CN114150496B - Flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing performances and preparation method thereof - Google Patents
Flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing performances and preparation method thereof Download PDFInfo
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- CN114150496B CN114150496B CN202111350682.5A CN202111350682A CN114150496B CN 114150496 B CN114150496 B CN 114150496B CN 202111350682 A CN202111350682 A CN 202111350682A CN 114150496 B CN114150496 B CN 114150496B
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- nanofiber membrane
- electromagnetic shielding
- flexible
- mxene
- piezoresistive sensing
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- 239000012528 membrane Substances 0.000 title claims abstract description 97
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- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 14
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- 229910052782 aluminium Inorganic materials 0.000 claims description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 15
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- 238000012986 modification Methods 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 5
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- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
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- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
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- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
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- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
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- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
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- D—TEXTILES; PAPER
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- 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
- D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/49—Oxides or hydroxides of elements of Groups 8, 9,10 or 18 of the Periodic Table; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
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- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- D06M11/58—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 nitrogen or compounds thereof, e.g. with nitrides
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- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
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Abstract
A flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing properties and a preparation method thereof belong to the technical field of multifunctional material preparation. Firstly, obtaining a polymer nanofiber membrane through an electrostatic spinning process, and then preparing MXene@Fe 3 O 4 And preparing the polymer nanofiber membrane with good hydrophilicity by using the dispersion liquid and then modifying the dopamine, and obtaining the target fiber membrane by combining a spraying process. Due to the excellent conductivity of MXene and the structural characteristics of the nanofibers, a conductive network is formed, fe 3 O 4 The nano particles cooperate to further realize the absorption of electromagnetic waves. The obtained fiber membrane has excellent electromagnetic shielding performance and sensing performance and good mechanical flexibility. Due to its ultra-thin,The light wearable property and the good mechanical property can be used for textile industry, military field, artificial intelligence and daily protection, and is a novel nano material with good application prospect.
Description
Technical Field
The invention belongs to the technical field of multifunctional material preparation, and particularly relates to a flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing performances and a preparation method thereof. The nanofiber membrane obtained by the invention is a composite fiber membrane, has excellent electromagnetic interference (EMI) shielding performance and good mechanical performance, and has good potential and application feasibility for developing flexible wearable electronic equipment.
Background
The propagation of electromagnetic waves does not depend on a medium, and the frequency is an important characteristic of electromagnetic waves, from low frequency to high frequency, and is mainly classified into radio waves, microwaves, infrared rays, visible light, ultraviolet rays, X-rays and gamma rays. With the rapid development of modern communication technology and portable electronic devices toward higher power, higher density and higher integration, it is becoming important to control electromagnetic radiation and reduce electromagnetic radiation pollution. Particularly, the rapid development of the fifth generation (5G) and sixth generation (6G) communication technologies has increased electromagnetic interference (EMI) and electromagnetic compatibility (EMC) problems, which threatens the health of people, and also causes serious interference to precise instruments, and in addition, the leakage of electromagnetic waves also endangers the information security. Electromagnetic waves become a fourth great nuisance after noise, air and water pollution, the research of electromagnetic shielding materials has important significance for social life, economic construction and national defense construction, and the related fields also put higher demands on the electromagnetic shielding materials.
Wearable electronic devices have received great attention over the past decades for their superior real-time monitoring capabilities and flexible interactive functions with the human body. High sensitivity, high precision components in wearable electronics and robotic systems can be strongly affected by electromagnetic radiation. Therefore, there is a need to develop a flexible shielding material that is as flexible and expandable as human skin but can effectively prevent electromagnetic waves. The increasing demand for shielded electronics has prompted the search for such multifunctional materials.
The common electromagnetic shielding materials mainly comprise metal, carbon materials, conductive polymers, metal oxides or nitrides, composite materials thereof and the like. However, the metal-based EMI shielding material has the disadvantages of high density, easy corrosion, difficult processing and the like, and limits the application of the metal-based EMI shielding material in most fields. One alternative to metal-based shielding materials is to use polymer-based materials with conductive fillers. Initial studies have incorporated metal particles as fillers into high weight fraction composites to increase electrical conductivity. For example, yan Dingxiang et al disclose a method for preparing a heat-resistant electromagnetic shielding material of carbon nanotubes (chinese patent application No. 201810506962.2), in which carbon nanotubes prepared by the method are distributed at the interface of polyphenylene sulfide particles to form a three-dimensional conductive network, and high electromagnetic shielding efficiency can be achieved with a lower filler content of the carbon nanotubes. However, the quality, cost and corrosiveness of polymer-metal composites are relatively high.
