CN115161995B - Conductive fabric material for single-walled carbon nanotube uniformly coated commercial cotton bandage and preparation method and application thereof - Google Patents
Conductive fabric material for single-walled carbon nanotube uniformly coated commercial cotton bandage and preparation method and application thereof Download PDFInfo
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- CN115161995B CN115161995B CN202110834583.8A CN202110834583A CN115161995B CN 115161995 B CN115161995 B CN 115161995B CN 202110834583 A CN202110834583 A CN 202110834583A CN 115161995 B CN115161995 B CN 115161995B
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- 239000002109 single walled nanotube Substances 0.000 title claims abstract description 116
- 239000004744 fabric Substances 0.000 title claims abstract description 99
- 229920000742 Cotton Polymers 0.000 title claims abstract description 61
- 239000000463 material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 105
- 238000002791 soaking Methods 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000006185 dispersion Substances 0.000 claims abstract description 25
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 25
- 238000001514 detection method Methods 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 18
- 238000009954 braiding Methods 0.000 claims abstract description 3
- 239000000853 adhesive Substances 0.000 claims description 44
- 230000001070 adhesive effect Effects 0.000 claims description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 239000008367 deionised water Substances 0.000 claims description 35
- 229910021641 deionized water Inorganic materials 0.000 claims description 35
- 238000012360 testing method Methods 0.000 claims description 28
- 239000011248 coating agent Substances 0.000 claims description 22
- 238000000576 coating method Methods 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 20
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 19
- 229910052709 silver Inorganic materials 0.000 claims description 18
- 239000004332 silver Substances 0.000 claims description 18
- 238000005520 cutting process Methods 0.000 claims description 17
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 16
- 229910052802 copper Inorganic materials 0.000 claims description 16
- 239000010949 copper Substances 0.000 claims description 16
- 238000013480 data collection Methods 0.000 claims description 15
- 238000003760 magnetic stirring Methods 0.000 claims description 15
- 230000035945 sensitivity Effects 0.000 claims description 12
- 238000000151 deposition Methods 0.000 claims description 11
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 239000000835 fiber Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims 4
- 238000011049 filling Methods 0.000 claims 1
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 claims 1
- 239000004020 conductor Substances 0.000 abstract description 33
- 230000004044 response Effects 0.000 abstract description 10
- 230000001351 cycling effect Effects 0.000 abstract description 9
- 239000007788 liquid Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000004094 surface-active agent Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 28
- 238000004458 analytical method Methods 0.000 description 13
- 230000008569 process Effects 0.000 description 8
- 230000008859 change Effects 0.000 description 6
- 230000008021 deposition Effects 0.000 description 6
- 238000005452 bending Methods 0.000 description 5
- 239000002041 carbon nanotube Substances 0.000 description 5
- 229910021393 carbon nanotube Inorganic materials 0.000 description 5
- 238000011056 performance test Methods 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 241000282414 Homo sapiens Species 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229920002334 Spandex Polymers 0.000 description 2
- 239000002134 carbon nanofiber Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004759 spandex Substances 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- CLOMYZFHNHFSIQ-UHFFFAOYSA-N clonixin Chemical compound CC1=C(Cl)C=CC=C1NC1=NC=CC=C1C(O)=O CLOMYZFHNHFSIQ-UHFFFAOYSA-N 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating 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
- D06M11/73—Treating 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
- D06M11/74—Treating 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
Abstract
The invention relates to a commercial Cotton Bandage (CB) solution method deposited single-walled carbon nanotube (SWCNT) conductive fabric material, a preparation method and application thereof. And adding the SWCNT into a surfactant Sodium Dodecyl Benzene Sulfonate (SDBS) solution, fully stirring and performing ultrasonic dispersion to obtain SWCNT dispersion liquid, and preparing the conductive fabric uniformly coated by the SWCNT by a solution soaking method. The multilayer braiding structure of CB is beneficial to maximizing the adsorption of SWCNT, wherein, when soaked for three times, the conductive bandage has good mechanical flexibility, wider strain response range, low strain detection limit, good cycling stability, washability and the like; when soaked for five times, the conductive bandage has good conductivity, high stretchability, excellent mechanical stretching stability and the like. The method for obtaining the conductive fabric material by the solution soaking method has the advantages of simple preparation process, low production cost, easy industrial scale and the like, and can be widely applied to flexible multidirectional strain sensors and elastic stretchable conductors.
Description
Technical Field
The invention relates to a conductive fabric material of a single-walled carbon nanotube coated cotton bandage and preparation and application thereof, belonging to the technical field of functional nano materials.
Background
The intelligent wearable field is a cross research field integrating multiple subjects and multiple categories, and is recently paid attention to by students. Recently, the conductive fiber is used as a pivot of intelligent wearable equipment, has wide application prospect in the intelligent wearable field due to excellent mechanical property, outstanding electrical and optical functional characteristics and the like, and becomes a research hotspot. The fabric is a material which is composed of fibers with layered structures and has special properties of high mechanical flexibility, strong air permeability, light weight, low bending stiffness, easy processing and the like. With the continued development of flexible electronics, conventional bulky or planar structures have failed to accommodate severe and complex deformations. In contrast, fabric structures offer unique and promising advantages. In order to meet the higher requirements of light weight, low cost, high flexibility, high air permeability, comfort, washability, suitability for complex deformation of various parts of human body and the like, strain sensors based on conductive fabrics are greatly developed.
