CN113607309A - Stretchable calotropis gigantea fiber graphene flexible sensor - Google Patents

Stretchable calotropis gigantea fiber graphene flexible sensor Download PDF

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Publication number
CN113607309A
CN113607309A CN202110899693.2A CN202110899693A CN113607309A CN 113607309 A CN113607309 A CN 113607309A CN 202110899693 A CN202110899693 A CN 202110899693A CN 113607309 A CN113607309 A CN 113607309A
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calotropis gigantea
conductive
calotropis
stretchable
yarn
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李刚
张君泽
李毓陵
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Suzhou University
Nantong Textile and Silk Industrial Technology Research Institute
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Suzhou University
Nantong Textile and Silk Industrial Technology Research Institute
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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
    • G01L1/18Measuring force or stress, in general using properties of piezo-resistive materials, i.e. materials of which the ohmic resistance varies according to changes in magnitude or direction of force applied to the material
    • 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
    • D06M11/73Treating 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 carbon or compounds thereof
    • D06M11/74Treating 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 carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
    • 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
    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • 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
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres

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  • Textile Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
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  • General Chemical & Material Sciences (AREA)
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  • General Physics & Mathematics (AREA)
  • Woven Fabrics (AREA)

Abstract

The invention relates to the technical field of a calotropis gigantea fabric flexible sensor, in particular to a stretchable calotropis gigantea fiber graphene flexible sensor which comprises a stretchable flexible sensor main body, electrodes and a lead; the stretchable flexible sensor main body is a conductive flexible calotropis gigantea fabric layer, and the conductive flexible calotropis gigantea fabric layer is formed by weaving conductive calotropis gigantea yarns; the conductive calotropis gigantea yarn is prepared from conductive calotropis gigantea fibers; the stretchable flexible sensor body is connected with an electrode; the electrode is connected with a lead. According to the stretchable calotropis gigantean fiber graphene flexible sensor with the antibacterial function and the durability, the calotropis gigantean yarns are coated by a padding method, the uniform and excellent conductivity of the calotropis gigantean yarns is achieved by regulating and controlling the process, and then the calotropis gigantean yarns are woven by a textile technology.

Description

Stretchable calotropis gigantea fiber graphene flexible sensor
Technical Field
The invention relates to the technical field of calotropis gigantea fabric flexible sensors, in particular to a stretchable calotropis gigantea fiber graphene flexible sensor.
Background
The traditional sensor based on metal and semiconductor has poor sensitivity, toughness and strain capacity, so that the application of the sensor is limited, and in order to overcome the defects, the multifunctional flexible wearable electronic textile is produced and is more and more widely applied to the aspects of flexible sensors, wearable electronic equipment, electromagnetic interference shielding and the like. However, most flexible sensors have high sensitivity and wide detection range, but neglect the properties of durability and antibacterial property. The mudar is natural antibacterial fiber, the graphene is excellent antibacterial and conductive material, and the combination of the two materials can not only enable the mudar fiber to have better conductivity, but also enable the flexible fabric sensor to have excellent antibacterial function. In order to further improve the durability performance of the flexible sensor, improvements must be made from the structure of the sensor.
The defects and shortcomings of the prior art are as follows:
chinese patent is granted publication No. CN111238696A, discloses a tensile force sensor and system based on graphene film, through the resistance change that the change of volume leads to and the corresponding relation between resistance change and pulling force under the effect of pulling force of graphite alkene layer, can be accurate obtain the pulling force that awaits measuring, graphite alkene layer volume change is showing, can measure pulling force on a relatively large scale, and sensitivity is higher. However, with the increase of the stretching times, the graphene film is not uniformly stretched, so that the accuracy of the tested tensile force is obviously reduced, and the durability is poor.
Chinese patent No. CN111592761A discloses a novel flexible intelligent fabric sensor, which adsorbs carbon black in a carbon black solution onto modified platinum catalytic silicone rubber to obtain a carbon black/platinum catalytic silicone rubber composite material, and obtains a carbon black/platinum catalytic silicone rubber composite material with high sensitivity and large restorable strain by adsorbing and combining firm carbon black on the surface of the modified platinum catalytic rubber, and avoids the carbon black from agglomerating on the surface of the composite material, but cannot obtain a conductive coating with uniform thickness, resulting in poor durability and no antibacterial function.
The Chinese patent granted publication No. CN110230142A discloses a woven structure resistance type carbon fiber fabric sensor and application thereof, wherein high-performance conductive carbon fibers and high-performance dielectric fibers are woven to form a deformable high-strength textile structure material, and the function of the sensor is realized by weaving a multilayer structure and deformation thereof. The sensor can realize ultrahigh change of resistance under a small strain degree, but conductive fibers or dielectric fibers are introduced into the radial weft direction, and when a fabric is stretched, friction force is generated in the stretching direction, so that the friction of the carbon fibers or the dielectric fibers is damaged, the sensing durability is poor, and the sensor does not have an antibacterial function.
