 is a graph showing the variation of the phase modulation amount with voltage of the liquid crystal S1 of the composition prepared in example 1 of the present application;
FIG. 2 is a graph showing the rising response time of the liquid crystal S1 of the composition prepared in example 1 of the present application at an operating voltage of 2.15V;
FIG. 3 is a graph showing the response time of the composition liquid crystal S1 prepared in example 1 of the present application at an operating voltage of 2.15V.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. It will be apparent that the described embodiments are some, but not all, embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
It should be noted that, in the examples of the present application, specific sources of the "compound T 1, compound T 2, compound T 3 and compound T 4" are not particularly limited, and may be obtained by commercially available methods or synthesized according to conventional methods well known in the related art. However, in order to improve the practical experience and effect of AR display, the gas chromatographic purities of the compounds T 1, T 2, T 3 and T 4 in the examples of the present application all reach 99.5% or more, and the resistivities are all greater than 10 13 Ω·cm.
Example 1
The embodiment provides a preparation method of a composition liquid crystal S1, which comprises the following steps of, based on 100% of total mass of the composition liquid crystal S1:
mixing a compound T 1%, a compound T 2%, a compound T 3% and a compound T 4%, putting the mixture into a borosilicate glass vessel, heating a flat plate to keep the temperature at 60 ℃, stirring and mixing for 1h until all solid matters are completely dissolved to be clear, slowly cooling, and assisting a mixing instrument to fully mix to obtain uniformly distributed composition liquid crystal S1;
Wherein, the compound T 1 has a chemical structure shown in formula (1):
compound T 2 has a chemical structure represented by formula (2):
Compound T 3 has a chemical structure represented by formula (3):
Compound T 4 has a chemical structure represented by formula (4):
In order to verify the physical properties of the composition liquid crystal S1, the performance of the composition liquid crystal S1 is tested according to the embodiment of the application, and the specific steps are as follows:
1.1 phase modulating voltage
After the composition liquid crystal S1 was poured into an antiparallel liquid crystal cell having a thickness of 5.17 μm, the phase modulation amount of the composition liquid crystal S1 in the liquid crystal cell was tested as a curve of voltage change at a temperature of 40℃to be shown in FIG. 1. Fig. 1 shows a voltage-dependent phase modulation amount of the liquid crystal composition S1.
As can be seen from fig. 1, the threshold voltage of the composition liquid crystal S1 is 1.3V, and the voltage to reach the 2pi phase modulation amount is 2.15V.
1.2 Response speed to rising at 2.15V Voltage
The rising response speed of the liquid crystal S1 of the composition at an operating voltage of 2.15V at a temperature of 40℃was measured, and the result is shown in FIG. 2. Among them, fig. 2 shows the rising response time of the composition liquid crystal S1 at an operating voltage of 2.15V.
As can be seen from fig. 2, the rising response time of the composition liquid crystal S1 at an operating voltage of 2.15V was 24.94ms.
1.3 Response speed to drop at 2.15V voltage
The response speed of the liquid crystal S1 of the test composition at an operating voltage of 2.15V was reduced at a temperature of 40℃and the result is shown in FIG. 3. Among them, fig. 3 shows the falling response time of the composition liquid crystal S1 at an operating voltage of 2.15V.
As can be seen from fig. 3, the response time of the composition liquid crystal S1 to the drop at 2.15V voltage was 11.57ms.
Response time at 1.42 pi phase modulation
The corresponding conversion of the measured rising response speed and falling response speed is carried out according to the literature (crystal, 2020,10,765) method, and it is known that the reflective liquid crystal on silicon device uses the composition liquid crystal S1, and then the response time of the measured 2 pi phase modulation amount is 1.26ms under the driving of the temperature of 40 ℃, the working wavelength of 633nm and the voltage of 5V, so that the phase type LCoS device can realize millisecond-level rapid response speed.
