CN107345840B - Preparation method of flexible force-sensitive sensor based on silver-loaded nanofiber - Google Patents

Preparation method of flexible force-sensitive sensor based on silver-loaded nanofiber Download PDF

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CN107345840B
CN107345840B CN201710568869.XA CN201710568869A CN107345840B CN 107345840 B CN107345840 B CN 107345840B CN 201710568869 A CN201710568869 A CN 201710568869A CN 107345840 B CN107345840 B CN 107345840B
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silver
sodium alginate
nano
flexible force
loaded
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CN107345840A (en
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龙云泽
胡伟鹏
张斌
王晓雄
张俊
罗维玲
张志广
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Qingdao 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
    • G01L1/22Measuring 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 using resistance strain gauges
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61BDIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B5/00Measuring for diagnostic purposes; Identification of persons
    • A61B5/68Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient
    • A61B5/6801Arrangements 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
    • A61B5/683Means for maintaining contact with the body
    • A61B5/6832Means for maintaining contact with the body using adhesives
    • A61B5/6833Adhesive patches
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/10Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/18Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/83Treating 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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles

Abstract

The invention discloses a flexible force-sensitive sensor based on silver-loaded nano-fibers and a preparation method thereof, wherein the sensor comprises a flexible force-sensitive resistance film, the flexible force-sensitive resistance film is connected with a power supply and an ammeter in series, the flexible force-sensitive resistance film comprises a silver-loaded nano-fiber film, the silver-loaded nano-fiber film consists of alginic acid/silver nano-particle composite nano-fibers, the alginic acid/silver nano-particle composite nano-fibers are sodium alginate nano-fibers prepared by an electrostatic spinning method, the alginic acid/silver nano-particle composite nano-fibers are prepared by ion exchange of sodium alginate nano-fibers, and then silver ions are reduced to prepare the sensor. The sensitive resistor of the sensor has good flexibility, can be directly adhered to the skin without hurting the skin, has good temperature property and sensitivity, and can realize the monitoring of physiological activities such as pulse, respiratory frequency, heartbeat and the like. Meanwhile, the antibacterial skin care product has an antibacterial effect and is safer to directly contact with the skin.

Description

Preparation method of flexible force-sensitive sensor based on silver-loaded nanofiber
Technical Field
The invention belongs to the field of sensors, and particularly relates to a preparation method of a flexible force-sensitive sensor based on silver-loaded nano fibers.
Background
Due to the urgent needs of modern society on health detection, man-machine communication, pressure distribution detection and the like, the flexible pressure sensor based on the working principle of the pressure sensor becomes an emerging research hotspot. At present, the application of the pressure sensor is not limited to the industrial production aspects of water conservancy and hydropower, railway transportation, intelligent buildings, production automatic control, aerospace, military industry, petrochemical industry, ships, machine tools, pipelines and the like. There is also a great demand in sports health, i.e. detecting movement status, respiration status, health indicators, etc. With the development of society, electronic devices are miniaturized to become a new research hotspot, and the traditional electronic devices are used for human skin and can cut or even infect bacteria, so that the traditional electronic devices are harmful to the health of human bodies. Flexibility becomes a hotspot of our attention. However, due to the limitations of material properties and manufacturing processes, research on flexible electronic devices based on pressure sensors is less, and electronic skins which are used on skins and have both flexibility and antibacterial property are still blank. The polymer material micro-nano fiber membrane prepared by the electrostatic spinning method has good flexibility, the composite nano fiber prepared by doping particles of a conductive material into an electrospinning precursor solution has certain conductivity, and has a potential application prospect in the aspect of flexible sensors, particularly the nano silver particles with antibacterial and conductive dual functions, the composite fiber obtained by taking the nano silver particles as a dopant theoretically has conductivity and antibacterial property and has good application prospect, however, the existing electrostatic spinning method has many defects in preparing silver-loaded nano fibers, and the doping amount of the silver nano particles is severely restricted by spinnability in the direct blending process; and the nano particles are easy to agglomerate, uniform spinning precursor liquid is not easy to obtain, so that the silver nano particles are not uniformly distributed in the material, and the prepared nano fibers have non-uniform diameters, thereby affecting the performance of the material.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides a preparation method of a flexible force-sensitive sensor based on silver-loaded nano-fibers. The sensor has the advantages of simple preparation method, low cost and suitability for large-scale production, the sensitive resistor of the sensor has good flexibility, can be directly adhered to the skin without damaging the skin, has good temperature property and sensitivity, and can realize the monitoring of physiological activities such as pulse, respiratory frequency, heartbeat and the like. Meanwhile, the antibacterial skin care product has an antibacterial effect and is safer to directly contact with the skin.