Chinese patent No. CN111055554A discloses a novel flexible intelligent fabric sensor and a method for manufacturing the same, wherein a carbon nanofiber with a slightly convex lattice is prepared by an electrospinning technique as a pressure sensitive material layer material, an electrode layer is coated with a conductive material, and a protective layer of the fabric sensor is prepared by using a high molecular elastic polymer, so that the flexible intelligent fabric sensor has high sensitivity, is softer, has a thinner thickness, and is also breathable and water-resistant, but due to the self limitation of the electrospun material, the sensor does not have an antibacterial function, and has poor durability.
The Chinese patent granted publication No. CN107233074A discloses a flexible wearable nanofiber fabric sensor and a preparation method thereof, wherein continuous nanofiber yarns prepared by electrostatic spinning are woven into a fabric through a weaving technology, gel films with conductive copper wires are compounded on the upper surface and the lower surface of the fabric, and the nanofiber fabric sensor with a sandwich structure is obtained.
Chinese patent No. CN107167180A discloses an elastic sensor and a method for manufacturing the same, in which graphene oxide-coated elastic fibers obtained by dipping in a graphene oxide solution are immersed in a tin chloride solution or a mixed solution of the tin chloride solution and the graphene oxide dispersion solution to perform a hydrothermal reaction, so as to obtain a conductive elastic fiber product, electrodes are fixed at both ends of the product to obtain the elastic sensor, the sensor has high wearing comfort, a wide detection range and high sensitivity, but the outer layer of the elastic fiber is made of fibers such as cotton, hemp, wool and the like, and has no antibacterial function, and when the graphene-coated fibers are stretched, surface graphene is easy to fall off after friction, and lacks a protective layer, so that the durability is poor.
Chinese patent No. CN108896199A discloses a stretchable yarn sensor and a method for manufacturing the same, in which a temperature sensitive material or a moisture sensitive material is coated on a cotton fiber or a silk fiber by dip coating, drop coating, lifting or spin coating to form an electrode yarn, and the electrode yarn is wound around an elastic yarn according to an "S" spiral, which is a yarn sensor that has good stability and high sensitivity and is light and thin and can be attached to the skin of a human body, but due to the characteristics of the substrate itself, the sensor does not have an antibacterial function and cannot be used for monitoring a human body for a long time.
Therefore, in order to overcome the problems of the flexible sensor, the invention provides a preparation method of a stretchable calotropis gigantea fiber graphene flexible sensor with antibacterial function and durability.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides a stretchable calotropis gigantea fiber graphene flexible sensor which comprises a stretchable flexible sensor main body, electrodes and a lead; the stretchable flexible sensor main body is a conductive flexible calotropis gigantea fabric layer, and the conductive flexible calotropis gigantea fabric layer is formed by weaving conductive calotropis gigantea yarns; the conductive calotropis gigantea yarn is prepared from conductive calotropis gigantea fibers; the stretchable flexible sensor body is connected with an electrode; the electrode is connected with a lead.
Preferably, the conductive flexible calotropis gigantea fabric layer comprises the following preparation steps: s1: placing the mudar floss in a surface cleaning agent and cleaning oil stains on the surface; combining the graphene oxide prepared by the redox method with the mudar horn fiber by a repeated padding method; finally, placing the conductive calotropis gigantea fiber in an ascorbic acid solution, and reducing the graphene oxide on the surface of the calotropis gigantea fiber to obtain the conductive calotropis gigantea fiber; s2: preparing conductive calotropis gigantea fibers into conductive calotropis gigantea yarns; and preparing the conductive calotropis gigantea yarn into a conductive flexible calotropis gigantea fabric layer by a weaving machine.
Preferably, the surface cleaning agent is Na2CO3The concentration of the solution, NaOH solution or oxalic acid solution is 10-30g/L, the washing time is 30-60min, the washing temperature is 30-60 ℃, and the washing bath ratio is 1 (300-500).
Preferably, the concentration of the graphene oxide solution is 3-7 mg/mL.
Preferably, the weight ratio of the ascorbic acid in the ascorbic acid solution to the graphene oxide on the yarn is (10-20): 1.
Preferably, the treatment time of the ascorbic acid solution is 12-36 h.
Preferably, in S1, the padding method includes soaking, padding and drying; the soaking time is 30-100min, and the drying time is 30-60 min; wherein, the steps from soaking, padding to drying are a padding cycle, and the padding cycle is processed for 4-10 times.
Preferably, in S2, the weft yarn is a conductive calotropis gigantea yarn processed from calotropis gigantea fiber, and the weft yarn is continuously inserted; the warp yarns are elastic spandex yarns.
Preferably, in S2, the conductive flexible calotropis gigantea fabric layer has a warp density of 100-.
Preferably, in S2, in the conductive flexible calotropis gigantea fabric layer, both weft yarns and warp yarns are 10-30 tex.