A recent class of research hotspot materials are carbides and nitrides of transition metals, known as mxnes. One of the main factors that MXene materials have rapidly evolved is its electrical conductivity: the conductivity is highest in all synthetic 2D materials, being ten or more times that of reduced graphene oxide (rGO) thin films. The material also has excellent electronic conduction and good mechanical property, can position MXene as a potential transduction material of a sensor such as strain, pressure, electrochemistry and the like, has unique characteristics, hydrophilicity and good dispersion stability, and widens the application of MXene in electromagnetic interference (EMI) shielding. Discovery from 2011First MXene (Ti 3 C 2 T x ) More than 30 different types of MXene have been synthesized so far, which have proved to have high electromagnetic shielding effectiveness as fillers or as films in polymeric matrices due to their comparable conductive properties of metals, their controllable surface chemistry, and their ability to be intercalated by other metal ions. For example: hong et al disclose an iron-based amorphous/MXenes composite electromagnetic shielding material for severe corrosion environments and application (Chinese patent application No. 201910525985.2), wherein iron-based amorphous and MXenes materials with different weight percentages are compounded, so that good shielding performance is achieved, and meanwhile, the defect that common metals are easy to corrode is overcome. However, although the electromagnetic shielding material reported at present has good shielding performance, the raw materials manufactured by the material are mostly powder or granular, agglomeration is easy to occur in large-scale production, and the mechanical performance of the material is poor, so that the material has the defects for practical application.
The electrostatic spinning technology is used as a simple technical means for solving the problems of uneven dispersion of raw materials and subsequent electromagnetic pollution by using reflection as a mechanism. In recent decades, the design of shielding materials has been developed towards thinning, light weight, wide frequency band, strong absorption and flexibility, and has made a great progress. The composite nanofiber membrane material prepared by the electrostatic spinning and post-treatment technology has better dispersibility and flexibility than powder, is low in density and easy to recycle, and has a better application prospect. Meanwhile, by combining different treatment technologies, organic nanofibers, inorganic nanofibers and organic/inorganic composite nanofibers with different structures can be obtained, wherein the inorganic/organic composite nanofibers have the functions of inorganic matters and the flexibility of polymers, so that electromagnetic waves can be reflected and absorbed between metal nanoparticles and the polymer nanofibers for multiple times, and therefore, the design of flexible electromagnetic shielding protective materials is considered widely.
The nano material has a series of special structures, so that the nano material can generate quality change in the aspects of physical properties such as light, electricity, magnetism and the like, can absorb electromagnetic waves more strongly, and is a material which is very advancedElectromagnetic shielding material in the way; and Fe (Fe) 3 O 4 Is considered to be one of the most popular materials because of its low cost, high content in the crust of the earth, and simple preparation. On the other hand, fe 3 O 4 The nano particles have the functions of relaxation regulation, magnetic resonance, electron jump, vortex, multiple scattering, impedance matching and the like, and can be widely applied to the fields of biomedicine, sensors and the like. Two-dimensional Ti 3 C 2 T x Nanosheets and Fe 3 O 4 Synergistic coordination between nanoparticles, MXene bonds to fibrous membranes to help form conductive networks, while Fe 3 O 4 The nanoparticles may further absorb microwave radiation by natural resonance, eddy currents, hysteresis losses, etc. Because it can prevent electromagnetic waves and sense pressure, we can also call this composite a multifunctional electromagnetic shielding skin. The nanofiber membrane provides a new thought for the development of next-generation flexible wearable equipment, and opens up a new way for the mass production of high-stability flexible electronic materials.
Disclosure of Invention
The invention aims to provide a flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing performances and a preparation method thereof, so as to solve the defects that the traditional metal electromagnetic shielding material is easy to corrode, has poor mechanical performance, serious pollution in the production process, nanoparticle agglomeration in the material preparation process, difficult recycling and the like, prolong the service life of the electromagnetic shielding material to the maximum extent, and enhance the practicability of the electromagnetic shielding material.
