CN115748241A - Preparation method of double-conducting-network super-hydrophobic fabric strain sensor - Google Patents
Preparation method of double-conducting-network super-hydrophobic fabric strain sensor Download PDFInfo
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- CN115748241A CN115748241A CN202211546898.3A CN202211546898A CN115748241A CN 115748241 A CN115748241 A CN 115748241A CN 202211546898 A CN202211546898 A CN 202211546898A CN 115748241 A CN115748241 A CN 115748241A
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- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 18
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Abstract
The invention discloses a preparation method of a double-conducting-network superhydrophobic fabric strain sensor, which comprises the following steps of: carrying out dopamine autopolymerization treatment on an original non-woven fabric to obtain a polydopamine fabric; and then soaking the carbon nano tube in a carbon nano tube dispersion liquid to obtain a carbon nano tube conductive fiber network, taking out the carbon nano tube conductive fiber network, drying the carbon nano tube conductive fiber network, soaking the carbon nano tube conductive fiber network in a silver trifluoroacetate solution, reducing the carbon nano tube conductive fiber network in an ascorbic acid solution to obtain a nano silver conductive fiber network, and placing the obtained fabric in a polydimethylsiloxane solution for hydrophobic treatment to obtain the strain sensor. The carbon nano tube and the nano silver conductive network constructed by the method improve the sensitivity, sensing range and durability and stability of the sensor, and in addition, the fabric strain sensor prepared by the method has good hydrophobic capacity and keeps excellent conductivity under acid, alkali and salt environments, so that a solution is provided for the fabric strain sensor to work in a complex environment.
Description
Technical Field
The invention relates to a preparation method of a fabric strain sensor, in particular to a preparation method of a double-conducting-network superhydrophobic fabric strain sensor.
Background
In recent years, with the rapid development of sensors, the wearable strain sensor has attracted wide attention in many fields, such as motion monitoring, medical monitoring, human-computer interfaces, artificial intelligence and the like, and has wide application prospects. The strain sensor can respond to the form change of external mechanical stimulation and convert the mechanical stimulation into resistance or current signals to be output, has the advantages of simple sensing mechanism, easy manufacture and low energy consumption, and has wide application prospect in wearable equipment. In order to improve the performance of the strain sensor, a great deal of research is carried out on the sensitivity and the sensing range of the sensor by means of material exploration, structural engineering and the like. Although optimization of sensing performance has been clearly recognized, it remains a challenge to fabricate strain sensors with a wide sensing range (> 50%), high sensitivity (> 100), good flexibility and good durability (> 2000 cycles). In addition, the harsh operating environment can cause decomposition or oxidation of the conductive material during long-term use, thereby reducing conductivity and causing irreversible damage to the sensor. Therefore, the development of a strain sensor with waterproof performance and high sensing performance has great significance for detection of acid, alkali, salt and underwater environment.
Patent 202010078702.7 prepares a super-hydrophobic strain sensor composite membrane. The strain sensor has excellent sensitivity and sensing range, and can maintain super-hydrophobic performance under the erosion of acid/alkali/salt solution. However, the strain sensor prepared by the method has the problems of poor air permeability, poor human skin fit and the like. Patent 201910226819.2 prepares a superhydrophobic paper-based flexible strain sensor. The strain sensor has good super-hydrophobic performance, but the strain sensing range is small, and the requirement for monitoring human motion in a large range is difficult to meet. Patent 202110968514.6 prepares a super-hydrophobic reduced graphene oxide/polyurethane sponge sensor. The sensor prepared by the method has a wider strain sensing range, but is low in sensitivity, thick in size and not suitable for monitoring the motion of a human body. Patent 202010443697.5 prepares a multi-response fabric sensor which is breathable and waterproof. The strain sensor has the characteristics of good hydrophobicity, air permeability, easiness in skin attachment and the like, but the sensitivity and the sensing range of the strain sensor are relatively low, and high-precision and large-range human motion monitoring is difficult to realize.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a preparation method of a double-conducting-network superhydrophobic fabric strain sensor with high sensitivity, wide sensing range and durable stability.
