CN112376266A - Composite fiber with shape memory performance and strain sensing performance and preparation method thereof - Google Patents
Composite fiber with shape memory performance and strain sensing performance and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
Abstract
The invention relates to a preparation method of a composite fiber with shape memory performance and strain sensing performance, which comprises the following steps: step one, premixing and batching ethylene-vinyl acetate copolymer containing vinyl acetate, triallyl isocyanurate and benzophenone, melting and extruding the mixture through a double-screw extruder, and performing radiation crosslinking under an ultraviolet lamp to obtain crosslinked EVA fibers; dispersing graphene oxide powder in a mixed solution of acetone and water, and performing ultrasonic treatment to prepare a GO dispersion liquid; step three, soaking the crosslinked EVA fibers in a toluene solution to swell the crosslinked EVA fibers, and soaking the swelled EVA fibers in GO dispersion liquid for ultrasonic treatment to prepare GO/EVA composite fibers; and (3) placing the GO/EVA composite fiber in hydroiodic acid for reduction to obtain the RGO/EVA composite fiber. The RGO/EVA composite fiber has shape memory performance and strain sensing performance.
Description
Technical Field
The invention belongs to the technical field of functional composite materials, and particularly relates to a composite fiber with shape memory performance and strain sensing performance and a preparation method thereof.
Background
With the increasing popularity of smart products, wearable devices have attracted great attention. The flexible strain sensor is used as an important component of wearable equipment, and has important application value in the aspects of electronic skin, human motion monitoring, human-computer interaction, intelligent textiles and the like. In order to meet both large recoverable deformation and flexibility requirements, flexible strain sensors are typically composed of two units of elastic polymer and conductive filler. Currently, the commonly used elastomeric polymer matrices (thermoplastic polyurethane, polydimethylsiloxane and copolyester) suffer from a significant drawback-hysteresis. Due to the hysteresis of the elastic polymer, the flexible strain sensor inevitably generates some residual strain after many stretch-relaxation cycles, which poses a great challenge to the dynamic durability and stability of the sensor. Moreover, this residual strain will increase with increasing cycle times, eventually leading to sensor failure, which greatly shortens the useful life of the strain sensor. Therefore, it is necessary to produce a flexible strain sensor having a repair function to repair sensor failure due to fatigue damage and hysteresis.
Currently, the repair mechanism of flexible strain sensors relies mainly on dynamic (reversible) covalent/non-covalent bonds to achieve the repair function. However, due to the defects of complex repairing process, long repairing time, low repairing efficiency and the like, the feasibility of the application of the wearable electronic device is greatly limited. Therefore, there is an urgent need to prepare a flexible strain sensor having a simple repair process, rapid repair, and high repair efficiency. In recent years, Shape Memory Polymers (SMPs) have been used for sensors, smart textiles and artificial muscles due to their excellent elasticity, large deformation and simple manufacturing process. In SMPF, commercial semi-crystalline EVA is low cost, elastic and easy to process into fibers. Research shows that EVA with a crystalline and cross-linked structure has the function of melt-induced shrinkage under constant and stress-free conditions, which provides power for self-repair of SMPF, so that a conductive network damaged by hysteresis effect is efficiently and quickly repaired. Therefore, flexible fiber strain sensors with shape memory properties are one of the ideal choices for the new generation of wearable devices.
At present, the flexible strain sensor is developing towards the direction of having a repair function, the shape memory performance and the strain sensing performance are combined, the repair function of the flexible strain sensor is hopefully realized through the shape memory performance of the flexible substrate, the aims of simple repair process, high repair speed, high repair efficiency and the like are realized, and the service life of the flexible strain sensor is greatly prolonged.
Disclosure of Invention
Based on the defects in the prior art, the invention provides a composite fiber with shape memory performance and strain sensing performance and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the composite fiber with the shape memory performance and the strain sensing performance comprises the following steps:
step one, premixing and batching ethylene-vinyl acetate copolymer containing vinyl acetate, triallyl isocyanurate and benzophenone, melting and extruding the mixture through a double-screw extruder, and performing radiation crosslinking under an ultraviolet lamp to obtain crosslinked EVA fibers;
dispersing graphene oxide powder in a mixed solution of acetone and water, and performing ultrasonic treatment to prepare a GO dispersion liquid;
step three, soaking the crosslinked EVA fibers in a toluene solution to swell the crosslinked EVA fibers, and soaking the swelled EVA fibers in GO dispersion liquid for ultrasonic treatment to prepare GO/EVA composite fibers; and (3) placing the GO/EVA composite fiber in hydroiodic acid for reduction to obtain the RGO/EVA composite fiber.