In order to solve the problems, the invention provides a preparation method of a flexible force-sensitive sensor based on silver-loaded nano-fibers, which comprises a flexible force-sensitive resistance film, the flexible force-sensitive resistance film is connected with a power supply and an ammeter in series, the flexible force-sensitive resistance film comprises a silver-loaded nanofiber film, and elastic protective films covering the upper and lower surfaces of the silver-loaded nanofiber membrane, wherein both ends of the silver-loaded nanofiber membrane are respectively connected with a lead, the silver-loaded nanofiber membrane consists of alginic acid/silver nanoparticle composite nanofibers, the alginic acid/silver nanoparticle composite nano-fiber is prepared by preparing sodium alginate nano-fiber by an electrostatic spinning method, preparing silver alginate nano-fiber by ion exchange, and reducing silver ions, the interior and the outer surface of the alginic acid/silver nanoparticle composite nanofiber are uniformly distributed with silver nanoparticles.
Preferably, when the flexible force-sensitive resistance film is deformed by pressure, the resistance changes along with the deformation degree, the larger the pressure is, the larger the deformation degree is, the smaller the resistance of the flexible force-sensitive resistance film is, and the larger the current displayed by the ammeter is.
When the inventor tests the electrical performance of the product, the resistance of the flexible force-sensitive resistance film of the invention decreases with the increase of the bending curvature of the film (i.e. the resistance of the flexible force-sensitive resistance film decreases with the increase of the deformation degree under the larger pressure), and the inventor thinks that the flexible force-sensitive resistance film has the property because: (1) when the silver-loaded nanofiber membrane is deformed under pressure, the fibers are in closer contact with each other, so that the number of indirect fiber contacts is increased, the conductivity of the material is enhanced, and the resistance is reduced; (2) in the process, the distance between silver nano particles on the silver-loaded nano fibers is reduced when the silver nano particles are pressed and bent, the particles are contacted more closely, the conductivity of the material is enhanced, the resistivity is reduced, the change of the pressure borne by the flexible force-sensitive resistance film can be analyzed and judged through the change of the current representation number of the sensor by utilizing the property, the sensitivity of the sensor is extremely high, the flexible force-sensitive resistance film of the sensor is adhered to the skin, and the monitoring on the physiological activities such as pulse, respiratory frequency, heartbeat and the like can be realized through the fluctuation of the flexible force-sensitive resistance film along with the skin. Meanwhile, based on the antibacterial property of the silver nanoparticles of the silver-loaded nanofibers, the flexible force-sensitive resistor film of the sensor is directly contacted with the skin, and the sensor is safer when being applied to the medical field.
Preferably, the sodium alginate nanofiber is a composite nanofiber of sodium alginate and a water-soluble polymer material.
The preparation of the pure sodium alginate fiber by the electrostatic spinning method has certain difficulty, the spinnability of the sodium alginate can be enhanced by adding the water-soluble polymer, the sodium alginate composite fiber can be prepared more easily, and the water-soluble polymer material in the sodium alginate composite fiber can be dissolved in the reaction liquid in the subsequent process of soaking in the reaction liquid for ion exchange to load silver ions, so that the composition of the finally obtained alginic acid/nano-silver composite nanofiber and the structural performance of the fiber can not be influenced.
Preferably, the water-soluble material is one or more of polyethylene oxide, polyvinylpyrrolidone and polyvinyl alcohol.
Preferably, the elastic protective film is a Polydimethylsiloxane (PDMS) elastic film.
