CN111678425A - Breathable and waterproof multi-response fabric sensor - Google Patents
Breathable and waterproof multi-response fabric sensor Download PDFInfo
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- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/16—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements
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- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
- G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
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Abstract
The invention discloses a breathable and waterproof multi-response fabric sensor. The MXene-based fabric sensor comprises a flexible elastic fabric substrate, an interface layer, a functional layer and a protective layer from inside to outside, wherein the interface layer is a polydopamine layer, the functional layer is an MXene network, and the protective layer is polydimethylsiloxane. The sensor of the invention is not only breathable and waterproof, but also can show corresponding resistance response under different external strains and temperatures; the preparation method is simple, large-scale production can be realized, and the multi-response fabric sensing device has excellent sensing performance and good environmental stability, and is very useful in the field of intelligent wearable clothing.
Description
Technical Field
The invention relates to a breathable waterproof wearable fabric sensor with photo-thermal response, temperature sensing and strain sensing, and belongs to the technical field of preparation of functional polymer composite materials.
Background
The development of 5G communication promotes the arrival of the world of everything interconnection, which also puts higher requirements on intelligent wearable electronic products, and the traditional wearable equipment is all based on a sensing device synthesized by an electronic mechanical gyroscope and an accelerometer. However, such a sensing device has problems of high cost, complicated instrument and single test. To overcome these difficulties, flexible wearable electronics have evolved. How to design frivolous, flexible, the wearable electron of various intelligent of performance is the research direction that people focus on more and more.
The preparation method of the flexible wearable electronic reported in literature at present generally selects a high-molecular flexible substrate to be compounded with a metal nano material, a carbon material (carbon nanotube, graphene, etc.) and a conductive polymer, however, the carbon nanotube and the graphene usually aggregate on a high-molecular substrate, the metal nanoparticle/nanowire is expensive and easy to corrode, and the conductivity of the intrinsic conductive polymer is not ideal and stable. With the development of 2D materials, two-dimensional transition metal carbide (MXene) materials have come into play and are attracting more and more attention, and show great potential applications in wearable electronics due to their unique properties, such as high conductivity of metalloids, large specific surface area, 2D layered structure and abundant hydrophilic functional groups on the surface. For example: liu et al prepared a Flexible MXene/AgNW composite fabric for EMI Shielding and moisture monitoring via a layer-by-layer spray assembly strategy (Liu L X, Chen W, Zhang H B, et al. Flexible and multifunctional Silk Textiles with a biomedical Leaf-Like MXene/Silver nanowirerope for Electromagnetic Interference screening, HumidyMonitoring, and Self-detailed hydrophilicity [ J ]. Advanced functional materials,2019, 29(44): 1905197.); cao et al developed multifunctional MXene-based fibers and Textiles with excellent photothermal, electrothermal and electromechanical responses using 3D printing methods, greatly expanding the field of application of MXene Materials (Cao W T, Ma C, Mao D S, et al, MXene-Reinforced Cellulose nanofiber Inksform 3D-Printed Smart fibers and Textiles [ J ]. Advanced Functional Materials,2019, 29(51): 1905898.).
However, according to practical application situations, some researchers find that MXene is easy to oxidize in air, and the performance is reduced correspondingly, which becomes a critical problem for restricting the application of MXene. In addition, the weak interface action between MXene and the polymer matrix is a non-negligible problem. More importantly, whether multiple tasks can be completed by one device, namely, the versatility, has important significance for the development of flexible devices.
Disclosure of Invention
The invention mainly aims to provide a breathable waterproof wearable fabric sensor with photo-thermal response, temperature sensing and strain sensing and a preparation method thereof, and provides a solution for preparing a multifunctional composite material. The multi-response fabric sensor prepared by the method is breathable and hydrophobic, can enable a wearer to keep comfortable and is convenient to clean, can make corresponding response to external light, temperature and mechanical movement, and has wide prospects in the field of wearable intelligent clothes.
The invention provides an MXene-based breathable waterproof multi-response fabric sensor which comprises a flexible elastic fabric substrate, an interface layer, a functional layer and a protective layer from inside to outside, wherein the interface layer is a polydopamine layer, the functional layer is an MXene network, and the protective layer is polydimethylsiloxane.