According to the stretchable calotropis gigantea fiber graphene flexible sensor with the antibacterial function and the durability, the calotropis gigantea yarn is coated by a padding method, the uniform and excellent conductivity of the calotropis gigantea yarn is obtained by regulating and controlling the process, and then the calotropis gigantea yarn is woven by a weaving technology.
According to the invention, the calotropis gigantea fiber is used as a base material for conducting functionalization, and the excellent antibacterial property of the calotropis gigantea fiber is combined with the antibacterial property of graphene, so that the prepared flexible sensor can obtain better antibacterial property.
According to the invention, the mudar horn yarn is coated by a repeated reciprocating padding method, so that the combination of the mudar horn fiber and the graphene is firmer, and the graphene can be uniformly and effectively distributed on the surface of the mudar horn fiber, thereby effectively improving the durability of the flexible sensor.
According to the stretchable calotropis gigantean fiber graphene flexible sensor, conductive calotropis gigantean yarns are used as weft yarns for continuous weft insertion, elastic spandex yarns are used as warp yarns for weaving into cloth, so that the stretchable calotropis gigantean fiber graphene flexible sensor obtains excellent radial tensile property, and the flexible sensor has better durability.
According to the stretchable calotropis gigantea fiber graphene flexible sensor, due to the structural design, abrasion and damage to the calotropis gigantea fiber surface graphene are effectively reduced, and the durability of the flexible sensor is effectively improved.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment 1 of a stretchable calotropis gigantea fiber graphene flexible sensor provided by the present invention;
FIG. 2 is a graph showing the rate of change of resistance according to the elongation during stretching in example 1;
FIG. 3 shows the corresponding resistance change rate of 500 cycles of stretching in example 1;
fig. 4 is a corresponding resistance change rate of a common calotropis gigantea elastic fabric sensor in the prior art when the sensor is stretched for 500 cycles;
FIG. 5 is an antibacterial test of the conductive Calotropis gigantean yarn of the present invention in example 1;
fig. 6 is an antibacterial experiment of a common cotton yarn in the prior art.
Detailed Description
The invention provides a stretchable calotropis gigantea fiber graphene flexible sensor which comprises a stretchable flexible sensor body 1, electrodes 2 and a lead 3; the stretchable flexible sensor body 1 is a conductive flexible calotropis gigantea fabric layer 4, and the conductive flexible calotropis gigantea fabric layer 4 is woven by conductive calotropis gigantea yarns 5; the conductive calotropis gigantea yarn 5 is prepared from conductive calotropis gigantea fibers 6;
the stretchable flexible sensor body 1 is connected with an electrode 2; the electrode 2 is connected with a lead 3.
According to the stretchable calotropis gigantea fiber graphene flexible sensor with the antibacterial function and the durability, the calotropis gigantea yarn is coated by a padding method, the uniform and excellent conductivity of the calotropis gigantea yarn is obtained by regulating and controlling the process, and then the calotropis gigantea yarn is woven by a weaving technology.
According to the invention, the calotropis gigantea fiber is used as a base material for conducting functionalization, and the excellent antibacterial property of the calotropis gigantea fiber is combined with the antibacterial property of graphene, so that the prepared flexible sensor can obtain better antibacterial property.
According to the invention, the mudar horn yarn is coated by a repeated reciprocating padding method, so that the combination of the mudar horn fiber and the graphene is firmer, and the graphene can be uniformly and effectively distributed on the surface of the mudar horn fiber, thereby effectively improving the durability of the flexible sensor.
According to the stretchable calotropis gigantean fiber graphene flexible sensor, the conductive calotropis gigantean yarns are used as weft yarns for continuous weft insertion, the elastic spandex yarns are used as warp yarns for weaving into cloth, and therefore the stretchable calotropis gigantean fiber graphene flexible sensor can obtain excellent radial tensile property and has better durability.
According to the stretchable calotropis gigantea fiber graphene flexible sensor, due to the structural design, abrasion and damage to the calotropis gigantea fiber surface graphene are effectively reduced, and the durability of the flexible sensor is effectively improved.