Example 2
The embodiment provides a preparation method of a composition liquid crystal S2, which comprises the following steps of, based on 100% of total mass of the composition liquid crystal S2:
Mixing a compound T 1%, a compound T 2%, a compound T 3% and a compound T 4% by weight, placing the mixture into a borosilicate glass vessel, heating the mixture to a constant temperature of 50 ℃, stirring and mixing for 1h until all solids are completely dissolved to be clear, slowly cooling, and assisting a mixing instrument to fully mix to obtain uniformly distributed composition liquid crystal S2;
Wherein, the compound T 1 has a chemical structure shown in formula (1):
compound T 2 has a chemical structure represented by formula (2):
Compound T 3 has a chemical structure represented by formula (3):
Compound T 4 has a chemical structure represented by formula (4):
In order to verify the physical properties of the composition liquid crystal S2, the performance of the composition liquid crystal S2 is tested according to the embodiment of the application, and the specific steps are as follows:
2.1 phase modulating voltage
After the composition liquid crystal S2 was poured into an antiparallel liquid crystal cell having a thickness of 5.12 μm, a curve of a phase modulation amount of the composition liquid crystal S2 in the liquid crystal cell with respect to a voltage was tested at a temperature of 40 ℃, and it was found that the threshold voltage of the composition liquid crystal S2 was 1.05V and a voltage reaching a2 pi phase modulation amount was 2.05V.
2.2 Response speed to rising at 2.05V Voltage
At a temperature of 40 ℃, the rising response speed of the composition liquid crystal S2 at an operating voltage of 2.05V is tested, and the test result shows that the rising response time of the composition liquid crystal S2 at the operating voltage of 2.05V is 17.96ms.
2.3 Response speed to drop at 2.05V Voltage
The response speed of the composition liquid crystal S2 to the decrease at the operating voltage of 2.05V was tested at a temperature of 40℃and the test result showed that the response time of the composition liquid crystal S2 to the decrease at the voltage of 2.05V was 8.95ms.
Response time at 2.42 pi phase modulation
The corresponding conversion of the measured rising response speed and falling response speed is carried out according to the literature (crystal 2020,10,765) method, and it is known that the reflective liquid crystal on silicon device uses the composition liquid crystal S2, and then the response time of the measured 2 pi phase modulation amount is 1.35ms under the driving of the temperature of 40 ℃, the working wavelength of 633nm and the voltage of 5V, so that the phase type LCoS device can realize millisecond-level rapid response speed.
Example 3
The embodiment provides a preparation method of a composition liquid crystal S3, which comprises the following steps of, based on 100% of total mass of the composition liquid crystal S3:
After mixing compound T 1.6%, compound T 2.7%, compound T 3.7% and compound T 4% and placing the mixture in a borosilicate glass vessel, stirring and mixing for 1h by heating a flat plate to constant temperature of 50 ℃ until all solid matters are completely dissolved to be clear, slowly cooling and fully mixing by an auxiliary mixing instrument to obtain uniformly distributed composition liquid crystal S3;
Wherein, the compound T 1 has a chemical structure shown in formula (1):
compound T 2 has a chemical structure represented by formula (2):
Compound T 3 has a chemical structure represented by formula (3):
Compound T 4 has a chemical structure represented by formula (4):
in order to verify the physical properties of the composition liquid crystal S3, the performance of the composition liquid crystal S3 is tested according to the embodiment of the application, and the specific steps are as follows:
3.1 phase modulating voltage
After the composition liquid crystal S3 was poured into an antiparallel liquid crystal cell having a thickness of 5.13 μm, a curve of the phase modulation amount of the composition liquid crystal S3 in the liquid crystal cell with respect to the voltage was tested at a temperature of 40℃and it was revealed that the threshold voltage of the composition liquid crystal S3 was 1.05V and the voltage at which the 2 pi phase modulation amount was reached was 1.95V.
3.2 Response speed to rising at 1.95V Voltage
The rising response speed of the composition liquid crystal S3 at an operating voltage of 1.95V was tested at a temperature of 40℃and the test result showed that the rising response time of the composition liquid crystal S3 at an operating voltage of 1.95V was 17.40ms.
