CN112941661B - High-tensile high-sensitivity piezoresistive fiber and preparation method and application thereof - Google Patents
High-tensile high-sensitivity piezoresistive fiber and preparation method and application thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
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Abstract
The invention discloses a high-tensile high-sensitivity piezoresistive fiber and a preparation method and application thereof. The method comprises the following steps: dispersing a carboxylated conductive filler into a thermoplastic polyurethane solution, and adding a certain amount of ammonia water to obtain a spinning solution; extruding the spinning solution into a coagulating bath containing a metal precursor through wet spinning to generate non-solvent induced phase transition, and substituting ammonium ions in the spinning solution by metal ions to obtain porous fibers containing the metal ions; and reducing to obtain the porous fiber containing the metal nano particles and the multidimensional synergic conductive network. The porous fiber shows high conductivity, high stretchability, and high responsiveness to compression set, and can be used as a highly stable, highly sensitive piezoresistive fiber. The porous fiber prepared by the invention has high pore density, adjustable pore size distribution and conductivity, and the preparation method is simple and feasible and can realize large-scale production. The method has wide application prospect in the fields of health monitoring, human-computer interaction, intelligent robots, electromagnetic shielding, thermoelectric materials and the like.
Description
Technical Field
The invention belongs to the field of piezoresistive sensing fibers, and particularly relates to a high-tensile high-sensitivity piezoresistive fiber and a preparation method and application thereof.
Background
Thermoplastic Polyurethane (TPU) contains soft and hard segments in its molecular chain, which imparts excellent flexibility and elasticity, good impact resistance, abrasion resistance, weather resistance, and the like. TPUs can be processed by melt processing, such as extrusion, blow molding, injection molding, and the like. Because of their many advantages and suitability for various processing techniques, TPU is widely used in the fields of automobiles, medicine, sporting goods, aerospace, electronics, and the like.
The porous fiber has the characteristics of large length-diameter ratio, low density, high specific surface area and the like, and the interconnected porous structures are favorable for loading and releasing molecular objects. So that the porous fiber has important application in energy storage and conversion, adsorption, separation, electromagnetic shielding and biological material. In addition, the three-dimensional porous fiber can be used as a high-performance flexible pressure sensor due to excellent mechanical compression and rebound resilience.
The traditional method for preparing the conductive composite material is to directly blend the conductive filler and the elastomer, and the prepared conductive composite material is poor in flexibility due to the problem that the filler is easy to agglomerate, so that the use of the conductive composite material is greatly limited. In order to solve the problem, one-dimensional nano materials with high conductivity and high length-diameter ratio, such as carbon nano tubes or silver nano wires, are added into elastomers such as silicon rubber and polyurethane, and a conductive network formed by the one-dimensional nano materials is utilized, so that the flexibility of the elastomer is kept by reducing the filling amount of the conductive filler as much as possible while the good conductivity is kept, but the single filler has great defects in reducing the using amount of the filler. The preparation of high-tensile and high-stability conductive composite materials is still an important problem to be solved urgently.
Fiber-type strain sensors are more easily integrated into fabrics than film-type strain sensors. In addition, the fiber has excellent flexibility, can be tightly attached to a human body to do complex actions, the fiber in the fabric can not generate crack propagation of a solid film or a block, the long-term use of the fabric can be improved, and the fabric is breathable, meets the comfortable feeling of long-term wearing, and is an ideal platform of a high-performance wearable flexible sensor. However, the current piezoresistive fiber has the problems of low sensitivity and poor conductivity caused by stretching in the use process, and the practical application of the piezoresistive fiber is greatly limited.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a preparation method of a high-tensile and high-sensitivity piezoresistive fiber.
According to the invention, the multi-dimensional synergetic conductive network containing metal nanoparticles is prepared by a chemical reduction method, and the porous fiber with adjustable pore diameter is subjected to wet spinning based on the non-solvent induced phase transition principle, so that the conductivity of the piezoresistive fiber in a high tensile state is improved, the problems of poor conductive stability, low sensitivity and the like of a piezoresistive sensing material during tensile are well solved, the wearable characteristic of a flexible sensor is further endowed, and further support is provided for the practical application of the material.
The invention also aims to provide a high-tensile high-sensitivity piezoresistive fiber prepared by the method.