The invention provides a preparation method of an MXene-based breathable waterproof multi-response fabric sensor, which comprises the following steps:
and 3, putting the elastic fabric with different MXene modification times obtained in the step 2 into a normal heptane solution of Polydimethylsiloxane (PDMS) for soaking and modifying for a period of time, and curing to obtain the breathable waterproof multi-response fabric sensor.
Preferably, in step 1, the dopamine alkaline solution is a dopamine Tris solution, wherein the concentration of dopamine is 0.2wt.%, and the pH is preferably 8.5.
Preferably, in step 2, the MXene colloidal solution is prepared as follows:
(1) adding lithium fluoride (LiF) into 9M dilute hydrochloric acid, and magnetically stirring to react for 15-30 minutes;
(2) adding MAX phase powder, and etching at 35 ℃ for 20-24 hours, wherein the mass ratio of MAX phase powder to lithium fluoride is 1: 1;
(3) and washing the etched product with deionized water until the pH value of the supernatant is more than or equal to 6, mixing the supernatant and the precipitate, performing ultrasonic treatment for 1h, centrifuging at 3500rpm for 1h, and collecting the upper black liquid to obtain the MXene colloidal solution.
Specifically, in the preparation of MXene colloidal solution, the MAX phase powder is preferably Ti3AlC2。
Preferably, in the step 2, the concentration of the MXene colloidal solution is preferably 4-7 mg/ml, and the immersion time is preferably 5-15 minutes.
Preferably, in step 2, the dipping and drying are repeated for more than 0 times, preferably 0 to 4 times, and the conductivity increases with the dipping times.
Preferably, in step 3, the n-heptane solution of polydimethylsiloxane is 1wt.%, and the modification time is 20-60 minutes.
Compared with the prior art, the invention has the following advantages:
(1) the multi-response composite fabric provided by the invention has the advantages of simple preparation process, mild and controllable reaction conditions, suitability for large-scale manufacturing and wide application prospect.
(2) The invention creatively explores the relationship between the resistance and the temperature of the MXene composite material and applies the MXene composite material to the field of temperature sensing.
(2) The multi-response composite fabric sensor prepared by the invention is breathable and waterproof, has an optimal contact angle of 152 degrees and excellent photo-thermal response performance, can be quickly heated to 58 ℃ under the energy density of 0.1W/cm 2, has stable strain and temperature sensing performance, and can be widely applied to the field of intelligent clothes for human body movement and body temperature monitoring and personal thermal management.
Drawings
Fig. 1 is a preparation diagram of the air-permeable hydrophobic smart fabric sensor of the present invention.
Fig. 2 is an XRD pattern of MXene prepared in example 1.
FIG. 3a is a scanning electron micrograph of an initial fabric; FIG. 3b is a scanning electron micrograph of a modified stretch fabric modified with Polydopamine (PDA); FIG. 3c is a scanning electron microscope image of the composite fabric with MXene impregnated 1 time; FIG. 3d is the scanning electron microscope image of the composite fabric with PDMS modification for 40 minutes and MXene immersion for 1 time.
Fig. 4 is an XPS plot of a multi-responsive fabric sensor prepared in example 1.
FIG. 5 shows a fabric sensor prepared in example 1 at 100 mW/cm2And under illumination, the photo-thermal performance is stable after repeated circulation.
Fig. 6 is the contact angle of MXene fabric soaked 3 times as a function of time of modified PDMS.
Fig. 7 is a graph demonstrating the air permeability of an MXene fabric sensor.
Fig. 8 shows the sensing signal response of the multi-response fabric sensor prepared in example 2 under different stretching conditions.
Fig. 9 is a stability test at 20% stretch for a multi-responsive fabric sensor made in example 2, with internal inset plots comparing the sensing response at 10 and 480 cycles of the stretch cycle, respectively.
Fig. 10 is a graph of the relative resistance change versus temperature for the multi-responsive fabric sensor prepared in example 3.
Fig. 11 is a graph showing temperature sensing stability in a plurality of tests of the fabric sensor prepared in example 3.
FIG. 12 shows the resistance change of PDMS-modified fabric sensor and non-PDMS-modified fabric exposed to air at a temperature of 20 ℃ and a humidity of about 60%.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes and modifications can be made by those skilled in the art after reading the teachings of the present invention, and equivalents also fall within the scope of the appended claims
Example 1
(1) Preparation of MXene:
1g of LiF and 20 ml of dilute hydrochloric acid (9M) are stirred thoroughly for 15 minutes, after which 1g of Ti3AlC2The powder was added slowly and stirring was continued at 35 ℃ for 24 h until etching was complete. And centrifuging and washing the MXene mixed solution for 5min at 3500rpm for multiple times by using deionized water until the pH value of a supernatant is more than or equal to 6. And mixing the supernatant and the precipitate, performing ultrasonic treatment for 1h, centrifuging at 3500rpm for 1h, and collecting the upper black liquid, namely MXene colloidal solution. Fig. 2 is the XRD patterns of MXene and MAX prepared in this example, and it can be seen that Al layer is completely etched and MXene is completely etched.