The performance of a strain sensor is primarily dependent on the electromechanical properties of its conductive material. The carbon nano tube has the advantages of good flexibility, electrical conductivity, light weight, chemical stability, easiness in chemical functionalization and the like, and can effectively meet the application requirements of flexible wearable electronic products. At present, a conductive material prepared by combining a carbon material and a fabric is widely reported to be applied to a sensor, but the preparation mode and the material stability of the conductive material are still more improved. The CNT elastic knitted cotton fabric material was prepared in literature (Mengyun Yang, junjie Pan, achang Xu, lei Luo, deshan Cheng, guard Cai, jinfeng Wang, bin Tang, and Xungai Wang, polymers 2018,10,568-580) using a soak method, and the strain detection range of the conductive fabric material prepared by this method was 100%, however, the sensitivity thereof was only 1.82 under a large strain condition and the strain direction was single. The strain detection range of the highly elastic conductive knitted fabric prepared by the integrated knitting process is 100%, the sensitivity of which is extremely small and only 0.4 and only one-way strain is mentioned in the literature (Javad Foroughi, geoffrey M. Spinks, shazed Aziz, azadeh Mirabedini, ali Jeiranikhameneh, gordon G. Wallace, mikhail E.Kozlov, and Ray H.Baughman, ACS Nano 2016,10,9129-9135) by taking Spandex (SPX)/Carbon Nanotube (CNT) fabric yarns as raw materials. The document (Jeng-Hun Lee, jungmo Kim, dan Liu, fengmei Guo, xi Shen, qingbin Zheng, seokwoo Jeon, and Jang-Kyo Kim, advanced Functional Materials 2019,29,1901623-1901634) adopts an electrostatic spinning method to prepare an anisotropic carbon nanofiber film, the anisotropy of the carbon nanofiber film is used for distinguishing the direction and strength of strain, the anisotropy can be used for multidirectional strain, the sensitivity of the fiber film is 180 at maximum, but the stretchability is only 30%. It is therefore necessary to achieve a sensor based on novel textile materials, structural design with high stretchability, high sensitivity and multi-directionality.
In order to improve the sensing performance of the strain sensor and simplify the preparation method, the method is easy to operate, the method successfully coats SWCNT on the commercial cotton bandage to prepare the conductive fabric material by adopting a solution soaking method based on the multi-layer woven structure of the cotton bandage and the strong interaction of Van der Waals force and the like between the multi-layer woven structure and the carbon nano tube, and meanwhile, the advantages of comfort and good linear strain response of the fabric are avoided by adopting polymer encapsulation.
Disclosure of Invention
Aiming at the defects of the existing fabric-based strain sensor conductive material, the invention provides a preparation method which is simple, can realize a wide strain range and high stable cycle performance, and is suitable for preparing a nano conductive fabric material by depositing an SWCNT coated cotton bandage by a solution soaking method in industrialized mass production. The technical problems solved by the invention are as follows: a preparation method for preparing a flexible conductive fabric material by depositing and coating SWCNT (SWCNT) on a commercial cotton bandage by a solution soaking method comprises the following steps: a proper amount of surfactant Sodium Dodecyl Benzene Sulfonate (SDBS) is purchased from Shanghai A Ding Shenghua technology Co., ltd, added into a certain amount of deionized water, and mixed and stirred uniformly; then adding a certain proportion of single-wall carbon nanotubes (SWCNTs) to purchase the SWCNTs from Nanjing Xianfeng nanomaterial technologies, inc., and performing ultrasonic dispersion at normal temperature to obtain SWCNT dispersion; immersing the commercial cotton bandage into the dispersion liquid, and regulating the immersing times to 3 or 5 times for 3-8min to obtain the flexible conductive fabric of the SWCNT uniformly coated cotton bandages with different contents.
Preferably, the soaking time is 5min, and the soaking times are 3 times or 5 times.
Preferably, the commercial cotton bandage is a woven structure formed by twisting fibers into yarns.
Preferably, the SWCNT solution is a uniform dispersion, and the preparation method is as follows: 0.3g of SDBS is filled into a beaker, 60mL of deionized water is added, then the mixture is stirred for 30min under magnetic stirring, 0.03g of SWCNT is added into the beaker, and the mixture is subjected to ultrasonic dispersion for 8h and stirring for 24h at normal temperature, so that a uniform dispersion of the SWCNT is obtained.
Preferably, the SWCNT solution is transferred to a surface dish with a diameter of 12cm, a cotton bandage with a size of 6cm x 6cm is put into the surface dish, soaked for 5min at normal temperature, then washed with deionized water, dried for 5h in a vacuum drying oven at 60 ℃, and the soaking is repeated for 3 times or 5 times according to the above steps to prepare the conductive fabric.
Preferably, the mass ratio of SDBS to SWCNT used is 10:1; in preparing the SWCNT dispersion, the desired ultrasonic temperature and stirring temperature are controlled at room temperature.
