CN112754464B - Application of MXene/fabric-based sensor with sandwich structure in respiration monitoring - Google Patents

Application of MXene/fabric-based sensor with sandwich structure in respiration monitoring Download PDF

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CN112754464B
CN112754464B CN202011406324.7A CN202011406324A CN112754464B CN 112754464 B CN112754464 B CN 112754464B CN 202011406324 A CN202011406324 A CN 202011406324A CN 112754464 B CN112754464 B CN 112754464B
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mxene
fabric
flexible
conductive
layer
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CN112754464A (en
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侯成义
吴钦鑫
刘芮
李耀刚
王宏志
张青红
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Donghua University
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B5/00—Measuring for diagnostic purposes; Identification of persons
    • A61B5/08—Detecting, measuring or recording devices for evaluating the respiratory organs
    • A61B5/0816—Measuring devices for examining respiratory frequency
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B5/00—Measuring for diagnostic purposes; Identification of persons
    • A61B5/68—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient
    • A61B5/6801—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient specially adapted to be attached to or worn on the body surface
    • A61B5/6802—Sensor mounted on worn items
    • A61B5/6803—Head-worn items, e.g. helmets, masks, headphones or goggles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
    • A61B2562/16—Details of sensor housings or probes; Details of structural supports for sensors
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
    • A61B2562/16—Details of sensor housings or probes; Details of structural supports for sensors
    • A61B2562/164—Details of sensor housings or probes; Details of structural supports for sensors the sensor is mounted in or on a conformable substrate or carrier

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  • Molecular Biology (AREA)
  • Heart & Thoracic Surgery (AREA)
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  • Measurement Of The Respiration, Hearing Ability, Form, And Blood Characteristics Of Living Organisms (AREA)

Abstract

The invention relates to application of an MXene/fabric-based sensor with a sandwich structure in respiration monitoring. The sensor comprises a flexible electrode layer, a flexible force-sensitive sensing layer and a flexible packaging layer, wherein the flexible force-sensitive sensing layer is made of MXene/fabric composite materials. The sensor has high sensitivity, quick response to external pressure change, better flexibility, better biocompatibility, better stability and durability, can be used for monitoring the respiratory frequency of a human body, and has wide application prospect in the field of health.