The technical scheme is as follows: the invention relates to a preparation method of a double-conducting-network superhydrophobic fabric strain sensor, which comprises the following steps of:
(1) Carrying out dopamine autopolymerization treatment on an original non-woven fabric to obtain a polydopamine fabric;
(2) Soaking the polydopamine fabric in a carbon nanotube dispersion liquid to obtain a carbon nanotube conductive fiber network, taking out and drying to obtain a polydopamine/carbon nanotube fabric;
(3) Soaking the polydopamine/carbon nanotube fabric in a silver trifluoroacetate solution, taking out and drying the polydopamine/carbon nanotube fabric, and reducing the polydopamine/carbon nanotube fabric in an ascorbic acid solution to obtain a nano-silver conductive fiber network, wherein the obtained fabric is a polydopamine/carbon nanotube/nano-silver fabric;
(4) And putting the polydopamine/carbon nano tube/nano silver fabric into a polydimethylsiloxane solution for hydrophobic treatment to obtain the strain sensor.
Wherein in the step (1), the concentration of the dopamine is 0.5-0.8 wt%, the pH value is 8-8.5, the reaction temperature is 25-40 ℃, and the reaction time is 12-24 hours. The poly-dopamine prepared under the reaction condition can be uniformly coated on the surface of the fiber. Through chemical polymerization of dopamine, the non-woven fabric is changed from a hydrophobic state to a hydrophilic state, so that the carbon nano tubes of a conductive substance are favorably deposited on the surface of the fiber, and the initial resistance of the fabric strain sensor is reduced.
In the step (2), the carbon nanotube is at least one of a multi-walled carbon nanotube, a single-walled carbon nanotube or a carboxylated carbon nanotube.
In the step (2), the concentration of the carbon nano tube dispersion liquid is 5-10 wt%, and a complete multi-walled carbon nano tube conductive network can be formed on the surface of the fiber under the concentration.
In the step (2), the polydopamine fabric is placed in the carbon nano tube dispersion liquid and is soaked for 40-70 min; wherein, the dipping is carried out for 10 to 20min under the ultrasonic condition, and then the dipping is carried out for 30 to 50min. This is more favorable for the carbon nanotubes to be adsorbed on the surface of the fiber.
Wherein, in the step (3), the concentration of the silver trifluoroacetate solution is 5-20wt%, and sufficient silver ions are provided for the solution.
In the step (3), the poly dopamine/carbon nanotube fabric is immersed in the silver trifluoroacetate solution for 30-60 min, so that enough silver ions are adsorbed on the surface of the fiber.
In the step (3), the concentration of the ascorbic acid solution is 3-10wt%, and the reduction time is 30-60 min, so that the silver ions on the surface of the fiber are completely reduced into silver particles.
In the step (4), the concentration of polydimethylsiloxane in the ethyl acetate solution is 0.5-2 wt%, and the dip-coating time is 30-60 min, so that the conductive fabric has super-hydrophobic capability, and the surface appearance of fibers, and the resistance and air permeability of the conductive fabric are not affected; the solvent of the polydimethylsiloxane solution is ethyl acetate and/or n-hexane.
The invention principle is as follows: in the invention, the polydopamine modified non-woven fabric changes the hydrophobic state of the non-woven fabric into the hydrophilic state, which is beneficial to the conductive material carbon nano tube and nano silver to be attached on the non-woven fabric. The double conductivity network of the carbon nano tube and the nano silver particle constructed by the carbon nano tube and the nano silver particle enables the sensor to have high sensitivity and wide sensing range, and simultaneously enables the fiber to have a rough microstructure. The low surface energy PDMS combines the rough fiber microstructure surface to enable the non-woven fabric sensor to have super-hydrophobic performance, and the corrosion resistance and the sensing stability of the sensor are also improved, so that the strain sensor can be applied to complex and worse external strip environments, and the stability of conductivity can be kept. The prepared strain sensor not only can realize the monitoring of daily human body movement, but also has excellent responsiveness to underwater movement.
Has the advantages that: compared with the prior art, the invention has the following remarkable effects: (1) The fabric strain sensor prepared by the method has high sensitivity, wide sensing range and durable stability; (2) The carbon nano tube and nano silver double-conductive network reduces the resistance of the fabric strain sensor, improves the conductivity, and enables the fabric strain sensor to have quick response, low detection limit and high sensitivity to tensile deformation. (3) After the hydrophobic treatment of the fabric strain sensor, the sensor has excellent resistance stability, and experiments show that the sensor still maintains higher conductivity after the treatment in chemical environments such as acid, alkali, salt and the like. After 7 hours of ultrasonic cleaning and 500 times of stretching cycles, the resistance of the sensor has small fluctuation, and good environmental stability is presented. (4) The hydrophobization fabric strain sensor can not only realize the monitoring of the motion of a common human body, but also realize the action recognition of fingers in acid, alkali, salt and other underwater environments and weak underwater vibration recognition. (5) The lower detection limit and wider monitoring range of the sensor can identify tiny deformation and wide movement range, which also enables the sensor to be applied to underwater monitoring occasions.