The invention solves the technical problem that the proposed another technical scheme is as follows: a commercial cotton bandage prepared according to any of the above methods was deposited coated SWCNT conductive fabric material.
The invention solves the technical problem that the proposed another technical scheme is as follows: the application of the commercial cotton bandage deposition coated SWCNT conductive fabric material can be effectively applied to flexible strain sensors or stretchable conductors.
Preferably, the SWCNTs are coated on the cotton bandage to obtain flexible conductive cotton fabrics, and the SWCNTs deposited on the cotton bandage are different in quantity through different soaking times; after three times of soaking, the SWCNT is uniformly coated on the surface of the fabric, so that the fabric has good mechanical flexibility, a wide strain range, low strain detection limit and good cycling stability, and is suitable for flexible wearable electronic equipment; after four times of soaking, the conductivity is continuously enhanced; after five times of soaking, the SWCNT wrapped by the conductive cotton bandage has the saturated content, good conductivity, high stretchability and excellent mechanical stretching stability, and is suitable for flexible stretchable conductors.
Preferably, the material is used for a preparation method of a flexible strain sensor or a stretchable conductor, and the preparation method comprises the following steps: a. the flexible conductive fabric material which is soaked for three or five times and is uniformly coated with SWCNT in 6cm size is dried for more than or equal to 5 hours in a vacuum drying oven at 60 ℃;
b. cutting conductive fabric material into rectangular shape with uniform size of 1.7cm 0.6cm, connecting two ends with copper wires by using conductive silver adhesive to serve as electrodes, drying in a vacuum drying oven at 60deg.C for 3h, further coating a layer of transparent adhesive on the conductive silver adhesive to strengthen the electrodes, and continuously drying in the vacuum drying oven at 60deg.C for 3h. Thus, a flexible strain sensor was obtained, mechanical properties were tested on a universal materials tester (Shanghai wing precision instruments limited HY-0350), and current signals were collected by a digital current source (Keithley 2450), after which data collection was completed, plotted and analyzed by origin software.
The prepared conductive fabric is used as a strain sensor for testing, the voltage is 3V, and the 5000 times circulation stability is good.
The size of the sensor in the step b is 1.7cm long and 0.6cm wide.
The beneficial effects are that:
compared with other methods for preparing carbon material fabric structural materials, the method for preparing the conductive fabric is simple, the adopted solution soaking method is suitable for large-scale production, no harmful substances are generated in the preparation reaction process, and the method accords with the concept of green chemistry. The prepared conductive fabric has a wider strain detection range (0-150%), higher sensitivity (6) and good cycle stability (5000 cycles), and is superior to most of SWCNT coated fabric conductive materials reported at present; meanwhile, the multi-layer structure of the fabric can realize multi-directional test and application.
The invention relates to design preparation and application of a commercial Cotton Bandage (CB) solution method deposited single-walled carbon nanotube (SWCNT) conductive fabric material. Adding SWCNT into a Sodium Dodecyl Benzene Sulfonate (SDBS) solution serving as a surfactant, fully stirring and mixing at room temperature, and performing ultrasonic dispersion to obtain a uniform SWCNT dispersion. And immersing CB in the dispersion liquid, and preparing the conductive fabric uniformly coated by SWCNT by a solution immersing method. The strong interaction between the SDBS and the SWCNTs can cause the SWCNTs to be uniformly dispersed and coated on the surface of the CB to become a part of the CB. The multilayer braid structure of CB is advantageous for maximizing adsorption of SWCNT while achieving resistance response in different strain directions. Wherein, when soaked for three times, the conductive bandage has good mechanical flexibility, wider strain response range, low strain detection limit, good cycling stability, washability and the like; when soaked for five times, the conductive bandage has good conductivity, high stretchability, excellent mechanical stretching stability and the like. The method for obtaining the conductive fabric material by the solution soaking method has the advantages of simple preparation process, low production cost, easy industrial scale and the like, and can be widely applied to flexible multidirectional strain sensors and elastic stretchable conductors.
The unique twisting and layering structure of the commercial cotton bandage increases the strain detection range, has the advantages of light weight, strong air permeability and the like, and can effectively improve the strain circulation stability of the conductive fabric due to the conductive path provided by the SWCNT and the strong force of the SWCNT and the cotton bandage. The woven layered structure is beneficial to coating the active material on the fabric, can realize that the electronic fabric is worn without any supporting substrate, is environment-friendly, has simple preparation process, and is suitable for large-scale production of flexible strain sensors.
The flexible conductive fabric can obtain SWCNTs with different deposition amounts on the commercial cotton bandage through different soaking times. After one and two times of soaking, the SWCNT is coated unevenly, and the conductivity is poor; after three times of soaking, the SWCNT is uniformly coated, has good conductivity and is suitable for flexible electronic materials; after four times of soaking, the conductivity is continuously enhanced; after five times of soaking, the SWCNT wrapped by the conductive cotton bandage reaches a saturated state, and is suitable for flexible and stretchable conductors. Demonstration of the combination examples this patent determines the optimal conditions for the preparation of a strain sensor when immersed three times, under which the conductive fabric has a wide strain sensing range, multidirectional response and high cycling stability; meanwhile, the conductive fabric is the optimal preparation condition of the stretchable conductor when soaked for five times, and the conductive fabric still has excellent conductivity under different deformation and good mechanical stretching stability under the condition.