Example one
As shown in fig. 1 to 3 and fig. 5, in the present invention, the conductive flexible calotropis gigantea fabric layer 4 comprises the following preparation steps:
s11: mixing Calotropis gigantea yarnThe wire is placed on Na2CO3Washing in solution, Na2CO3The concentration of the solution is 20g/L, the washing time is 50min, the washing temperature is 45 ℃, the washing bath ratio is 1:300, the mudar yarn is washed by deionized water after washing, the impurities remained on the surface of the mudar yarn are removed, and then the mudar yarn is placed in a drying oven to be dried for 1h at the temperature of 60 ℃;
s12 mixing 1-4g of graphite and 1-4g of NaNO3Mixed in 100mL of H2SO4Continuously stirring in an ice bath, adding 3-12g of potassium permanganate during stirring, adding 150-600mL of deionized water in portions after stirring is finished, and adding a proper amount of H2O2Terminating the reaction, obtaining a graphene oxide solution through high-speed centrifugation of HCL and water, and adjusting the concentration of the graphene oxide solution to be 5 mg/mL;
s13: soaking the mudar floss cleaned in the step S11 in the graphene oxide solution in the step S12 for 60min, removing redundant graphene oxide solution on the surface of the mudar fiber through a small padder after the mudar yarn is fully soaked, enabling the graphene oxide to be uniformly distributed on the surface of the mudar fiber, and pressing part of the graphene oxide solution into the mudar fiber;
s14: placing the mudar yarns processed by the padder in the S13 into an oven to be dried for 1 hour, wherein the drying temperature is 60 ℃;
wherein, S13 and S14 are a cycle of handling the calotropis gigantea yarn, and the process needs to be cycled for 10 times;
s15: placing the calotropis gigantea yarn treated in the S14 into an ascorbic acid solution for treatment, preparing the ascorbic acid solution according to the mass ratio of 10:1 of the ascorbic acid to the graphene oxide on the surface of the calotropis gigantea yarn, treating for 24 hours at the treatment temperature of 80 ℃, after the treatment is finished, placing the calotropis gigantea yarn into a drying oven for treatment for 1 hour at the drying temperature of 60 ℃, and obtaining the conductive calotropis gigantea yarn;
s16: weaving the conductive calotropis gigantea yarns in the S15 into fabric by using a weaving method, wherein the conductive calotropis gigantea yarns are used as weft yarns, the spandex core-spun yarns are used as warp yarns, the fabric is in a twill weave structure, the warp density is 140 pieces/10 cm, the weft density is 600 pieces/10 cm, and the thicknesses of the warp yarns and the weft yarns are both 20 tex;
s17: connecting two ends of the conductive elastic calotropis gigantea fabric woven in the S16 with conductive copper wires, coating silver paste on the connecting points, placing the conductive elastic calotropis gigantea fabric in an oven for processing for 1 hour, and drying at the temperature of 60 ℃ to obtain the stretchable calotropis gigantea fiber graphene flexible sensor, wherein the length of the sensor is 20mm, and the width of the sensor is 10 mm;
as can be seen from fig. 2, the stretchable calotropis gigantea fiber graphene flexible sensor prepared by the method can meet the basic requirements of the sensor;
as can be seen from fig. 3, after the stretchable calotropis gigantea fiber graphene flexible sensor prepared by the invention is stretched 500 times under the condition that the elongation is 50%, the resistance change rate is kept better, and the stretchable calotropis gigantea fiber graphene flexible sensor shows better durability.
As can be seen from fig. 5, the mudar yarn has a good antibacterial property.
Meanwhile, in the prior art, as can be seen from fig. 4, after the ordinary sensor is stretched for 500 times under the condition of 50% of elongation, the durability of the sensor is inferior to that of the stretchable calotropis gigantea fiber graphene flexible sensor in the invention. As can be seen from fig. 6, the conventional cotton yarn has no antibacterial property.
Example two
In the invention, the conductive flexible calotropis gigantea fabric layer 4 comprises the following preparation steps:
s21: putting the calotropis gigantea yarn into NaOH solution for cleaning, wherein the concentration of the NaOH solution is 20g/L, the cleaning time is 60min, the cleaning temperature is 30 ℃, the cleaning bath ratio is 1:500, after cleaning, the calotropis gigantea yarn is cleaned by deionized water, and after removing impurities remained on the surface of the calotropis gigantea yarn, the calotropis gigantea yarn is placed in an oven for drying for 1h at the temperature of 30 ℃;
s22: mixing 1-4g of graphite and 1-4g of NaNO3Mixing in 100mLH2SO4Continuously stirring in an ice bath, adding 3-12g of potassium permanganate during stirring, adding 150-600mL of deionized water in portions after stirring is finished, and adding a proper amount of H2O2Terminating the reaction, obtaining a graphene oxide solution through high-speed centrifugation of HCL and water, and adjusting the concentration of the graphene oxide solution to be 3 mg/mL;
s23: soaking the mudar floss cleaned in the S21 in the graphene oxide solution in the S22 for 100min, removing redundant graphene oxide solution on the surface of the mudar fiber through a small padder after the mudar yarn is fully soaked, enabling the graphene oxide to be uniformly distributed on the surface of the mudar fiber, and pressing part of the graphene oxide solution into the mudar fiber;
s24: placing the mudar yarn processed by the padder in the S23 into an oven to be dried for 50min, wherein the drying temperature is 60 ℃;
wherein, S23 and S24 are a cycle of handling the calotropis gigantea yarn, and the process needs 7 cycles;
s25: placing the calotropis gigantea yarn treated in the S24 into an ascorbic acid solution for treatment, preparing the ascorbic acid solution according to the mass ratio of 15:1 of the ascorbic acid to the graphene oxide on the surface of the calotropis gigantea yarn, treating for 12 hours at the treatment temperature of 80 ℃, after the treatment is finished, placing the calotropis gigantea yarn into a drying oven for treatment for 1 hour at the drying temperature of 60 ℃, and obtaining the conductive calotropis gigantea yarn;
s26: weaving the conductive calotropis gigantea yarn in the S25 into a fabric by using a weaving method, wherein the conductive calotropis gigantea yarn is used as weft yarn, the spandex core-spun yarn is used as warp yarn, the core yarn is calotropis gigantea yarn, the fabric has a plain weave structure, the warp density is 100 pieces/10 cm, the weft density is 500 pieces/10 cm, and the thicknesses of the warp yarn and the weft yarn are both 30 tex;
s27: connecting two ends of the conductive elastic calotropis gigantea fabric woven in the S26 with conductive copper wires, coating silver paste on the connecting points, and placing the conductive elastic calotropis gigantea fabric in a drying oven for processing for 1 hour, wherein the drying temperature is 60 ℃;
s28: the conductive elastic calotropis gigantea fabric prepared in S27 is wrapped by high-elasticity polymer PDMS, air bubbles in the conductive elastic calotropis gigantea fabric are removed through a vacuum drying oven after the conductive elastic calotropis gigantea fabric is wrapped, the extraction time is 1h, the drying temperature is 40 ℃, the vacuum degree is 0.99MPa, the stretchable calotropis gigantea fiber graphene flexible sensor is obtained, the length of the sensor is 20mm, and the width of the sensor is 10 mm.