The invention relates to a preparation method of a flexible nanofiber membrane with electromagnetic shielding and piezoresistance sensing performance, which comprises the steps of firstly obtaining a polymer nanofiber membrane through an electrostatic spinning process, then adopting a method in a document (DOI 10.1021/acs. Chemnater.7b02847) to etch MAX phase to obtain a few-layer MXene nanosheet, and performing hydrothermal synthesis on Fe 3 O 4 Nanometer particle (DOI 10.1039/d0nr09228 b) to obtain MXene@Fe 3 O 4 And (3) a dispersion. By adjusting Fe 3 O 4 The addition amount of the nano particles can obtain MXene@Fe with different proportions 3 O 4 And (3) a dispersion. And then preparing the PPAN nanofiber membrane with good hydrophilicity by utilizing dopamine modification treatmentAnd combining a spraying process to obtain the target fiber membrane. Due to the excellent conductivity of MXene and the structural characteristics of the nanofibers, a conductive network is formed, fe 3 O 4 The nano particles cooperate to further realize the absorption of electromagnetic waves. The obtained fiber membrane has excellent electromagnetic shielding performance and sensing performance and good mechanical flexibility. Due to the ultrathin and portable wearable property, the nano-material can be used for textile industry, military field, artificial intelligence and daily protection, and is a novel nano-material with good application prospect.
The invention relates to a preparation method of a flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing performances, which comprises the following steps:
(1) Dissolving a high molecular polymer in an organic solvent, and uniformly stirring to obtain a clear precursor solution; filling the obtained precursor solution into an injector of electrostatic spinning equipment, taking a stainless steel needle as an anode, taking a planar aluminum foil as a cathode to receive an electrostatic spinning product, keeping the distance between the needle and a receiving plate to be 10-20 cm, and carrying out electrostatic spinning for 10-24 hours under the voltage of 8-18 kV to obtain a polymer nanofiber membrane on the planar aluminum foil;
(2) Stripping 100-150 mg of the polymer nanofiber membrane obtained in the step (1) from the planar aluminum foil, then putting the stripped polymer nanofiber membrane into 80-120 mL of alcohol reagent, and carrying out infiltration treatment for 0.5-2.0 h;
(3) Putting the polymer nanofiber membrane subjected to the infiltration treatment in the step (2) into 50-100 mL of dopamine solution (the solvent is pH=8.5 and 50mM Tris-HCl buffer solution) with the concentration of 7.5-8.0 mg/mL, reacting for 12-48 hours at room temperature, taking out, sequentially washing the reacted film with distilled water and the same alcohol reagent as in the step (2) for 3-5 times respectively, and drying in vacuum to obtain the polymer nanofiber membrane subjected to the polydopamine modification treatment;
(4) Preparation of MXene nanosheet Dispersion and Fe 3 O 4 NPs, fe 3 O 4 NPs are added into MXene dispersion liquid to prepare Fe 3 O 4 MXene@Fe with mass fraction of NPs of 1-5% 3 O 4 A dispersion;
(5) The step (4) is carried outMXene@Fe of (C) 3 O 4 And (3) depositing the dispersion liquid on the surface of the polymer nanofiber membrane obtained in the step (3) by using a spraying method, and cleaning and drying to obtain the flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing properties.