The cotton bandage prepared by the experiment is deposited and coated with SWCNT for three times, the soaking time is 5 min/time, the prepared conductive fabric material can bear larger deformation, relatively higher sensitivity is obtained after the test is applied to a sensor, the strain range can be up to 150%, the relative resistance change is large, the cycling stability is good, meanwhile, the cotton bandage has multiple directions, can be used for detecting subtle and severe multidirectional movements of human beings, and shows great potential in the application of wearable electronic products.
The preparation method is basically the same as that of example 3, except that the performance test of the conductive fabric material prepared by coating SWCNT by deposition of a commercial cotton bandage (soaking three times for 3min and 8 min) is not greatly different from the performance test of the conductive fabric material prepared in example 3 (soaking three times for 5 min), can bear larger deformation, and the strain range obtained after the test is applied to a sensor is wider, the cycling stability is good, the fluctuation range of sensitivity is small, and the difference of relative resistance change is not great.
The cotton bandage prepared by the experiment is coated for five times in a deposition way, the soaking time is 5 min/time, the prepared conductive fabric has high conductivity (resistance: 12 omega), excellent flexibility (deformation such as stretching, bending and torsion), strong stretchability (strain range: 150%), and excellent mechanical stretching stability, and the stretchable conductor can be used in the intelligent fields such as wearable equipment due to the super elasticity.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a scanning electron microscope image of a cotton bandage of example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of a commercial cotton bandage deposited coated SWCNT after three dips in example 3 of the present invention;
FIG. 3 is a Raman image of a commercial cotton bandage deposited coated SWCNT after three dips in example 3 of the present invention;
FIG. 4 is a graph showing the performance of strain sensors of SWCNT wrapped cotton bandages with varying numbers of dips in example 1 of the present invention, wherein the relative resistance changes ΔR/R 0 (ΔR＝R-R 0 R is instantaneous resistance, R 0 Initial resistance), sensitivity (GF= (DeltaR/R) 0 )/ε，ε＝L-L 0 /L 0 Length after stretching L 0 Initial length);
FIG. 5 is a graph showing the change in resistance response of a conductive fabric material coated with SWCNTs deposited on a commercial cotton bandage after three times of soaking in example 3 of the present invention under different strain conditions at the same frequency;
FIG. 6 is a stability test of a commercial cotton bandage deposition coated SWCNT strain sensor after three dips in example 3 of the present invention;
FIG. 7 is a multi-directional test of the conductive material deposited over SWCNT with a commercial cotton bandage after three dips in example 3 of the present invention (left: vertical elastic fabric orientation; right: network weave structure angle 45 °);
FIG. 8 is a response signal for monitoring different fingers of a human body in a bending state in embodiment 3 of the present invention;
FIG. 9 is a tensile conductor test of a conductive material coated with SWCNT deposited with a commercial cotton bandage after five times of soaking in example 5 of the present invention in a deformed state such as stretched, bent, twisted, etc.;
FIG. 10 is a tensile and mechanical tensile stability test of a stretchable conductor of the conductive material of the commercial cotton bandage deposited coated SWCNTs after five dips in example 5 of the present invention;
Detailed Description
The technical solution of the present invention will be further described with reference to examples, which should not be construed as limiting the technical solution.
1. Preparation of SWCNT solutions
And adding a proper amount of surfactant Sodium Dodecyl Benzene Sulfonate (SDBS) into a proper amount of deionized water, and uniformly mixing and stirring. Then adding a certain proportion of single-wall carbon nano tube (SWCNT), mixing, performing ultrasonic dispersion for 8 hours at normal temperature, and stirring for 24 hours to obtain SWCNT dispersion liquid.
2. Application of SWCNT (SWCNT) coated cotton bandage to preparation of sensor conductive material
The SWCNT dispersion is transferred to a 12cm diameter surface dish, a 6cm x 6cm size cotton bandage is placed in the surface dish, soaked for 5min at normal temperature, then washed with deionized water, dried for 5h in a vacuum drying oven at 60 ℃ and repeatedly operated for three times.
3. Application of SWCNT (SWCNT) coated cotton bandage to preparation of stretchable conductor conductive material
The SWCNT dispersion was transferred to a 12cm diameter petri dish, a 6cm x 6cm size cotton bandage was placed in the petri dish, soaked for 5min at room temperature, then washed with deionized water, dried in a vacuum oven at 60℃for 5h, and the operation was repeated five times.
4. Application of SWCNT (SWCNT) coated cotton bandage to preparation of sensor or stretchable conductor
Cutting the conductive fabric material by scissors, cutting the conductive fabric material into rectangular shapes with the size of 1.7cm and 0.6cm, connecting two ends of the conductive fabric material with copper wires to serve as electrodes by using conductive silver adhesive, drying the electrodes in a vacuum drying oven at 60 ℃ for 3 hours, further coating a layer of transparent adhesive on the conductive silver adhesive to strengthen the electrodes, and drying the electrodes in the vacuum drying oven at 60 ℃ for 3 hours.