Preferably, in the first step, the content of vinyl acetate in the ethylene-vinyl acetate copolymer is 18-40 wt%.
Preferably, in the first step, the mass ratio of the ethylene-vinyl acetate copolymer, the triallyl isocyanurate and the benzophenone is 100: (5-8): (5-8).
Preferably, in the first step, the radiation crosslinking time is 1-2 h.
Preferably, in the second step, the ratio of the graphene oxide powder, acetone and water is (100-300 mg): (5-20 mL): (80-95 mL).
Preferably, in the second step, the time of ultrasonic treatment is 1-2 h.
Preferably, in the third step, the soaking time is 2-3 h.
Preferably, in the third step, the time of the ultrasonic soaking treatment is 2-3 h.
Preferably, in the third step, the reduction time of the hydroiodic acid is 1-3 h.
The invention also provides a composite fiber with shape memory performance and strain sensing performance, which is prepared by the preparation method of any scheme.
Compared with the prior art, the invention has the beneficial effects that:
the RGO/EVA composite fiber prepared by the invention has the advantages of knittability, light weight, small size, excellent elasticity, simple manufacturing process and the like. Moreover, the RGO/EVA composite fiber with the crystallization and crosslinking structure has the function of melting induced shrinkage under the constant and stress-free conditions, which provides power for the self-repairing behavior of the flexible strain sensor, so that the RGO conductive network damaged by the hysteresis effect is efficiently and quickly repaired. Therefore, flexible strain sensor composite fibers with shape memory properties are one of the ideal choices for the new generation of wearable devices.
Drawings
FIG. 1 is a scanning electron micrograph of a cross section of an RGO/EVA composite fiber prepared in example 1 of the present invention;
FIG. 2 is a stress-strain plot of RGO/EVA composite fibers of example 1 of the present invention at various VA contents;
FIG. 3 is a bar graph of the retained spring rate of RGO/EVA composite fibers of example 1 of the invention at various VA contents after cyclic stretch-relaxation;
FIG. 4 is a graph of five heating-cooling cycles that the RGO/EVA composite fiber made in example 1 of the present invention undergoes between 20 ℃ and 80 ℃.
Detailed Description
The technical solution of the present invention will be further explained by the following specific examples.
Example 1:
the preparation method of the composite material of the embodiment specifically comprises the following steps:
(1) ethylene-vinyl acetate copolymer EVA having a vinyl acetate VA content of 40 wt%, triallyl isocyanurate and benzophenone in a ratio of 100 g: 5 g: 5g of the EVA fibers are mixed according to a mass ratio, the mixture is added into a micro double-screw extruder for melt extrusion and is subjected to radiation crosslinking for 1 hour under an ultraviolet lamp, and crosslinked EVA fibers are obtained;
(2) dispersing 300mg of GO in a mixed solution of 5mL of acetone and 95mL of deionized water, and carrying out ultrasonic treatment for 1 hour by using a probe ultrasonic instrument to obtain a uniformly dispersed GO solution;
(3) placing the crosslinked EVA fibers in 100mL of toluene solution to be soaked for 2 hours for swelling, soaking the swollen EVA fibers in uniform GO dispersion liquid for ultrasonic treatment for 2 hours to obtain graphene oxide/ethylene-vinyl acetate GO/EVA composite fibers, and placing the obtained GO/EVA composite fibers in hydroiodic acid for reduction for 3 hours to obtain the reduced graphene oxide/ethylene-vinyl acetate RGO/EVA composite fibers.
FIG. 1 is a SEM image of the cross section of the prepared RGO/EVA composite fiber. As can be seen from the figure, the RGO is uniformly distributed on the surface of the EVA fiber, and a perfect conductive network is constructed.
FIG. 2 is a stress-strain curve of RGO/EVA composite fibers with different VA contents, and it can be seen that RGO/EVA composite fibers with 40 wt% VA content have better flexibility and maximum elongation at break.