The polymer in the step (1) is one of polymethyl methacrylate, polystyrene, polyacrylonitrile, sulfonated polyether ether ketone or polyacrylamide; the organic solvent is one or a mixture of more of N, N-dimethylformamide, N-dimethylacetamide, dimethyl sulfoxide, acetone, chloroform, dichloromethane and ethanol, and the mass fraction of the polymer in the precursor solution is 6-10%;
the alcohol reagent in the step (2) and the step (3) is one or more than two of ethanol, n-propanol, n-butanol, glycol and glycerol;
the average thickness of the MXene nano-sheet in the step (4) is 5.0+/-0.5 nm, fe 3 O 4 The particle size distribution of NPs is 282.57 +/-6 nm;
the spraying speed in the step (5) is 300-500 rpm/min, and the spraying time is 1.5-3.0 min;
fe is adopted in the step (5) 3 O 4 MXene@Fe with mass fraction of NPs of 1-5% 3 O 4 After the dispersion liquid is sprayed, the obtained composite fiber membrane has a multi-level coarse structure (one-dimensional PAN is taken as a fiber framework, and the surface is tightly covered with two-dimensional MXene shell layers and zero-dimensional Fe) 3 O 4 The nano particles are randomly distributed on the nano particles, as shown in the figure 2), and the average diameter of the nano particles is 333-431 nm; the obtained flexible nanofiber membrane has flexibility, can be folded, can not be broken after being repeatedly bent for more than 500 times, and has almost no loss of conductivity;
the flexible nanofiber membrane obtained in the step (5) can be applied to the fields of electromagnetic shielding protection, sensors, photocatalysis and the like.
The flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing performances is prepared by the method.
The invention has the advantages that:
the invention uses poly dopamineBased on modified polymer nanofiber membrane, MXene@Fe with different proportions is sprayed 3 O 4 And (3) preparing the dispersion liquid to obtain the nanofiber membrane with excellent flexible electromagnetic shielding performance. The nanofiber membrane with a certain thickness has an electromagnetic shielding effect similar to that of a traditional metal protective material, and the secondary structure of the fiber membrane is realized to form a 3D conductive network, so that the electromagnetic wave is reflected and absorbed for multiple times inside, and the shielding effect of the electromagnetic wave is enhanced. Meanwhile, the flexible nanofiber membrane has the characteristics of low density, comfort in wearing and soft texture, overcomes the defects of poor flexibility, insufficient environmental protection and easiness in damaging human health of the traditional metal material, and prolongs the service life of the material. Meanwhile, compared with the electromagnetic shielding protective material reported in the past, the flexible electromagnetic shielding protective and pressure sensing nanofiber membrane provided by the invention ensures excellent electromagnetic shielding performance, has long and continuous fiber, soft and flexible texture, can be bent at will, has certain mechanical strength and Fe 3 O 4 The nano particles are uniformly dispersed and have stable performance. The composite fiber membrane is easy to recycle after use, can be reused for photocatalytic degradation of pollutants or used as devices such as a temperature sensor, a capacitor and the like after recycling, has good conductivity, can serve as a wire and the like in an emergency condition, can exert the function of a material to the maximum extent, realizes 'one-membrane multipurpose', can create economic value in the whole life cycle, has high efficiency and is environment-friendly, and has higher operability and practical applicability. In addition, the structure on the obtained composite nanofiber can be regulated and controlled by changing the reaction condition, the obtained composite nanofiber can be loaded with nano particles, nano sheets and the like, the application range and the application potential of the material are greatly improved, and the flexible nanofiber membrane provided by the invention can be applied to various fields such as electromagnetic shielding protective clothing, human body sensing and the like. Finally, the preparation method provided by the invention has the advantages of easily available raw materials, simple and safe operation and easy realization of industrial mass production.
