CN111419217A - Preparation method and application of electrode based on flexible conductive fabric - Google Patents

Preparation method and application of electrode based on flexible conductive fabric Download PDF

Info

Publication number
CN111419217A
CN111419217A CN202010246781.8A CN202010246781A CN111419217A CN 111419217 A CN111419217 A CN 111419217A CN 202010246781 A CN202010246781 A CN 202010246781A CN 111419217 A CN111419217 A CN 111419217A
Authority
CN
China
Prior art keywords
flexible conductive
fabric
conductive fabric
electrode
placing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202010246781.8A
Other languages
Chinese (zh)
Other versions
CN111419217B (en
Inventor
肖渊
贠伟博
马丽萍
潘晓
代阳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xian Polytechnic University
Original Assignee
Xian Polytechnic University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xian Polytechnic University filed Critical Xian Polytechnic University
Priority to CN202010246781.8A priority Critical patent/CN111419217B/en
Publication of CN111419217A publication Critical patent/CN111419217A/en
Application granted granted Critical
Publication of CN111419217B publication Critical patent/CN111419217B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61BDIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B5/00Measuring for diagnostic purposes; Identification of persons
    • A61B5/24Detecting, measuring or recording bioelectric or biomagnetic signals of the body or parts thereof
    • A61B5/25Bioelectric electrodes therefor
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/08Materials for coatings
    • A61L31/082Inorganic materials
    • A61L31/088Other specific inorganic materials not covered by A61L31/084 or A61L31/086
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/14Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • 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
    • 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
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2420/00Materials or methods for coatings medical devices
    • A61L2420/02Methods for coating medical devices

Landscapes

  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Surgery (AREA)
  • Animal Behavior & Ethology (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Veterinary Medicine (AREA)
  • Heart & Thoracic Surgery (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Vascular Medicine (AREA)
  • Epidemiology (AREA)
  • Textile Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Biophysics (AREA)
  • Molecular Biology (AREA)
  • Medical Informatics (AREA)
  • Biomedical Technology (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing Of Electric Cables (AREA)

Abstract

The invention discloses a preparation method of an electrode based on a flexible conductive fabric, which comprises the following steps of firstly, preprocessing, and then preparing a precursor solution and a metal salt solution; taking a proper amount of precursor solution to completely wet the fabric; then placing the metal salt solution in a nozzle of a micro-droplet jetting device, and controlling a three-dimensional motion control platform and the nozzle to drop by drop print the metal salt solution on the upper surface of the fabric; repeatedly cleaning the printed fabric by respectively adopting deionized water and absolute ethyl alcohol, drying the fabric in an oven after removing impurities, and cooling to obtain the flexible conductive fabric; and finally, preparing a mixed solution, dripping the mixed solution on the bottom surface and the upper surface of the flexible conductive fabric, and curing to obtain the flexible conductive fabric with the PDMS packaging layers on the upper part and the lower part, so as to obtain the flexible conductive fabric-based electrode. The invention relates to a preparation method of an electrode based on a flexible conductive fabric, which solves the problems of poor use comfort, weak signals and poor conductivity of the conventional electrocardiosignal acquisition electrode.