(2) Preparing a multifunctional MXene fabric sensor:
and (3) fully mixing 0.24 g of Tris powder and 0.4 g of dopamine in 200 ml of deionized water, then putting the flexible elastic fabric into the solution, magnetically stirring and reacting for 6 hours, taking out the flexible elastic fabric after reaction, fully washing the flexible elastic fabric with the deionized water, and drying the flexible elastic fabric in an oven at 40 ℃ for 12 hours. The PDA modified stretch fabric was immersed in a 5 wt.% concentration of MXene colloidal solution for 10 minutes, then the fabric was removed and dried at 40 ℃ for 30min to make a fabric with 1 impregnation of MXene. To impart superhydrophobic properties to the fabric and maintain the intrinsic breathability of the fabric itself, the fabric impregnated with MXene 1 time was immersed in a 1wt.% solution of Polydimethylsiloxane (PDMS) in n-heptane for 20min and cured at 60 ℃ for 1h to give a waterproof and breathable fabric sensor. As shown in fig. 3a, the fiber surface of the initial fabric is flat, but after PDA modification, as shown in fig. 3b, the fiber surface becomes rough, and the highly chemically active PDA layer provides active sites for adsorption of MXene nanosheets, and strengthens the interfacial bonding ability between the MXene layer and the fiber. Abundant active hydrophilic functional groups on the surface of MXene can form hydrogen bond interaction with hydroxyl groups on PDA, so that MXene nanosheets can be firmly adsorbed on the surface of the modified fiber, and a wrinkled MXene conductive network is formed by assembly (as shown in FIG. 3 c). After the modification of PDMS, the interface between MXene becomes fuzzy, and the interaction between MXene layer and fiber is strengthened better (as shown in FIG. 3 d). XPS analysis of the prepared fabric is carried out, and characteristic peaks of Ti and Si can be observed by XPS full spectrum scanning in figure 4, which shows that MXene and PDMS are successfully modified on the fabric.
(3) And (3) testing: photothermal test using 100 mW/cm2The xenon lamp of (1) simulates the illumination of 1 solar light intensity, and the sample fabric (40 mm × 10 mm) prepared in example 1 was placed on a substrate 50cm below the xenon lamp for photothermal testing, as shown in FIG. 5, at 100 mW/cm2And (2) carrying out illumination heating and cooling on the sample under the energy density, wherein after illumination is applied, the temperature-time curve of the fabric sensor shows that the temperature rises rapidly firstly and then slowly rises to the saturation temperature, and after the illumination is removed, the fabric sensor is cooled rapidly firstly and then slowly reduced to the room temperature. And maintains good stability after multiple cycles. The excellent photothermal conversion performance enables the fabric sensor to be applied to a personal intelligent thermal management system.
Example 2
(1) Preparation of MXene:
the preparation process and conditions were the same as in step (1) of example 1.
(2) Preparing a multifunctional MXene fabric sensor:
and (3) fully mixing 0.24 g of Tris powder and 0.4 g of dopamine in 200 ml of deionized water, then putting the flexible elastic fabric into the solution, magnetically stirring and reacting for 6 hours, taking out the flexible elastic fabric after reaction, fully washing the flexible elastic fabric with the deionized water, and drying the flexible elastic fabric in an oven at 40 ℃ for 12 hours. The PDA modified stretch fabric was dipped in MXene colloidal solution with a concentration of 5 wt.% for 10 minutes, taken out and dried at 40 c for 30min, and then the above dipping and drying process was repeated 2 times to make MXene dipped fabric 3 times. To impart superhydrophobic properties to the fabric and maintain the intrinsic breathability of the fabric itself, the fabric impregnated with MXene 3 times was immersed in a 1wt.% solution of PDMS in n-heptane for 40 min and cured at 60 ℃ for 1h to give a waterproof and breathable fabric sensor.