The invention further aims to provide application of the high-tensile high-sensitivity piezoresistive fiber in electronic textiles and intelligent wearable electronic equipment.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a high-tensile high-sensitivity piezoresistive fiber comprises the following steps:
(1) Dispersing a carboxylated conductive filler into a thermoplastic polyurethane solution, and adding a certain amount of ammonia water to obtain a spinning solution;
(2) Extruding the spinning solution obtained in the step (1) into a coagulating bath containing a metal precursor through wet spinning, standing for a period of time, so that a solvent in the coagulating bath and a solvent in the spinning solution are exchanged with each other, the solvent in the spinning solution is extracted in the diffusion process, the thermoplastic polyurethane is gradually solidified, meanwhile, a solution with metal ions enters the fibers, and the metal ions replace ammonium ions and are loaded on the fibers to obtain the fibers loaded with the metal ions;
(3) Drying the fiber loaded with the metal ions in the step (2) to obtain porous composite fiber loaded with the metal ions;
(4) And (4) reducing the porous composite fiber loaded with the metal ions in the step (3) to reduce the metal ions into metal nano particles, cleaning and drying to obtain the porous piezoresistive fiber.
Preferably, the carboxylated conductive filler in the step (1) is at least one of one-dimensional carboxylated carbon nanotube, two-dimensional carboxylated graphene and two-dimensional carboxylated MXene.
More preferably, the carboxylated conductive filler is a one-dimensional carboxylated carbon nanotube and a two-dimensional carboxylated graphene and/or two-dimensional carboxylated MXene mixture, wherein the mass ratio of the one-dimensional filler to the two-dimensional filler is 1.
Preferably, the mass ratio of the carboxylated conductive filler to the thermoplastic polyurethane in the step (1) is 0.1-5: 15 to 40
Preferably, the mass concentration of the thermoplastic polyurethane solution in the step (1) is 15-40%.
Preferably, the solvent of the thermoplastic polyurethane solution in the step (1) is at least one of N, N-dimethylformamide, tetrahydrofuran, acetone and dimethyl sulfoxide.
Preferably, the pH of the mixed solution after adding the ammonia water in the step (1) is 11-14.
Preferably, the metal in the coagulation bath of the metal-containing precursor in the step (2) is at least one of copper and silver; the metal precursor is silver trifluoroacetate (AgCOOF) 3 ) Copper trifluoroacetate (Cu (COOF) 3 ) 2 ) And copper acetate.
Preferably, the solvent of the coagulation bath containing the metal precursor in the step (2) is at least one of water, methanol, ethanol and isopropanol. More preferably, the solvent of the coagulation bath containing the metal precursor is water and one of isopropanol, methanol and ethanol in a volume ratio of 1:4 to 4: 1.
Preferably, the mass concentration of the metal precursor in the coagulating bath containing the metal precursor in the step (2) is 5-30 wt%.
Preferably, the standing time of the step (2) is at least 30min; more preferably 30min to 12h.
Preferably, the drying temperature in the step (3) is 25-60 ℃ and the time is 8-24 h.
Preferably, the reduction treatment in step (4) is: the porous composite fiber loaded with metal ions is placed in hydrazine hydrate steam or hydroiodic acid steam at the temperature of 70-100 ℃ for 5 min-1 h.
More preferably, the concentration of the hydrazine hydrate steam or the hydroiodic acid steam is 1 to 10g/m 3 。
The piezoresistive fiber with high tensile and high sensitivity is prepared by the method.
The piezoresistive fiber shows high conductivity, high stretchability, and high responsiveness to compression set, and can be used as a highly stable, highly sensitive piezoresistive fiber.
The application of the high-tensile high-sensitivity piezoresistive fiber in electronic textiles and intelligent wearable equipment is provided.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1) By constructing a 0D/1D, 0D/2D and 0D/1D/2D multi-dimensional cooperative network, the adding amount of the filler is greatly reduced, the influence of the filler on the flexibility of the material is avoided, and the problem of fiber tensile property reduction caused by adding the filler in the prior art is improved; the carboxyl treated conductive filler is beneficial to dispersion in a polymer solution, the 0D metal nanoparticles are introduced by utilizing the fact that the bonding force of metal ions and carboxylate radicals is larger than that of ammonium radicals and carboxylate radicals, the metal ions replace the ammonium radicals and the carboxylate radicals to form a new complex, and the reduced metal nanoparticles can be uniformly distributed in fibers, so that the damage of the metal nanoparticles to the flexibility of the material is avoided; in addition, when the piezoresistive sensing fiber is stretched at high tension, the multidimensional fillers are mutually bridged, and the conductivity of the fiber under high tension is ensured by the synergistic effect.
