CN114605827A - Sensor material based on liquid crystal elastomer and application thereof - Google Patents
Sensor material based on liquid crystal elastomer and application thereof Download PDFInfo
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- CN114605827A CN114605827A CN202210223551.9A CN202210223551A CN114605827A CN 114605827 A CN114605827 A CN 114605827A CN 202210223551 A CN202210223551 A CN 202210223551A CN 114605827 A CN114605827 A CN 114605827A
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- 239000004997 Liquid crystal elastomers (LCEs) Substances 0.000 title claims abstract description 45
- 239000000463 material Substances 0.000 title claims abstract description 18
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 31
- 239000004917 carbon fiber Substances 0.000 claims abstract description 31
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 17
- -1 tetra (3-mercaptopropionic acid) pentaerythritol ester Chemical class 0.000 claims abstract description 11
- HCZMHWVFVZAHCR-UHFFFAOYSA-N 2-[2-(2-sulfanylethoxy)ethoxy]ethanethiol Chemical compound SCCOCCOCCS HCZMHWVFVZAHCR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004132 cross linking Methods 0.000 claims abstract description 9
- ISSYGWIDLYOJEN-UHFFFAOYSA-N [3-methyl-4-[4-(3-prop-2-enoyloxypropoxy)benzoyl]oxyphenyl] 4-(3-prop-2-enoyloxypropoxy)benzoate Chemical compound C=1C=C(OC(=O)C=2C=CC(OCCCOC(=O)C=C)=CC=2)C(C)=CC=1OC(=O)C1=CC=C(OCCCOC(=O)C=C)C=C1 ISSYGWIDLYOJEN-UHFFFAOYSA-N 0.000 claims abstract description 5
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 10
- WEHWNAOGRSTTBQ-UHFFFAOYSA-N dipropylamine Chemical compound CCCNCCC WEHWNAOGRSTTBQ-UHFFFAOYSA-N 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 7
- JOBBTVPTPXRUBP-UHFFFAOYSA-N [3-(3-sulfanylpropanoyloxy)-2,2-bis(3-sulfanylpropanoyloxymethyl)propyl] 3-sulfanylpropanoate Chemical compound SCCC(=O)OCC(COC(=O)CCS)(COC(=O)CCS)COC(=O)CCS JOBBTVPTPXRUBP-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000000178 monomer Substances 0.000 claims description 7
- 230000000977 initiatory effect Effects 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000002525 ultrasonication Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 8
- 239000011540 sensing material Substances 0.000 abstract description 7
- 239000000758 substrate Substances 0.000 abstract 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000000527 sonication Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
- C08G75/02—Polythioethers
- C08G75/04—Polythioethers from mercapto compounds or metallic derivatives thereof
- C08G75/045—Polythioethers from mercapto compounds or metallic derivatives thereof from mercapto compounds and unsaturated compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2381/02—Polythioethers; Polythioether-ethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a sensor material based on a liquid crystal elastomer and application thereof. The preparation method utilizes a simple and feasible secondary crosslinking mode, takes tetra (3-mercaptopropionic acid) pentaerythritol ester, 3, 6-dioxa-1, 8-octane dithiol and 1, 4-bis- [4- (3-acryloyloxy propoxy) benzoyloxy ] -2-methylbenzene as substrates, and compounds the substrates with carbon fibers in different proportions to finally form the carbon fiber-doped composite liquid crystal elastomer sensing material. The prepared carbon fiber/liquid crystal elastomer composite film connecting circuit is used for manufacturing a sensor and can be used for collecting human finger action signals. In addition, the mechanical property of the prepared sensor material based on the liquid crystal elastomer is greatly improved compared with that of the traditional liquid crystal elastomer. The invention provides a new idea for designing and preparing the novel flexible sensor, simultaneously overcomes the problems of complex preparation process, easy corrosion, poor mechanical property and the like in the prior art, and has wide application prospect.
Description
Technical Field
The invention belongs to the field of high polymer materials, and particularly relates to a sensor material based on a liquid crystal elastomer, and a preparation method and application thereof.
Background
In recent years, flexible sensors have been widely used in the fields of human-computer interaction, soft robots, medical treatment, and the like, because of their excellent characteristics such as high sensitivity and high flexibility. However, the flexible sensor cannot be produced and utilized in a large scale due to the problems of complex preparation process, high preparation cost, poor stretchability and the like, and the application of the flexible sensor in reality is limited.