Description

Preparation method and application of electrode based on flexible conductive fabric
Technical Field
The invention belongs to the technical field of electrode preparation, and particularly relates to a preparation method of a flexible conductive fabric-based electrode.
Background
At present, the most commonly used electrocardiosignal acquisition electrode is a silver chloride (Ag/AgCl) electrode, but the electrode can cause skin allergy after long-time use, and the conductive gel is easy to weaken signals after being dried; existing dry contact electrodes can also cause skin discomfort due to their rigid structure. Therefore, an acquisition electrode which can effectively reduce the stimulation to the skin of a human body and can realize long-term monitoring of electrocardiosignals is urgently needed to be designed.
Disclosure of Invention
The invention aims to provide a preparation method of an electrode based on a flexible conductive fabric, which solves the problems of poor use comfort, weak signal and poor conductivity of the conventional electrocardiosignal acquisition electrode.
The invention also aims to provide application of the electrode based on the flexible conductive fabric, and the problems of poor use comfort and weak signals of the conventional electrocardiosignal acquisition electrode are solved.
The invention adopts a technical scheme that a preparation method based on a flexible conductive fabric electrode is implemented according to the following steps:
step 1, pretreatment
Selecting a proper metal substrate, polishing the metal substrate by using 2000-mesh abrasive paper, removing surface oxides, and tightly attaching the metal substrate to a three-dimensional motion control platform; selecting a proper fabric, removing burrs, and attaching the fabric to a metal substrate for later use;
step 2, preparing precursor solution
Dissolving the raw material A in deionized water, adding a dispersing agent, dispersing uniformly by an ultrasonic oscillator, and filtering to obtain a precursor solution for later use;
step 3, preparing a metal salt solution
Dissolving the raw material B in deionized water, dispersing uniformly by an ultrasonic oscillator, and filtering to obtain a metal salt solution for later use;
step 4, taking a proper amount of precursor solution to completely wet the fabric for later use;
step 5, placing the metal salt solution into a nozzle of a micro-droplet jetting device, controlling a three-dimensional motion control platform and the nozzle to drop by drop the metal salt solution on the upper surface of the fabric in the step 4, printing 1-6 layers of the metal salt solution on the upper surface of the fabric, and standing;
step 6, repeatedly cleaning the printed fabric by respectively adopting deionized water and absolute ethyl alcohol, drying the fabric in an oven after removing impurities, and cooling to obtain the flexible conductive fabric;
step 7, uniformly mixing polydimethylsiloxane and a curing agent in a mass ratio of 10-12: 1 to obtain a mixed solution for later use;
step 8, dripping the mixed liquid on the bottom surface of the flexible conductive fabric, automatically leveling, placing the mixed liquid in a grinding tool, placing the mould in an oven for curing treatment, cooling to normal temperature, taking out the grinding tool, and obtaining the flexible conductive fabric with the PDMS packaging layer at the bottom for later use;
and 9, placing a metal buckle on the upper surface of the flexible conductive fabric, dripping the mixed liquid on the upper surface of the flexible conductive fabric, automatically leveling, placing the flexible conductive fabric into a grinding tool, placing the mould into an oven for solidification treatment, cooling to normal temperature, taking out the grinding tool to obtain the flexible conductive fabric with the PDMS packaging layers on the upper part and the lower part, and obtaining the electrode based on the flexible conductive fabric.
The invention is also characterized in that:
the fabric is any one of plain weave fabric, satin weave fabric and twill weave fabric; the metal base is made of any one of aluminum, zinc, iron, tin and copper.
In the step 2, the raw material A is any one of ascorbic acid, hydrazine hydrate and ethylene glycol, and the mass volume concentration of the precursor solution is 20-30% w/v.
In the step 2, the mass ratio of the raw material A to the dispersing agent is 6-8: 1, the dispersing agent is polyvinylpyrrolidone, and the mass volume concentration of the polyvinylpyrrolidone is 4-8% w/v.
In the step 3, the raw material B is any one of silver nitrate powder, silver ammonia powder and silver laurate powder, and the mass volume concentration of the metal salt solution is 50-80% w/v.
The droplet jetting device is a piezoelectric droplet on-demand jetting device, the diameter of a nozzle is 50-80 microns, and the jetting frequency is 1-10 Hz.
In step 6, the temperature of the drying treatment is 60-100 ℃, and the time is 5 min.
In the steps 8 and 9, the temperature of the curing treatment is 60-100 ℃, and the time is 30-60 min.
The metal button extends out of the PDMS packaging layer on the upper part of the flexible conductive fabric.
The invention adopts another technical scheme that the flexible conductive fabric-based electrode is applied to a flexible wearable electronic device to acquire electrocardiosignals of a human body.
The invention has the beneficial effects that:
the invention relates to a preparation method based on a flexible conductive fabric electrode, which takes an aqueous metal salt solution as a spraying material, takes a fabric soaked by a precursor solution as a reaction substrate, takes the metal material as a substrate, generates a silver simple substance through the redox reaction of the precursor solution and a silver nitrate solution, and simultaneously utilizes the natural porosity of the fabric to ensure that part of the generated silver contacts the lower-layer metal material substrate to form the reaction of a chemical primary battery, thereby improving the overall reaction rate, increasing the compactness of a silver layer and leading the generated silver to be capable of forming effective coating on yarns among the fabrics;