2) The porous polyurethane fiber is equivalent to a three-dimensional porous framework built in the polyurethane, and the conductive filler is coated or embedded in the three-dimensional porous framework; when the two lapped conductive porous structures are subjected to external pressure, the contact degree of the inner hole walls of the fibers and the change of the contact area of the fibers can be quickly caused, so that the conductive path is changed, and the purpose of sensing is achieved; the introduction of a porous structure can greatly weaken the hysteresis viscoelastic behavior of polyurethane, increase the sensitivity of the polyurethane, reduce the response time and the relaxation time and greatly improve the sensing performance; when the porous conductive fiber is stretched, the fiber is contracted in the radial direction due to the poisson's ratio, and the conductive fillers in the pores are contacted with each other, thereby ensuring the conductive stability in a high-stretching state.
3) The prepared piezoresistive fiber is a one-dimensional elastic fiber, is more fine and convenient to carry, can be processed into various shapes more conveniently, for example, a two-dimensional electronic fabric is prepared by weaving, and meanwhile, the fiber has excellent skin adhesion and air permeability, so that the piezoresistive fiber has a wide application prospect in intelligent wearable equipment.
4) The porous fiber prepared by the invention has high pore density, adjustable pore size distribution and conductivity, and the preparation method is simple and feasible and can realize large-scale production.
Drawings
FIG. 1 is a cross-section of a porous composite fiber prepared by using coagulation baths prepared from water and isopropanol in different volume ratios in example 4.
FIG. 2 is a comparison of the elongation at break of porous composite fibers prepared from coagulation baths formulated with different volume ratios of water and isopropanol in example 4.
FIG. 3 is the electron microscope image of piezoresistive fibers after reduction in example 1.
FIG. 4 is a stress-strain curve of piezoresistive fibers prepared in example 2.
FIG. 5 is a graph comparing the stability of electrical conductivity when solid conductive fibers made in comparative example 1 using acetone as a coagulation bath and piezoresistive fibers made in example 3 were drawn.
FIG. 6 shows the coagulation bath of example 4 as water: isopropanol =2:3, the two piezoresistive fibers prepared by the method have the compressive sensing performance when being lapped at different stretching lengths.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
Those who do not specify specific conditions in the examples of the present invention follow conventional conditions or conditions recommended by the manufacturer. The raw materials, reagents and the like which are not indicated for manufacturers are all conventional products which can be obtained by commercial purchase.
Example 1
Preparation method of high-tensile high-sensitivity piezoresistive fiber
1) Adding 3g of thermoplastic polyurethane into 17g of N, N-Dimethylformamide (DMF), stirring and dissolving, then adding 200mg of one-dimensional carboxylated multi-walled carbon nanotubes (MWCNT) into the solution, stirring and dispersing, slowly adding ammonia water into the solution while stirring to make the pH value reach 12, and finally forming the stably-dispersed spinning solution.
2) With 15wt% silver trifluoroacetate (AgCOOF) 3 ) The isopropyl alcohol (IPA) solution was used as a coagulation bath. The spinning solution was extruded into a coagulation bath by wet spinning at normal temperature.
3) Standing the fiber obtained by spinning in a coagulating bath for 12h to fully exchange DMF and IPA, gradually solidifying the thermoplastic polyurethane, and simultaneously Ag + Ion substituted NH 4 + 。
4) And taking out the fiber in the coagulating bath, placing the fiber in a fume hood, and drying for 24h to volatilize the solvent in the fiber to obtain the fiber with a porous structure.
5) The dried porous fiber is put into hydrazine hydrate steam (the concentration is 5 g/m) 3 ) Reducing at 80 deg.C for 10min to obtain Ag + Reduced to silver nanoparticles (AgNPs) to give porous fibers containing a 0D AgNPs and 1D carboxylated MWCNT cooperative conducting network.
Example 2
Preparation method of high-tensile high-sensitivity piezoresistive fiber
1) Adding 3g of thermoplastic polyurethane into 4.5g of dimethyl sulfoxide (DMSO), stirring and dissolving, adding 10mg of two-dimensional carboxylated Graphene (GE) and 40mg of one-dimensional carboxylated single-walled Carbon Nanotubes (CNT), stirring and dispersing, and slowly adding ammonia water into the solution while stirring to enable the pH value to reach 11, thus forming the stably-dispersed spinning solution.