Drawings
FIG. 1 is a SEM image of the fiber surface of a nonwoven fabric according to example 1 of the present invention;
FIG. 2 is a static contact angle chart of a nonwoven fabric of example 1 of the present invention;
FIG. 3 is a SEM image of the fiber surface of a PDA modified nonwoven fabric of example 1 in accordance with the invention;
FIG. 4 is a SEM image of the fiber surface of a PDA/MWNTs nonwoven fabric of example 1 of the present invention;
FIG. 5 is a fiber surface SEM image of a PDA/MWNTs/AgNPs/PDMS nonwoven fabric according to example 1 of the present invention;
FIG. 6 is a graph of the static contact angle of the PDA/MWNTs/AgNPs/PDMS nonwoven fabric of example 1 of the present invention;
FIG. 7 shows the wettability of the PDA/MWNTs/AgNPs/PDMS nonwoven fabric for various solutions in example 1 of the present invention;
FIG. 8 shows the hydrophobic properties and conductive abilities of the non-woven PDA/MWNTs/AgNPs/PDMS fabric in different external environments according to example 1 of the present invention;
FIG. 9 shows the signal identification of the PDA/MWNTs/AgNPs/PDMS non-woven fabric strain sensor for finger motion and the identification of intermittent ultrasonic signals under acid, alkali and salt solutions in the embodiment 1 of the invention.
Detailed Description
The present invention is described in further detail below.
Example 1
(1) Placing 5 × 5cm non-woven fabric in 0.5wt% dopamine solution with pH of 8.5, setting temperature at 35 deg.C, shaking with constant temperature water bath shaker for 24 hr, washing residue with deionized water, placing in 60 deg.C vacuum drying oven, and taking out after 15min for use.
(2) And (2) immersing the polydopamine fabric prepared in the step (1) into 5wt% of multi-walled carbon nanotube aqueous dispersion, performing ultrasonic immersion for 20min, then performing natural immersion for 30min, putting into a vacuum drying oven at 60 ℃, and taking out for 15min for later use.
(3) And (3) soaking the polydopamine/carbon nanotube fabric prepared in the step (2) in a 5wt% silver trifluoroacetate solution for 30min, drying in a 60 ℃ vacuum drying oven, taking out the polydopamine/carbon nanotube fabric for 15min, soaking the polydopamine/carbon nanotube fabric in a 3wt% ascorbic acid solution for 30min, placing the polydopamine/carbon nanotube fabric in a 60 ℃ vacuum drying oven, and taking out the polydopamine/carbon nanotube fabric for 15min for later use.
(4) And (3) soaking the polydopamine/multi-walled carbon nanotube/nano-silver fabric prepared in the step (3) into a 0.5wt% PDMS solution for 1h, putting the polydopamine/multi-walled carbon nanotube/nano-silver fabric into a 70 ℃ vacuum drying oven, and taking out the polydopamine/multi-walled carbon nanotube/nano-silver fabric after 60min to successfully prepare the high-durability super-hydrophobic fabric strain sensor.
Fig. 1 is an SEM of the surface of the fibers of the nonwoven fabric, from which it can be seen that the fibers are in a smooth state, and fig. 2 is a static contact angle of the nonwoven fabric, 134 °, from which it can be seen that the nonwoven fabric is in a hydrophobic state. Through PDA modification of the non-woven fabric, the hydrophobic non-woven fabric is changed into a hydrophilic state, so that MWNTs can be attached to the surface of the fiber. Fig. 3 is a diagram of the PDA material attached to the surface of the fiber, and it can be observed that the PDA is wrapped on the surface of the fiber and has a uniform shape. Fig. 4 shows that MWNTs are tightly wrapped on the surface of the PDA fiber, and it can be observed that MWNTs are wrapped on the PDA fiber, and the tight connection forms a complete conductive channel. FIG. 5 shows AgNPs and PDMS attached to the surface of the fiber, and it can be seen that PDMS does not affect the morphology of the fiber surface. The double-conductive network constructed by MWNTs and AgNPs not only improves the conductivity and the sensing performance of the fabric, but also increases the roughness of the fiber. The combination of the rough fiber surface and PDMS provided the nonwoven fabric with super-hydrophobic property, and as shown in FIG. 6, the static contact angle of the prepared PDA/MWNTs/AgNPs/PDMS nonwoven fabric was 156 °. FIG. 7 shows that the PDA/MWNTs/AgNPs/PDMS nonwoven fabric has anti-wetting ability to various solutions. FIG. 8 shows that the PDA/MWNTs/AgNPs/PDMS nonwoven fabric still maintains the super-hydrophobic capability after 500 times of fatigue resistance tests. FIG. 9 shows the state where the PDA/MWNTs/AgNPs/PDMS nonwoven fabric can identify underwater ultrasonic source signals and underwater finger joint motion. Therefore, the super-hydrophobic fabric with good conductivity prepared by the method has good application value in wearable electronic equipment, heaters and underwater sensing monitoring.