Drawings
Fig. 1: the optical photograph of the folding and resetting of the flexible nanofiber membrane obtained in example 1 shows objective flexibility;
fig. 2: fe obtained in example 3 3 O 4 Transmission electron micrographs of (figure a) and flexible nanofiber membrane (figure b) and corresponding elemental analysis maps, and the obtained product is a coated MXene shell structure, fe 3 O 4 A nanoparticle-supported flexible nanofiber membrane with a diameter distribution of 390.51 +/-1 nm; the elemental analysis map results show that: C. the O, fe and Ti elements are uniformly distributed, which indicates that Fe on the PPAN film 3 O 4 Successful introduction of MXene;
fig. 3: electromagnetic shielding efficiency curves (sequence 1, sequence 2 and sequence 3 curves correspond to the examples 1, 2 and 3 respectively) of the flexible nanofiber membranes obtained in the examples 1, 2 and 3 on electromagnetic waves when the single-layer thickness is (48 μm is uniformly selected);
electromagnetic shielding effectiveness (EMI SE) is a measure of the ability of a material to attenuate electromagnetic waves, the Total electromagnetic shielding effectiveness (Total EMI SE) (SE T ) Is defined as the logarithm of the ratio of the incident power (Pi) to the transmitted power (Pm) of an electromagnetic wave, in decibels (dB). The abscissa is the electromagnetic wave frequency and the ordinate is the shielding effectiveness, defined as se=20 lg (E 1 /E 2 ) (dB), a ZV3672B-S type vector network analyzer of the middle electric forty-one station is used for testing by using rectangular waveguides, the electromagnetic wave frequency band is an X wave band (8-12.4 GHz), a Ku wave band (12-18 GHz) and a K wave band (18-26.5 GHz), and each wave band is tested by using a corresponding rectangular waveguide adapter, so that the result can be obtained that along with Fe 3 O 4 An increase in the amount of nanoparticles added, the electromagnetic shielding efficiency of which was gradually improved, fe in example 2 3 O 4 The electromagnetic shielding efficiency reached the maximum at 3% by mass and was further increased to 5% (example 3), which was a decrease in shielding performance. From this result, it can be concluded that the flexible nanofiber membrane described in example 2 has the best electromagnetic shielding properties;
fig. 4: different ratios of MXene@Fe used in examples 1, 2, 3 3 O 4 Bar graph of Zeta potential test of the dispersion and of MXene dispersion at a concentration of 2 mg/mL; the results show that: with Fe 3 O 4 An increase in the amount of addition, the two oppositely charged nanomaterials attract each other andself-assembly, different proportions of MXene@Fe 3 O 4 The Zeta (ζ) potential of the dispersion gradually increases, and the stability of the dispersion deteriorates, but they all exhibit the same electronegativity.
Fig. 5: tensile strength curves of the flexible nanofiber membranes obtained in examples 1, 2, 3; testing by adopting a tensile testing machine AGS-H, wherein the tensile speed is as follows: 3mm/min, gauge length: 20mm, sample width: 10mm, the results show that: with Fe 3 O 4 The content is increased, the elongation at break of the fiber membrane is gradually reduced, and the strength is increased. Mainly because of a large number of defects on the surface of the film, the flexibility of the film is reduced, but Fe 3 O 4 But the introduction of (c) can increase its mechanical strength.
Fig. 6: electromagnetic shielding efficiency curves of flexible nanofiber membranes prepared in example 1 with different layers (1, 3,5,7 layers were selected) on electromagnetic waves; it was found that as the number of layers increases, the thickness of the fiber film also increases, and the overall electromagnetic shielding efficiency increases gradually. The test is still carried out by using a ZV3672B-S type vector network analyzer of the middle electric forty-one institute and utilizing rectangular waveguide to test, the electromagnetic wave frequency band is an X wave band (8-12.4 GHz), a Ku wave band (12-18 GHz) and a K wave band (18-26.5 GHz), and each wave band is tested by using a corresponding rectangular waveguide adapter. Since the conductivity of the fiber film is hardly changed, the corresponding reflection loss is slightly increased, indicating that increasing the thickness to increase the EMI SE is mainly achieved by increasing the absorption loss. The thickness increases, the propagation path of electromagnetic waves inside the material increases, the multiple reflection increases, and the action time with the material increases, thereby accompanying an increase in absorption loss.
Fig. 7: an optical photograph of the conductive ability of the flexible nanofiber membrane obtained in example 2 under bending; the results show that: the LED bulb can be lightened as a lead no matter the fiber film is in a flat state or is bent, which indicates that the fiber film has better durability.
Fig. 8: the response rate curve of the flexible nanofiber membrane obtained in example 3 (graph a) and the monitoring curve of the sensor device on human body signals (graph b, throat sounding) under different pressures; the results show that: the sensor has better real-time response under the ultra-wide pressure range of 0.53-250 k Pa. When the sensor is compressed, the resistance decreases and when the pressure is released, the resistance increases significantly. Meanwhile, figure b shows the response of the throat when "hello" is emitted, indicating that the sensor can fully distinguish the human body signals in real time.
Detailed Description
For a better understanding of the present invention, the following examples are set forth to illustrate the present invention, but are not to be construed as limiting the scope of the invention.