2) With 30wt% copper trifluoroacetate (Cu (COOF) 3 ) 2 ) The volume ratio of the deionized water to the methanol is 1:1 as a coagulation bath. The spinning solution was extruded into a coagulation bath by wet spinning at normal temperature.
3) The fiber obtained by spinning stays in a coagulating bath for 30min, so that the DMSO is fully exchanged with the solvent in the coagulating bath, the thermoplastic polyurethane is gradually solidified, and meanwhile, the Cu is added 2+ Ion substituted NH 4 + 。
4) And taking out the fiber in the coagulating bath, and drying in an oven at 60 ℃ for 8h to volatilize the solvent in the fiber to obtain the fiber with a porous structure.
5) The dried porous fiber is put into hydrazine hydrate steam (the concentration is 5 g/m) 3 ) Reducing at 70 deg.C for 20min to obtain Cu 2+ Reduction to copper nanoparticles (CuNPs) resulted in porous fibers containing 0D CuNPs in conjunction with 1D CNTs, 2D GE conductive network.
Example 3
Preparation method of high-tensile high-sensitivity piezoresistive fiber
1) Adding 3g of thermoplastic polyurethane into 12g of acetone, stirring and dissolving, adding 100mg of two-dimensional carboxylated MXene into the mixture, stirring, and slowly adding ammonia water into the solution while stirring to enable the pH value to reach 11 so as to form the stably dispersed spinning solution.
2) With 20wt% copper acetate (Cu (CH) 3 COO) 2 ) The volume ratio of ethanol to isopropanol is 1:3 as a coagulating bath. The spinning solution was extruded into a coagulation bath by wet spinning at room temperature.
3) The fiber obtained by spinning stays in the coagulating bath for 6 hours, so that the acetone and the solvent in the coagulating bath are fully exchanged, the thermoplastic polyurethane is gradually solidified, and simultaneously Cu is added 2+ Ion substituted NH 4 + 。
4) And taking out the fiber in the coagulating bath, and drying in a fume hood for 24h to volatilize the solvent in the fiber to obtain the fiber with a porous structure.
5) Placing the dried porous fiber in hydriodic acid steam (concentration is 5 g/m) 3 ) Reducing at medium 80 deg.C for 10min to obtain Cu 2+ Reducing the solution into copper nano particles (CuNPs) to obtain the porous fiber containing 0D CuNPs and 2D MXene cooperative conductive network.
Example 4
Preparation method of high-tensile high-sensitivity piezoresistive fiber
1) Adding 3g of thermoplastic polyurethane into 7g of N, N-Dimethylformamide (DMF), stirring and dissolving, adding 100mg of two-dimensional carboxylated Graphene (GE) and 50mg of one-dimensional carboxylated single-walled Carbon Nanotubes (CNT), stirring and dispersing, and slowly adding ammonia water into the solution while stirring to make the pH value reach 13, thereby forming the uniform spinning solution.
2) With 20wt% silver trifluoroacetate (AgCOOF) 3 ) The mixed solution of deionized water and isopropyl alcohol (1, 4, 2, 3, 1, 4 and 0. The spinning solution was extruded into a coagulation bath by wet spinning at normal temperature.
3) The fiber obtained by spinning stays in the coagulating bath for 6 hours, so that the DMF and the solvent in the coagulating bath are fully exchanged, the thermoplastic polyurethane is gradually solidified, and simultaneously the Ag + Ion substituted NH 4 + 。
4) And taking out the fiber in the coagulating bath, and drying in a fume hood for 24h to volatilize the solvent in the fiber to obtain the fiber with a porous structure.
5) Putting the dried porous fiber into hydrazine hydrate steam(concentration 5 g/m) 3 ) Reducing at 80 deg.C for 10min to obtain Ag + Reduction to silver nanoparticles (AgNPs) resulted in porous fibers with 0D AgNPs in conjunction with 1D CNTs, 2D GE conductive network.
6) The two piezoresistive fibers are mutually overlapped, and the compression sensing performance of the fibers is respectively tested on a tensile machine when the fibers are stretched to different lengths.