FIG. 3 shows the resilience retained after cyclic stretching-relaxation of RGO/EVA composite fibers with different VA contents, and it can be seen that EVA fibers with 40 wt% of VA content retain the highest resilience (92%) after cyclic stretching-relaxation, and the requirement of the flexible strain sensor on the elastic substrate material is met.
FIG. 4 is a graph of five heating-cooling cycles experienced by RGO/EVA composite fibers having a VA content of 40 wt% between 20 ℃ and 80 ℃. Calculation of RGO/EVA composite fiber at Each heatingR during the cooling cyclefAnd Rr(see Table 1), it was found that the RGO/EVA composite fiber has excellent shape fixation rate and shape recovery rate in each heating-cooling cycle, which provides a theoretical basis for the self-repair function of the RGO/EVA composite fiber.
TABLE 1 Performance Table for RGO/EVA composite fiber cycling several times
Example 2:
the preparation method of the composite material of the embodiment specifically comprises the following steps:
(1) EVA with a VA content of 25 wt%, triallyl isocyanurate and benzophenone in a ratio of 100 g: 5 g: 5g of the above-mentioned components were mixed in a mass ratio. Adding the mixture into a micro double-screw extruder for melt extrusion and performing radiation crosslinking for 1 hour under an ultraviolet lamp to obtain crosslinked EVA fibers;
(2) dispersing 300mg GO in a mixed solution of 5mL acetone and 80mL deionized water, and carrying out ultrasonic treatment for 1 hour by using a probe ultrasonic instrument to obtain a uniformly dispersed RGO solution;
(3) the crosslinked EVA fibers are placed in 100mL of toluene solution and soaked for 2 hours to swell. And immersing the swollen EVA fibers into the uniform GO dispersion liquid for ultrasonic treatment for 2 hours to obtain GO/EVA composite fibers, and placing the obtained GO/EVA composite fibers in hydroiodic acid for reduction for 3 hours to obtain RGO/EVA.
The RGO/EVA composite fiber of this example was characterized in the same manner as in example 1, and the results showed that the shape memory property of the composite fiber was similar to that exhibited by the composite fiber obtained in example 1, and 80% of the spring back rate was retained after cyclic stretch-relaxation.
Example 3:
the preparation method of the composite material of the embodiment specifically comprises the following steps:
(1) EVA having a VA content of 40 wt%, triallyl isocyanurate and benzophenone in a ratio of 100 g: 8 g: 8g of the above-mentioned mixture was mixed. Adding the mixture into a micro double-screw extruder for melt extrusion and performing radiation crosslinking for 1.5 hours under an ultraviolet lamp to obtain crosslinked EVA fibers;
(2) dispersing 100mg GO in a mixed solution of 10mL acetone and 90mL deionized water, and carrying out ultrasonic treatment for 1 hour by using a probe ultrasonic instrument to obtain a uniformly dispersed GO solution;
(3) and placing the crosslinked EVA fibers in 100mL of toluene solution to be soaked for 2 hours for swelling, soaking the swollen EVA fibers in the uniform GO dispersion liquid for ultrasonic treatment for 2 hours to obtain GO/EVA composite fibers, and placing the obtained GO/EVA composite fibers in hydroiodic acid for reduction for 3 hours to obtain the RGO/EVA composite fibers.
The RGO/EVA fibers of this example were characterized in the same manner as in example 1, and the results showed that the shape memory property and the spring back rate of the composite fibers were similar to those of the composite fibers obtained in example 1.
Example 4:
the preparation method of the composite material of the embodiment specifically comprises the following steps:
(1) EVA having a VA content of 40 wt%, triallyl isocyanurate and benzophenone in a ratio of 100 g: 7 g: 7g of the above-mentioned mixture was mixed. Melting and extruding the mixture through a micro double-screw extruder, and performing radiation crosslinking for 1 hour under an ultraviolet lamp to obtain crosslinked EVA fibers;
(2) dispersing 200mg GO in a mixed solution of 15mL acetone and 85mL deionized water, and carrying out ultrasonic treatment for 1 hour by using a probe ultrasonic instrument to obtain a uniformly dispersed GO solution;
(3) the crosslinked EVA fibers are placed in 100mL of toluene solution and soaked for 2 hours to swell. And immersing the swollen EVA fibers into the uniform GO dispersion liquid for ultrasonic treatment for 2 hours to obtain GO/EVA composite fibers, and placing the obtained GO/EVA composite fibers in hydroiodic acid for reduction for 3 hours to obtain the RGO/EVA composite fibers.