EXAMPLE III
In the invention, the conductive flexible calotropis gigantea fabric layer 4 comprises the following preparation steps:
s31: placing Calotropis gigantea yarn in Na2CO3Washing in solution, Na2CO3The concentration of the solution is 30g/L, the washing time is 40min, the washing temperature is 60 ℃, the washing bath ratio is 1:400, the mudar yarn is washed by deionized water after washing, the impurities remained on the surface of the mudar yarn are removed, and then the mudar yarn is placed in an oven to be dried for 1h at 50 ℃;
s33: mixing 1-4g of graphite and 1-4g of NaNO3Mixing in 100mLH2SO4Continuously stirring in an ice bath, adding 3-12g of potassium permanganate during stirring, adding 150-600mL of deionized water in portions after stirring is finished, and adding a proper amount of H2O2Terminating the reaction, obtaining a graphene oxide solution through high-speed centrifugation of HCL and water, and adjusting the concentration of the graphene oxide solution to be 7 mg/mL;
s33: soaking the mudar floss cleaned in the S31 in the graphene oxide solution in the S32 for 80min, removing redundant graphene oxide solution on the surface of the mudar fiber through a small padder after the mudar yarn is fully soaked, enabling the graphene oxide to be uniformly distributed on the surface of the mudar fiber, and pressing part of the graphene oxide solution into the mudar fiber;
s34: placing the mudar yarn processed by the padder in the S33 into an oven to be dried for 40min, wherein the drying temperature is 60 ℃;
wherein, S33 and S34 are a cycle of handling the calotropis gigantea yarn, and the process needs to be cycled for 4 times;
s35: placing the calotropis gigantea yarn treated in the S34 into an ascorbic acid solution for treatment, preparing the ascorbic acid solution according to the mass ratio of 20:1 of the ascorbic acid to the graphene oxide on the surface of the calotropis gigantea yarn, wherein the treatment time is 36h, the treatment temperature is 80 ℃, after the treatment is finished, placing the calotropis gigantea yarn into a drying oven for treatment for 1h, and the drying temperature is 60 ℃ to obtain the conductive calotropis gigantea yarn;
s36: weaving the conductive calotropis gigantea yarn in the S35 into a fabric by using a weaving method, wherein the conductive calotropis gigantea yarn is used as weft yarn, the spandex core-spun yarn is used as warp yarn, the fabric is in a twill weave structure, the warp density is 200 pieces/10 cm, the weft density is 400 pieces/10 cm, and the thicknesses of the warp yarn and the weft yarn are both 10 tex;
s37: connecting two ends of the conductive elastic calotropis gigantea fabric woven in the S36 with conductive copper wires, coating silver paste on the connecting points, and placing the conductive elastic calotropis gigantea fabric in a drying oven for processing for 1 hour, wherein the drying temperature is 60 ℃;
s38: wrapping the conductive elastic calotropis gigantea fabric prepared in the S37 by using a high-elasticity polymer Ecoflex, and after wrapping, removing air bubbles in the conductive elastic calotropis gigantea fabric by using a vacuum drying oven, wherein the extraction time is 0.5h, the drying temperature is 80 ℃, and the vacuum degree is 0.99MPa, so that the stretchable calotropis gigantea fiber graphene flexible sensor is obtained, and the length of the sensor is 20mm, and the width of the sensor is 10 mm.
