CN112556899B - Flexible pressure sensor and preparation method thereof - Google Patents

Flexible pressure sensor and preparation method thereof Download PDF

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Publication number
CN112556899B
CN112556899B CN202011428481.8A CN202011428481A CN112556899B CN 112556899 B CN112556899 B CN 112556899B CN 202011428481 A CN202011428481 A CN 202011428481A CN 112556899 B CN112556899 B CN 112556899B
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sericin
pressure sensor
flexible substrate
flexible
nano tube
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CN112556899A (en
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毕曙光
姜伟冬
杜进操
倪佳节
黄婉昕
张鹏宇
张国梁
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Wuhan Textile University
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Wuhan Textile University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01LMEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L1/00Measuring force or stress, in general
    • G01L1/20Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81BMICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B7/00Microstructural systems; Auxiliary parts of microstructural devices or systems
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • B81C1/00134Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems comprising flexible or deformable structures
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01LMEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L9/00Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
    • G01L9/02Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81BMICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B2201/00Specific applications of microelectromechanical systems
    • B81B2201/02Sensors
    • B81B2201/0264Pressure sensors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C2203/00Forming microstructural systems

Abstract

The invention belongs to the technical field of flexible pressure sensing materials, and particularly relates to a flexible pressure sensor which is environment-friendly, low in cost and simple in process and a preparation method thereof. The invention takes sericin (SS) as a dispersing agent and a binding agent, prepares a sericin dispersed carbon nano tube (SSCNT) aqueous solution by a simple physical method, and immerses Melamine Foam (MF) as an elastic substrate in the SSCNT aqueous solution to design and prepare a resistance-type flexible pressure sensor with a three-dimensional conductive network.