Description

Application of MXene/fabric-based sensor with sandwich structure in respiration monitoring
Technical Field
The invention belongs to the application field of force-sensitive sensors, and particularly relates to an application of an MXene/fabric-based sensor with a sandwich structure in respiratory monitoring.
Background
The flexible sensor is made of flexible materials, has good flexibility and ductility, can even be freely bent or folded, has flexible and various structural forms, can be arranged according to the measurement conditions and the requirements of a test object, makes up the defects of the rigid sensor, and can effectively and quickly detect. The novel flexible sensor is widely applied to the fields of electronic skin, medical care, electronic products, textiles, aerospace, environmental monitoring and the like.
The flexible wearable force-sensitive sensor is mainly formed by combining a conductive network and a flexible substrate. In recent years, nanomaterials are widely used in the preparation of flexible force-sensitive sensors, such as metal nanoparticles, carbon nanotubes, metal nanowires, polymer nanofibers, graphene, etc., due to their excellent mechanical flexibility and electrical conductivity. MXene is a two-dimensional layered nano material with large specific surface area, good hydrophilicity and high conductivity, and can be widely applied to the fields of electrochemical energy storage, transparent electrode materials, nano composite materials and the like. Although multilayer MXene composite meshes have a large specific surface area and strong electrical conductivity, they are rarely used to make flexible force-sensitive sensors.
Disclosure of Invention
The invention aims to solve the technical problem of providing the application of the MXene/fabric-based sensor with a sandwich structure in respiratory monitoring so as to fill the blank in the prior art.
The invention provides an application of an MXene/fabric-based sensor with a sandwich structure in respiratory monitoring.
The MXene/fabric-based sensor with the sandwich structure is used for a mask with an air valve. The method specifically comprises the following steps: the MXene/fabric-based sensor with the sandwich structure is fixed at the air valve of the mask.
The MXene/fabric-based sensor with the sandwich structure comprises a flexible electrode layer, a flexible force-sensitive sensing layer and a flexible packaging layer, wherein the flexible force-sensitive sensing layer is made of an MXene/fabric composite material.
The flexible electrode layer is an interdigital electrode screen-printed on a flexible substrate.
The flexible packaging layer is an insulating adhesive tape.
The flexible substrate is one of non-woven fabric, nylon, pure cotton cloth and terylene.
The electrode material of the flexible electrode layer is one of conductive ink, conductive silver paste and conductive carbon black.
The insulating adhesive tape is a VHB adhesive tape or a PI adhesive tape.
The preparation method of the MXene/fabric-based sensor with the sandwich structure comprises the following steps: (1) Dipping the fabric in MXene dispersion liquid, and drying to obtain MXene conductive fabric; (2) And (2) superposing the MXene conductive fabric and the flexible interdigital electrode in the step (1) from top to bottom, contacting an interdigital electrode surface with the MXene conductive fabric, connecting two ends of the interdigital electrode by using silver wires and fixing the interdigital electrode by using conductive silver paste, fixing the interdigital electrode into a sandwich structure by using an insulating adhesive tape, and packaging to obtain the conductive interdigital electrode.
The fabric in the step (1) is one of non-woven fabric, nylon, pure cotton cloth and terylene.
The preparation method of the MXene dispersion liquid in the step (1) comprises the following steps: mixing MAX phase (Ti) 3 AlC 2 ) Adding the mixture into an etching solution of ultrapure water, hydrochloric acid and hydrofluoric acid, etching, centrifuging for the first time, dispersing the obtained precipitate in deionized water, centrifuging for the second time, and taking the upper-layer dispersion solution to obtain the catalyst, wherein the mass ratio of the ultrapure water, the hydrochloric acid, the hydrofluoric acid and the MAX phase is 4.0-9.0: 10.0-18.0: 1.0-3.0: 0.5-1.0.
The first centrifugation is as follows: centrifuging for many times until the pH of the supernatant is close to 7, wherein the speed of centrifuging for many times is 3500 to 4000 r/min, and the centrifuging time is 3 to 7min each time.
The etching temperature is 25 to 35 ℃, the etching time is 24 to 30h, and the stirring speed in the etching process is 400 to 1000 r/min.
The second centrifugation speed is 3500 to 4000 r/min, and the centrifugation time is 1 to 5 min.
The active sensing material of the flexible force-sensitive sensing layer is MXene.
Advantageous effects
(1) The breathing frequency detection sensor material based on MXene has the advantages of high sensitivity, quick response to external pressure change, good flexibility, good biocompatibility, good stability and durability, can be used for monitoring the breathing frequency of a human body, and has wide application prospect in the field of health;
(2) The invention is simple, non-toxic, harmless and low in cost, and provides a low-cost and portable method for detecting the respiratory rate.
Drawings
FIG. 1 is a time-current graph of the sensor breathing frequency test in example 1.
Fig. 2 is an XRD pattern of MXene prepared in example 1-2.
Fig. 3 is an SEM image of the flexible interdigital electrode in example 1.