The RGO/EVA composite fiber of this example was characterized in the same manner as in example 1, and the results showed that the shape memory property and the spring back rate of the composite fiber were similar to those of the composite fiber obtained in example 1.
Example 5:
the preparation method of the composite material of the embodiment specifically comprises the following steps:
(1) EVA with a VA content of 18 wt%, triallyl isocyanurate and benzophenone in a ratio of 100 g: 8 g: 6g of the above-mentioned mixture was mixed. Adding the mixture into a micro double-screw extruder for melt extrusion and performing radiation crosslinking for 1.5 hours under an ultraviolet lamp to obtain crosslinked EVA fibers;
(2) dispersing 200mg GO in a mixed solution of 10mL acetone and 90mL deionized water, and carrying out ultrasonic treatment for 1.5 hours by using a probe ultrasonic instrument to obtain a uniformly dispersed GO solution;
(3) the crosslinked EVA fibers were soaked in 100mL of toluene for 2.5 hours to swell. And immersing the swollen EVA fibers into the uniform GO dispersion liquid for ultrasonic treatment for 2.5 hours to obtain GO/EVA composite fibers, and reducing the obtained GO/EVA composite fibers in hydroiodic acid for 2 hours to obtain the RGO/EVA composite fibers.
The CNTs/EVA composite fiber of this example was characterized in the same manner as in example 1, and the results showed that the shape memory property and the spring back rate of the composite fiber were similar to those of the composite fiber obtained in example 1.
Example 6:
the preparation method of the composite material of the embodiment specifically comprises the following steps:
(1) EVA having a VA content of 40 wt%, triallyl isocyanurate and benzophenone in a ratio of 100 g: 6 g: 7g of the above-mentioned mixture was mixed. Adding the mixture into a miniature double-screw extruder for melt extrusion and radiating and crosslinking for 2 hours under an ultraviolet lamp;
(2) dispersing 300mg of GO in a mixed solution of 20mL of acetone and 95mL of deionized water, and carrying out ultrasonic treatment for 2 hours by a probe ultrasonic instrument to obtain a uniformly dispersed GO solution.
(3) The crosslinked EVA fibers were soaked in 100mL of toluene for 3 hours to swell. And immersing the swollen EVA fibers into the uniform GO dispersion liquid for ultrasonic treatment for 3 hours to obtain GO/EVA composite fibers, and placing the obtained GO/EVA composite fibers in hydroiodic acid for reduction for 1 hour to obtain the RGO/EVA composite fibers.
The RGO/EVA composite fiber of this example was characterized in the same manner as in example 1, and the results showed that the shape memory property and the spring back rate of the composite fiber were similar to those of the composite fiber obtained in example 1.
Comparative example 1:
the preparation method of the composite material of the comparative example specifically comprises the following steps:
(1) EVA with a VA content of 16 wt%, triallyl isocyanurate and benzophenone in a ratio of 100 g: 5 g: 5g of the above-mentioned components were mixed in a mass ratio. Adding the mixture into a miniature double-screw extruder for melt extrusion and radiating and crosslinking for 1 hour under an ultraviolet lamp;
(2) 100mg of GO was dispersed in a mixed solution of 5mL acetone and 95mL deionized water and sonicated for 1 hour by a probe sonicator. We then obtained a homogeneously dispersed GO solution.
(3) The crosslinked EVA fibers are placed in 100mL of toluene solution and soaked for 2 hours to swell. And immersing the swollen EVA fibers into the uniform GO dispersion liquid for ultrasonic treatment for 2 hours to obtain GO/EVA composite fibers, and placing the obtained GO/EVA composite fibers in hydroiodic acid for reduction for 3 hours to obtain RGO/EVA.
The RGO/EVA composite fiber of this example was characterized in the same manner as in example 1, and the results showed that the shape memory property of the composite fiber was similar to that exhibited by the composite fiber obtained in example 1. However, only 68% elastic recovery remains after cyclic stretch-relaxation, and the low elastic recovery greatly limits the application of RGO/EVA composite fibers with 18 wt% VA content to flexible strain sensors.