Description

Flexible pressure sensor and preparation method thereof
Technical Field
The invention relates to the technical field of sensor materials, in particular to a flexible pressure sensor and a preparation method thereof.
Background
In recent years, the flexible pressure sensor has attracted attention in the fields of medical systems, intelligent robots, electronic skins, wearable electronic devices and the like because of the advantages of elastic deformation, good biocompatibility, conversion of mechanical signals into visual electric signals by sensing surface acting force and the like. Most flexible sensing materials are mainly carbon-based materials, such as carbon nanotubes synthesized in situ by Chemical Vapor Deposition (CVD), carbon nanotubes dispersed by chemical reagents, reduced graphene oxide prepared by high-temperature heat treatment, and the like. However, the flexible sensors prepared by the methods have the problems of high cost, complex process, environmental pollution and the like. Therefore, the problem to be solved by those skilled in the art is how to provide a method for properly modifying a carbon nanotube and applying the modified carbon nanotube to the preparation of a flexible resistive pressure sensor with low cost, simple process, environmental friendliness, and stable performance.
Disclosure of Invention
The invention aims to provide a preparation method of a flexible pressure sensor, which is simple to operate, mild in condition, low in cost and stable in performance.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a flexible pressure sensor, which comprises a flexible substrate, a carbon nanotube layer dispersed by sericin and a lead, wherein the carbon nanotube layer is a carbon nanotube layer; the sericin dispersed carbon nanotube layer is attached to the surface of the flexible substrate.
The invention provides a preparation method of a flexible pressure sensor, which comprises the following steps:
(1) dipping a flexible substrate in an aqueous solution of sericin dispersed carbon nanotubes (SSCNT) to form a sericin dispersed carbon nanotube layer on the surface of the flexible substrate;
(2) and connecting the lead with two ends of the obtained flexible substrate containing the carbon nanotube layer to obtain the flexible pressure sensor.
Further, the concentration of the aqueous solution of the sericin dispersed carbon nanotube in the step (1) is 1-4 mg/mL.
Further, the dipping time in the step (1) is 10-50 min, and the dipping temperature is 20-30 ℃.
Further, the flexible substrate is Melamine Foam (MF).
Further, the aqueous solution of sericin dispersed carbon nanotubes in the step (1) is obtained by adding a surfactant into a mixed solution of carbon nanotubes and sericin.
Further, the surfactant is sodium dodecyl benzene sulfonate.
Further, the mass ratio of the carbon nano tube to the sericin to the surfactant is 2-5: 2-6: 1.
the invention has the beneficial effects that:
the invention utilizes the non-covalent modification and dispersion effect of sericin on the carbon nano tube, not only ensures that the carbon nano tube is dispersed more uniformly without influencing the self conductivity and has the excellent function of a biological base, but also ensures that the dispersion liquid is better absorbed on a flexible matrix and has excellent sensing performance. Meanwhile, sericin has a strong adhesion effect, the fastness between the flexible substrate and the carbon nano tube is enhanced, and an adhesive is not additionally added.
Drawings
FIG. 1 is a schematic diagram of a flexible pressure sensor according to the present invention;
FIG. 2 is a scanning electron micrograph of SSCNT loaded flexible matrix made according to the present invention;
FIG. 3 is a graph of conductivity curves for flexible substrates of different SSCNT loadings made in accordance with the present invention;
FIG. 4 is an X-ray diffraction curve of sericin and a carbon nanotube prepared by the method;
FIG. 5 is an IR spectrum of sericin and carbon nanotubes prepared according to the present invention;
FIG. 6 is a thermogravimetric plot of sericin and carbon nanotubes prepared according to the invention;
FIG. 7 is a drawing sensitivity analysis of the flexible substrate treated with the carbon nanotube solution prepared according to the present invention.
Detailed Description
The invention provides a flexible pressure sensor, which comprises a flexible substrate, a carbon nanotube layer dispersed by sericin and a lead, wherein the carbon nanotube layer comprises sericin; the sericin dispersed carbon nanotube layer is attached to the surface of the flexible substrate.
The invention provides a preparation method of a flexible pressure sensor, which comprises the following steps:
(1) dipping a flexible substrate in an aqueous solution of sericin dispersed carbon nanotubes (SSCNT) to form a sericin dispersed carbon nanotube layer on the surface of the flexible substrate;
(2) and connecting the lead with two ends of the obtained flexible substrate containing the carbon nanotube layer to obtain the flexible pressure sensor.
In the invention, the concentration of the sericin dispersed carbon nanotube aqueous solution in the step (1) is 1-4 mg/mL, preferably 3 mg/mL.
In the invention, the dipping time in the step (1) is 10-50 min, preferably 30 min; the dipping temperature is 20-30 ℃, and preferably 25 ℃.
In the present invention, the flexible substrate is preferably Melamine Foam (MF).
In the invention, the aqueous solution of the sericin dispersed carbon nano tube in the step (1) is obtained by adding a surfactant into a mixed solution of the carbon nano tube and the sericin.
In the present invention, the surfactant is preferably sodium dodecylbenzenesulfonate.
In the invention, the mass ratio of the carbon nano tube, the sericin and the surfactant is 2-5: 2-6: 1, preferably 3: 4: 1.
the technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) Dipping the pretreated flexible substrate into 1mg/mL aqueous solution of sericin dispersed carbon nanotubes (SSCNT) for ultrasonic treatment, then putting the flexible substrate into an oven for drying, then putting the flexible substrate into a constant temperature forced air drying oven for drying, wherein the drying temperature is 50 ℃, taking out after complete curing and drying, and calculating the MF of the SSCNT (load capacity of 10 percent).
(2) And connecting wires at the upper end and the lower end of the SSCNT/MF to manufacture the elastic three-dimensional foam-based pressure sensor.
The pretreatment in the step (1) comprises the following steps: immersing the flexible substrate in a Soxhlet extractor containing acetone solution, raising the temperature of the acetone solution from 0 ℃ to 50 ℃, stabilizing the solution to 50 ℃, putting the flexible substrate in the Soxhlet extractor containing the acetone solution for circulating reflux, carrying out one-time cleaning of the reflux, and carrying out reflux cleaning on the flexible substrate for 2 hours.
The 1mg/mL sericin dispersed carbon nanotube aqueous solution is obtained by adding sodium dodecyl benzene sulfonate into a carbon nanotube and sericin mixed solution subjected to probe ultrasonic treatment, magnetically stirring for 20min, and centrifuging at 2000rpm for 5 min. The mass ratio of the carbon nano tube to the sericin to the surfactant is 3: 4: 1.
example 2
(1) Dipping the pretreated flexible substrate into a 2mg/mL sericin dispersed carbon nanotube (SSCNT) water solution for ultrasonic treatment, then putting the flexible substrate into an oven for drying, then putting the flexible substrate into a constant temperature air blast drying oven for drying, wherein the drying temperature is 50 ℃, taking out after complete curing and drying, and calculating as the MF of the SSCNT (load capacity of 40%).
(2) And connecting leads at the upper end and the lower end of the SSCNT/MF to manufacture the elastic three-dimensional foam-based pressure sensor.
The pretreatment in step (1) was the same as in example 1.
The 2mg/mL sericin dispersed carbon nanotube aqueous solution is obtained by adding sodium dodecyl benzene sulfonate into a carbon nanotube and sericin mixed solution subjected to probe ultrasonic treatment, magnetically stirring for 25min, and centrifuging at 2000rpm for 5 min. The mass ratio of the carbon nano tube to the sericin to the surfactant is 3: 4: 1.
example 3
(1) Dipping the pretreated flexible substrate into a 3mg/mL aqueous solution of sericin dispersed carbon nanotubes (SSCNT) for ultrasonic treatment, then putting the flexible substrate into an oven for drying, then putting the flexible substrate into a constant temperature forced air drying oven for drying at a drying temperature of 50 ℃, taking out the flexible substrate after complete curing and drying, and calculating the MF of the SSCNT (80% of the loading).
(2) And connecting wires at the upper end and the lower end of the SSCNT/MF to manufacture the elastic three-dimensional foam-based pressure sensor.
The pretreatment in step (1) was the same as in example 1.
The aqueous solution of the sericin dispersed carbon nano tube of 3mg/mL is obtained by adding sodium dodecyl benzene sulfonate into a mixed solution of the carbon nano tube and the sericin treated by the probe by ultrasonic, magnetically stirring for 30min, and centrifuging for 5min at 2000 rpm. The mass ratio of the carbon nano tube to the sericin to the surfactant is 3: 4: 1.
example 4
(1) Dipping the pretreated flexible substrate into a 4mg/mL sericin dispersed carbon nanotube (SSCNT) aqueous solution for ultrasonic treatment, then putting the flexible substrate into an oven for drying, then putting the flexible substrate into a constant temperature air blast drying oven for drying, wherein the drying temperature is 50 ℃, taking out after complete curing and drying, and calculating the MF of the SSCNT (load capacity 110 percent).
(2) And connecting wires at the upper end and the lower end of the SSCNT/MF to manufacture the elastic three-dimensional foam-based pressure sensor.
The pretreatment in step (1) was the same as in example 1.
The 4mg/mL sericin dispersed carbon nanotube aqueous solution is obtained by adding sodium dodecyl benzene sulfonate into a carbon nanotube and sericin mixed solution subjected to probe ultrasonic treatment, magnetically stirring for 30min, and centrifuging at 2000rpm for 5 min. The mass ratio of the carbon nano tube to the sericin to the surfactant is 3: 4: 1.
it can be seen in fig. 2 that the sericin dispersed carbon nanotubes are uniformly supported on the surface of the flexible substrate.
As can be seen in FIG. 3, the conductivity of the resulting pressure sensor of the present application can be as high as 140 μ S/cm.
FIG. 4: x-ray diffraction was performed on the dried films of pristine carbon nanotubes, sericin and 50 wt% carbon nanotubes, indicating that the original crystal structure of CNTs was not altered by sericin treatment, and the high conductivity of carbon nanotubes was retained.
FIG. 5: and performing infrared spectrum curve on the original carbon nano tube, sericin and a sericin non-covalent carbon nano tube drying film to show that sericin is adsorbed on the surface of the carbon nano tube.
FIG. 6: thermogravimetric analysis was performed on pristine carbon nanotubes, sericin and sericin non-covalent carbon nanotubes.
As can be seen from fig. 7, the flexible pressure sensor with a load of 110% has the characteristics of strong tensile sensitivity and strong flexibility.
According to the embodiment, the flexible pressure sensor and the preparation method thereof are low in cost, simple in process, green and environment-friendly, and the prepared flexible pressure sensor is stable in performance and has wide application prospects.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (6)