according to the preparation method of the flexible conductive fabric electrode, the prepared fabric electrode has physical properties such as flexibility, elasticity and air permeability of common textiles, and still has stable electrochemical performance and washing resistance under different deformation conditions;
according to the preparation method based on the flexible conductive fabric electrode, the prepared electrode based on the flexible conductive fabric has good electrical properties, lays a foundation for collecting physiological signals of electrocardio and the like of a human body, and is simple in preparation process and low in raw material price; the problem of traditional electrode need clean before using, polish local skin and conducting resin dry up influence electrocardiosignal is solved.
Drawings
FIG. 1 is a schematic diagram of a method of making a flexible conductive fabric-based electrode according to the present invention;
FIG. 2 is a schematic diagram of a flexible conductive fabric-based electrode according to the present invention;
FIG. 3 is a scanning electron microscope image of a flexible conductive fabric-based electrode prepared by the preparation method of the flexible conductive fabric-based electrode of the invention;
fig. 4 is a sheet resistance diagram of the electrode based on the flexible conductive fabric prepared by the preparation method of the electrode based on the flexible conductive fabric.
In the figure, 1, a metal button, 2, a PDMS packaging layer, 3, a flexible conductive fabric, 4, a nozzle, 5, a precursor solution, 6, a fabric, 7, a metal substrate and 8, a three-dimensional motion control platform.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of an electrode based on a flexible conductive fabric, which is implemented according to the following steps as shown in figure 1:
step 1, pretreatment
Selecting a proper metal substrate 7, polishing the metal substrate by using 2000-mesh abrasive paper, removing surface oxides, and tightly attaching the metal substrate to a three-dimensional motion control platform 8; selecting a proper fabric 6, removing burrs, and attaching the fabric to a metal substrate 7 for later use;
wherein, the fabric 6 is any one of plain weave fabric, satin weave fabric and twill weave fabric; the metal base 7 is made of any one of aluminum, zinc, iron, tin and copper;
step 2, preparing precursor solution 5
Dissolving the raw material A in deionized water, adding a dispersing agent, dispersing uniformly by an ultrasonic oscillator, and filtering to obtain a precursor solution 5 for later use;
wherein the raw material A is any one of ascorbic acid, hydrazine hydrate and ethylene glycol, and the mass volume concentration of the precursor solution 5 is 20-30% w/v; the mass ratio of the raw material A to the dispersing agent is 6-8: 1, the dispersing agent is polyvinylpyrrolidone, and the mass volume concentration of the polyvinylpyrrolidone is 4-8% w/v;
step 3, preparing a metal salt solution
Dissolving the raw material B in deionized water, dispersing uniformly by an ultrasonic oscillator, and filtering to obtain a metal salt solution for later use;
wherein the raw material B is any one of silver nitrate powder, silver ammonia powder and silver laurate powder, and the mass volume concentration of the metal salt solution is 50-80% w/v;
step 4, taking a proper amount of precursor solution 5 to completely wet the fabric 6 for later use;
step 5, placing the metal salt solution into a nozzle 4 of a micro-droplet jetting device, controlling a three-dimensional motion control platform 8 and the nozzle 4 to drop by drop print the metal salt solution on the upper surface of the fabric 6 in the step 4, printing 1-6 layers of the metal salt solution on the upper surface of the fabric 6, and standing;
wherein the droplet jetting device is a piezoelectric droplet on-demand jetting device, the diameter of the nozzle 4 is 50-80 μm, and the jetting frequency is 1-10 Hz; the droplet injection device and the three-dimensional motion control platform 8 are both connected with the controller;
step 6, repeatedly cleaning the printed fabric 6 by respectively adopting deionized water and absolute ethyl alcohol, drying the fabric in an oven after removing impurities, and cooling to obtain the flexible conductive fabric 3;
wherein the drying treatment temperature is 60-100 ℃, and the drying treatment time is 5 min;
step 7, uniformly mixing polydimethylsiloxane and a curing agent in a mass ratio of 10-12: 1 to obtain a mixed solution for later use;
step 8, dripping the mixed liquid on the bottom surface of the flexible conductive fabric 3, automatically leveling, placing the mixed liquid in a grinding tool, placing the mould in an oven for curing treatment, cooling to normal temperature, taking out the grinding tool to obtain the flexible conductive fabric 3 with the PDMS packaging layer 2 at the bottom for later use;
step 9, placing the metal buckle 1 on the upper surface of the flexible conductive fabric 3, dripping the mixed liquid on the upper surface of the flexible conductive fabric 3, automatically leveling, placing the mixed liquid in a grinding tool, placing the mould in an oven for curing treatment, cooling to normal temperature, taking out the grinding tool to obtain the flexible conductive fabric 3 with the PDMS packaging layers 2 on the upper part and the lower part, and obtaining the flexible conductive fabric-based electrode as shown in figure 2;
wherein, in the steps 8 and 9, the temperature of the curing treatment is 60-100 ℃, and the time is 30-60 min; the metal button 1 extends out of the PDMS encapsulation layer 2 on the upper part of the flexible conductive fabric 3.
The invention also relates to an application of the flexible conductive fabric-based electrode, and the flexible conductive fabric-based electrode is used for a flexible wearable electronic device to acquire electrocardiosignals of a human body.