Example four
In the invention, the conductive flexible calotropis gigantea fabric layer 4 comprises the following preparation steps:
placing Calotropis gigantea yarn in Na2CO3Cleaning in a solution, wherein the concentration of an oxalic acid solution is 10g/L, the cleaning time is 40min, the cleaning temperature is 30 ℃, the cleaning bath ratio is 1:500, cleaning the mudar yarn by deionized water after cleaning, removing the impurities remained on the surface of the mudar yarn, and then placing the mudar yarn in an oven to dry for 1h at 40 ℃;
mixing 1-4g of graphite and 1-4g of NaNO3Mixing in 100mLH2SO4Continuously stirring in an ice bath, adding 3-12g of potassium permanganate during stirring, adding 150-600mL of deionized water in portions after stirring is finished, and adding a proper amount of H2O2And (3) stopping the reaction, obtaining a graphene oxide solution by high-speed centrifugation of HCL and water, and adjusting the concentration of the graphene oxide solution to be 5 mg/mL.
The method comprises the following steps: soaking the cleaned calotropis gigantea yarn in a graphene oxide solution for 30min, removing redundant graphene oxide solution on the surface of calotropis gigantea fibers by a small padder after the calotropis gigantea yarn is fully soaked, enabling the graphene oxide to be uniformly distributed on the surface of the calotropis gigantea fibers, and pressing part of the graphene oxide solution into the calotropis gigantea fibers;
step two: placing the mudar yarn processed by the padder into an oven to be dried for 30min, wherein the drying temperature is 60 ℃;
wherein, the step one and the step two are a cycle of handling the mudar yarn, and the process needs to be cycled for 10 times;
placing the treated calotropis gigantea yarn into an ascorbic acid solution for treatment, preparing the ascorbic acid solution according to the mass ratio of 10:1 of the ascorbic acid to the graphene oxide on the surface of the calotropis gigantea yarn, treating for 24 hours at the treatment temperature of 80 ℃, placing the calotropis gigantea yarn into a drying oven for treatment for 1 hour at the drying temperature of 60 ℃ to obtain the conductive calotropis gigantea yarn;
weaving the conductive calotropis gigantea yarns into fabric by using a weaving method, wherein the conductive calotropis gigantea yarns are used as weft yarns, the spandex core-spun yarns are used as warp yarns, the fabric is in a satin weave structure, the warp density is 200 pieces/10 cm, the weft density is 600 pieces/10 cm, and the thicknesses of the warp yarns and the weft yarns are both 20 tex;
connecting two ends of the woven conductive elastic calotropis gigantea fabric with conductive copper wires, coating silver paste on the connecting points, and placing the fabric in a drying oven for processing for 1 hour, wherein the drying temperature is 60 ℃; the stretchable calotropis gigantea fiber graphene flexible sensor is obtained, the length of the sensor is 20mm, and the width of the sensor is 10 mm.
EXAMPLE five
In the invention, the conductive flexible calotropis gigantea fabric layer 4 comprises the following preparation steps:
placing Calotropis gigantea yarn in Na2CO3Washing in solution, Na2CO3The concentration of the solution is 20g/L, the washing time is 30min, the washing temperature is 40 ℃, the washing bath ratio is 1:300, the mudar yarn is washed by deionized water after washing, the impurities remained on the surface of the mudar yarn are removed, and then the mudar yarn is placed in a drying oven to be dried for 1h at 40 ℃;
mixing 1-4g of graphite and 1-4g of NaNO3Mixing in 100mLH2SO4Continuously stirring in an ice bath, adding 3-12g of potassium permanganate during stirring, adding 150-600mL of deionized water in portions after stirring is finished, and adding a proper amount of H2O2And (3) stopping the reaction, obtaining a graphene oxide solution by high-speed centrifugation of HCL and water, and adjusting the concentration of the graphene oxide solution to be 7 mg/mL.
The method comprises the following steps: soaking the cleaned calotropis gigantea yarn in a graphene oxide solution for 30min, removing redundant graphene oxide solution on the surface of calotropis gigantea fibers by a small padder after the calotropis gigantea yarn is fully soaked, enabling the graphene oxide to be uniformly distributed on the surface of the calotropis gigantea fibers, and pressing part of the graphene oxide solution into the calotropis gigantea fibers;
step two: placing the mudar yarn processed by the padder into an oven to be dried for 30min, wherein the drying temperature is 60 ℃;
wherein, the step one and the step two are a cycle of handling the mudar yarn, and the process needs to be cycled for 10 times;
placing the treated calotropis gigantea yarn into an ascorbic acid solution for treatment, preparing the ascorbic acid solution according to the mass ratio of 10:1 of the ascorbic acid to the graphene oxide on the surface of the calotropis gigantea yarn, treating for 24 hours at the treatment temperature of 80 ℃, placing the calotropis gigantea yarn into a drying oven for treatment for 1 hour at the drying temperature of 60 ℃ to obtain the conductive calotropis gigantea yarn;
feeding conductive calotropis gigantea yarns into a weft knitting machine to be woven into a fabric by using a knitting method, wherein the fabric has the structure of weft plain needles with the technical parameters of 1+1 rib, the needle type of 12 needles/25.4 mm, and the thickness of the yarns is 20 tex;
connecting two ends of the weft-knitted conductive calotropis gigantea fabric with conductive copper wires, coating silver paste on the connecting points, and placing the fabric in a drying oven for processing for 1 hour, wherein the drying temperature is 60 ℃; the stretchable calotropis gigantea fiber graphene flexible sensor is obtained, the length of the sensor is 20mm, and the width of the sensor is 10 mm.