Example 1
0.3g of SDBS is filled into a beaker, 60mL of deionized water is added, then the mixture is stirred for 30min under magnetic stirring, 0.03g of SWCNT is added into the beaker, and the mixture is subjected to ultrasonic dispersion for 8h and stirring for 24h at normal temperature, so that a uniform dispersion of the SWCNT is obtained.
The SWCNT solution was transferred to a 12cm diameter petri dish, a 6cm x 6cm size cotton bandage was placed in the petri dish, soaked for 5min at normal temperature, then washed with deionized water, and dried in a vacuum oven at 60 ℃ for 5h.
Cutting the conductive fabric into the same length (length 1.7cm, width 0.6 cm) according to the woven hierarchical structure, connecting two ends with copper wires through conductive silver adhesive to serve as electrodes, drying, coating a transparent adhesive fixed electrode, performing mechanical property test on a universal material tester (HY-0350 of Shanghai scale wing precision instruments Co., ltd.), collecting current signals by a current source (Keithley 2450), and performing drawing and analysis by an origin software after data collection.
The sensor has extremely poor conductivity, extremely small strain detection range, and failure of the conductive path in the strain process and disconnection.
Example 2
0.3g of SDBS is filled into a beaker, 60mL of deionized water is added, then the mixture is stirred for 30min under magnetic stirring, 0.03g of SWCNT is added into the beaker, and the mixture is sonicated for 8h and stirred for 24h at normal temperature, thus obtaining a uniform dispersion of SWCNT.
The SWCNT solution was transferred to a 12cm diameter petri dish, a 6cm x 6cm size cotton bandage was placed in the petri dish, soaked for 5min at normal temperature, then washed with deionized water, and dried in a vacuum oven at 60 ℃ for 5h. And (3) repeatedly soaking for two times according to the steps to prepare the conductive fabric.
Cutting the conductive fabric into the same length (length 1.7cm, width 0.6 cm) according to the woven hierarchical structure, connecting two ends with copper wires through conductive silver adhesive to serve as electrodes, drying, coating a transparent adhesive fixed electrode, performing mechanical property test on a universal material tester (HY-0350 of Shanghai scale wing precision instruments Co., ltd.), collecting current signals by a current source (Keithley 2450), and performing drawing and analysis by an origin software after data collection.
The sensor exhibits a very small strain detection range, and the conductive path is unstable during strain.
Example 3
0.3g of SDBS is filled into a beaker, 60mL of deionized water is added, then the mixture is stirred for 30min under magnetic stirring, 0.03g of SWCNT is added into the beaker, and the mixture is subjected to ultrasonic dispersion for 8h and stirring for 24h at normal temperature, so that a uniform dispersion of the SWCNT is obtained.
The SWCNT solution was transferred to a 12cm diameter petri dish, a 6cm x 6cm size cotton bandage was placed in the petri dish, soaked for 5min at normal temperature, then washed with deionized water, and dried in a vacuum oven at 60 ℃ for 5h. According to the steps, the conductive fabric is prepared by repeatedly soaking for three times.
Cutting the conductive fabric into the same length (length 1.7cm, width 0.6 cm) according to the woven hierarchical structure, connecting two ends with copper wires through conductive silver adhesive to serve as electrodes, drying, coating a transparent adhesive fixed electrode, carrying out mechanical property test on the transparent adhesive fixed electrode, collecting current signals by a current source, and carrying out drawing and analysis by origin software after data collection.
The sensor shows a wide detection range (0-150%), excellent cycle stability (5000 cycles), high sensitivity (gf=6), and other excellent properties. Meanwhile, multi-direction test can be carried out, and the strain in the direction vertical to the elastic fabric can reach 5%; the strain range of the network braiding structure in the 45-degree direction can reach 110%.
Example 4
0.3g of SDBS is filled into a beaker, 60mL of deionized water is added, then the mixture is stirred for 30min under magnetic stirring, 0.03g of SWCNT is added into the beaker, and the mixture is subjected to ultrasonic dispersion for 8h and stirring for 24h at normal temperature, so that a uniform dispersion of the SWCNT is obtained.
The SWCNT solution was transferred to a 12cm diameter petri dish, a 6cm x 6cm size cotton bandage was placed in the petri dish, soaked for 5min at normal temperature, then washed with deionized water, and dried in a vacuum oven at 60 ℃ for 5h. The conductive fabric is prepared by repeatedly soaking four times according to the steps.
Cutting the conductive fabric into the same length (length 1.7cm, width 0.6 cm) according to the woven hierarchical structure, connecting two ends with copper wires through conductive silver adhesive to serve as electrodes, drying, coating a transparent adhesive fixed electrode, carrying out mechanical property test on the transparent adhesive fixed electrode, collecting current signals by a current source, and carrying out drawing and analysis by origin software after data collection.
The sensor exhibits a large strain detection range, and the conductive path is stable during strain, whereas the resistance response value becomes small.