The Liquid Crystal Elastomer (LCE) is a high polymer material which has the orientation order of liquid crystal and the entropy elasticity of the traditional elastomer, and has the biggest characteristic of realizing reversible deformation under the external stimulation. The two-way shape memory characteristic of LCE has a large application space in the aspects of sensors, artificial muscles, soft robots and the like. However, the conventional liquid crystal elastomer has poor mechanical properties and is limited in use in a wider environment.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a sensor material based on a liquid crystal elastomer, and a preparation method and application thereof. The material is used for a flexible sensor, can overcome the problems of complex process, poor response effect, poor mechanical property and the like in the prior art, and has great application prospect in sensing devices.
The technical scheme is as follows: the invention discloses a sensor material based on a liquid crystal elastomer, which comprises the following main raw materials: pentaerythritol tetra (3-mercaptopropionate), 3, 6-dioxa-1, 8-octanedithiol, an acrylate monomer RM257, carbon fiber and dipropylamine; wherein, the structure of the tetra (3-mercaptopropionic acid) pentaerythritol ester is as follows:
the 3, 6-dioxa-1, 8-octane dithiol has the structure as follows:
the structure of the 1, 4-bis- [4- (3-acryloyloxypropoxy) benzoyloxy ] -2-methylbenzene is as follows:
the dipropylamine structure is as follows:
the invention also discloses a preparation method of the sensor material based on the liquid crystal elastomer, which comprises the following steps:
(1) adding pentaerythritol tetrakis (3-mercaptopropionate), 3, 6-dioxa-1, 8-octane dithiol, an acrylate monomer, carbon fiber and dichloromethane into a strain bottle, and carrying out ultrasonic crushing;
(2) adding dipropylamine into the mixed solution obtained in the step (1), and then carrying out ultrasonic treatment;
(3) pouring the mixed solution obtained in the step (2) into a polytetrafluoroethylene groove, removing bubbles, putting into an oven, and thermally initiating pre-crosslinking to form a film;
(4) after film forming, taking out the film from the groove, and partially cutting four edges of the film;
(5) stretching and orienting the film cut in the step (4), fixing and then placing to realize secondary crosslinking; finally, forming a carbon fiber/liquid crystal elastomer composite film;
(6) the carbon fiber/liquid crystal elastomer composite film is cut into a proper size, fixed at the joint of a human finger and connected to a microcomputer control electronic universal testing machine.
Further, in the step (1), the time for ultrasonic disruption is 10-15 min.
Further, in the step (3), the temperature of the oven is 25-35 ℃, and the time for placing the oven in the oven is 2-3 h.
Further, in the step (5), the film is stretched to 200% -300% of the original length.
Further, in the step (5), the stretched film is fixedly placed for not less than 10 hours.
The carbon fiber/liquid crystal elastomer film is applied to the aspect of sensing.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages:
(1) the carbon fiber/liquid crystal elastomer composite sensing material prepared by the invention can realize quick response under the stretching condition, and has stable sensing performance after a plurality of stretching cycles. Can be used as a flexible sensing material and applied to the aspects of medical treatment, human-computer interaction and the like.
(2) According to the invention, the carbon fiber is introduced into the liquid crystal elastomer material to form the composite film, a classical two-step crosslinking mode is adopted, the reaction condition is mild, the operation is convenient, and the large-scale production can be realized.
(3) The liquid crystal elastomer composite film prepared by the invention is a carbon fiber/liquid crystal elastomer composite sensing material obtained by introducing carbon fibers in a physical doping mode. The composite material overcomes the defect of poor mechanical property of the traditional liquid crystal elastomer.
Drawings
FIG. 1 is a schematic diagram of a carbon fiber/liquid crystal elastomer preparation process;
FIG. 2 is a diagram of a carbon fiber/liquid crystal elastomer as a finger sensor and a relative change rate of resistance;
FIG. 3 illustrates the sensing stability of the carbon fiber/liquid crystal elastomer sensing material when stretched;
fig. 4 shows the breaking strength of the carbon fiber/liquid crystal elastomer.