The invention also discloses a preparation method of the flexible force-sensitive sensor based on the silver-loaded nano fiber, which comprises the following steps:
(1) electrospinning sodium alginate nanofiber: preparing spinning precursor solution containing sodium alginate, and preparing a sodium alginate nanofiber membrane by using an electrostatic spinning method;
(2) loading silver ions: soaking the sodium alginate nano-fiber prepared in the step (1) in a silver nitrate solution to perform ion exchange between sodium ions and silver ions of the fiber to form a silver alginate nano-fiber, taking out a sample, and washing the sample with deionized water;
(3) reducing silver ions: soaking the sample obtained in the step (2) in a reducing agent solution to reduce silver ions in and on the fiber, washing the sample with deionized water after a silver nanoparticle coating shell layer is formed on the surface of the sodium alginate nanofiber, and drying the sample to obtain the silver-loaded nanofiber membrane;
(4) assembling the force sensitive resistor: connecting two ends of the silver-loaded nanofiber membrane obtained in the step (3) with a lead through silver adhesive, and coating elastic protective films on the upper surface and the lower surface of the silver-loaded nanofiber membrane to obtain a flexible force-sensitive resistor film;
(5) assembling devices: and (4) connecting the flexible force-sensitive resistance film obtained in the step (4) with a power supply and an ammeter in series to obtain the flexible force-sensitive sensor.
In the preparation process of the silver-loaded nanofiber membrane, the sodium alginate nanofiber is prepared by adopting electrostatic spinning, and then ion exchange and in-situ reduction self-assembly are combined, so that the limit of spinnability on the doping amount of the nano silver particles is successfully overcome, the problem of agglomeration of the nano silver particles in the electrospinning process is avoided, the method can realize large-scale production of the composite fiber containing nano silver, the sodium alginate nanofiber has small diameter and large specific surface area and can be fully contacted with a silver nitrate solution for ion exchange, silver ions are fully loaded in the fiber and on the surface of the fiber, and the loaded silver ions are further reduced into silver nanoparticles, so that the content of the silver nanoparticles in the obtained silver-loaded alginate nanofiber is high, the nano silver particles are uniformly distributed in the fiber and on the surface of the fiber, the composite fiber is directly nano-scale, and has larger specific surface area, so that more contact sites are formed among the fibers, so that the material has excellent electrical properties. In addition, the particle size of the nano silver particles of the composite nano fiber can be controlled by adjusting the test parameters of the silver ion loading in the step (2) and the silver ion reduction in the step (3), so that the performance and the appearance of the material can be flexibly adjusted.
Preferably, the step (1) of electrospinning sodium alginate nanofibers: weighing 0.5-2 g of sodium alginate powder at normal temperature, adding the sodium alginate powder into a container, adding 0.1-0.2 g of polyethylene oxide, 0.4-0.5 g of triton, 2-3 g of dimethyl sulfoxide and 30-40 g of deionized water, stirring the mixture at normal temperature until the solution is uniform and transparent to obtain a spinning precursor solution, injecting the spinning precursor solution into an electrostatic spinning device, preparing sodium alginate nanofibers by an electrostatic spinning method, wherein the spinning voltage is 10-15 kV, the spinning distance is 12-18 cm, the spinning time is 20-30 min, and drying the sodium alginate nanofibers obtained by electrospinning in an oven at 40-60 ℃ for 1-3 h.
Preferably, the step (1) of electrospinning sodium alginate nanofibers: weighing 1-2 g of sodium alginate powder at normal temperature, adding the sodium alginate powder into a container, adding 0.5-1 g of polyvinyl alcohol, 0.4-0.5 g of triton, 2-3 g of dimethyl sulfoxide and 30-40 g of deionized water, stirring the mixture at normal temperature until the solution is uniform and transparent to obtain a spinning precursor solution, injecting the spinning precursor solution into an electrostatic spinning device, preparing sodium alginate nanofibers by using an electrostatic spinning method, wherein the spinning voltage is 12-18 kV, the spinning distance is 10-15 cm, the spinning time is 20-30 min, placing the sodium alginate nanofibers obtained by electrospinning into an oven, and drying the sodium alginate nanofibers for 1-3 h at 40-60 ℃ in the oven
Preferably, the step (2) is characterized in that the silver ion loading: preparing a silver nitrate aqueous solution, wherein the content of silver nitrate in the silver nitrate aqueous solution is 20-30 wt%, soaking the sodium alginate nanofiber prepared in the step (1) in the silver nitrate aqueous solution for 20-30 minutes, taking out, and washing with deionized water for 2-3 times.