Example 1:
(1) 2.00g of Polyacrylonitrile (PAN) was dissolved in 18.00g of N, N-Dimethylformamide (DMF) and stirred mechanically at 45℃for 10h to prepare a homogeneous clear precursor solution. And cooling the obtained spinning solution to room temperature, then loading the spinning solution into an electrostatic spinning injector, taking a stainless steel needle as an anode, taking a planar aluminum foil as a cathode to receive an electrostatic spinning product, keeping the distance between the needle and a receiving plate to be 17cm, carrying out electrostatic spinning for 20h under 18kV voltage, and obtaining the PAN nanofiber membrane on the planar aluminum foil.
(2) 120mg of the PAN nanofiber membrane obtained in the step (1) was put into 100mL of absolute ethyl alcohol, and subjected to infiltration treatment for 1.5 hours.
(3) And (3) peeling the fiber membrane subjected to the infiltration treatment in the step (2) from the planar aluminum foil, putting the peeled fiber membrane into a dopamine solution (the solvent is pH=8.5 and 50mM Tris-HCl buffer solution) with the volume of 7.88mg/mL, reacting for 24 hours at room temperature, taking out the reacted film, sequentially washing the reacted film with distilled water and absolute ethyl alcohol for 3 times respectively, and then putting the film into a vacuum dryer for drying to obtain the PAN nanofiber membrane subjected to the polydopamine modification treatment, and naming the PAN nanofiber membrane as PPAN.
(4) Preparation of MXene nanosheet Dispersion (DOI 10.1021/acs. Chemnater.7b02847) and Fe according to methods in the literature 3 O 4 NPs (DOI 10.1039/d0nr09228 b) with Fe regulation 3 O 4 Amount of NPs to produce Fe 3 O 4 MXene@Fe with mass fraction of NPs of 1% 3 O 4 And (3) a dispersion. Reference is made to the document, namely to first prepare MXene nanoplatelets and then to prepare MXene dispersionsFe is then prepared by reference 3 O 4 NPs, finally Fe 3 O 4 NPs are added into MXene dispersion liquid to obtain Fe 3 O 4 MXene@Fe with mass fraction of NPs of 1% 3 O 4 And (3) a dispersion. The average thickness of the MXene nano-sheet is 5.0+/-0.5 nm, fe 3 O 4 The particle size distribution of NPs was 282.57.+ -.6 nm.
(5) The MXene@Fe obtained in the step (4) is treated 3 O 4 The dispersion is deposited on the surface of the PPAN fiber film by a spraying method. The spraying time is 2min, the spraying speed is 400rpm/min, then distilled water and absolute ethyl alcohol are respectively used for cleaning for 3 times, and a vacuum drying oven is used for drying, so that the flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing performances, named PPAN-M-1% Fe, can be obtained 3 O 4 (M represents MXene) and the average diameter of the fiber was 333nm.
The average density of the single-layer flexible nanofiber membrane prepared in this example was 1.35g/cm 3 The thickness was 33. Mu.m. The electromagnetic shielding efficiency of the electromagnetic wave K wave band, the Ku wave band and the X wave band is tested by using the single-layer flexible nanofiber membrane, so that a certain electromagnetic shielding protection effect can be achieved, and SE (selective electromagnetic) of the single-layer flexible nanofiber membrane is achieved T Up to 27.6dB. Meanwhile, the flexible cable is good in flexibility, does not have fracture phenomenon after being bent for 500 times, and has no obvious protection efficiency loss.
Example 2:
(1) 2.00g of polyacrylonitrile was dissolved in 18.00g of N, N-Dimethylformamide (DMF), and the mixture was mechanically stirred at 45℃for 10 hours to prepare a homogeneous and clear precursor solution. And cooling the obtained spinning solution to room temperature, then loading the spinning solution into an electrostatic spinning injector, taking a stainless steel needle as an anode, taking a planar aluminum foil as a cathode to receive an electrostatic spinning product, keeping the distance between the needle and a receiving plate to be 17cm, carrying out electrostatic spinning for 20h under 18kV voltage, and obtaining the PAN nanofiber membrane on the planar aluminum foil.
(2) 120mg of the nanofiber membrane obtained in the step (1) was peeled off from the planar aluminum foil, and then, the nanofiber membrane was put into 100mL of absolute ethyl alcohol, and subjected to a soaking treatment for 1.5 hours.