Example 5
0.3g of SDBS is filled into a beaker, 60mL of deionized water is added, then the mixture is stirred for 30min under magnetic stirring, 0.03g of SWCNT is added into the beaker, and the mixture is subjected to ultrasonic dispersion for 8h and stirring for 24h at normal temperature, so that a uniform dispersion of the SWCNT is obtained.
The SWCNT solution was transferred to a 12cm diameter petri dish, a 6cm x 6cm size cotton bandage was placed in the petri dish, soaked for 5min at normal temperature, then washed with deionized water, and dried in a vacuum oven at 60 ℃ for 5h. The conductive fabric is prepared by repeatedly soaking for five times according to the steps.
Cutting the conductive fabric into the same length (length 1.7cm, width 0.6 cm) according to the woven hierarchical structure, connecting two ends with copper wires through conductive silver adhesive to serve as electrodes, drying, coating a transparent adhesive fixed electrode, carrying out mechanical property test on the transparent adhesive fixed electrode, collecting current signals by a current source, and carrying out drawing and analysis by origin software after data collection.
The conductive fabric reaches a saturated state, the conductive path is stable in the strain process, the stretchable conductor shows a larger detection range (0-150%), the brightness of the LED lamp does not change in the deformation (stretching, bending and torsion) process, the stretching property and the mechanical stretching stability are excellent (the conductive fabric can be circularly stable 5000 times when the strain is 10%,30%,50%,70% and 90%), and the conductive fabric can be used for the stretchable conductor.
Example 6
0.3g of SDBS is filled into a beaker, 60mL of deionized water is added, then the mixture is stirred for 30min under magnetic stirring, 0.03g of SWCNT is added into the beaker, and the mixture is subjected to ultrasonic dispersion for 8h and stirring for 24h at normal temperature, so that a uniform dispersion of the SWCNT is obtained.
The SWCNT solution was transferred to a 12cm diameter petri dish, a 6cm x 6cm size cotton bandage was placed in the petri dish, soaked for 1min at normal temperature, then washed with deionized water, and dried in a vacuum oven at 60 ℃ for 5h. According to the steps, the conductive fabric is prepared by repeatedly soaking for three times.
Cutting the conductive fabric into the same length (length 1.7cm, width 0.6 cm) according to the woven hierarchical structure, connecting two ends with copper wires through conductive silver adhesive to serve as electrodes, drying, coating a transparent adhesive fixed electrode, carrying out mechanical property test on the transparent adhesive fixed electrode, collecting current signals by a current source, and carrying out drawing and analysis by origin software after data collection.
The sensor exhibits a small strain detection range, and the conductive path fails during the strain to form an open circuit condition.
Example 7
0.3g of SDBS is filled into a beaker, 60mL of deionized water is added, then the mixture is stirred for 30min under magnetic stirring, 0.03g of SWCNT is added into the beaker, and the mixture is subjected to ultrasonic dispersion for 8h and stirring for 24h at normal temperature, so that a uniform dispersion of the SWCNT is obtained.
The SWCNT solution was transferred to a 12cm diameter petri dish, a 6cm x 6cm size cotton bandage was placed in the petri dish, soaked for 10min at normal temperature, then washed with deionized water, and dried in a vacuum oven at 60 ℃ for 5h. According to the steps, the conductive fabric is prepared by repeatedly soaking for three times.
Cutting the conductive fabric into the same length (length 1.7cm, width 0.6 cm) according to the woven hierarchical structure, connecting two ends with copper wires through conductive silver adhesive to serve as electrodes, drying, coating a transparent adhesive fixed electrode, carrying out mechanical property test on the transparent adhesive fixed electrode, collecting current signals by a current source, and carrying out drawing and analysis by origin software after data collection.
The sensor exhibits a large strain detection range, with a stable conductive path during strain, but a small resistance response.
Example 8
0.3g of SDBS is filled into a beaker, 60mL of deionized water is added, then the mixture is stirred for 30min under magnetic stirring, 0.03g of SWCNT is added into the beaker, and the mixture is subjected to ultrasonic dispersion for 8h and stirring for 24h at normal temperature, so that a uniform dispersion of the SWCNT is obtained.
The SWCNT solution was transferred to a 12cm diameter petri dish, a 6cm x 6cm size cotton bandage was placed in the petri dish, soaked for 1min at normal temperature, then washed with deionized water, and dried in a vacuum oven at 60 ℃ for 5h. The conductive fabric is prepared by repeatedly soaking for five times according to the steps.
Cutting the conductive fabric into the same length (length 1.7cm, width 0.6 cm) according to the woven hierarchical structure, connecting two ends with copper wires through conductive silver adhesive to serve as electrodes, drying, coating a transparent adhesive fixed electrode, carrying out mechanical property test on the transparent adhesive fixed electrode, collecting current signals by a current source, and carrying out drawing and analysis by origin software after data collection.
The stretchable conductor shows a large strain detection range, the conductive path is stable during strain, however, the conductivity is poor, the conductive fabric does not reach a saturated state, and the conductive fabric cannot be used for the stretchable conductor.