1. A flexible pressure sensor is characterized by comprising a flexible substrate, a sericin dispersed carbon nanotube layer and a lead; the sericin dispersed carbon nanotube layer is attached to the surface of the flexible substrate;
the preparation method of the flexible pressure sensor comprises the following steps:
(1) dipping a flexible substrate into a sericin dispersed carbon nanotube aqueous solution to form a sericin dispersed carbon nanotube layer on the surface of the flexible substrate;
(2) connecting a lead with two ends of the obtained flexible substrate containing the carbon nanotube layer to obtain a flexible pressure sensor;
the aqueous solution of the sericin dispersed carbon nano tube in the step (1) is obtained by adding a surfactant into a mixed solution of the carbon nano tube and the sericin;
the mass ratio of the carbon nano tube to the sericin to the surfactant is 2-5: 2-6: 1.
2. a method of making a flexible pressure sensor as claimed in claim 1, comprising the steps of:
(1) dipping a flexible substrate into a sericin dispersed carbon nanotube aqueous solution to form a sericin dispersed carbon nanotube layer on the surface of the flexible substrate;
(2) connecting a lead with two ends of the obtained flexible substrate containing the carbon nano tube layer to obtain a flexible pressure sensor;
the aqueous solution of the sericin dispersed carbon nano tube in the step (1) is obtained by adding a surfactant into a mixed solution of the carbon nano tube and the sericin;
the mass ratio of the carbon nano tube to the sericin to the surfactant is 2-5: 2-6: 1.
3. the method for preparing a flexible pressure sensor according to claim 2, wherein the concentration of the aqueous solution of sericin dispersed carbon nanotubes in the step (1) is 1-4 mg/mL.
4. The method for preparing the flexible pressure sensor according to claim 3, wherein the dipping time in the step (1) is 10-50 min, and the dipping temperature is 20-30 ℃.
5. Method for producing a flexible pressure sensor according to claim 4, characterized in that the flexible substrate is melamine foam.
6. The method of claim 5, wherein the surfactant is sodium dodecylbenzenesulfonate.
CN202011428481.8A 2020-12-09 2020-12-09 Flexible pressure sensor and preparation method thereof Active CN112556899B (en)

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CN104622787A (en) * 2014-11-25 2015-05-20 陶虎 Sericin protein microneedle for drug delivery and preparation method thereof
CN104451933B (en) * 2014-12-09 2016-04-13 浙江天濮环保科技有限公司 The method of the nano-fiber material of preparation containing sericin/nano-sized carbon
CN109401337A (en) * 2018-09-30 2019-03-01 厦门大学 A kind of flexible compound conductive film and preparation method thereof
CN110251110A (en) * 2019-04-22 2019-09-20 太原理工大学 Composite and flexible carbon nano-tube film, pliable pressure sensor and preparation method thereof
CN110455176A (en) * 2019-07-19 2019-11-15 南京邮电大学 The preparation method of flexible strain transducer
CN110699949B (en) * 2019-11-01 2021-10-08 电子科技大学 Flexible self-adhesive cloth with pressure/friction force sensing function, flexible mechanical sensor and preparation method of flexible mechanical sensor
CN111926563B (en) * 2020-07-03 2022-12-09 武汉纺织大学 Strain sensing fabric and preparation method thereof
CN111941985B (en) * 2020-08-26 2022-09-30 武汉纺织大学 Flexible strain sensing material and preparation method thereof

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