(3) And (3) testing: the contact angle test comprises the steps of testing the contact angle of a silver-plated fabric by using an OCA20 contact angle measuring instrument, dripping 5 mu L of distilled water on the surface of the fabric, testing for 5 times to ensure the accuracy of the result, averaging, recording the contact angle of the corresponding composite fabric by regulating and controlling the PDMS modification time in order to explore the influence of PDMS on the material wettability in detail, wherein when the modification time reaches 20min, the contact angle of the composite fabric reaches 152 degrees, the contact angle is slightly reduced along with the increase of time, the thickness of a hydrophobic layer is increased due to excessive PDMS, and the surface of folded MXene becomes flat, so that the hydrophobicity is slightly reduced (as shown in figure 6); the air permeability proves that: the composite fabric was secured to the opening of the vial under the beaker with a rubber band as shown in fig. 7. It can be seen from the figure that water vapor can pass through the composite textile from a vial containing hot water: (>80) Cutting the composite fabric into 40 mm × 10 mm, fixing 2 copper wires at two ends of a sample as electrodes by conductive silver paste, monitoring temperature sensing signals by a KEYSIGHT 6517B electrometer, and using a KEYSIGHT 6517B electrometer to monitor temperature sensing signalsR-R 0/R 0To represent the sensing signal of the fabric sensor. By applying 10%, 30%, 50% and 70% strain to this fabric sensor, respectively, it was observed that the fabric sensor exhibited increasing response signals, as shown in fig. 8, which could be used for detection of different strains. In order to test the sensing stability of the fabric sensor, the fabric sensor is subjected to 500 times of cycle tests under 20% tensile strain (as shown in fig. 9), and the relative resistance of the composite fabric is basically kept unchanged, so that the fabric sensor can be repeatedly used in practical application. The multifunctional composite fabric is expected to be applied to human motion monitoring due to the excellent sensing performance.
Example 3
(1) Preparation of MXene:
the preparation process and conditions were the same as in step (1) of example 1.
(2) Preparing a multifunctional MXene fabric sensor:
and (3) fully mixing 0.24 g of Tris powder and 0.4 g of dopamine in 200 ml of deionized water, then putting the flexible elastic fabric into the solution, magnetically stirring and reacting for 6 hours, taking out the flexible elastic fabric after reaction, fully washing the flexible elastic fabric with the deionized water, and drying the flexible elastic fabric in an oven at 40 ℃ for 12 hours. The PDA modified stretch fabric was immersed in 5 wt.% concentration of MXene colloidal solution for 10 minutes, removed and dried at 40 ℃ for 30min, followed by 4 repetitions of the dip drying process to make MXene dipped 5 times fabric. To impart superhydrophobic properties to the fabric and maintain the inherent breathability of the fabric itself, the fabric impregnated 5 times with MXene was immersed in a 1wt.% solution of Polydimethylsiloxane (PDMS) in n-heptane for 60 min and cured at 60 ℃ for 1h to give a waterproof and breathable fabric sensor.
(3) (test of temperature sensing Performance) cutting the composite fabric into 40 mm × 10 mm, fixing 2 copper wires as electrodes at two ends of the sample with conductive silver paste, respectively placing the multifunctional fabric sensor prepared in example 3 in different temperature environments, observing the resistance change, and finding out the relative resistance change ((R-R 0/R 0) Decreases with increasing temperature (as shown in fig. 10), exhibiting a negative temperature coefficient behavior. The relationship between the relative resistance and the temperature was explored by fitting. Fig. 11 is a temperature-sensitive sensing performance stability test of a fabric sensor that can maintain stable sensing signals over multiple heating and cooling cycles. Owing to the excellent temperature sensitivity of the composite fabric in the range of 20-50 ℃, the multifunctional fabric sensor is expected to be applied to real-time monitoring of the body temperature of a human body.
Comparative example 1
(1) Preparation of MXene:
the preparation process and conditions were the same as in step (1) of example 1.