Comparative example 2:
the preparation method of the composite material of the comparative example specifically comprises the following steps:
(1) EVA having a VA content of 40 wt%, triallyl isocyanurate and benzophenone in a ratio of 100 g: 5 g: 5g of the above-mentioned components were mixed in a mass ratio. Adding the mixture into a miniature double-screw extruder for melt extrusion and radiating and crosslinking for 1 hour under an ultraviolet lamp;
(2) 100mg GO was dispersed in a mixed solution of 5mL acetone and 95mL deionized water and sonicated for 1 hour by a probe sonicator. We then obtained a homogeneously dispersed GO solution.
(3) The crosslinked EVA fibers are placed in 100mL of toluene solution and soaked for 2 hours to swell. And immersing the swollen EVA fibers into the uniform GO dispersion liquid for ultrasonic treatment for 2 hours to obtain GO/EVA composite fibers, and placing the obtained GO/EVA composite fibers in hydroiodic acid for reduction for 0.1 hour to obtain RGO/EVA.
The RGO/EVA composite fiber of this example was characterized in the same manner as in example 1, and the results showed that the shape memory property of the composite fiber was similar to that exhibited by the composite fiber obtained in example 1. However, the sensitivity of the RGO/EVA composite fiber flexible strain sensor is too low due to the short time for reducing GO with hydroiodic acid, and the application of the RGO/EVA composite fiber flexible strain sensor in the wearable field is greatly limited.
The foregoing has outlined rather broadly the preferred embodiments and principles of the present invention and it will be appreciated that those skilled in the art may devise variations of the present invention that are within the spirit and scope of the appended claims.
Claims (10)
1. The preparation method of the composite fiber with the shape memory performance and the strain sensing performance is characterized by comprising the following steps of:
step one, premixing and batching ethylene-vinyl acetate copolymer containing vinyl acetate, triallyl isocyanurate and benzophenone, melting and extruding the mixture through a double-screw extruder, and performing radiation crosslinking under an ultraviolet lamp to obtain crosslinked EVA fibers;
dispersing graphene oxide powder in a mixed solution of acetone and water, and performing ultrasonic treatment to prepare a GO dispersion liquid;
step three, soaking the crosslinked EVA fibers in a toluene solution to swell the crosslinked EVA fibers, and soaking the swelled EVA fibers in GO dispersion liquid for ultrasonic treatment to prepare GO/EVA composite fibers; and (3) placing the GO/EVA composite fiber in hydroiodic acid for reduction to obtain the RGO/EVA composite fiber.
2. The preparation method according to claim 1, wherein in the first step, the content of vinyl acetate in the ethylene-vinyl acetate copolymer is 18 to 40 wt%.
3. The method according to claim 1, wherein in the first step, the mass ratio of the ethylene-vinyl acetate copolymer, the triallyl isocyanurate and the benzophenone is 100: (5-8): (5-8).
4. The preparation method according to claim 1, wherein in the first step, the radiation crosslinking time is 1-2 h.
5. The preparation method according to claim 1, wherein in the second step, the ratio of the graphene oxide powder to the acetone to the water is (100-300 mg): (5-20 mL): (80-95 mL).
6. The preparation method according to claim 1, wherein in the second step, the time of ultrasonic treatment is 1-2 h.
7. The preparation method according to claim 1, wherein the soaking time in the third step is 2-3 h.
8. The preparation method according to claim 1, wherein in the third step, the time for the ultrasonic immersion treatment is 2-3 h.
9. The preparation method according to claim 1, wherein in the third step, the reduction time of the hydroiodic acid is 1-3 h.
10. Composite fibers having shape memory properties and strain sensing properties, obtainable by the process according to any one of claims 1 to 9.
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| CN113073394A (en) * | 2021-03-29 | 2021-07-06 | 浙江理工大学 | Thermal driving type twisted artificial muscle composite fiber and preparation method thereof |
| CN113943439A (en) * | 2021-05-08 | 2022-01-18 | 天津科技大学 | Method for preparing GO/rGO micro-wrinkle humidity-sensitive film by biodegradable shape memory material |
| CN115058046A (en) * | 2022-07-12 | 2022-09-16 | 浙江理工大学 | CNT/EVA shape memory composite material and preparation method thereof |
| WO2023217065A1 (en) * | 2022-05-10 | 2023-11-16 | 江南大学 | Preparation method for electrically and thermally stimulated shape memory fpc electromagnetic shielding film |
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