3.3 Response speed to drop at 1.95V Voltage
The response speed of the composition liquid crystal S3 was measured at 40℃under an operating voltage of 1.95V, and the measurement result showed that the response time of the composition liquid crystal S3 under an operating voltage of 1.95V was 12.48ms.
Response time at 3.42 pi phase modulation
The corresponding conversion of the measured rising response speed and falling response speed is carried out according to the literature (crystal 2020,10,765) method, and it is known that the reflective liquid crystal on silicon device uses the composition liquid crystal S3, and then the response time of the measured 2 pi phase modulation amount is 1.62ms under the driving of the temperature of 40 ℃, the working wavelength of 633nm and the voltage of 5V, so that the phase type LCoS device can realize millisecond-level rapid response speed.
Various embodiments in this specification are described in an incremental manner, and identical or similar parts of the various embodiments are referred to each other, with each embodiment focusing on differences from the other embodiments.
The above embodiments are only for illustrating the technical solution of the present application, and not for limiting the present application; although the application has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced with equivalents; such modifications and substitutions do not depart from the spirit of the application.
Claims (7)
1. A fast response liquid crystal composition for AR display is characterized by comprising the following raw material components in percentage by weight relative to 100% of the total mass of the liquid crystal composition:
15-25% of compound T 1; 15-25% of compound T 2;
15-25% of compound T 3; 25-50% of compound T 4;
Wherein:
compound T 1 has a chemical structure represented by formula (1):
compound T 2 has a chemical structure represented by formula (2):
Compound T 3 has a chemical structure represented by formula (3):
Compound T 4 has a chemical structure represented by formula (4):
2. The fast response liquid crystal composition for AR display according to claim 1, which is prepared by mixing compound T 1, compound T 2, compound T 3 and compound T 4.
3. The fast response liquid crystal composition for AR display according to claim 2, wherein the mass ratio of compound T 1, compound T 2, compound T 3 and compound T 4 is 1:1:1:1-3.
4. The fast response liquid crystal composition for AR display according to claim 1, wherein the raw material components thereof comprise, based on 100% by mass relative to the total mass of the liquid crystal composition:
25% of compound T 1; 25% of compound T 2;
25% of compound T 3; 25% of compound T 4.
5. The fast response liquid crystal composition for AR display according to any one of claims 1 to 4, wherein the gas chromatographic purities of the compound T 1, the compound T 2, the compound T 3 and the compound T 4 are all more than 99.5%, and the resistivities are all more than 10 13 Ω & cm.
6. A method for preparing the fast response liquid crystal composition for AR display according to any one of claims 1 to 5, comprising:
And mixing the compound T 1, the compound T 2, the compound T 3 and the compound T 4, stirring at constant temperature until the four compounds are completely dissolved, and slowly cooling under full mixing to obtain the fast response liquid crystal composition for AR display.
7. The method according to claim 6, wherein the constant temperature stirring is carried out at 50-60 ℃ for 1 hour.
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| CN107474856A (en) * | 2017-09-21 | 2017-12-15 | 中国科学院长春光学精密机械与物理研究所 | A kind of mixing formula of Millisecond fast response liquid crystal material |
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| CN107721811A (en) * | 2017-11-06 | 2018-02-23 | 陕西师范大学 | A kind of biphenyl diluent of fluorine-type containing side and its synthetic method for high birefringence rate liquid crystal |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103725294A (en) * | 2013-12-19 | 2014-04-16 | 中国科学院长春光学精密机械与物理研究所 | Molecular design and mixing formula of quick liquid crystal material for liquid crystal wavefront corrector |
| CN107474856A (en) * | 2017-09-21 | 2017-12-15 | 中国科学院长春光学精密机械与物理研究所 | A kind of mixing formula of Millisecond fast response liquid crystal material |
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| CN107721811A (en) * | 2017-11-06 | 2018-02-23 | 陕西师范大学 | A kind of biphenyl diluent of fluorine-type containing side and its synthetic method for high birefringence rate liquid crystal |
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