Detailed Description
The technical scheme of the invention is further explained by combining the attached drawings.
Example 1
(1) 16.00mg of pentaerythritol tetrakis (3-mercaptopropionate), 119.38mg of 3, 6-dioxa-1, 8-octanedithiol, 423.99mg of an acrylate monomer, 55.32mg of carbon fibers and 2.5ml of dichloromethane were put in a seed bottle, and the carbon fibers accounted for 9% of the composite liquid crystal elastomer. Performing ultrasonic disruption for 10-15 min.
(2) Adding 7. mu.l of dipropylamine to the mixed solution obtained in the step (1), followed by sonication for 30 seconds.
(3) Pouring the mixed solution obtained in the step (2) into polytetrafluoroethylene grooves with the inner diameters of 2cm x 3cm respectively, removing air bubbles, putting the polytetrafluoroethylene grooves into a baking oven with the temperature of 25-35 ℃, and carrying out heat initiation for 2 hours to form a pre-crosslinked film.
(4) And after film formation, taking out the film from the groove, and partially cutting four sides of the film.
(5) And (4) stretching and orienting the film cut in the step (4) to 250% of the original length, and standing after fixing to realize secondary crosslinking. Finally, the carbon fiber/liquid crystal elastomer composite film is formed. The sample is labeled S1.
(6) Cutting the S1 sample into proper size, fixing at the joint of human finger, and connecting to the microcomputer control electronic universal tester.
Example 2
(1) 16.00mg of pentaerythritol tetrakis (3-mercaptopropionate), 119.38mg of 3, 6-dioxa-1, 8-octanedithiol, 423.99mg of an acrylate monomer, 76.28mg of carbon fibers and 2.5ml of dichloromethane were put in a seed bottle, and the carbon fibers accounted for 12% of the composite liquid crystal elastomer. Performing ultrasonic disruption for 10-15 min.
(2) To the mixed solution obtained in step (1), 7. mu.l of dipropylamine was added, followed by sonication for 30 seconds.
(3) Pouring the mixed solution obtained in the step (2) into polytetrafluoroethylene grooves with the inner diameters of 2cm x 3cm respectively, removing air bubbles, putting the polytetrafluoroethylene grooves into a baking oven with the temperature of 25-35 ℃, and carrying out heat initiation for 2 hours to form a pre-crosslinked film.
(4) And after film formation, taking out the film from the groove, and partially cutting four sides of the film.
(5) And (4) stretching and orienting the film cut in the step (4) to 250% of the original length, and standing after fixing to realize secondary crosslinking. Finally, the carbon fiber/liquid crystal elastomer composite film is formed. The sample is labeled S2.
(6) Cutting the S2 sample into proper size, fixing at the joint of human finger, and connecting to the microcomputer control electronic universal tester.
Example 3
(1) 16.00mg of pentaerythritol tetrakis (3-mercaptopropionate), 119.38mg of 3, 6-dioxa-1, 8-octanedithiol, 423.99mg of an acrylate monomer, 98.71mg of carbon fibers and 2.5ml of dichloromethane were put into a seed bottle, and the carbon fibers accounted for 15% of the composite liquid crystal elastomer. Performing ultrasonic disruption for 10-15 min.
(2) Adding 7. mu.l of dipropylamine to the mixed solution obtained in the step (1), followed by sonication for 30 seconds.
(3) Pouring the mixed solution obtained in the step (2) into polytetrafluoroethylene grooves with the inner diameters of 2cm x 3cm respectively, removing air bubbles, putting the polytetrafluoroethylene grooves into a baking oven with the temperature of 25-35 ℃, and carrying out heat initiation for 2 hours to form a pre-crosslinked film.
(4) And after film formation, taking out the film from the groove, and partially cutting four sides of the film.
(5) And (4) stretching and orienting the film cut in the step (4) to 250% of the original length, and standing after fixing to realize secondary crosslinking. Finally, the carbon fiber/liquid crystal elastomer composite film is formed. The sample is labeled S3.
(6) Cutting the S3 sample into proper size, fixing at the joint of human finger, and connecting to the microcomputer control electronic universal tester.