EXAMPLE six
In the invention, the conductive flexible calotropis gigantea fabric layer 4 comprises the following preparation steps:
putting the calotropis gigantea yarn into NaOH solution for cleaning, wherein the concentration of the NaOH solution is 20g/L, the cleaning time is 60min, the cleaning temperature is 30 ℃, the cleaning bath ratio is 1:500, after cleaning, the calotropis gigantea yarn is cleaned by deionized water, and after removing impurities remained on the surface of the calotropis gigantea yarn, the calotropis gigantea yarn is placed in an oven for drying for 1h at the temperature of 30 ℃;
mixing 1-4g of graphite and 1-4g of NaNO3Mixing in 100mLH2SO4In the process, the mixture is continuously stirred in an ice bath, 3 to 12g of potassium permanganate are added during the stirring, and after the stirring is finished, 150-600mL of potassium permanganate are added in portionsIonized water is added, and a proper amount of H is added2O2And (3) stopping the reaction, obtaining a graphene oxide solution by high-speed centrifugation of HCL and water, and adjusting the concentration of the graphene oxide solution to be 3 mg/mL.
The method comprises the following steps: soaking the cleaned calotropis gigantea yarn in a graphene oxide solution for 100min, removing redundant graphene oxide solution on the surface of calotropis gigantea fibers by a small padder after the calotropis gigantea yarn is fully soaked, enabling the graphene oxide to be uniformly distributed on the surface of the calotropis gigantea fibers, and pressing part of the graphene oxide solution into the calotropis gigantea fibers;
step two: placing the mudar yarn processed by the padder into an oven to be dried for 50min, wherein the drying temperature is 60 ℃;
wherein, the step one and the step two are a cycle of handling the mudar yarn, and the process needs 7 cycles;
placing the treated calotropis gigantea yarn into an ascorbic acid solution for treatment, preparing the ascorbic acid solution according to the mass ratio of 15:1 of the ascorbic acid to the graphene oxide on the surface of the calotropis gigantea yarn, treating for 12 hours at the treatment temperature of 80 ℃, placing the calotropis gigantea yarn into a drying oven for treatment for 1 hour at the drying temperature of 60 ℃ to obtain the conductive calotropis gigantea yarn;
feeding conductive calotropis gigantea yarns into a warp knitting machine by using a knitting method to weave into a fabric, wherein the structure of the fabric is a warp flat structure, the needle type is 12 needles/25.4 mm of process parameters, and the thickness of the yarns is 20 tex;
connecting two ends of the warp-knitted conductive calotropis gigantea fabric with conductive copper wires, coating silver paste on connecting points, placing in an oven for processing for 1h, and drying at the temperature of 60 ℃ to obtain the stretchable calotropis gigantea fiber graphene flexible sensor, wherein the length of the sensor is 20mm, and the width of the sensor is 10 mm.
EXAMPLE seven
In the invention, the conductive flexible calotropis gigantea fabric layer 4 comprises the following preparation steps:
placing Calotropis gigantea yarn in Na2CO3Washing in solution, Na2CO3The solution concentration is 20g/L, the washing time is 50min, and the washing temperature is 45 DEG CWashing the mudar yarn with deionized water at a washing bath ratio of 1:300, removing residual impurities on the surface of the mudar yarn, and drying the mudar yarn in a drying oven at 60 ℃ for 1 h;
mixing 1-4g of graphite and 1-4g of NaNO3Mixing in 100mLH2SO4Continuously stirring in an ice bath, adding 3-12g of potassium permanganate during stirring, adding 150-600mL of deionized water in portions after stirring is finished, and adding a proper amount of H2O2And (3) stopping the reaction, obtaining a graphene oxide solution by high-speed centrifugation of HCL and water, and adjusting the concentration of the graphene oxide solution to be 5 mg/mL.