Preferably, the step (3) reduces silver ions: immersing the sample obtained in the step (2) in a dimethylamino borane aqueous solution to reduce silver ions inside and on the surface of the fiber, wherein the content of the methylamino borane in the dimethylamino borane aqueous solution is 5 multiplied by 10-2And (3) soaking for 10-20 minutes in wt%, taking out, washing with deionized water for 3-4 times, and drying in an oven at 50 ℃ for 2-5 hours to obtain the silver-loaded nanofiber membrane.
The invention has the beneficial effects that: the invention provides a preparation method of a flexible force-sensitive sensor based on silver-loaded nano fibers. The sensor has the advantages of simple preparation method, low cost and suitability for large-scale production, the sensitive resistor of the sensor has good flexibility, can be directly adhered to the skin without damaging the skin, has good temperature property and sensitivity, and can realize the monitoring of physiological activities such as pulse, respiratory frequency, heartbeat and the like. Meanwhile, the antibacterial skin care product has an antibacterial effect and is safer to directly contact with the skin.
(1) When the inventor tests the electrical performance of the product, the resistance of the flexible force-sensitive resistance film of the invention decreases with the increase of the bending curvature of the film (i.e. the resistance of the flexible force-sensitive resistance film decreases with the increase of the deformation degree under the larger pressure), and the inventor thinks that the flexible force-sensitive resistance film has the property because: (1) when the silver-loaded nanofiber membrane is deformed under pressure, the fibers are in closer contact with each other, so that the number of indirect fiber contacts is increased, the conductivity of the material is enhanced, and the resistance is reduced; (2) in the process, the distance between silver nano particles on the silver-loaded nano fibers is reduced when the silver nano particles are pressed and bent, the particles are contacted more closely, the conductivity of the material is enhanced, the resistivity is reduced, the change of the pressure borne by the flexible force-sensitive resistance film can be analyzed and judged through the change of the current representation number of the sensor by utilizing the property, the sensitivity of the sensor is extremely high, the flexible force-sensitive resistance film of the sensor is adhered to the skin, and the monitoring on the physiological activities such as pulse, respiratory frequency, heartbeat and the like can be realized through the fluctuation of the flexible force-sensitive resistance film along with the skin. Meanwhile, based on the antibacterial property of the silver nanoparticles of the silver-loaded nanofibers, the flexible force-sensitive resistor film of the sensor is directly contacted with the skin, and the sensor is safer when being applied to the medical field.
(2) In the preparation process of the silver-loaded nanofiber membrane, the sodium alginate nanofiber is prepared by adopting electrostatic spinning, and then ion exchange and in-situ reduction self-assembly are combined, so that the limit of spinnability on the doping amount of the nano silver particles is successfully overcome, the problem of agglomeration of the nano silver particles in the electrospinning process is avoided, the method can realize large-scale production of the composite fiber containing nano silver, the sodium alginate nanofiber has small diameter and large specific surface area and can be fully contacted with a silver nitrate solution for ion exchange, silver ions are fully loaded in the fiber and on the surface of the fiber, and the loaded silver ions are further reduced into silver nanoparticles, so that the content of the silver nanoparticles in the obtained silver-loaded alginate nanofiber is high, the nano silver particles are uniformly distributed in the fiber and on the surface of the fiber, the composite fiber is directly nano-scale, and has larger specific surface area, so that more contact sites are formed among the fibers, so that the material has excellent electrical properties. In addition, the particle size of the nano silver particles of the composite nano fiber can be controlled by adjusting the test parameters of the silver ion loading in the step (2) and the silver ion reduction in the step (3), so that the performance and the appearance of the material can be flexibly adjusted.
Drawings
FIG. 1: TEM photograph of silver-loaded nanofiber membrane of pressure sensor of example 1;
FIG. 2: I-U diagrams of the pressure sensor of example 1 under different pressures;
FIG. 3: stability test curve of the pressure sensor of example 1;
FIG. 4: breath test curve.
Detailed Description
In order to clearly illustrate the technical features of the present solution, the following explains the present solution by way of embodiments.