Example 1
(1) Pretreatment
Selecting a metal substrate 7 made of aluminum material, cutting the metal substrate 7 into a specification of 50mm × mm, polishing the metal substrate by using 2000-mesh sand paper, removing surface oxides, and tightly attaching the metal substrate to a three-dimensional motion control platform 8;
(2) preparation of precursor solution 5
Dissolving ascorbic acid in deionized water, adding polyvinylpyrrolidone, dispersing uniformly by an ultrasonic oscillator, filtering to obtain a precursor solution with the mass volume concentration of 20% w/v, wherein the mass ratio of the ascorbic acid to the polyvinylpyrrolidone is 8:1, the mass volume concentration of the polyvinylpyrrolidone is 4% w/v, and taking a proper amount of the precursor solution 5 to completely wet the plain woven fabric;
(3) preparation of Metal salt solutions
Dissolving silver nitrate powder in deionized water, dispersing uniformly by an ultrasonic oscillator, and filtering to obtain a metal salt solution with the mass volume concentration of 50% w/v;
(4) printing and curing
Placing a metal salt solution in a nozzle 4 of a micro-droplet spraying device, controlling a three-dimensional motion control platform 8 and the nozzle 4 to drop by drop the metal salt solution on the upper surface of the wetted plain weave fabric, printing 1 layer of the metal salt solution on the upper surface of the plain weave fabric, and standing; wherein the diameter of the nozzle 4 is 50 μm, and the spraying frequency is 10 Hz; then respectively adopting deionized water and absolute ethyl alcohol to repeatedly clean the printed plain weave fabric, removing impurities, then placing the plain weave fabric in an oven to dry for 5min at the temperature of 60 ℃, and cooling to obtain a flexible conductive fabric 3;
(5) preparing a mixed solution
Uniformly mixing polydimethylsiloxane and a curing agent in a mass ratio of 10:1 to obtain a mixed solution;
(6) dripping the mixed liquid on the bottom surface of the flexible conductive fabric 3, automatically leveling, placing in a grinding tool, placing the mould in an oven, curing for 60min at 60 ℃, cooling to normal temperature, and taking out the grinding tool to obtain the flexible conductive fabric 3 with the PDMS packaging layer 2 at the bottom;
and then placing the metal buckle 1 on the upper surface of the flexible conductive fabric 3, dripping the mixed liquid on the upper surface of the flexible conductive fabric 3, automatically leveling, placing in a grinding tool, placing the mould in an oven, curing for 60min at 60 ℃, cooling to normal temperature, taking out the grinding tool, and obtaining the flexible conductive fabric 3 with the PDMS packaging layers 2 on the upper part and the lower part, thus obtaining the electrode based on the flexible conductive fabric.
Example 2
(1) Pretreatment
Selecting a zinc material metal substrate 7, cutting the zinc material metal substrate into a specification of 50mm × mm, polishing the zinc material metal substrate by using 2000-mesh sand paper, removing surface oxides, and tightly attaching the zinc material metal substrate to a three-dimensional motion control platform 8;
(2) preparation of precursor solution 5
Dissolving ascorbic acid in deionized water, adding polyvinylpyrrolidone, dispersing uniformly by using an ultrasonic oscillator, filtering to obtain a precursor solution with the mass volume concentration of 25% w/v, wherein the mass ratio of the ascorbic acid to the polyvinylpyrrolidone is 7:1, the mass volume concentration of the polyvinylpyrrolidone is 6% w/v, and taking a proper amount of the precursor solution 5 to completely wet the twill fabric;
(3) preparation of Metal salt solutions
Dissolving silver nitrate powder in deionized water, dispersing uniformly by an ultrasonic oscillator, and filtering to obtain a metal salt solution with the mass volume concentration of 65% w/v;
(4) printing and curing
Placing a metal salt solution in a nozzle 4 of a micro-droplet jetting device, controlling a three-dimensional motion control platform 8 and the nozzle 4 to drop by drop the metal salt solution on the upper surface of the wetted twill fabric, printing 3 layers of the metal salt solution on the upper surface of the twill fabric, and standing; wherein, the diameter of the nozzle 4 is 60 μm, and the spraying frequency is 8 Hz; then respectively adopting deionized water and absolute ethyl alcohol to repeatedly clean the printed twill fabric, removing impurities, then placing the twill fabric in an oven to dry for 5min at 70 ℃, and cooling to obtain a flexible conductive fabric 3;
(5) preparing a mixed solution
Uniformly mixing polydimethylsiloxane and a curing agent in a mass ratio of 10:1 to obtain a mixed solution;
(6) dripping the mixed liquid on the bottom surface of the flexible conductive fabric 3, automatically leveling, placing in a grinding tool, placing the mould in an oven, curing for 45min at 80 ℃, cooling to normal temperature, and taking out the grinding tool to obtain the flexible conductive fabric 3 with the PDMS packaging layer 2 at the bottom;
and then placing the metal buckle 1 on the upper surface of the flexible conductive fabric 3, dripping the mixed liquid on the upper surface of the flexible conductive fabric 3, automatically leveling, placing in a grinding tool, placing the mould in an oven, curing for 45min at 80 ℃, cooling to normal temperature, taking out the grinding tool, and obtaining the flexible conductive fabric 3 with the PDMS packaging layers 2 on the upper part and the lower part, thus obtaining the electrode based on the flexible conductive fabric.
Example 3
(1) Pretreatment
Selecting a copper metal substrate 7, cutting the copper metal substrate into a specification of 50mm × mm, polishing the copper metal substrate by using 2000-mesh sand paper, removing surface oxides, and tightly attaching the copper metal substrate to a three-dimensional motion control platform 8;
(2) preparation of precursor solution 5