The method comprises the following steps: soaking the cleaned calotropis gigantea yarn in a graphene oxide solution for 60min, removing redundant graphene oxide solution on the surface of calotropis gigantea fibers by a small padder after the calotropis gigantea yarn is fully soaked, enabling the graphene oxide to be uniformly distributed on the surface of the calotropis gigantea fibers, and pressing part of the graphene oxide solution into the calotropis gigantea fibers;
step two: placing the mudar yarns processed by the padder into an oven to be dried for 1 hour, wherein the drying temperature is 60 ℃;
wherein, the step one and the step two are a cycle of handling the mudar yarn, and the process needs to be circulated for 4 times;
placing the treated calotropis gigantea yarn into an ascorbic acid solution for treatment, preparing the ascorbic acid solution according to the mass ratio of 10:1 of the ascorbic acid to the graphene oxide on the surface of the calotropis gigantea yarn, treating for 24 hours at the treatment temperature of 80 ℃, placing the calotropis gigantea yarn into a drying oven for treatment for 1 hour at the drying temperature of 60 ℃ to obtain the conductive calotropis gigantea yarn;
weaving conductive calotropis gigantea yarns into a sheet fabric by using a plane weaving method, wherein warp yarns are spandex core-spun yarns, weft yarns are conductive calotropis gigantea yarns, the yarns are alternately woven into the conductive calotropis gigantea fabric with the length of 2cm and the width of 1cm according to a plain weaving method, and the thickness of the warp yarns and the thickness of the weft yarns are both 30 tex;
connecting two ends of the woven conductive elastic calotropis gigantea fabric with conductive copper wires, coating silver paste on the connecting points, and placing the conductive elastic calotropis gigantea fabric in a drying oven for processing for 1 hour, wherein the drying temperature is 60 ℃;
wrapping the prepared conductive elastic calotropis gigantea fabric by using a high-elasticity polymer PDMS, and after wrapping, removing air bubbles in the conductive elastic calotropis gigantea fabric by using a vacuum drying oven, wherein the extraction time is 1h, the drying temperature is 40 ℃, and the vacuum degree is 0.99MPa, so that the stretchable calotropis gigantea fiber graphene flexible sensor is obtained, and the length of the sensor is 20mm, and the width of the sensor is 10 mm.
The embodiments of the present invention have been described in detail with reference to the drawings, but the present invention is not limited thereto, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention.

Claims (9)

1. A stretchable calotropis gigantea fiber graphene flexible sensor is characterized by comprising a stretchable flexible sensor main body (1), electrodes (2) and a lead (3); the stretchable flexible sensor main body (1) is a conductive flexible calotropis gigantea fabric layer (4), and the conductive flexible calotropis gigantea fabric layer (4) is formed by weaving conductive calotropis gigantea yarns (5); the conductive calotropis gigantea yarn (5) is prepared from conductive calotropis gigantea fibers (6);
the stretchable flexible sensor body (1) is connected with an electrode (2); the electrode (2) is connected with a lead (3).
2. A stretchable calotropis gigantea fiber graphene flexible sensor according to claim 1, characterized in that the conductive flexible calotropis gigantea fabric layer (4) comprises the following preparation steps:
s1: placing the mudar floss in a surface cleaning agent and cleaning oil stains on the surface; combining the graphene oxide prepared by the redox method with the mudar horn fiber by a repeated padding method; finally, placing the conductive calotropis gigantea fiber in an ascorbic acid solution, and reducing the graphene oxide on the surface of the calotropis gigantea fiber to obtain the conductive calotropis gigantea fiber (6);
s2: preparing the conductive calotropis gigantea fibers (6) into conductive calotropis gigantea yarns (5); and preparing the conductive calotropis gigantea yarn (5) into a conductive flexible calotropis gigantea fabric layer (4) by a weaving machine.
3. A stretchable calotropis gigantea fiber graphene flexible sensor according to claim 2, characterized in that the surface cleaning agent is Na2CO3The concentration of the solution, NaOH solution or oxalic acid solution is 10-30g/L, the washing time is 30-60min, the washing temperature is 30-60 ℃, and the washing bath ratio is 1 (300-500).
4. A stretchable calotropis gigantea fiber graphene flexible sensor according to claim 2, wherein the concentration of the graphene oxide solution is 3-7 mg/mL.
5. A stretchable calotropis gigantea fiber graphene flexible sensor according to claim 2, characterized in that the ratio of the ascorbic acid weight of the ascorbic acid solution to the graphene oxide weight on the yarn is (10-20):1, and the processing time is 12-36 h.
6. A stretchable calotropis gigantea fiber graphene flexible sensor according to claim 2, wherein in S1, the padding method comprises soaking, padding and drying; the soaking time is 30-100min, and the drying time is 30-60 min; wherein, the steps from soaking, padding to drying are a padding cycle, and the padding cycle is processed for 4-10 times.
7. A stretchable calotropis gigantea fiber graphene flexible sensor according to claim 2, characterized in that in S2, the weft yarn is a conductive calotropis gigantea yarn (5) processed by calotropis gigantea fiber, and the weft yarn is continuously inserted; the warp yarns are elastic spandex yarns.
8. The stretchable calotropis gigantea fiber graphene flexible sensor according to claim 2, wherein in S2, the warp density of the conductive flexible calotropis gigantea fabric layer (4) is 200 pieces/10 cm, and the weft density is 400 pieces/10 cm.
9. A stretchable calotropis gigantea fiber graphene flexible sensor according to claim 2, characterized in that in S2, in the conductive flexible calotropis gigantea fabric layer (4), both weft yarns and warp yarns are 10-30 tex.
CN202110899693.2A 2021-08-06 2021-08-06 Stretchable calotropis gigantea fiber graphene flexible sensor Pending CN113607309A (en)

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