Example 9
0.3g of SDBS is filled into a beaker, 60mL of deionized water is added, then the mixture is stirred for 30min under magnetic stirring, 0.03g of SWCNT is added into the beaker, and the mixture is subjected to ultrasonic dispersion for 8h and stirring for 24h at normal temperature, so that a uniform dispersion of the SWCNT is obtained.
The SWCNT solution was transferred to a 12cm diameter petri dish, a 6cm x 6cm size cotton bandage was placed in the petri dish, soaked for 10min at normal temperature, then washed with deionized water, and dried in a vacuum oven at 60 ℃ for 5h. The conductive fabric is prepared by repeatedly soaking for five times according to the steps.
Cutting the conductive fabric into the same length (length 1.7cm, width 0.6 cm) according to the woven hierarchical structure, connecting two ends with copper wires through conductive silver adhesive to serve as electrodes, drying, coating a transparent adhesive fixed electrode, carrying out mechanical property test on the transparent adhesive fixed electrode, collecting current signals by a current source, and carrying out drawing and analysis by origin software after data collection.
The stretchable conductor shows a larger strain detection range, the conductivity is good, the conductive fabric reaches a supersaturation state, but the conductive material can fall off during the test process, so that a conductive path is unstable during the strain process, and the conductive fabric cannot be used for the stretchable conductor.
Example 10
0.3g of SDBS is filled into a beaker, 60mL of deionized water is added, then the mixture is stirred for 30min under magnetic stirring, 0.03g of SWCNT is added into the beaker, and the mixture is subjected to ultrasonic dispersion for 8h and stirring for 24h at normal temperature, so that a uniform dispersion of the SWCNT is obtained.
The SWCNT solution was transferred to a 12cm diameter petri dish, a 6cm x 6cm size cotton bandage was placed in the petri dish, soaked for 3min at normal temperature, then washed with deionized water, and dried in a vacuum oven at 60 ℃ for 5h. According to the steps, the conductive fabric is prepared by repeatedly soaking for three times.
Cutting the conductive fabric into the same length (length 1.7cm, width 0.6 cm) according to the woven hierarchical structure, connecting two ends with copper wires through conductive silver adhesive to serve as electrodes, drying, coating a transparent adhesive fixed electrode, carrying out mechanical property test on the transparent adhesive fixed electrode, collecting current signals by a current source, and carrying out drawing and analysis by origin software after data collection.
The sensor can bear larger deformation, and the strain range obtained after the sensor is applied to the sensor is smaller through testing, so that the cycling stability is better.
Example 11
0.3g of SDBS is filled into a beaker, 60mL of deionized water is added, then the mixture is stirred for 30min under magnetic stirring, 0.03g of SWCNT is added into the beaker, and the mixture is subjected to ultrasonic dispersion for 8h and stirring for 24h at normal temperature, so that a uniform dispersion of the SWCNT is obtained.
The SWCNT solution was transferred to a 12cm diameter petri dish, a 6cm x 6cm size cotton bandage was placed in the petri dish, soaked for 8min at normal temperature, then washed with deionized water, and dried in a vacuum oven at 60 ℃ for 5h. According to the steps, the conductive fabric is prepared by repeatedly soaking for three times.
Cutting the conductive fabric into the same length (length 1.7cm, width 0.6 cm) according to the woven hierarchical structure, connecting two ends with copper wires through conductive silver adhesive to serve as electrodes, drying, coating a transparent adhesive fixed electrode, carrying out mechanical property test on the transparent adhesive fixed electrode, collecting current signals by a current source, and carrying out drawing and analysis by origin software after data collection.
The sensor shows larger deformation, and the strain range obtained after the sensor is applied to the sensor is wider through testing, so that the cycling stability is good.
Example 12
0.6g of SDBS is filled into a beaker, 60mL of deionized water is added, then the mixture is stirred for 30min under magnetic stirring, 0.06g of SWCNT is added into the beaker, and the mixture is subjected to ultrasonic dispersion for 8h and stirring for 24h at normal temperature, so that a uniform dispersion of the SWCNT is obtained.
The SWCNT solution was transferred to a 12cm diameter petri dish, a 6cm x 6cm size cotton bandage was placed in the petri dish, soaked for 5min at normal temperature, then washed with deionized water, and dried in a vacuum oven at 60 ℃ for 5h. According to the steps, the conductive fabric is prepared by repeatedly soaking for three times.
Cutting the conductive fabric into the same length (length 1.7cm, width 0.6 cm) according to the woven hierarchical structure, connecting two ends with copper wires through conductive silver adhesive to serve as electrodes, drying, coating a transparent adhesive fixed electrode, carrying out mechanical property test on the transparent adhesive fixed electrode, collecting current signals by a current source, and carrying out drawing and analysis by origin software after data collection.
The conductive fabric shows a larger strain detection range, has good conductivity, and has smaller resistance response change in the strain process.
Example 12
0.6g of SDBS is filled into a beaker, 60mL of deionized water is added, then the mixture is stirred for 30min under magnetic stirring, 0.06g of SWCNT is added into the beaker, and the mixture is subjected to ultrasonic dispersion for 8h and stirring for 24h at normal temperature, so that a uniform dispersion of the SWCNT is obtained.