According to the figure 2, the carbon fiber/liquid crystal elastomer sensing material is connected to a finger, and can stably sense and output a finger motion signal. Meanwhile, as can be seen from fig. 3, the sensing signal is still stable after the material is repeatedly stretched 100 times. As shown in FIG. 4, as the doping ratio of the carbon fiber increases, the mechanical properties of the samples S1-S3 are gradually increased, and are greatly improved compared with the undoped pure liquid crystal elastomer. The method fully shows that the sensing material based on the liquid crystal elastomer is prepared by the scheme, the sensing performance with high sensitivity and high stability is realized in a simpler mode, and meanwhile, the greatly improved mechanical property is obtained, so that the practical requirements of most flexible sensors can be met.
Claims (7)
1. A sensor material based on a liquid crystal elastomer is characterized in that the main raw materials comprise: pentaerythritol tetra (3-mercaptopropionate), 3, 6-dioxa-1, 8-octanedithiol, an acrylate monomer RM257, carbon fiber and dipropylamine; wherein, the structure of the tetra (3-mercaptopropionic acid) pentaerythritol ester is as follows:
the 3, 6-dioxa-1, 8-octane dithiol has the structure as follows:
the structure of the 1, 4-bis- [4- (3-acryloyloxypropoxy) benzoyloxy ] -2-methylbenzene is as follows:
the dipropylamine structure is as follows:
2. a method for preparing a liquid crystal elastomer-based sensor material according to claim 1, comprising the steps of:
(1) adding pentaerythritol tetrakis (3-mercaptopropionate), 3, 6-dioxa-1, 8-octane dithiol, an acrylate monomer, carbon fiber and dichloromethane into a strain bottle, and carrying out ultrasonic crushing;
(2) adding dipropylamine into the mixed solution obtained in the step (1), and then carrying out ultrasonic treatment;
(3) pouring the mixed solution obtained in the step (2) into a polytetrafluoroethylene groove, removing bubbles, putting into an oven, and thermally initiating pre-crosslinking to form a film;
(4) after film forming, taking out the film from the groove, and partially cutting four edges of the film;
(5) stretching and orienting the film cut in the step (4), fixing and then placing to realize secondary crosslinking; finally, forming a carbon fiber/liquid crystal elastomer composite film;
(6) the carbon fiber/liquid crystal elastomer composite film is cut into a proper size, fixed at the joint of a human finger and connected to a microcomputer control electronic universal testing machine.
3. The method for preparing a liquid crystal elastomer-based sensor material according to claim 2, wherein in the step (1), the time for the ultrasonication is 10 to 15 min.
4. The method for preparing a sensor material based on a liquid crystal elastomer, according to claim 2, wherein in the step (3), the oven temperature is 25-35 ℃, and the time for placing the sensor material in the oven is 2-3 h.
5. The method for preparing a liquid crystal elastomer-based sensor material according to claim 2, wherein in the step (5), the film is stretched to 200 to 300% of its original length.
6. The method for preparing a liquid crystal elastomer-based sensor material according to claim 2, wherein in the step (5), the stretched film is fixedly placed for not less than 10 hours.
7. Use of the carbon fiber/liquid crystal elastomer film of claim 2 for sensing.
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CN115710354A (en) * | 2022-11-25 | 2023-02-24 | 东南大学 | Liquid crystal elastomer composite film and preparation method and application thereof |
CN115806689A (en) * | 2022-11-30 | 2023-03-17 | 东南大学 | Preparation method and application of silver nanowire-based conductive liquid crystal elastomer material |
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CN113698518A (en) * | 2021-08-24 | 2021-11-26 | 东南大学 | Liquid crystal elastomer material based on liquid metal nano droplets |
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CN113698518A (en) * | 2021-08-24 | 2021-11-26 | 东南大学 | Liquid crystal elastomer material based on liquid metal nano droplets |
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CN115710354A (en) * | 2022-11-25 | 2023-02-24 | 东南大学 | Liquid crystal elastomer composite film and preparation method and application thereof |
CN115710354B (en) * | 2022-11-25 | 2024-04-05 | 东南大学 | Liquid crystal elastomer composite film and preparation method and application thereof |
CN115806689A (en) * | 2022-11-30 | 2023-03-17 | 东南大学 | Preparation method and application of silver nanowire-based conductive liquid crystal elastomer material |
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Application publication date: 20220610 |