Example 1
A flexible force-sensitive sensor based on silver-loaded nano-fiber comprises a flexible force-sensitive resistance film, wherein the flexible force-sensitive resistance film is connected with a power supply and an ammeter in series, the flexible force-sensitive resistance film comprises a silver-loaded nano-fiber film and elastic protective films covering the upper surface and the lower surface of the silver-loaded nano-fiber film, two ends of the silver-loaded nano-fiber film are respectively connected with a lead, the silver-loaded nano-fiber film consists of alginic acid/silver nano-particle composite nano-fiber, the alginic acid/silver nano-particle composite nano-fiber is sodium alginate nano-fiber prepared by an electrostatic spinning method, silver alginate nano-fiber is prepared by ion exchange, silver ions are reduced, nano-silver particles are uniformly distributed inside and on the outer surface of the alginic acid/silver nano-particle composite nano-fiber, and the preparation method of the flexible force-sensitive sensor, the method comprises the following steps:
(1) electrospinning sodium alginate nanofiber: weighing 1.3g of sodium alginate powder at normal temperature, adding the sodium alginate powder into a container, adding 0.7g of polyvinyl alcohol, 0.5g of triton, 2g of dimethyl sulfoxide and 33g of deionized water, stirring the mixture at normal temperature until the solution is uniform and transparent to obtain spinning precursor solution, injecting the spinning precursor solution into an electrostatic spinning device, preparing sodium alginate nanofibers by an electrostatic spinning method, wherein the spinning voltage is 15kV, the spinning distance is 12cm, the spinning time is 30min, placing the sodium alginate nanofibers obtained by electrospinning into an oven, drying the sodium alginate nanofibers for 3h at 40 ℃, and cutting the obtained fiber membrane into small pieces of 2 x 2cm for later use;
(2) loading silver ions: preparing a silver nitrate aqueous solution, wherein the content of silver nitrate in the silver nitrate aqueous solution is 30 wt%, soaking the sodium alginate nanofiber prepared in the step (1) in the silver nitrate aqueous solution for 20 minutes, taking out, and washing with deionized water for 3 times;
(3) reducing silver ions: immersing the sample obtained in the step (2) in a dimethylamino borane aqueous solution to reduce silver ions inside and on the surface of the fiber, wherein the content of the methylamino borane in the dimethylamino borane aqueous solution is 5 multiplied by 10-2Soaking for 15 minutes in wt%, taking out, washing with deionized water for 3 times, and drying in a 50 ℃ oven for 3 hours to obtain the silver-loaded nanofiber membrane, wherein the morphological characteristics of the obtained silver-loaded nanofiber membrane are shown in figure 1, and the average diameter of the fibers is 182 nm;
(4) assembling the force sensitive resistor: connecting two ends of the silver-loaded nanofiber membrane obtained in the step (3) with a lead through silver glue, and coating polydimethylsiloxane PDMS elastic protective films on the upper surface and the lower surface of the silver-loaded nanofiber membrane to obtain a flexible force-sensitive resistor film;
(5) assembling devices: and (4) connecting the flexible force-sensitive resistance film obtained in the step (4) with a power supply and an ammeter in series to obtain the flexible force-sensitive sensor.
And (3) testing electrical properties: the inventor tests the current-voltage curve (I-U curve, as shown in fig. 2) of the force sensor of this embodiment when the force sensor deforms under different pressures, and as can be seen from fig. 2, the resistance of the force sensor decreases with the increase of the pressure, and when the pressure does not change, the voltage and the current are in direct proportion, and the resistance does not change. The stability of the pressure sensor is shown in fig. 3, and the stability remains substantially unchanged after thousands of trial and error. The pressure sensor of the invention has high sensitivity besides good stability, for example, the flexible force sensitive resistance film of the pressure sensor is adhered to the abdominal skin, so that the breathing frequency change can be tested, and the test result is shown in fig. 4.