(2) Preparing a multifunctional MXene fabric sensor:
and (3) fully mixing 0.24 g of Tris powder and 0.4 g of dopamine in 200 ml of deionized water, then putting the flexible elastic fabric into the solution, magnetically stirring and reacting for 6 hours, taking out the flexible elastic fabric after reaction, fully washing the flexible elastic fabric with the deionized water, and drying the flexible elastic fabric in an oven at 40 ℃ for 12 hours. The PDA modified stretch fabric was immersed in a 5 wt.% concentration of MXene colloidal solution for 10 minutes, then the fabric was removed and dried at 40 ℃ for 30min to make a fabric with 1 impregnation of MXene. Unlike example 1, the surface of the fabric impregnated with MXene 1 times is not treated by hydrophobic PDMS, the contact angle of MXene fabric prepared in comparative example 1 is 0 ° and the relative resistance is increased to 36.5 after 136 h, while the relative resistance of the super-hydrophobic composite fabric prepared in example 1 is only increased to about 3 and gradually kept stable, and the detailed data is shown in FIG. 12. Therefore, the MXene fabric can be endowed with super-hydrophobic performance by PDMS modification, and the MXene layer can be protected from being oxidized to a certain extent, so that the conductivity of the MXene fabric is prevented from being greatly reduced.
Comparative example 2
(1) Preparation of MXene:
the preparation process and conditions were the same as in step (1) of example 1.
(2) Preparing a multifunctional MXene fabric sensor:
the flexible stretch fabric without PDA finish was immersed in a 5 wt.% concentration of MXene colloidal solution for 10 minutes, followed by taking out the fabric and drying at 40 ℃ for 30min to make MXene impregnated 1-time fabric. To impart superhydrophobic properties to the fabric and maintain the intrinsic breathability of the fabric itself, the fabric impregnated with MXene 1 time was immersed in a 1wt.% solution of Polydimethylsiloxane (PDMS) in n-heptane for 20min and cured at 60 ℃ for 1h to give a waterproof and breathable fabric sensor. The fabric sensor of comparative example 1 had a lower conductivity, only one fifth of the conductivity of the fabric sensor of example 1, compared to the interface-modified multifunctional fabric sensor of example 1. The modification of PDA can provide a large number of active sites on the surface of inert fabric fibers, and hydrophilic functional groups on the surface of MXene can form hydrogen bonding action with the active sites, so that the MXene is firmly adsorbed on the surface of the fibers, the interface action between the MXene and the fibers is enhanced, and the conductivity of the MXene is greatly improved.
Claims (9)
1. The breathable waterproof multi-response fabric sensor is characterized by comprising a flexible elastic fabric substrate, an interface layer, a functional layer and a protective layer from inside to outside, wherein the interface layer is a poly-dopamine layer, the functional layer is an MXene network, and the protective layer is polydimethylsiloxane.
2. A preparation method of a breathable waterproof multi-response fabric sensor is characterized by comprising the following steps:
step 1, immersing a flexible elastic fabric into a dopamine alkaline solution, and stirring to perform a self-polymerization reaction of dopamine;
step 2, placing the elastic fabric modified by the polydopamine obtained in the step 1 into MXene colloidal solution for soaking for a period of time, taking out and drying, and repeating the soaking and drying process to obtain the elastic fabric with different MXene modification times;
and 3, putting the elastic fabric with different MXene modification times obtained in the step 2 into an n-heptane solution of polydimethylsiloxane for soaking and modifying for a period of time, and curing to obtain the breathable waterproof multi-response fabric sensor.
3. The method of claim 2, wherein in step 1, the alkaline solution of dopamine is a Tris solution of dopamine, wherein the concentration of dopamine is 0.2wt.% and the pH is 8.5.
4. The method of claim 2, wherein the MXene colloidal solution is prepared as follows in step 2:
(1) adding lithium fluoride into 9M dilute hydrochloric acid, and reacting for 15-30 minutes by magnetic stirring;
(2) adding MAX phase powder, and etching at 35 ℃ for 20-24 hours, wherein the mass ratio of MAX phase powder to lithium fluoride is 1: 1;
(3) and (3) washing the etched product with deionized water until the pH value of the supernatant is more than or equal to 6, mixing the supernatant and the precipitate, performing ultrasonic treatment for 1h, and centrifuging at 3500rpm for 1h to obtain the MXene colloidal solution.
5. The method of claim 4, wherein the MAX phase powder is Ti3AlC2。
6. The method of claim 2, wherein the concentration of MXene colloidal solution in step 2 is 4-7 mg/ml, and the immersion time is 5-15 minutes.
7. The method of claim 2, wherein the dip drying is repeated 0 or more times in step 2.
8. The method of claim 2, wherein the dip drying is repeated 0 to 4 times in step 2.
9. The method of claim 2, wherein in step 3, the polydimethylsiloxane is 1wt.% in n-heptane and the modification time is 20 to 60 minutes.
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