The SWCNT solution was transferred to a 12cm diameter petri dish, a 6cm x 6cm size cotton bandage was placed in the petri dish, soaked for 5min at normal temperature, then washed with deionized water, and dried in a vacuum oven at 60 ℃ for 5h. The conductive fabric is prepared by repeatedly soaking for five times according to the steps.
Cutting the conductive fabric into the same length (length 1.7cm, width 0.6 cm) according to the woven hierarchical structure, connecting two ends with copper wires through conductive silver adhesive to serve as electrodes, drying, coating a transparent adhesive fixed electrode, carrying out mechanical property test on the transparent adhesive fixed electrode, collecting current signals by a current source, and carrying out drawing and analysis by origin software after data collection.
The stretchable conductor shows a large strain detection range and high conductivity, and the conductive fabric reaches a supersaturation state, but the conductive material can fall off in strain testing, so that a conductive path is unstable in the strain process, and the conductive fabric cannot be used for the stretchable conductor.
The conductive fabric material prepared by depositing and coating the SWCNT on the commercial cotton bandage in example 3 can reach a strain detection range of 150%, has high sensitivity (gf=6), has a cyclic stability of 5000 times, can perform multi-directional test, has a simple preparation process, and is more suitable for mass production.
The conductive fabric material prepared by depositing the coated SWCNT on the commercial cotton bandage of example 5 can be used as a drawn conductor, and can be drawn by 150%, and has 5000 cycles stability, and can be applied to various deformations (drawing, bending, torsion, etc.).
The preparation method is basically the same as that of example 3, except that the performance test of the conductive fabric material prepared by coating SWCNT by deposition of a commercial cotton bandage (soaking three times for 3min and 8 min) is not greatly different from the performance test of the conductive fabric material prepared in example 3 (soaking three times for 5 min), can bear larger deformation, and the strain range obtained after the test is applied to a sensor is wider, the cycling stability is good, the fluctuation range of sensitivity is small, and the difference of relative resistance change is not great.
The invention is not limited to the specific technical solutions described in the above embodiments, and all technical solutions formed by adopting equivalent substitution are the protection scope of the invention.
Claims (1)
1. A preparation method for preparing a flexible conductive fabric material for a flexible strain sensor by depositing and coating SWCNT (SWCNT) on a commercial cotton bandage through a solution soaking method is characterized by comprising the following steps of:
the preparation of the flexible conductive fabric material comprises the following steps: filling 0.3g sodium dodecyl benzene sulfonate SDBS into a beaker, adding 60mL deionized water, stirring for 30min under magnetic stirring, adding 0.03g single-walled carbon nanotube SWCNT into the beaker, performing ultrasonic dispersion at normal temperature for 8h, and stirring for 24h to obtain SWCNT uniform dispersion; transferring SWCNT solution into 12cm diameter surface dish, placing 6cm ×6cm commercial cotton bandage into the surface dish, soaking at room temperature for 5min, washing with deionized water, washing with water, and washing with deionized water, washing with high temperature, and concentrating o Drying 5h in a vacuum drying oven, repeatedly soaking for three times according to the steps to prepare a conductive fabric, wherein the commercial cotton bandage is formed by twisting fibers into yarns and forming a woven structure;
the preparation method of the flexible conductive fabric material for the flexible strain sensor comprises the following steps:
cutting the conductive fabric into the same length of 1.7cm and width of 0.6cm according to the woven layered structure, connecting the two ends with copper wires by using conductive silver paste to serve as electrodes, and then at 60 oC Drying 3h in vacuum drying oven, further coating transparent adhesive on conductive silver gel to strengthen electrode, continuing at 60 oC Drying 3h in a vacuum drying oven, thus obtaining a flexible strain sensor, testing the mechanical property of the flexible strain sensor, collecting current signals by a current source, and drawing and analyzing by origin software after data collection is completed;
the flexible strain sensor has a wider detection range of 0-150%, excellent cycle stability of 5000 cycles and high sensitivity GF=6, and can perform multi-direction test, and the strain in the direction perpendicular to the elastic fabric can reach 5%; the strain range of the network braiding structure in the 45-degree direction can reach 110%.
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| CN107887181A (en) * | 2017-11-16 | 2018-04-06 | 东华大学 | A kind of preparation method of cotton base carbon fibre flexible electrode |
| CN107988787A (en) * | 2017-12-19 | 2018-05-04 | 安徽工程大学 | A kind of preparation method for inhaling wave mode Electromagnetically shielding fabrics |
| CN110983532A (en) * | 2019-11-25 | 2020-04-10 | 武汉纺织大学 | Preparation method of spiral yarn with sensing and capacitance characteristics |
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| CN107887181A (en) * | 2017-11-16 | 2018-04-06 | 东华大学 | A kind of preparation method of cotton base carbon fibre flexible electrode |
| CN107988787A (en) * | 2017-12-19 | 2018-05-04 | 安徽工程大学 | A kind of preparation method for inhaling wave mode Electromagnetically shielding fabrics |
| CN110983532A (en) * | 2019-11-25 | 2020-04-10 | 武汉纺织大学 | Preparation method of spiral yarn with sensing and capacitance characteristics |
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