Example 2
A flexible force-sensitive sensor based on silver-loaded nano-fibers has a structure similar to that of the flexible force-sensitive sensor in embodiment 1, and is different from the flexible force-sensitive sensor in that the preparation method of the flexible force-sensitive sensor comprises the following steps:
(1) electrospinning sodium alginate nanofiber: weighing 0.64g of sodium alginate powder at normal temperature, adding the sodium alginate powder into a container, adding 0.16g of polyethylene oxide (PEO), 0.4g of triton, 2g of dimethyl sulfoxide and 36.8g of deionized water, stirring for 3 hours at normal temperature to obtain spinning precursor solution, injecting the spinning precursor solution into an electrostatic spinning device, preparing sodium alginate nano-fiber by an electrostatic spinning method, wherein the spinning voltage is 12kV, the spinning distance is 15cm, the spinning time is 25min, placing the sodium alginate nano-fiber obtained by electrospinning in an oven at 50 ℃ for drying for 2 hours, and cutting the obtained fiber membrane into 2 x 2cm2The small pieces are ready for use;
(2) loading silver ions: preparing a silver nitrate aqueous solution, wherein the content of silver nitrate in the silver nitrate aqueous solution is 30 wt%, soaking the sodium alginate nanofiber prepared in the step (1) in the silver nitrate aqueous solution for 20 minutes, taking out, and washing with deionized water for 3 times;
(3) reducing silver ions: immersing the sample obtained in the step (2) in a dimethylamino borane aqueous solution to reduce silver ions inside and on the surface of the fiber, wherein the content of the methylamino borane in the dimethylamino borane aqueous solution is 5 multiplied by 10-2Soaking for 15 minutes in wt%, taking out, washing with deionized water for 3 times, and drying in a 50 ℃ oven for 3 hours to obtain the silver-loaded nanofiber membrane, wherein the average diameter of the silver-loaded nanofiber is 207 nm;
(4) assembling the force sensitive resistor: connecting two ends of the silver-loaded nanofiber membrane obtained in the step (3) with a lead through silver glue, and coating PDMS elastic protective films on the upper surface and the lower surface of the silver-loaded nanofiber membrane to obtain a flexible force-sensitive resistor film;
(5) assembling devices: and (4) connecting the flexible force-sensitive resistance film obtained in the step (4) with a power supply and an ammeter in series to obtain the flexible force-sensitive sensor.
The embodiments of the present invention are provided only for understanding the present invention, and are not intended to limit the technical solutions of the present invention, and one skilled in the relevant art may make various changes or modifications based on the technical solutions described in the claims, and all equivalent changes or modifications should be covered within the scope of the claims of the present invention. The present invention is not described in detail, but is known to those skilled in the art.

Claims (9)

1. A method for preparing a flexible force-sensitive sensor based on silver-loaded nano-fibers is characterized by comprising a flexible force-sensitive resistance film, the flexible force-sensitive resistance film is connected with a power supply and an ammeter in series, the flexible force-sensitive resistance film comprises a silver-loaded nanofiber film, and elastic protective films covering the upper and lower surfaces of the silver-loaded nanofiber membrane, wherein both ends of the silver-loaded nanofiber membrane are respectively connected with a lead, the silver-loaded nanofiber membrane consists of alginic acid/silver nanoparticle composite nanofibers, the alginic acid/silver nanoparticle composite nano-fiber is prepared by preparing sodium alginate nano-fiber by an electrostatic spinning method, preparing silver alginate nano-fiber by ion exchange, and reducing silver ions, the interior and the outer surface of the alginic acid/silver nanoparticle composite nanofiber are uniformly distributed with silver nanoparticles; the preparation method of the flexible force-sensitive sensor based on the silver-loaded nano fiber comprises the following steps:
(1) electrospinning sodium alginate nanofiber: preparing spinning precursor solution containing sodium alginate, and preparing a sodium alginate nanofiber membrane by using an electrostatic spinning method;
(2) loading silver ions: soaking the sodium alginate nano-fiber prepared in the step (1) in a silver nitrate solution to perform ion exchange between sodium ions and silver ions of the fiber to form a silver alginate nano-fiber, taking out a sample, and washing the sample with deionized water;
(3) reducing silver ions: soaking the sample obtained in the step (2) in a reducing agent solution to reduce silver ions in and on the fiber, washing the sample with deionized water after a silver nanoparticle coating shell layer is formed on the surface of the sodium alginate nanofiber, and drying the sample to obtain the silver-loaded nanofiber membrane;
(4) assembling the force sensitive resistor: connecting two ends of the silver-loaded nanofiber membrane obtained in the step (3) with a lead through silver adhesive, and coating elastic protective films on the upper surface and the lower surface of the silver-loaded nanofiber membrane to obtain a flexible force-sensitive resistor film;
(5) assembling devices: and (4) connecting the flexible force-sensitive resistance film obtained in the step (4) with a power supply and an ammeter in series to obtain the flexible force-sensitive sensor.
2. The method for preparing the flexible force-sensitive sensor based on the silver-loaded nanofiber as claimed in claim 1, wherein the resistance of the flexible force-sensitive resistance film changes along with the deformation degree when the flexible force-sensitive resistance film is deformed under pressure, and the larger the pressure is, the larger the deformation degree is, the smaller the resistance of the flexible force-sensitive resistance film is, and the larger the current displayed by an ammeter is.
3. The method for preparing the flexible force-sensitive sensor based on the silver-loaded nanofiber as claimed in claim 1, wherein the sodium alginate nanofiber is a composite nanofiber of sodium alginate and a water-soluble polymer material.
4. The method for preparing the flexible force-sensitive sensor based on the silver-loaded nano-fiber according to claim 3, wherein the water-soluble material is one or more of polyethylene oxide, polyvinylpyrrolidone and polyvinyl alcohol.
5. The method for preparing the flexible force-sensitive sensor based on the silver-loaded nano fiber according to claim 1, wherein the elastic protective film is a Polydimethylsiloxane (PDMS) elastic film.
6. The method for preparing the flexible force-sensitive sensor based on the silver-loaded nanofiber as claimed in claim 1, wherein the step (1) of electrospinning sodium alginate nanofiber comprises the following steps: weighing 0.5-2 g of sodium alginate powder at normal temperature, adding the sodium alginate powder into a container, adding 0.1-0.2 g of polyethylene oxide, 0.4-0.5 g of triton, 2-3 g of dimethyl sulfoxide and 30-40 g of deionized water, stirring the mixture at normal temperature until the solution is uniform and transparent to obtain a spinning precursor solution, injecting the spinning precursor solution into an electrostatic spinning device, preparing sodium alginate nanofibers by an electrostatic spinning method, wherein the spinning voltage is 10-15 kV, the spinning distance is 12-18 cm, the spinning time is 20-30 min, and drying the sodium alginate nanofibers obtained by electrospinning in an oven at 40-60 ℃ for 1-3 h.
7. The method for preparing the flexible force-sensitive sensor based on the silver-loaded nanofiber as claimed in claim 1, wherein the step (1) of electrospinning sodium alginate nanofiber comprises the following steps: weighing 1-2 g of sodium alginate powder at normal temperature, adding the sodium alginate powder into a container, adding 0.5-1 g of polyvinyl alcohol, 0.4-0.5 g of triton, 2-3 g of dimethyl sulfoxide and 30-40 g of deionized water, stirring the mixture at normal temperature until the solution is uniform and transparent to obtain a spinning precursor solution, injecting the spinning precursor solution into an electrostatic spinning device, preparing sodium alginate nanofibers by using an electrostatic spinning method, wherein the spinning voltage is 12-18 kV, the spinning distance is 10-15 cm, the spinning time is 20-30 min, and drying the sodium alginate nanofibers obtained by electrospinning in an oven at 40-60 ℃ for 1-3 h.
8. The method for preparing the flexible force-sensitive sensor based on the silver-loaded nano-fiber according to claim 1, wherein the step (2) is carried out by loading silver ions: preparing a silver nitrate aqueous solution, wherein the content of silver nitrate in the silver nitrate aqueous solution is 20-30 wt%, soaking the sodium alginate nanofiber prepared in the step (1) in the silver nitrate aqueous solution for 20-30 minutes, taking out, and washing with deionized water for 2-3 times.
9. The method for preparing a flexible force-sensitive sensor based on silver-loaded nanofibers according to claim 1, wherein the step (3) of reducing silver ions: immersing the sample obtained in the step (2) in a dimethylamino borane aqueous solution to reduce silver ions inside and on the surface of the fiber, wherein the content of the methylamino borane in the dimethylamino borane aqueous solution is 5 multiplied by 10-2And (3) soaking for 10-20 minutes in wt%, taking out, washing with deionized water for 3-4 times, and drying in an oven at 50 ℃ for 2-5 hours to obtain the silver-loaded nanofiber membrane.
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