Comparative example 1
Preparation method of high-tensile high-sensitivity piezoresistive fiber
1) 3g of thermoplastic polyurethane is added into 12g of acetone and stirred for dissolution, then 100mg of two-dimensional carboxylated MXene is added into the acetone and stirred, and ammonia water is slowly added into the solution while stirring to make the pH value reach 11, thus forming the stably dispersed spinning solution.
2) With 20wt% copper acetate (Cu (CH) 3 COO) 2 ) The acetone solution was used as a coagulation bath. The spinning solution was extruded into a coagulation bath by wet spinning at room temperature.
3) The fiber obtained by spinning stays in the coagulating bath for 6 hours, so that the acetone and the solvent in the coagulating bath are fully exchanged, the thermoplastic polyurethane is gradually solidified, and simultaneously Cu is added 2+ Ion substituted NH 4 + 。
4) And taking out the fiber in the coagulating bath, and drying in a fume hood for 24h to volatilize the solvent in the fiber to obtain the fiber.
5) The dried fibers were placed in a stream of hydroiodic acid (5 g/m concentration) 3 ) Reducing at medium 80 ℃ for 10min to obtain Cu 2+ Reducing the solution into copper nano particles (CuNPs) to obtain solid fibers containing 0D CuNPs and 2D MXene cooperative conductive network.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. A preparation method of piezoresistive fiber is characterized by comprising the following steps:
(1) Dispersing the carboxylated conductive filler into a thermoplastic polyurethane solution, and adding a certain amount of ammonia water to obtain a spinning solution;
(2) Extruding the spinning solution obtained in the step (1) into a coagulating bath containing a metal precursor through wet spinning and standing for at least 30min to obtain a fiber loaded with metal ions;
(3) Drying the fiber loaded with the metal ions in the step (2) to obtain porous composite fiber loaded with the metal ions;
(4) Reducing the porous composite fiber loaded with metal ions in the step (3) to reduce the metal ions into metal nano particles, cleaning and drying to obtain the porous piezoresistive fiber;
the solvent of the coagulating bath containing the metal precursor is water and one of isopropanol, methanol and ethanol according to the volume ratio of 1:4 to 4: 1;
the mass ratio of the carboxylated conductive filler to the thermoplastic polyurethane in the step (1) is 0.1-5: 15 to 40 percent;
adding ammonia water into the mixed solution in the step (1), and then adjusting the pH of the mixed solution to 11-14;
the mass concentration of the metal precursor in the coagulating bath containing the metal precursor in the step (2) is 5-30 wt%;
the carboxylated conductive filler in the step (1) is at least one of one-dimensional carboxylated carbon nanotube, two-dimensional carboxylated graphene and two-dimensional carboxylated MXene;
and (3) the metal in the coagulating bath containing the metal precursor in the step (2) is at least one of copper and silver.
2. The method for preparing piezoresistive fibers according to claim 1, wherein the solvent of the thermoplastic polyurethane solution in step (1) is at least one of N, N-dimethylformamide, tetrahydrofuran, acetone and dimethyl sulfoxide.
3. The method for preparing piezoresistive fiber according to claim 1, wherein the carboxylated conductive filler in step (1) is one-dimensional carboxylated carbon nanotube and two-dimensional carboxylated graphene and/or two-dimensional carboxylated MXene mixture, wherein the mass ratio of the one-dimensional conductive filler to the two-dimensional conductive filler is 1;
and (3) the metal precursor in the coagulating bath containing the metal precursor in the step (2) is at least one of silver trifluoroacetate, copper trifluoroacetate and copper acetate.
4. The method for preparing piezoresistive fibers according to claim 1, wherein the mass concentration of the thermoplastic polyurethane solution in the step (1) is 15-40%.
5. The method for preparing piezoresistive fibers according to claim 1, wherein the standing time in step (2) is 30min to 12h; the drying temperature in the step (3) is 25-60 ℃, and the drying time is 8-24 h; the reduction treatment in the step (4) comprises the following steps: placing the porous composite fiber loaded with metal ions in hydrazine hydrate steam or hydroiodic acid steam at 70-100 ℃ for 5 min-1 h, wherein the concentration of the hydrazine hydrate steam or the hydroiodic acid steam is 1-10 g/m 3 。
6. A piezoresistive fiber produced by the method of any of claims 1-5.
7. Use of piezoresistive fiber according to claim 6 in electronic textiles and smart wearable devices.
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