(3) And (3) putting the fiber membrane subjected to the infiltration treatment in a dopamine solution (the solvent is pH=8.5 and 50mM Tris-HCl buffer solution) with the volume of 80mL and the concentration of 7.88mg/mL, reacting at room temperature for 24 hours, taking out, sequentially washing the film subjected to the reaction with distilled water and absolute ethyl alcohol for 3 times respectively, and drying in a vacuum dryer to obtain the PPAN nanofiber membrane subjected to the polydopamine modification treatment.
(4) Preparation of MXene nanosheet Dispersion and Fe according to methods in literature 3 O 4 NPs, while regulating Fe 3 O 4 Amount of NPs preparation of MXene@Fe with mass fraction of 3% 3 O 4 And (3) a dispersion.
(5) The MXene@Fe obtained in (4) is used for preparing 3 O 4 The dispersion is deposited on the surface of the PPAN fiber film by a spraying method. The spraying time is 2min, the spraying speed is 400rpm/min, then distilled water and absolute ethyl alcohol are respectively used for cleaning for 3 times, and a vacuum drying oven is used for drying, so that the flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing performances, named PPAN-M-3% Fe, can be obtained 3 O 4 . The average diameter of the fibers was 390nm.
(6) The average density of the single-layer flexible nanofiber membrane prepared in this example was 1.44g/cm 3 The thickness was 40. Mu.m. The electromagnetic shielding efficiency of the electromagnetic wave K wave band, the Ku wave band and the X wave band is tested by using the single-layer flexible nanofiber membrane, so that a certain electromagnetic shielding protection effect can be achieved, and SE (selective electromagnetic) of the single-layer flexible nanofiber membrane is achieved T Can reach 43.8dB, and can realize the shielding effectiveness of more than 99.999999 percent. Meanwhile, the flexible cable is good in flexibility, does not have fracture phenomenon after being bent for 500 times, and has no obvious protection efficiency loss.
Example 3:
(1) 2.00g of polyacrylonitrile was dissolved in 18.00g of N, N-Dimethylformamide (DMF), and the mixture was mechanically stirred at 45℃for 10 hours to prepare a homogeneous and clear precursor solution. And cooling the obtained spinning solution to room temperature, then loading the spinning solution into an electrostatic spinning injector, taking a stainless steel needle as an anode, taking a planar aluminum foil as a cathode to receive an electrostatic spinning product, keeping the distance between the needle and a receiving plate to be 17cm, carrying out electrostatic spinning for 20h under 18kV voltage, and obtaining the PAN nanofiber membrane on the planar aluminum foil.
(2) 120mg of the nanofiber membrane obtained in the step (1) was peeled off from the planar aluminum foil, and then, the nanofiber membrane was put into 100mL of absolute ethyl alcohol, and subjected to a soaking treatment for 1.5 hours.
(3) And (3) putting the fiber membrane subjected to the infiltration treatment in a dopamine solution (the solvent is pH=8.5 and 50mM Tris-HCl buffer solution) with the volume of 80mL and the concentration of 7.88mg/mL, reacting at room temperature for 24 hours, taking out, sequentially washing the film subjected to the reaction with distilled water and absolute ethyl alcohol for 3 times respectively, and drying in a vacuum dryer to obtain the PPAN nanofiber membrane subjected to the polydopamine modification treatment.
(4) Preparation of MXene nanosheet Dispersion and Fe according to methods in literature 3 O 4 NPs, while regulating Fe 3 O 4 Amount of NPs preparation of MXene@Fe with mass fraction of 5% 3 O 4 And (3) a dispersion.
(5) The MXene@Fe obtained in (4) is used for preparing 3 O 4 The dispersion is deposited on the surface of the PPAN fiber film by a spraying method. The spraying time is 2min, the spraying speed is 400rpm/min, then distilled water and absolute ethyl alcohol are respectively used for cleaning for 3 times, and a vacuum drying oven is used for drying, so that the flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing performances, named PPAN-M-5% Fe, can be obtained 3 O 4 . The average diameter of the fibers was 431nm.