Example 2
(1) Placing 5 × 5cm non-woven fabric in 0.5wt% dopamine solution with pH of 8 and temperature of 35 deg.C, shaking with constant temperature water bath shaker for 24 hr, washing residue with deionized water, placing in 60 deg.C vacuum drying oven, and taking out after 15min for use.
(2) And (2) immersing the polydopamine fabric prepared in the step (1) into 5wt% of multi-walled carbon nanotube aqueous dispersion, performing ultrasonic immersion for 20min, then performing natural immersion for 30min, putting into a vacuum drying oven at 60 ℃, and taking out for 15min for later use.
(3) And (3) soaking the polydopamine/multi-walled carbon nanotube fabric prepared in the step (2) in a 20wt% silver trifluoroacetate solution for 30min, drying in a 60 ℃ vacuum drying oven, taking out the polydopamine/multi-walled carbon nanotube fabric after 15min, soaking in a 3wt% ascorbic acid solution for 30min, putting in a 60 ℃ vacuum drying oven, and taking out the polydopamine/multi-walled carbon nanotube fabric for 15min to reserve.
(4) And (4) soaking the polydopamine/multi-walled carbon nanotube/nano-silver fabric prepared in the step (3) into a 0.5wt% PDMS solution for 1h, putting the solution into a 70 ℃ vacuum drying oven, and taking out the solution after 60min, thereby successfully preparing the high-durability super-hydrophobic fabric strain sensor.
Example 3
(1) Placing 5 × 5cm non-woven fabric in 0.8wt% dopamine solution with pH of 8.5, setting temperature at 35 deg.C, shaking in constant temperature water bath for 24 hr, washing residue with deionized water, placing in 60 deg.C vacuum drying oven, and taking out after 15min for use.
(2) And (2) soaking the polydopamine fabric prepared in the step (1) into 10wt% of single-walled carbon nanotube aqueous dispersion, performing ultrasonic immersion for 20min, then performing natural immersion for 30min, putting into a vacuum drying oven at 60 ℃, and taking out for 15min for later use.
(3) And (3) soaking the polydopamine/single-walled carbon nanotube fabric prepared in the step (2) in a 20wt% silver trifluoroacetate solution for 30min, putting the polydopamine/single-walled carbon nanotube fabric into a 60 ℃ vacuum drying oven to be dried, taking out the polydopamine/single-walled carbon nanotube fabric after 15min, soaking the polydopamine/single-walled carbon nanotube fabric into a 5wt% ascorbic acid solution for 30min, putting the polydopamine/single-walled carbon nanotube fabric into a 60 ℃ vacuum drying oven, and taking out the polydopamine/single-walled carbon nanotube fabric for standby after 15 min.
(4) And (3) soaking the polydopamine/single-walled carbon nanotube/nano-silver fabric prepared in the step (3) into ethyl acetate solution with the content of 2wt% PDMS for 1h, putting the polydopamine/single-walled carbon nanotube/nano-silver fabric into a vacuum drying oven with the temperature of 70 ℃, taking out the polydopamine/single-walled carbon nanotube/nano-silver fabric after 60min, and successfully preparing the high-durability super-hydrophobic fabric strain sensor.
Example 4
(1) Placing 5 × 5cm non-woven fabric in 0.6wt% dopamine solution with pH of 8.5, setting temperature at 35 deg.C, shaking in constant temperature water bath for 24 hr, washing residue with deionized water, placing in 60 deg.C vacuum drying oven, and taking out after 15min for use.
(2) And (2) soaking the polydopamine fabric prepared in the step (1) into 10wt% of carboxylated carbon nanotube aqueous dispersion, performing ultrasonic soaking for 20min, then naturally soaking for 30min, placing in a vacuum drying oven at 60 ℃, and taking out for later use after 15 min.