Dissolving ascorbic acid in deionized water, adding polyvinylpyrrolidone, dispersing uniformly by an ultrasonic oscillator, filtering to obtain a precursor solution with the mass volume concentration of 30% w/v, wherein the mass ratio of the ascorbic acid to the polyvinylpyrrolidone is 8:1, the mass volume concentration of the polyvinylpyrrolidone is 8% w/v, and taking a proper amount of the precursor solution 5 to completely wet the plain woven fabric;
(3) preparation of Metal salt solutions
Dissolving silver nitrate powder in deionized water, dispersing uniformly by an ultrasonic oscillator, and filtering to obtain a metal salt solution with the mass volume concentration of 80% w/v;
(4) printing and curing
Placing a metal salt solution in a nozzle 4 of a micro-droplet jetting device, controlling a three-dimensional motion control platform 8 and the nozzle 4 to drop by drop the metal salt solution on the upper surface of the wetted plain weave fabric, printing 4 layers of the metal salt solution on the upper surface of the plain weave fabric, and standing; wherein the diameter of the nozzle 4 is 70 μm, and the spraying frequency is 5 Hz; then respectively adopting deionized water and absolute ethyl alcohol to repeatedly clean the printed plain weave fabric, removing impurities, then placing the plain weave fabric in an oven to dry for 5min at 80 ℃, and cooling to obtain a flexible conductive fabric 3;
(5) preparing a mixed solution
Uniformly mixing polydimethylsiloxane and a curing agent in a mass ratio of 10:1 to obtain a mixed solution;
(6) dripping the mixed liquid on the bottom surface of the flexible conductive fabric 3, automatically leveling, placing in a grinding tool, placing the mould in an oven, curing for 30min at 100 ℃, cooling to normal temperature, and taking out the grinding tool to obtain the flexible conductive fabric 3 with the PDMS packaging layer 2 at the bottom;
and then placing the metal buckle 1 on the upper surface of the flexible conductive fabric 3, dripping the mixed liquid on the upper surface of the flexible conductive fabric 3, automatically leveling, placing in a grinding tool, placing the mould in an oven, curing for 30min at 100 ℃, cooling to normal temperature, taking out the grinding tool, and obtaining the flexible conductive fabric 3 with the PDMS packaging layers 2 on the upper part and the lower part, thus obtaining the electrode based on the flexible conductive fabric.
Example 4
(1) Pretreatment
Selecting a metal substrate 7 made of an iron material, cutting the metal substrate into a specification of 50mm × mm, polishing the metal substrate by using 2000-mesh sand paper, removing surface oxides, and tightly attaching the metal substrate to a three-dimensional motion control platform 8;
(2) preparation of precursor solution 5
Dissolving hydrazine hydrate in deionized water, adding polyvinylpyrrolidone, dispersing uniformly by using an ultrasonic oscillator, filtering to obtain a precursor solution with the mass volume concentration of 22% w/v, wherein the mass ratio of the hydrazine hydrate to the polyvinylpyrrolidone is 6:1, the mass volume concentration of the polyvinylpyrrolidone is 5% w/v, and taking a proper amount of the precursor solution 5 to completely wet the satin fabric;
(3) preparation of Metal salt solutions
Dissolving silver ammonia powder in deionized water, dispersing uniformly by an ultrasonic oscillator, and filtering to obtain a metal salt solution with mass volume concentration of 66% w/v;
(4) printing and curing
Placing a metal salt solution in a nozzle 4 of a micro-droplet jetting device, controlling a three-dimensional motion control platform 8 and the nozzle 4 to drop by drop the metal salt solution on the upper surface of the wetted satin fabric, printing 5 layers of the metal salt solution on the upper surface of the satin fabric, and standing; wherein the diameter of the nozzle 4 is 70 μm, and the spraying frequency is 4 Hz; then repeatedly cleaning the printed satin fabric by respectively adopting deionized water and absolute ethyl alcohol, drying the satin fabric for 5min at 100 ℃ in an oven after removing impurities, and cooling to obtain a flexible conductive fabric 3;
(5) preparing a mixed solution
Uniformly mixing polydimethylsiloxane and a curing agent in a mass ratio of 12:1 to obtain a mixed solution;
(6) dripping the mixed liquid on the bottom surface of the flexible conductive fabric 3, automatically leveling, placing in a grinding tool, placing the mould in an oven, curing at 80 ℃ for 40min, cooling to normal temperature, and taking out the grinding tool to obtain the flexible conductive fabric 3 with the PDMS packaging layer 2 at the bottom;
and then placing the metal buckle 1 on the upper surface of the flexible conductive fabric 3, dripping the mixed liquid on the upper surface of the flexible conductive fabric 3, automatically leveling, placing in a grinding tool, placing the mould in an oven, curing at 80 ℃ for 40min, cooling to normal temperature, taking out the grinding tool, and obtaining the flexible conductive fabric 3 with the PDMS packaging layers 2 on the upper part and the lower part, thus obtaining the electrode based on the flexible conductive fabric.
Example 5
(1) Pretreatment
Selecting a metal substrate 7 made of a tin material, cutting the metal substrate into a specification of 50mm × mm, polishing the metal substrate by using 2000-mesh sand paper, removing surface oxides, and tightly attaching the plain woven fabric to a three-dimensional motion control platform 8;
(2) preparation of precursor solution 5
Dissolving ethylene glycol in deionized water, adding polyvinylpyrrolidone, dispersing uniformly by an ultrasonic oscillator, filtering to obtain a precursor solution with the mass volume concentration of 24% w/v, wherein the mass ratio of the ethylene glycol to the polyvinylpyrrolidone is 7:1, the mass volume concentration of the polyvinylpyrrolidone is 6% w/v, and taking a proper amount of the precursor solution 5 to completely wet the plain woven fabric;