Fig. 4 is a physical diagram of the flexible interdigital electrode in example 1.
FIG. 5 is SEM images of the flexible force-sensitive sensing layers (b, d) of the cotton fabrics (a, c) and MXene/cotton of example 1-2 at different magnifications.
Fig. 6 is a flow chart of the structure and preparation of a sandwich-structured MXene/fabric-based respiration monitoring sensor of example 1-2.
Fig. 7 is a graph of the sensitivity of the MXene/fabric-based respiration monitoring sensor of example 1.
Fig. 8 is a graph of the sensitivity of the MXene/fabric-based respiration monitoring sensor of example 2.
Fig. 9 is a time-current plot of the sensor breathing rate test in example 2.
Fig. 10 is an SEM image of the flexible interdigital electrode of example 2.
Fig. 11 is a physical diagram of the flexible interdigital electrode in example 2.
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. Further, it should be understood that various changes or modifications of the present invention can be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the claims appended to the present application.
Example 1
(1) Preparation process of MXene:
5.0 g, 12 g and 2.5 g of ultrapure water, hydrochloric acid and HF are sequentially added into a reagent bottle to obtain etching solution, the etching solution is fully stirred, and then 1g of MAX phase Ti is added into the etching solution for a plurality of times in small amount 3 AlC 2 And continuously stirring the powder for etching for 24 hours until the etching is complete. Washing was performed by multiple centrifugations at 3500 r/min until the supernatant pH was close to 7. And then fully dispersing the obtained precipitate in deionized water, centrifuging at 3500 r/min for 5 min, and collecting the upper black liquid, namely MXene dispersion liquid. Fig. 2 is an XRD pattern of MXene prepared in this example, which shows that MXene is completely etched.
(2) The preparation process of the flexible interdigital electrode comprises the following steps:
the nylon is placed under the silk screen plate, and the two are fixed well. Pouring a certain amount of conductive silver paste on the screen plate, applying a certain pressure on the conductive silver paste on the screen plate by using a scraper, moving towards the other side of the screen plate, and extruding the conductive silver paste on a nylon flexible substrate from meshes of a circuit part by the scraper in the moving process to obtain a clear circuit, so that the flexible interdigital electrode is obtained, wherein the microstructure of the flexible interdigital electrode is shown in figure 3, and the physical diagram of the flexible interdigital electrode is shown in figure 4.
(3) Preparing a flexible force-sensitive sensing layer of MXene/pure cotton:
placing a pure cotton fabric with the size of 3 x 3cm into a culture dish containing the MXene aqueous dispersion (18 mg/ml) obtained in the step (1), soaking for 2h, and drying with cold air.
(4) Repeating the step (3) for 3 times to obtain the MXene/pure cotton flexible force-sensitive sensing layer with uniform adhesion, wherein the surface appearance is shown in FIG. 5, the surface of the pure cotton fiber is smooth, the MXene/pure cotton composite fabric has wrinkles on the fiber surface, and the MXene with the sheet layer on the surface is coated on the fiber surface.
(5) Preparing an MXene-based respiratory rate detection sensor:
and (3) connecting the flexible interdigital electrode obtained in the step (2) with the MXene/pure cotton flexible force-sensitive sensing layer obtained in the step (4), fixing the two ends of the interdigital electrode by using silver wires and conductive silver paste, finally packaging by using a VHB adhesive tape, and obtaining the MXene-based respiratory rate detection sensor as a flow chart shown in fig. 6.
(6) The application of the breathing frequency detection sensor based on MXene is shown in FIG. 7, and the calculation formula of the sensitivity is S = (delta I/I) 0 ) Δ P, where Δ I is the change from the initial current after load pressure, I 0 Is the initial current value, Δ P is the pressure differential value. The sensor is placed at an air valve of the mask, the sensor is placed at a vent valve of the mask, a response time current curve can be obtained through expiration and inspiration, and the peak value of the curve shown in figure 1 is stable, so that the respiratory frequency times per minute of a human body are calculated.
FIG. 7 shows that: the sensitivity of a flexible force sensitive sensor consists of three regions: the sensitivity coefficients of S1, S2, S3 and S4 are respectively 1.287, 10.025, 18.023 and 5.367 kPa when S1 is in a low-pressure range (347-1248 Pa), S2 is 1477-3082kPa when S2 is in a pressure range, S3 is 3.5-7.6 kPa when S3 is in a pressure range, and S4 is 8.6-17.1 kPa when S4 is in a pressure range -1 。
Example 2
According to the embodiment 1, the nylon in the preparation process of the flexible interdigital electrode in the embodiment 1 is modified into pure cotton, the rest is the same as the embodiment 1, the MXene-based respiration rate detection is obtained, the sensitivity is shown in the graph 8, and the sensitivity is S 1 、S 2 Two zones of 0.339kPa each -1 And 0.514kPa -1 The sensor is placed at an air valve of the mask, and the sensor breathes in a normal state and breathes in a post-exercise state to obtain a response time current curve, as shown in fig. 9, so that the breathing frequency times of the human body per minute are calculated.
Fig. 10 is an SEM image of interdigital electrodes on a pure cotton fabric, and fig. 11 is an actual image, which shows that the screen-printed electrodes are not well bonded to the pure cotton fabric, and the electrodes are easily detached.