(3) And (3) soaking the polydopamine/carboxylated carbon nanotube fabric prepared in the step (2) into a 5wt% silver trifluoroacetate solution for 30min, putting the polydopamine/carboxylated carbon nanotube fabric into a 60 ℃ vacuum drying oven to be dried, taking out the polydopamine/carboxylated carbon nanotube fabric for 15min, soaking the polydopamine/carboxylated carbon nanotube fabric into a 3wt% ascorbic acid solution for 30min, putting the polydopamine/carboxylated carbon nanotube fabric into a 60 ℃ vacuum drying oven, and taking out the polydopamine/carboxylated carbon nanotube fabric for 15min to be reserved.
(4) And (3) soaking the polydopamine/carboxylated carbon nanotube/nano-silver fabric prepared in the step (3) into 0.5wt% of ethyl acetate solution of PDMS for 1h, putting the polydopamine/carboxylated carbon nanotube/nano-silver fabric into a 70 ℃ vacuum drying oven, and taking out the polydopamine/carboxylated carbon nanotube/nano-silver fabric after 60min, thereby successfully preparing the high-durability superhydrophobic fabric strain sensor.
Claims (10)
1. A preparation method of a double-conductive-network super-hydrophobic fabric strain sensor is characterized by comprising the following steps:
(1) Carrying out dopamine autopolymerization treatment on an original non-woven fabric to obtain a polydopamine fabric;
(2) Soaking the polydopamine fabric in the carbon nanotube dispersion liquid to obtain a carbon nanotube conductive fiber network, taking out and drying to obtain a polydopamine/carbon nanotube fabric;
(3) Soaking the polydopamine/carbon nanotube fabric in a silver trifluoroacetate solution, taking out and drying the polydopamine/carbon nanotube fabric, and reducing the polydopamine/carbon nanotube fabric in an ascorbic acid solution to obtain a nano-silver conductive fiber network, wherein the obtained fabric is a polydopamine/carbon nanotube/nano-silver fabric;
(4) And (3) placing the polydopamine/carbon nanotube/nano-silver fabric into a polydimethylsiloxane solution for hydrophobic treatment to obtain the hydrophobic strain sensor.
2. The preparation method of the double-conducting-network superhydrophobic fabric strain sensor according to claim 1, wherein in the step (1), the concentration of dopamine is 0.5-0.8 wt%, the pH value is 8-8.5, the reaction temperature is 20-40 ℃, and the reaction time is 12-24 hours.
3. The method for preparing the double-conducting-network superhydrophobic fabric strain sensor according to claim 1, wherein in the step (2), the carbon nanotubes are at least one of multi-walled carbon nanotubes, single-walled carbon nanotubes or carboxylated carbon nanotubes.
4. The method for preparing the double-conducting-network superhydrophobic fabric strain sensor according to claim 1, wherein in the step (2), the concentration of the carbon nanotube dispersion is 5-10 wt%.
5. The method for preparing the double-conducting-network superhydrophobic fabric strain sensor according to claim 1, wherein in the step (2), the poly-dopamine fabric is placed in the carbon nanotube dispersion liquid, ultrasonic treatment is performed for 10-20 min, and then the poly-dopamine fabric is continuously immersed for 30-50min.
6. The method for preparing the double-conducting-network superhydrophobic fabric strain sensor according to claim 1, wherein in the step (3), the concentration of the silver trifluoroacetate solution is 5-20wt%.
7. The method for preparing the double-conducting-network superhydrophobic fabric strain sensor according to claim 1, wherein in the step (3), the poly-dopamine/carbon nanotube fabric is immersed in a silver trifluoroacetate solution for 30-60 min.
8. The method for preparing the double-conductive-network superhydrophobic fabric strain sensor according to claim 1, wherein in the step (3), the concentration of the ascorbic acid solution is 3-10wt%, and the reduction time is 30-60 min.
9. The method for preparing the double-conducting-network superhydrophobic fabric strain sensor according to claim 1, wherein in the step (4), the concentration of the polydimethylsiloxane solution is 0.5-2 wt%.
10. The method for preparing the double-conducting-network superhydrophobic fabric strain sensor according to claim 1, wherein in the step (4), the solvent required for preparing the polydimethylsiloxane solution is ethyl acetate and/or n-hexane.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112501905A (en) * | 2020-11-19 | 2021-03-16 | 嘉兴立一新材料有限公司 | Super-hydrophobic electromagnetic shielding fabric and preparation method thereof |
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