(3) preparation of Metal salt solutions
Dissolving silver nitrate powder in deionized water, dispersing uniformly by an ultrasonic oscillator, and filtering to obtain a metal salt solution with mass volume concentration of 76% w/v;
(4) printing and curing
Placing a metal salt solution in a nozzle 4 of a micro-droplet spraying device, controlling a three-dimensional motion control platform 8 and the nozzle 4 to drop by drop the metal salt solution on the upper surface of the wetted plain weave fabric, printing 6 layers of the metal salt solution on the upper surface of the plain weave fabric, and standing; wherein, the diameter of the nozzle 4 is 72 μm, and the spraying frequency is 1 Hz; then respectively adopting deionized water and absolute ethyl alcohol to repeatedly clean the printed plain weave fabric, removing impurities, then placing the plain weave fabric in an oven to dry for 5min at 80 ℃, and cooling to obtain a flexible conductive fabric 3;
(5) preparing a mixed solution
Uniformly mixing polydimethylsiloxane and a curing agent in a mass ratio of 11:1 to obtain a mixed solution;
(6) dripping the mixed liquid on the bottom surface of the flexible conductive fabric 3, automatically leveling, placing in a grinding tool, placing the mould in an oven, curing at 90 ℃ for 35min, cooling to normal temperature, and taking out the grinding tool to obtain the flexible conductive fabric 3 with the PDMS packaging layer 2 at the bottom;
and then placing the metal buckle 1 on the upper surface of the flexible conductive fabric 3, dripping the mixed liquid on the upper surface of the flexible conductive fabric 3, automatically leveling, placing in a grinding tool, placing the mould in an oven, curing at 90 ℃ for 35min, cooling to normal temperature, taking out the grinding tool, and obtaining the flexible conductive fabric 3 with the PDMS packaging layers 2 on the upper part and the lower part, thus obtaining the electrode based on the flexible conductive fabric.
In summary, example 3 is the best embodiment of the present invention, by spraying and printing silver nitrate solution on the fabric surface completely wetted by ascorbic acid solution, and placing the metal substrate 7 made of copper material on the lower layer of the fabric. Silver nitrate reacts with ascorbic acid solution to generate a silver simple substance, the silver simple substance and copper material on the lower layer of the fabric form a copper-silver primary battery, silver ions in the silver nitrate are directionally deposited on a cathode (one pole of the silver simple substance) of the primary battery, and the generation efficiency of the silver simple substance in a reaction system is improved. The problems of weak signal transmission and poor conductivity are improved.
Fig. 3 is a scanning electron microscope image (magnification of 2000 times) of the electrode based on the flexible conductive fabric prepared by the preparation method of the electrode based on the flexible conductive fabric of the present invention, and the preparation method is as shown in example 3, as can be seen from fig. 3, in the image, silver-white particles are silver particles generated on the surface of the fabric after chemical deposition reaction, and it can be seen that, as the number of printing layers increases, the more silver particles are generated, the more complete the growth is, the more uniform and dense the distribution of the silver particles is, and the higher the silver glossiness of the printed electrode based on the flexible conductive fabric is.
Moreover, the distribution of silver particles and the glossiness of silver when printing 2 layers are obviously improved compared with those when printing 1 layer, because the amount of silver nitrate used is far insufficient when printing 1 layer, the reaction with ascorbic acid is not complete; and when the number of printing layers is increased to 5-6, the silver particles on the fabric gradually tend to be in a saturated state. In addition, as can be seen from the figure, as the number of printing layers increases, the number of yarns exposed outside without being covered by the silver layer in the fabric structure gradually decreases until the number of printing layers reaches 4, and the yarns are completely covered; the reason is that with the increase of the number of printing layers, the crystal mode of the silver deposited on the flexible conductive fabric 3 is changed from dendritic silver to blocky silver to flaky silver under the influence of the generation amount and the fabric structure, so that the continuity and the electrical property of the formed conductive circuit are ensured.
Fig. 4 is a sheet resistance diagram of a flexible conductive fabric electrode prepared by the method of the present invention, the method is shown in example 3, and the data is shown in table 1:
table 1 sheet resistance based on flexible conductive fabric electrode based on different number of printing layers of copper silver nitrate solution
Number of silver nitrate printing layers Mean square resistance value omega/□ Standard deviation omega/□ of sheet resistance
1 0.852175 0.574616617
2 0.1338 0.121050444
3 0.09685 0.02441009
4 0.02995 0.008995693
5 0.015125 0.004401349
6 0.0116 0.006984984
As can be seen from fig. 4 and table 1, as the number of printed layers increases, the mean value and the standard deviation of the sheet resistance based on the surface of the flexible conductive fabric electrode are both gradually reduced, and when the number of printed layers reaches 4, the mean value and the standard deviation of the sheet resistance based on the surface of the flexible conductive fabric electrode basically tend to be stable. The electrode based on the flexible conductive fabric prepared by the invention has good conductivity, provides a base stone for effective and stable transmission of signals, and combines the PDMS packaging layer to package the electrode, so that the use comfort of the electrode is effectively improved, and a foundation is laid for preparing the flexible fabric sensor.