(6) The single-layer flexible nanofiber membrane prepared in this example had an average density of 1.51g/cm 3 The thickness was 45. Mu.m. The electromagnetic shielding efficiency of the electromagnetic wave K wave band, the Ku wave band and the X wave band is tested by using the single-layer flexible nanofiber membrane, so that a certain electromagnetic shielding protection effect can be achieved, and SE (selective electromagnetic) of the single-layer flexible nanofiber membrane is achieved T Up to 37.6dB. Meanwhile, the flexible cable is good in flexibility, does not have fracture phenomenon after being bent for 500 times, and has no obvious protection efficiency loss.
Claims (9)
1. A preparation method of a flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing properties comprises the following steps:
(1) Dissolving high molecular polymer in organic solvent, stirring uniformly at 30-60 ℃ to obtain clear precursor solution; cooling the obtained precursor solution to room temperature, then loading the cooled precursor solution into an injector of electrostatic spinning equipment, taking a stainless steel needle as an anode, taking a planar aluminum foil as a cathode to receive an electrostatic spinning product, keeping the distance between the needle and a receiving plate to be 10-20 cm, and carrying out electrostatic spinning for 10-24 hours under the voltage of 10-20 kV to obtain a polymer nanofiber membrane on the planar aluminum foil;
(2) Stripping 100-150 mg of the polymer nanofiber membrane obtained in the step (1) from the planar aluminum foil, then putting the stripped polymer nanofiber membrane into 80-120 mL of alcohol reagent, and carrying out infiltration treatment for 0.5-2.0 h;
(3) Putting the polymer nanofiber membrane subjected to the infiltration treatment in the step (2) into 50-100 mL of dopamine solution with the concentration of 7.5-8.0 mg/mL, reacting for 12-48 hours at room temperature, taking out, sequentially washing the reacted film with distilled water and the same alcohol reagent as in the step (2) for 3-5 times respectively, and then drying under vacuum to obtain the polymer nanofiber membrane subjected to the polydopamine modification treatment;
(4) Fe is added to 3 O 4 NPs are added into MXene dispersion liquid to prepare Fe 3 O 4 MXene@Fe with mass fraction of NPs of 1-5% 3 O 4 A dispersion;
(5) The MXene@Fe obtained in the step (4) is treated 3 O 4 The dispersion liquid is deposited on the surface of the polymer nanofiber membrane obtained in the step (3) by a spraying method; and (3) respectively cleaning the polymer nanofiber membrane with distilled water and the same alcohol reagent in the step (2) for 3-5 times, and drying under vacuum to obtain the flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing properties.
2. The method for preparing the flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing properties according to claim 1, wherein the method comprises the following steps: the polymer in the step (1) is one of polymethyl methacrylate, polystyrene, polyacrylonitrile, sulfonated polyether ether ketone or polyacrylamide.
3. The method for preparing the flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing properties according to claim 1, wherein the method comprises the following steps: the organic solvent in the step (1) is one or a mixture of more of N, N-dimethylformamide, N-dimethylacetamide, dimethyl sulfoxide, acetone, chloroform, dichloromethane and ethanol.
4. The method for preparing the flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing properties according to claim 1, wherein the method comprises the following steps: the mass fraction of the polymer in the precursor solution in the step (1) is 6-10%.
5. The method for preparing the flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing properties according to claim 1, wherein the method comprises the following steps: the alcohol reagent in the step (2) and the step (3) is one or more than two of absolute ethyl alcohol, n-propyl alcohol, n-butyl alcohol, ethylene glycol and glycerol.
6. The method for preparing the flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing properties according to claim 1, wherein the method comprises the following steps: the average thickness of the MXene nano-sheet in the step (4) is 5.0+/-0.5 nm, fe 3 O 4 The particle size distribution of NPs was 282.57.+ -.6 nm.
7. The method for preparing the flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing properties according to claim 1, wherein the method comprises the following steps: the spraying speed in the step (5) is 300-500 rpm/min, and the spraying time is 1.5-3.0 min.
8. A flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing properties, characterized by: is prepared by the method of any one of claims 1 to 7.
9. A flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing properties according to claim 8, wherein: the fiber membrane has a multi-stage coarse structure, and the average diameter of the fiber membrane is 333-431 nm.
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