Claims (7)

1. The MXene/fabric-based sensor with the sandwich structure comprises a flexible electrode layer, a flexible force-sensitive sensing layer and a flexible packaging layer, wherein the flexible force-sensitive sensing layer is made of MXene/fabric composite materials;
the preparation method of the MXene/fabric-based sensor with the sandwich structure comprises the following steps: (1) Dipping the fabric in MXene dispersion liquid, and drying to obtain MXene conductive fabric; (2) Superposing the MXene conductive fabric and the flexible interdigital electrode in the step (1) up and down, contacting an interdigital electrode surface with the MXene conductive fabric, connecting two ends of the interdigital electrode by silver wires and fixing by conductive silver paste, fixing into a sandwich structure by using an insulating adhesive tape, and packaging to obtain the conductive interdigital electrode;
the preparation method of the MXene dispersion liquid in the step (1) comprises the following steps: adding the MAX phase into an etching solution of ultrapure water, hydrochloric acid and hydrofluoric acid, etching, centrifuging for the first time, dispersing the obtained precipitate in deionized water, centrifuging for the second time, and taking the upper layer dispersion solution to obtain the nano-silver/zinc alloy composite material, wherein the mass ratio of the ultrapure water, the hydrochloric acid, the hydrofluoric acid and the MAX phase is 4.0 to 9.0: 10.0 to 18.0: 1.0 to 3.0: 0 to 5: 1.0.
2. The use according to claim 1, wherein the sandwich of MXene/fabric based sensors is used for masks with air valves.
3. The use according to claim 1, wherein the flexible electrode layer is an interdigitated electrode screen printed on a flexible substrate; the flexible packaging layer is an insulating adhesive tape.
4. The use of claim 3, wherein the flexible substrate is one of non-woven fabric, nylon, cotton, and polyester; the electrode material of the flexible electrode layer is one of conductive ink, conductive silver paste and conductive carbon black.
5. Use according to claim 3, wherein the insulating tape is a VHB tape or a PI tape.
6. The use of claim 1, wherein the fabric in step (1) is one of non-woven fabric, nylon, cotton, and dacron.
7. The application of the composition as claimed in claim 1, wherein the etching temperature is 25 to 35 ℃, and the etching time is 24 to 30h; the stirring time is 1 to 2 hours.
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Publication number Priority date Publication date Assignee Title
CN113907744A (en) * 2021-12-14 2022-01-11 河北工业大学 Paper-based pressure sensor and wearable device capable of monitoring respiration

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108469319A (en) * 2018-03-20 2018-08-31 西南交通大学 A kind of flexible force sensitive sensor and preparation method thereof, array device and application
CN109793520A (en) * 2019-02-01 2019-05-24 电子科技大学 The flexible fabric respiration transducer and preparation method thereof of humidity and strain collaboration sensitivity
CN110726496A (en) * 2019-10-11 2020-01-24 东华大学 MXene coated textile force-sensitive sensor and preparation method thereof
CN111671426A (en) * 2020-05-13 2020-09-18 北京航空航天大学 Human body respiration state monitoring system and method based on flexible sensing and deep learning
CN111678425A (en) * 2020-05-22 2020-09-18 扬州大学 Breathable and waterproof multi-response fabric sensor
CN111759315A (en) * 2020-06-19 2020-10-13 南京邮电大学 Preparation method of self-powered electronic skin system based on laser reduction graphene/MXene composite material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108469319A (en) * 2018-03-20 2018-08-31 西南交通大学 A kind of flexible force sensitive sensor and preparation method thereof, array device and application
CN109793520A (en) * 2019-02-01 2019-05-24 电子科技大学 The flexible fabric respiration transducer and preparation method thereof of humidity and strain collaboration sensitivity
CN110726496A (en) * 2019-10-11 2020-01-24 东华大学 MXene coated textile force-sensitive sensor and preparation method thereof
CN111671426A (en) * 2020-05-13 2020-09-18 北京航空航天大学 Human body respiration state monitoring system and method based on flexible sensing and deep learning
CN111678425A (en) * 2020-05-22 2020-09-18 扬州大学 Breathable and waterproof multi-response fabric sensor
CN111759315A (en) * 2020-06-19 2020-10-13 南京邮电大学 Preparation method of self-powered electronic skin system based on laser reduction graphene/MXene composite material

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