Claims (10)

1. A preparation method based on a flexible conductive fabric electrode is characterized by comprising the following steps:
step 1, pretreatment
Selecting a proper metal substrate (7), polishing the substrate by using 2000-mesh abrasive paper, removing surface oxides, and tightly attaching the surface oxides to a three-dimensional motion control platform (8); selecting a proper fabric (6), removing burrs, and attaching the fabric to a metal substrate (7) for later use;
step 2, preparing precursor solution (5)
Dissolving the raw material A in deionized water, adding a dispersing agent, dispersing uniformly by an ultrasonic oscillator, and filtering to obtain a precursor solution (5) for later use;
step 3, preparing a metal salt solution
Dissolving the raw material B in deionized water, dispersing uniformly by an ultrasonic oscillator, and filtering to obtain a metal salt solution for later use;
step 4, taking a proper amount of the precursor solution (5) to completely wet the fabric (6) for later use;
step 5, placing the metal salt solution in a nozzle (4) of a microdroplet spraying device, controlling a three-dimensional motion control platform (8) and the nozzle (4) to print the metal salt solution on the upper surface of the fabric (6) in the step 4 drop by drop, printing 1-6 layers of the metal salt solution on the upper surface of the fabric (6), and standing;
step 6, repeatedly cleaning the printed fabric (6) by respectively adopting deionized water and absolute ethyl alcohol, drying the fabric in an oven after removing impurities, and cooling to obtain the flexible conductive fabric (3);
step 7, uniformly mixing polydimethylsiloxane and a curing agent in a mass ratio of 10-12: 1 to obtain a mixed solution for later use;
8, dripping the mixed liquid on the bottom surface of the flexible conductive fabric (3), automatically leveling, placing in a grinding tool, placing the mould in an oven for curing, cooling to normal temperature, and taking out the grinding tool to obtain the flexible conductive fabric (3) with the PDMS packaging layer (2) at the bottom for later use;
and 9, placing the metal buckle (1) on the upper surface of the flexible conductive fabric (3), dripping the mixed liquid on the upper surface of the flexible conductive fabric (3), automatically leveling, placing the mixed liquid in a grinding tool, placing the mould in an oven for curing, cooling to normal temperature, taking out the grinding tool to obtain the flexible conductive fabric (3) with the PDMS packaging layers (2) on the upper part and the lower part, and obtaining the electrode based on the flexible conductive fabric.
2. The preparation method of the electrode based on the flexible conductive fabric according to claim 1, wherein the fabric (6) is any one of plain fabric, satin fabric and twill fabric; the metal substrate (7) is made of any one of aluminum, zinc, iron, tin and copper.
3. The method for preparing the electrode based on the flexible conductive fabric according to claim 1, wherein in the step 2, the raw material A is any one of ascorbic acid, hydrazine hydrate and ethylene glycol, and the mass volume concentration of the precursor solution (5) is 20% w/v to 30% w/v.
4. The preparation method of the electrode based on the flexible conductive fabric as claimed in claim 3, wherein in the step 2, the mass ratio of the raw material A to the dispersing agent is 6-8: 1, and the dispersing agent is polyvinylpyrrolidone, and the mass volume concentration of the polyvinylpyrrolidone is 4-8% w/v.
5. The method for preparing the electrode based on the flexible conductive fabric as claimed in claim 1, wherein in the step 3, the raw material B is any one of silver nitrate powder, silver ammonia powder and silver laurate powder, and the mass volume concentration of the metal salt solution is 50% w/v to 80% w/v.
6. The method for preparing the electrode based on the flexible conductive fabric according to claim 1, wherein the droplet spraying device is a piezoelectric droplet on demand spraying device, the diameter of the nozzle (4) is 50 μm to 80 μm, and the spraying frequency is 1Hz to 10 Hz.
7. The method for preparing the electrode based on the flexible conductive fabric according to claim 1, wherein in the step 6, the drying treatment temperature is 60-100 ℃ and the drying treatment time is 5 min.
8. The preparation method of the electrode based on the flexible conductive fabric according to claim 1, wherein in the steps 8 and 9, the curing treatment temperature is 60-100 ℃ and the curing treatment time is 30-60 min.
9. The method for preparing the electrode based on the flexible conductive fabric according to claim 1, wherein the metal button (1) extends out of the PDMS encapsulation layer (2) on the upper part of the flexible conductive fabric (3).
10. The application of the flexible conductive fabric-based electrode is characterized in that the flexible conductive fabric-based electrode according to any one of claims 1 to 9 is used for a flexible wearable electronic device to acquire electrocardiosignals of a human body.
CN202010246781.8A 2020-03-31 2020-03-31 Preparation method and application of electrode based on flexible conductive fabric Active CN111419217B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010246781.8A CN111419217B (en) 2020-03-31 2020-03-31 Preparation method and application of electrode based on flexible conductive fabric

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010246781.8A CN111419217B (en) 2020-03-31 2020-03-31 Preparation method and application of electrode based on flexible conductive fabric

Publications (2)

Publication Number Publication Date
CN111419217A true CN111419217A (en) 2020-07-17
CN111419217B CN111419217B (en) 2023-06-20

Family

ID=71550254

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010246781.8A Active CN111419217B (en) 2020-03-31 2020-03-31 Preparation method and application of electrode based on flexible conductive fabric

Country Status (1)

Country Link
CN (1) CN111419217B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111885841A (en) * 2020-07-31 2020-11-03 西安工程大学 Preparation method of flexible stretchable conductive circuit
CN114224595A (en) * 2021-11-12 2022-03-25 福建江夏学院 Cloth structure with electric heating warm keeping and electric stimulation coating and preparation method thereof
CN114379069A (en) * 2020-10-20 2022-04-22 西安工程大学 Controllable wrinkle shape preparation method
CN114883513A (en) * 2022-03-30 2022-08-09 南京邮电大学 Fabric electrode and rapid preparation method and application thereof

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002020941A (en) * 2000-07-10 2002-01-23 Asahi Kasei Corp Base fabric for plating metal and metal-plated wove fabric
US20030124256A1 (en) * 2000-04-10 2003-07-03 Omnishield, Inc. Omnishield process and product
WO2016139529A1 (en) * 2015-03-04 2016-09-09 D.B. Textile S.R.L. Metallized textile substrates, process for preparing the same and related apparatus
CN106049035A (en) * 2016-09-06 2016-10-26 复旦大学 Establishment method of conductive circuit on surface of flexible fabric
CN109183401A (en) * 2018-09-30 2019-01-11 西安工程大学 The preparation method and device of fabric sensor based on droplet need based jet technology
CN109859961A (en) * 2018-10-29 2019-06-07 哈尔滨工业大学(深圳) A kind of preparation method of the flexible super capacitor electrode based on chemical & blended fabric
CN110063724A (en) * 2019-04-26 2019-07-30 清华大学 Flexible biological electrode and preparation method thereof
CN110248477A (en) * 2019-06-12 2019-09-17 西安工程大学 A kind of manufacturing method of embedded compliant conductive route

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030124256A1 (en) * 2000-04-10 2003-07-03 Omnishield, Inc. Omnishield process and product
JP2002020941A (en) * 2000-07-10 2002-01-23 Asahi Kasei Corp Base fabric for plating metal and metal-plated wove fabric
WO2016139529A1 (en) * 2015-03-04 2016-09-09 D.B. Textile S.R.L. Metallized textile substrates, process for preparing the same and related apparatus
CN106049035A (en) * 2016-09-06 2016-10-26 复旦大学 Establishment method of conductive circuit on surface of flexible fabric
CN109183401A (en) * 2018-09-30 2019-01-11 西安工程大学 The preparation method and device of fabric sensor based on droplet need based jet technology
CN109859961A (en) * 2018-10-29 2019-06-07 哈尔滨工业大学(深圳) A kind of preparation method of the flexible super capacitor electrode based on chemical & blended fabric
CN110063724A (en) * 2019-04-26 2019-07-30 清华大学 Flexible biological electrode and preparation method thereof
CN110248477A (en) * 2019-06-12 2019-09-17 西安工程大学 A kind of manufacturing method of embedded compliant conductive route

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
肖渊: "织物表面微滴喷射打印沉积过程试验研究" *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111885841A (en) * 2020-07-31 2020-11-03 西安工程大学 Preparation method of flexible stretchable conductive circuit
CN111885841B (en) * 2020-07-31 2023-04-07 西安工程大学 Preparation method of flexible stretchable conductive circuit
CN114379069A (en) * 2020-10-20 2022-04-22 西安工程大学 Controllable wrinkle shape preparation method
CN114224595A (en) * 2021-11-12 2022-03-25 福建江夏学院 Cloth structure with electric heating warm keeping and electric stimulation coating and preparation method thereof
CN114224595B (en) * 2021-11-12 2023-09-19 徐州市海格德生物科技有限公司 Cloth structure with electrothermal heat-preserving and electro-stimulation coating and preparation method thereof
CN114883513A (en) * 2022-03-30 2022-08-09 南京邮电大学 Fabric electrode and rapid preparation method and application thereof
CN114883513B (en) * 2022-03-30 2024-02-23 南京邮电大学 Fabric electrode, and rapid preparation method and application thereof

Also Published As

Publication number Publication date
CN111419217B (en) 2023-06-20

Similar Documents

Publication Publication Date Title
CN111419217A (en) Preparation method and application of electrode based on flexible conductive fabric
CN111432560B (en) Manufacturing method of ultra-low resistance flexible conductive circuit
CN105133293B (en) A kind of preparation method of conductive nano composite material
CN106134299B (en) Printed wiring board substrate, printed wiring board and the method for manufacturing printed wiring board substrate
CN108517696B (en) Preparation method of patterned flexible conductive graphene cloth
KR20120116004A (en) Fine silver-plated copper powder and method for producing same
CN110730760A (en) Apparatus and method for providing a plurality of nanowires
CN101660264A (en) Method for preparing polyimide/silver composite conductive fiber
CN109468686A (en) Electrostatic spinning apparatus, the porous Gr/PAN composite nano fiber of orientation and preparation method thereof
CN108797098A (en) A method of based on cellulosic fabric surface printing conducting wire
CN110342563A (en) A kind of cupric oxide nano line and its preparation method and application
CN110248477A (en) A kind of manufacturing method of embedded compliant conductive route
CN107020374B (en) A kind of Ti3SiC2The preparation method of/Cu composite conductive powder
KR101273346B1 (en) Silver-plated nanoweb and dry-type electrode using there of
CN108064120B (en) The preparation method and preparation facilities of a kind of flexible circuit or electrode
CN108076591B (en) The preparation method and preparation facilities of a kind of flexible circuit or electrode
CN109520648A (en) A kind of wearable piezoresistive pressure sensor and its preparation method and application
KR101392932B1 (en) Nano-structure carbon layer foamed Aluminium Foil current collector with high electro-conductivity and Fabrication Method thereof
CN107243630B (en) A kind of Ti3SiC2The preparation method of/Ag composite conductive powder
CN111863310A (en) MXene preparation method and application of MXene as conductive silver paste reinforcing phase
CN108538864A (en) A kind of flexible wearable formula system and its manufacturing method based on inkjet printing technology
JP2008274404A (en) Manufacturing method of silver powder
CN106049035A (en) Establishment method of conductive circuit on surface of flexible fabric
CN111479396A (en) Preparation method of fabric-based high-conductivity circuit
CN101922001A (en) Method for manufacturing printed circuit board by power triggering electroless plating addition process

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant