CN111809439A - Flexible high-strength MXene-based electromagnetic shielding composite film and preparation method thereof - Google Patents
Flexible high-strength MXene-based electromagnetic shielding composite film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a flexible high-strength MXene-based electromagnetic shielding composite film which comprises a conductive layer Ti3C2TxMXene/silver nanowire and polymer reinforced layer aramid nanofiber, Ti3C2TxThe mass fraction of the MXene/silver nanowire conducting layer is 10-80%; ti3C2TxThe mass ratio of MXene to the silver nanowires is 10: 0.5-10: 1.5. The invention also discloses a preparation method of the flexible high-strength MXene-based electromagnetic shielding composite film, and the composite film prepared by the invention has excellent flexibility and mechanical properties, good conductivity and wide-frequency high electromagnetic shielding efficiency, and can meet the requirements of aerospace, military engineering and artificial intelligenceCan be applied to the field of flexible wearable electronic equipment.
Description
Technical Field
The invention belongs to the technical field of electromagnetic shielding composite materials, relates to a flexible high-strength MXene-based electromagnetic shielding composite film, and further relates to a preparation method of the film.
Background
With the rapid development of high-power, high-density and high-integration technologies of electronic and communication equipment, the problems of electromagnetic radiation, electromagnetic interference, information leakage and the like caused by electromagnetic waves are increasingly serious, the development of the fields of aerospace, military engineering, artificial intelligence, flexible wearable electronic equipment and the like is limited, and meanwhile, the health of human bodies is threatened. In order to guarantee the operation reliability and information safety of precise electronic components and protect human health, high-efficiency electromagnetic shielding materials are needed to attenuate electromagnetic wave energy. Particularly, with the rapid development and wide application of the fifth generation (5G) and sixth generation (6G) communication technologies, the related fields put higher demands on electromagnetic shielding materials. Metal materials are widely used for electromagnetic shielding materials due to their high electrical conductivity and high electromagnetic shielding effectiveness, but their disadvantages of high density, low flexibility, poor chemical resistance and poor workability severely limit their application in some special fields. The polymer-based conductive composite material composed of the polymer matrix and the conductive filler (such as graphene, multi-walled carbon nanotubes, metal nanoparticles, nanowires and hybrids thereof) has the advantages of light weight, chemical corrosion resistance, easiness in processing and forming, stable shielding performance and the like, but has the defects of low conductivity, poorer Electromagnetic shielding performance (EMI SE) than that of a metal material and the like. Since the polymer-based conductive composite has a high percolation threshold, a high filler content and a large thickness are generally required to obtain a desired conductivity and electromagnetic shielding property, resulting in a decrease in mechanical properties (particularly flexibility and strength) and processability thereof.
MXenes is a novel two-dimensional (2D) transition metal carbide and/or nitride nano material with the molecular formula of Mn+1XnTxWherein M is a transition metal element, X is a carbon and/or nitrogen element, TxAre functional surface end groups (e.g., -O, -F, and-OH). Due to excellent metal conductivity, hydrophilicity and good interface interaction with polymers, MXenes is widely used in the fields of energy storage, strain sensing, electric heating, wave absorption (MA), electromagnetic shielding and the like. However, although the MXene-based electromagnetic shielding material has high conductivity and high electromagnetic shielding effectiveness, its low flexibility and mechanical properties limit the application of the material in the fields of aerospace, military engineering, artificial intelligence, flexible wearable electronic devices, and the like. The incorporation of polymers (such as polyvinyl alcohol, PEDOT: PSS, polyaniline) and one-dimensional (1D) organic nanofibers (such as nanocellulose) into MXene films is a common method of reinforcing MXene films. The MXene film is reinforced and toughened by the polymer molecular chain and the organic nano-fiber through mechanical interlocking. However, the mechanical properties of the currently used polymer and organic nanofiber are low, and the interface interaction with MXene is weak, so that the reinforcing and toughening effects on MXene films are limited. In addition, the introduced polymer molecular chains and organic nanofibers increase the contact resistance between adjacent MXene sheet layers, thereby causing the reduction of the conductivity and electromagnetic shielding performance of the composite film.
Therefore, there is an urgent need to simply and effectively prepare an MXene-based electromagnetic shielding material with ultra-flexibility, high strength, broad frequency and high electromagnetic shielding performance while maintaining high conductivity of MXene.
Disclosure of Invention
The invention aims to provide a flexible high-strength MXene-based electromagnetic shielding composite film which has excellent flexibility and mechanical properties, good conductivity and broadband high electromagnetic shielding efficiency and can meet the application requirements in the fields of aerospace, military engineering, artificial intelligence and flexible wearable electronic equipment.
The first technical scheme adopted by the invention is that the flexible high-strength MXene-based electromagnetic shielding composite film comprisesConductive layer Ti3C2TxMXene/silver nanowire and polymer reinforced layer aramid nanofiber, Ti3C2TxThe mass fraction of the MXene/silver nanowire conducting layer is 10-80%; ti3C2TxThe mass ratio of MXene to the silver nanowires is 10: 0.5-10: 1.5.
The first technical solution adopted by the present invention is further characterized in that,
Ti3C2TxMXene is prepared from MAX-phase ceramic with 200-400 meshes as a raw material in a mixed solution of hydrochloric acid and lithium fluoride, and the size of a lamella is 100-300 nm.
The silver nanowires have a diameter of 20-50 nm and a length-diameter ratio of 500-1000.
The aramid nano-fiber is prepared from one of para-aramid yarn fiber, para-aramid chopped fiber and para-aramid fabric fiber serving as a raw material in a potassium hydroxide and dimethyl sulfoxide mixed solution system, and is 5-20 nm in diameter and 5-20 microns in length.
The hot-pressing pressure of the flexible high-strength MXene-based electromagnetic shielding composite film is 0.5-5 MPa, and the hot-pressing temperature is 50-80 ℃.
The second technical scheme adopted by the invention is that the preparation method of the flexible high-strength MXene-based electromagnetic shielding composite film comprises the following steps:
step 1, adding para-aramid fibers into a potassium hydroxide and dimethyl sulfoxide mixed solution, and stirring at room temperature to obtain a deep red aramid nanofiber dispersion liquid;
step 2, adding MAX ceramic powder into a mixed solution of hydrochloric acid and lithium fluoride, stirring at 35 ℃ to obtain a black solution, and centrifugally cleaning to obtain blackish green Ti3C2TxMXene dispersion liquid;
step 3, dispersing silver nanowires with the diameter of 20-50 nm and the length-diameter ratio of 500-1000 into deionized water, and performing ultrasonic dispersion to obtain a silver nanowire dispersion liquid;
step 4, Ti obtained in the step 23C2TxMXene dispersion and step 3The silver nanowire dispersion liquid is blended and subjected to ultrasonic dispersion to obtain Ti3C2TxMXene/silver nanowire mixed dispersion liquid;
step 5, carrying out vacuum-assisted suction filtration on the aramid nano-fiber dispersion liquid obtained in the step 1 through an organic filter membrane with the aperture of 0.22-0.45 mu m to obtain a colloidal aramid nano-fiber sheet;
step 6, the Ti obtained in the step 4 is treated3C2TxAdding the MXene/silver nanowire mixed dispersion liquid, and continuously performing vacuum-assisted suction filtration to obtain the colloid Ti with the double-layer structure3C2TxMXene/silver nanowire-aramid nanofiber sheet;
step 7, the colloidal double-layer structure Ti obtained in the step 6 is processed3C2TxCarrying out vacuum hot-pressing drying on the MXene/silver nanowire-aramid nanofiber sheet at the temperature of 50-80 ℃ for 24h to obtain the Ti with the flexible high-strength double-layer structure3C2TxMXene/silver nanowire-aramid nanofiber electromagnetic shielding composite film.
The second technical solution of the present invention is also characterized in that,
in the step 1, the aramid nano-fiber is prepared in a potassium hydroxide and dimethyl sulfoxide mixed solution system by taking one of para-aramid yarn fiber, para-aramid chopped fiber and para-aramid fabric fiber as a raw material, wherein the proportion of the para-aramid fiber, the potassium hydroxide and the dimethyl sulfoxide is 0.5-1.5 g: 1-2 g: 100-1000 mL.
In the step 1, the aramid nano-fiber dispersion liquid can be uniformly dispersed in water, the diameter of the aramid nano-fiber is 5-20 nm, the length of the aramid nano-fiber is 5-20 microns, the concentration of the aramid nano-fiber is 0.2-2 mg/mL, the stirring speed is 500-1000 r/min, and the stirring time is 3-7 days.
Step 2 of Ti3C2TxMXene is prepared by taking MAX-phase ceramic with 200-400 meshes as a raw material in a mixed solution of hydrochloric acid and lithium fluoride, wherein the ratio of MAX-phase ceramic to lithium fluoride to hydrochloric acid is 1-2 g: 20-40 mL, and Ti3C2TxThe size of the MXene lamella is 100-300 nm;
in the step 2, the stirring speed is 500-1000 r/min, the stirring time is 20-24 h, the centrifugal speed is 3000-4000 r/min, and the centrifugal time is 50-80 min;
in the step 3, the concentration of the silver nanowires in the silver nanowire dispersion liquid is 0.5-5 mg/mL, and the ultrasonic power is 200-300W.
And 7, the hot pressure intensity is 0.5-5 MPa.
The invention has the beneficial effects that the invention adopts high-conductivity two-dimensional Ti3C2TxMXene nanosheet layer and high length-diameter ratio one-dimensional silver nanowire are used as conductive materials to construct a three-dimensional conductive network structure, and Ti3C2TxHydroxyl on the surface of MXene and carbonyl on the surface of the silver nanowire form hydrogen bond action to endow Ti3C2TxThe MXene-based electromagnetic shielding composite film has excellent conductivity and electromagnetic shielding performance; uses flexible high-strength aramid nano-fiber as high-performance polymer reinforced layer, because of Ti3C2TxStrong hydrogen bond action is formed between hydroxyl on the MXene surface and carbonyl in the aramid nano-fiber, so that Ti is formed3C2TxThe MXene-based electromagnetic shielding composite film has good interface interaction and high mechanical property. The design of the double-layer structure ensures that the prepared ultrathin Ti3C2TxThe MXene-based electromagnetic shielding composite film not only has Ti3C2TxThe MXene/silver nanowire conducting layer has high conductivity and high electromagnetic shielding efficiency, and the ultra-flexibility and high mechanical property of the aramid nanofiber reinforcing layer, so that the ultra-thin Ti is realized3C2TxThe MXene-based electromagnetic shielding composite film is cooperatively modified with high mechanical property and high electromagnetic shielding property. The preparation method adopted by the invention is simple and effective, has strong operation controllability, can be used for large-scale manufacturing and is easy for commercial production. Prepared ultrathin Ti3C2TxThe MXene-based electromagnetic shielding composite film has good flexibility, excellent mechanical property, high conductivity and outstanding broadband electromagnetic shielding performance, and is suitable for the fields of aerospace, military engineering, artificial intelligence, flexible wearable electronic equipment and the like.
Drawings
FIG. 1 shows a double-layer Ti structure obtained in example 2 of the method for preparing a flexible high-strength MXene-based electromagnetic shielding composite film according to the present invention3C2TxDigital photos provided by the MXene/silver nanowire-aramid nanofiber composite film;
FIG. 2 shows a double-layer Ti structure obtained in embodiment 2 of the method for preparing a flexible high-strength MXene-based electromagnetic shielding composite film of the present invention3C2TxA surface electron Scanning Electron Microscope (SEM) image provided by the MXene/silver nanowire-aramid nanofiber composite film;
FIG. 3 shows a double-layer Ti structure obtained in embodiment 2 of the method for preparing a flexible high-strength MXene-based electromagnetic shielding composite film of the present invention3C2TxAnd a section electron Scanning Electron Microscope (SEM) image provided by the MXene/silver nanowire-aramid nanofiber composite film.
FIG. 4 shows a double-layer Ti structure obtained in examples 1 to 5 of a method for preparing a flexible high-strength MXene-based electromagnetic shielding composite film according to the present invention3C2TxSchematic microstructure diagram of MXene/silver nanowire-aramid nanofiber composite film.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a flexible high-strength MXene-based electromagnetic shielding composite film, which comprises Ti3C2TxMXene, silver nanowires and aramid nanofibers; flexible high-strength MXene-based electromagnetic shielding composite film and Ti3C2TxMXene/silver nanowire is a high-conductivity layer, and aramid nanofiber with flexibility and high strength is used as a high-performance enhancement layer; ti in flexible high-strength MXene-based electromagnetic shielding material3C2TxThe mass fraction of the MXene/silver nanowire is 10-80%; ti in flexible high-strength MXene-based electromagnetic shielding material3C2TxThe mass ratio of MXene to the silver nanowires is 10: 0.5-10: 1.5; the aramid nano-fiber is prepared from one of para-aramid yarn fiber, para-aramid chopped fiber and para-aramid fabric fiber serving as a raw material in a potassium hydroxide and dimethyl sulfoxide mixed solution systemThe diameter of the aramid nano fiber is 5-20 nm, and the length of the aramid nano fiber is 5-20 mu m; ti3C2TxMXene is prepared by taking MAX-phase ceramic with 200-400 meshes as a raw material in a mixed solution of hydrochloric acid and lithium fluoride, and the size of a lamella is 100-300 nm; the diameter of the silver nanowire is 20-50 nm, and the length-diameter ratio is 500-1000; the hot-pressing pressure of the flexible high-strength MXene-based electromagnetic shielding composite film is 0.5-5 MPa, and the hot-pressing temperature is 50-80 ℃; silver nanowires in the flexible high-strength MXene-based electromagnetic shielding composite film are uniformly distributed in Ti3C2TxBetween MXene two-dimensional lamellae, and Ti3C2TxMXene constructs a high-efficiency three-dimensional conductive network, so that the conductivity and the electromagnetic shielding performance of the composite film are obviously improved; the aramid nanofibers in the flexible high-strength MXene-based electromagnetic shielding composite film are used as a high-performance polymer reinforcing layer, so that the flexibility and the mechanical property of the composite film are effectively improved.
The invention discloses a preparation method of a flexible high-strength MXene-based electromagnetic shielding composite film, which comprises the following steps:
step 1, soaking para-aramid fibers into a mixed solution of potassium hydroxide and dimethyl sulfoxide, and stirring at room temperature to obtain a deep red aramid nanofiber dispersion liquid; the diameter of the aramid nano-fiber in the aramid nano-fiber dispersion liquid is 5-20 nm, and the length of the aramid nano-fiber in the aramid nano-fiber dispersion liquid is 5-20 mu m;
in the step 1, the aramid nano-fiber is prepared in a potassium hydroxide and dimethyl sulfoxide mixed solution system by taking one of para-aramid yarn fiber, para-aramid chopped fiber and para-aramid fabric fiber as a raw material, wherein the proportion of the para-aramid fiber, the potassium hydroxide and the dimethyl sulfoxide is 0.5-1.5 g: 1-2 g: 100-1000 mL;
the aramid nano-fiber dispersion liquid in the step 1 can be uniformly dispersed in deionized water, the diameter of the aramid nano-fiber is 5-20 nm, the length of the aramid nano-fiber is 5-20 microns, and the concentration of the aramid nano-fiber is 0.2-2 mg/mL;
wherein the stirring speed in the step 1 is 500-1000 r/min, and the stirring time is 3-7 days.
Step 2, adding MAX phase ceramic powder into mixed solution of hydrochloric acid and lithium fluorideStirring at 35 deg.C to obtain black solution, centrifuging, and cleaning to obtain dark green Ti3C2TxMXene dispersion liquid; ti3C2TxTi in MXene dispersion3C2TxThe size of the MXene lamella is 100-300 nm;
wherein in step 2 Ti3C2TxMXene is prepared by taking MAX-phase ceramic with 200-400 meshes as a raw material in a mixed solution system of hydrochloric acid and lithium fluoride, wherein the ratio of MAX-phase ceramic to lithium fluoride to hydrochloric acid is 1-2 g: 20-40 mL;
wherein in step 2 Ti3C2TxMXene can be uniformly dispersed in deionized water, Ti3C2TxThe size of the MXene lamella is 100-300 nm;
wherein the stirring speed in the step 2 is 500-1000 r/min, and the stirring time is 24-48 h;
wherein the centrifugation speed in the step 2 is 3000-4000 r/min, and the centrifugation time is 50-80 min.
Step 3, dispersing silver nanowires with the diameter of 20-50 nm and the length-diameter ratio of 500-1000 into deionized water, and performing ultrasonic dispersion to obtain a silver nanowire dispersion liquid;
wherein the concentration of the silver nanowires in the silver nanowire dispersion liquid in the step 3 is 0.5-5 mg/mL, and the ultrasonic power is 200-300W;
step 4, Ti obtained in the step 23C2TxMixing MXene dispersion liquid with the silver nanowire dispersion liquid obtained in the step 3, and performing ultrasonic dispersion to obtain Ti3C2TxMXene/silver nanowire mixed dispersion liquid;
wherein in step 4 Ti3C2TxTi in MXene/silver nanowire mixed dispersion liquid3C2TxThe mass ratio of MXene to the silver nanowires is 10: 0.5-10: 1.5.
Step 5, carrying out vacuum-assisted suction filtration on the aramid nano-fiber dispersion liquid obtained in the step 1 through an organic filter membrane with the aperture of 0.22-0.45 mu m to obtain a colloidal aramid nano-fiber sheet;
step 6, step 4Obtained Ti3C2TxAdding the MXene/silver nanowire mixed dispersion liquid, and continuously performing vacuum-assisted suction filtration to obtain the colloid Ti with the double-layer structure3C2TxMXene/silver nanowire-aramid nanofiber sheet;
step 7, the colloidal double-layer structure Ti obtained in the step 6 is processed3C2TxCarrying out vacuum hot-pressing drying on the MXene/silver nanowire-aramid nanofiber sheet at the temperature of 50-80 ℃ for 24h to obtain the Ti with the flexible high-strength double-layer structure3C2TxMXene/silver nanowire-aramid nanofiber electromagnetic shielding composite film;
and (4) the hot-pressing pressure of the flexible high-strength MXene-based electromagnetic shielding composite film obtained in the step (7) is 0.5-5 MPa.
Example 1
A flexible high-strength MXene-based electromagnetic shielding composite film contains Ti3C2TxMXene, silver nanowires and aramid nanofibers; ti in flexible high-strength MXene-based electromagnetic shielding composite film3C2TxThe mass fraction of MXene/silver nanowires is 10 percent; ti in flexible high-strength MXene-based electromagnetic shielding composite film3C2TxThe mass ratio of MXene to silver nanowires is 10: 0.5; the aramid nano-fiber is prepared by taking para-aramid yarn fiber as a raw material in a potassium hydroxide and dimethyl sulfoxide mixed solution, and the diameter of the aramid nano-fiber is 5-20 nm, and the length of the aramid nano-fiber is 5-20 mu m; ti3C2TxThe size of the MXene lamella is 100-300 nm; the diameter of the silver nanowire is 20-50 nm, and the length-diameter ratio is 500-1000; the hot-pressing pressure of the flexible high-strength MXene-based electromagnetic shielding composite film is 0.5 MPa.
The preparation method of the flexible high-strength MXene-based electromagnetic shielding composite film comprises the following steps: adding para-aramid yarn into a potassium hydroxide and dimethyl sulfoxide solution system, controlling the proportion of the para-aramid yarn to be 0.5g, 2g and 100mL, stirring for 7 days at room temperature, and adding deionized water to obtain a deep red aramid nanofiber dispersion liquid with the concentration of 0.2mg/mL, wherein the diameter of the aramid nanofiber is 5-20 nm, and the length of the aramid nanofiber is 5-20 microns; adding 400-mesh MAX ceramic powder into hydrochloric acid for neutralizing lithium fluoride mixed solutionControlling the ratio of the three components to be 1g:2g:40mL, and stirring the mixture for 24 hours at 35 ℃ to obtain black Ti3C2TxCentrifuging MXene solution with 3500r/min deionized water to obtain dark green Ti3C2TxMXene dispersion liquid, wherein the size of the prepared MXene lamella is 100-300 nm; dispersing silver nanowires with the diameter of 20-50 nm and the length-diameter ratio of 500-1000 into deionized water, and performing ultrasonic treatment at 200W to obtain silver nanowire dispersion liquid with the concentration of 0.5 mg/mL; mixing Ti3C2TxMixing MXene dispersion liquid and silver nanowire dispersion liquid, and performing 100W ultrasonic dispersion; carrying out vacuum-assisted suction filtration on the aramid nano-fiber dispersion liquid through an organic filter membrane with the aperture of 0.22 mu m to obtain a colloidal aramid nano-fiber sheet; mixing Ti3C2TxAdding the MXene/silver nanowire dispersion liquid, and continuously performing suction filtration to obtain the colloidal double-layer structure Ti3C2TxMXene/silver nanowire-aramid nanofiber sheet; the obtained colloidal bilayer structure Ti3C2TxHot-pressing and drying the MXene/silver nanowire-aramid nanofiber sheet at the temperature of 50 ℃ for 24 hours at the hot-pressing pressure of 0.5MPa to obtain Ti3C2TxThe mass fraction of MXene/silver nanowire is 10 percent and the Ti content is3C2TxFlexible high-strength double-layer structure Ti with MXene/silver nanowire mass ratio of 10:0.53C2TxMXene/silver nanowire-aramid nanofiber electromagnetic shielding composite film. Obtained Ti3C2TxThe MXene-based electromagnetic shielding composite film has the conductivity of 152.6S/cm, the tensile strength of 213.7MPa, the tensile modulus of 3.4GPa and the electromagnetic shielding effectiveness of 36.8dB in an X-band (8.2-12.4 GHz).
Example 2
The flexible high-strength MXene-based electromagnetic shielding composite film comprises Ti3C2TxMXene, silver nanowires and aramid nanofibers; ti in flexible high-strength MXene-based electromagnetic shielding composite film3C2TxThe mass fraction of MXene/silver nanowires is 20 percent; ti in flexible high-strength MXene-based electromagnetic shielding composite film3C2TxThe mass ratio of MXene to silver nanowires is 10: 1; aramid fiber sodiumThe rice fiber is prepared by taking para-aramid chopped fiber as a raw material in a potassium hydroxide and dimethyl sulfoxide mixed solution, and the aramid nano-fiber has the diameter of 5-20 nm and the length of 5-20 microns; ti3C2TxThe size of the MXene lamella is 100-300 nm; the diameter of the silver nanowire is 20-50 nm, and the length-diameter ratio is 500-1000; the hot-pressing pressure of the flexible high-strength MXene-based electromagnetic shielding composite film is 1 MPa.
A preparation method of a flexible high-strength MXene-based electromagnetic shielding composite film comprises the following steps: adding para-aramid chopped fibers into a potassium hydroxide and dimethyl sulfoxide solution system, controlling the proportion of the para-aramid chopped fibers to be 1g:1.5g:500mL, stirring at room temperature for 7 days, and adding deionized water to obtain a deep red aramid nanofiber dispersion liquid with the concentration of 0.5mg/mL, wherein the diameter of the aramid nanofiber is 5-20 nm, and the length of the aramid nanofiber is 5-20 microns; adding 400-mesh MAX ceramic powder into hydrochloric acid and lithium fluoride mixed solution, controlling the proportion of the three to be 1g:1g:20mL, and stirring at 35 ℃ for 24h to obtain black Ti3C2TxCentrifuging MXene solution with 3500r/min deionized water to obtain dark green Ti3C2TxMXene dispersion liquid, wherein the size of the prepared MXene lamella is 100-300 nm; dispersing silver nanowires with the diameter of 20-50 nm and the length-diameter ratio of 500-1000 into deionized water, and performing ultrasonic treatment at 200W to obtain silver nanowire dispersion liquid with the concentration of 1 mg/mL; mixing Ti3C2TxMixing MXene dispersion liquid and silver nanowire dispersion liquid, and performing 250W ultrasonic dispersion; carrying out vacuum-assisted suction filtration on the aramid nano-fiber dispersion liquid through an organic filter membrane with the aperture of 0.22 mu m to obtain a colloidal aramid nano-fiber sheet; mixing Ti3C2TxAdding the MXene/silver nanowire dispersion liquid, and continuously performing suction filtration to obtain the colloidal double-layer structure Ti3C2TxMXene/silver nanowire-aramid nanofiber sheet; the obtained colloidal bilayer structure Ti3C2TxHot-pressing and drying the MXene/silver nanowire-aramid nanofiber sheet at the temperature of 60 ℃ for 24h under the hot-pressing pressure of 1MPa to obtain Ti3C2TxMXene/silver nanowire mass fraction of 20% and Ti3C2TxMXeneFlexible high-strength double-layer structure Ti with silver nanowire mass ratio of 10:13C2TxMXene/silver nanowire-aramid nanofiber electromagnetic shielding composite film. Obtained Ti3C2TxThe MXene-based electromagnetic shielding composite film has the conductivity of 922S/cm, the tensile strength of 235.9MPa, the tensile modulus of 4.1GPa and the electromagnetic shielding effectiveness of 48.1dB in an X-wave band (8.2-12.4 GHz).
Example 2 obtained double layer Structure Ti3C2TxA digital photo provided by the MXene/silver nanowire-aramid nanofiber composite film is shown in FIG. 1; example 2 obtained double layer Structure Ti3C2TxScanning Electron Microscope (SEM) images of the surface and the cross section provided by the MXene/silver nanowire-aramid nanofiber composite film are respectively shown in fig. 2 and fig. 3.
Example 3
The flexible high-strength MXene-based electromagnetic shielding composite film comprises Ti3C2TxMXene, silver nanowires and aramid nanofibers; ti in flexible high-strength MXene-based electromagnetic shielding composite film3C2TxThe mass fraction of MXene/silver nanowires is 40%; ti in flexible high-strength MXene-based electromagnetic shielding composite film3C2TxThe mass ratio of MXene to silver nanowires is 10: 1.5; the aramid nano-fiber is prepared by taking para-aramid fabric fiber as a raw material in a potassium hydroxide and dimethyl sulfoxide mixed solution, and the diameter of the aramid nano-fiber is 5-20 nm, and the length of the aramid nano-fiber is 5-20 mu m; ti3C2TxThe size of the MXene lamella is 100-300 nm; the diameter of the silver nanowire is 20-50 nm, and the length-diameter ratio is 500-1000; the hot-pressing pressure and the hot-pressing temperature of the flexible high-strength MXene-based electromagnetic shielding composite film are respectively 2MPa and 80 ℃.
The preparation method of the flexible high-strength MXene-based electromagnetic shielding composite film comprises the following steps: adding para-aramid fabric fibers into a potassium hydroxide and dimethyl sulfoxide solution system, controlling the proportion of the para-aramid fabric fibers to be 1g:1.5g:1000mL, stirring for 7 days at room temperature, adding deionized water to obtain a deep red aramid nanofiber dispersion liquid with the concentration of 0.5mg/mL, wherein the diameter of the aramid nanofiber is 5-20 nm, and the length of the aramid nanofiber is 5-E20 μm; adding 400-mesh MAX ceramic powder into hydrochloric acid and lithium fluoride mixed solution, controlling the proportion of the three to be 1g:1g:20mL, and stirring at 35 ℃ for 24h to obtain black Ti3C2TxCentrifuging MXene solution with 3500r/min deionized water to obtain dark green Ti3C2TxMXene dispersion, Ti obtained3C2TxThe size of the MXene lamella is 100-300 nm; dispersing silver nanowires with the diameter of 20-50 nm and the length-diameter ratio of 500-1000 into deionized water, and performing 300W ultrasonic treatment to obtain silver nanowire dispersion liquid with the concentration of 2 mg/mL; mixing Ti3C2TxMixing MXene dispersion liquid and silver nanowire dispersion liquid, and performing 250W ultrasonic dispersion; carrying out vacuum-assisted suction filtration on the aramid nano-fiber dispersion liquid through an organic filter membrane with the aperture of 0.45 mu m to obtain a colloidal aramid nano-fiber sheet; mixing Ti3C2TxAdding the MXene/silver nanowire dispersion liquid, and continuously performing suction filtration to obtain the colloidal double-layer structure Ti3C2TxMXene/silver nanowire-aramid nanofiber sheet; the obtained colloidal bilayer structure Ti3C2TxHot-pressing and drying the MXene/silver nanowire-aramid nanofiber sheet at the temperature of 70 ℃ for 24 hours at the hot-pressing pressure of 2MPa to obtain Ti3C2TxMXene/silver nanowire mass fraction of 40% and Ti3C2TxFlexible high-strength double-layer structure Ti with MXene/silver nanowire mass ratio of 10:1.53C2TxMXene/silver nanowire-aramid nanofiber electromagnetic shielding composite film. Obtained Ti3C2TxThe MXene-based electromagnetic shielding composite film has the conductivity of 1847.5S/cm, the tensile strength of 176.5MPa, the tensile modulus of 3.8GPa and the electromagnetic shielding effectiveness of 56.2dB in an X-wave band (8.2-12.4 GHz).
Example 4
The flexible high-strength MXene-based electromagnetic shielding composite film comprises Ti3C2TxMXene, silver nanowires and aramid nanofibers; ti in flexible high-strength MXene-based electromagnetic shielding composite film3C2TxThe mass fraction of MXene/silver nanowires is 60 percent; flexible high-strength MXene baseTi in electromagnetic shielding composite film3C2TxThe mass ratio of MXene to silver nanowires is 10: 0.5; the aramid nano-fiber is prepared by taking para-aramid fabric fiber as a raw material in a potassium hydroxide and dimethyl sulfoxide mixed solution, and the diameter of the aramid nano-fiber is 5-20 nm, and the length of the aramid nano-fiber is 5-20 mu m; ti3C2TxThe size of the MXene lamella is 100-300 nm; the diameter of the silver nanowire is 20-50 nm, and the length-diameter ratio is 500-1000; the hot-pressing pressure of the flexible high-strength MXene-based electromagnetic shielding composite film is 4 MPa.
The preparation method of the flexible high-strength MXene-based electromagnetic shielding composite film comprises the following steps: adding para-aramid fabric fibers into a potassium hydroxide and dimethyl sulfoxide solution system, controlling the proportion of the para-aramid fabric fibers to be 1g:2g:200mL, stirring at room temperature for 7 days, and adding deionized water to obtain a deep red aramid nanofiber dispersion liquid with the concentration of 2mg/mL, wherein the diameter of the aramid nanofiber is 5-20 nm, and the length of the aramid nanofiber is 5-20 microns; adding 400-mesh MAX ceramic powder into hydrochloric acid and lithium fluoride mixed solution, controlling the proportion of the three to be 2g:1g:40mL, and stirring for 24h at 35 ℃ to obtain black Ti3C2TxCentrifuging MXene solution with 3500r/min deionized water to obtain dark green Ti3C2TxMXene dispersion liquid, wherein the size of the prepared MXene lamella is 100-300 nm; dispersing silver nanowires with the diameter of 20-50 nm and the length-diameter ratio of 500-1000 into deionized water, and performing ultrasonic treatment at 200W to obtain silver nanowire dispersion liquid with the concentration of 4 mg/mL; mixing Ti3C2TxMixing MXene dispersion liquid and silver nanowire dispersion liquid, and performing 250W ultrasonic dispersion; carrying out vacuum-assisted suction filtration on the aramid nano-fiber dispersion liquid through an organic filter membrane with the aperture of 0.22 mu m to obtain a colloidal aramid nano-fiber sheet; mixing Ti3C2TxAdding the MXene/silver nanowire dispersion liquid, and continuously performing suction filtration to obtain the colloidal double-layer structure Ti3C2TxMXene/silver nanowire-aramid nanofiber sheet; the obtained colloidal bilayer structure Ti3C2TxHot-pressing and drying the MXene/silver nanowire-aramid nanofiber sheet at the temperature of 80 ℃ for 24 hours at the hot-pressing pressure of 4MPa to obtain Ti3C2TxMXene/silver nanowire mass fraction of 60% and Ti3C2TxFlexible high-strength double-layer structure Ti with MXene/silver nanowire mass ratio of 10:0.53C2TxMXene/silver nanowire-aramid nanofiber electromagnetic shielding composite film. Obtained Ti3C2TxThe MXene-based electromagnetic shielding composite film has the conductivity of 2690.3S/cm, the tensile strength of 159.6MPa, the tensile modulus of 2.9GPa and the electromagnetic shielding effectiveness of 65.3dB in an X-wave band (8.2-12.4 GHz).
Example 5
The flexible high-strength MXene-based electromagnetic shielding composite film comprises Ti3C2TxMXene, silver nanowires and aramid nanofibers; ti in flexible high-strength MXene-based electromagnetic shielding composite film3C2TxThe mass fraction of MXene/silver nanowires is 80 percent; ti in flexible high-strength MXene-based electromagnetic shielding composite film3C2TxThe mass ratio of MXene to silver nanowires is 10: 1; the aramid nano-fiber is prepared by taking para-aramid fabric fiber as a raw material in a potassium hydroxide and dimethyl sulfoxide mixed solution, and the diameter of the aramid nano-fiber is 5-20 nm, and the length of the aramid nano-fiber is 5-20 mu m; ti3C2TxThe size of the MXene lamella is 100-300 nm; the diameter of the silver nanowire is 20-50 nm, and the length-diameter ratio is 500-1000; the hot-pressing pressure of the flexible high-strength MXene-based electromagnetic shielding composite film is 5 MPa.
The preparation method of the flexible high-strength MXene-based electromagnetic shielding composite film comprises the following steps: adding para-aramid fabric fibers into a potassium hydroxide and dimethyl sulfoxide solution system, controlling the proportion of the para-aramid fabric fibers to be 1g:1.5g:500mL, stirring at room temperature for 7 days, and adding deionized water to obtain a deep red aramid nanofiber dispersion liquid with the concentration of 0.5mg/mL, wherein the diameter of the aramid nanofiber is 5-20 nm, and the length of the aramid nanofiber is 5-20 microns; adding 400-mesh MAX ceramic powder into hydrochloric acid and lithium fluoride mixed solution, controlling the proportion of the three to be 1g:1g:20mL, and stirring at 35 ℃ for 24h to obtain black Ti3C2TxCentrifuging MXene solution with 3500r/min deionized water to obtain dark green Ti3C2TxMXene dispersion, Ti obtained3C2TxThe size of the MXene lamella is 100-300 nm; dispersing silver nanowires with the diameter of 20-50 nm and the length-diameter ratio of 500-1000 into deionized water, and performing ultrasonic treatment at 200W to obtain silver nanowire dispersion liquid with the concentration of 5 mg/mL; mixing Ti3C2TxMixing MXene dispersion liquid and silver nanowire dispersion liquid, and performing 250W ultrasonic dispersion; carrying out vacuum-assisted suction filtration on the aramid nano-fiber dispersion liquid through an organic filter membrane with the aperture of 0.45 mu m to obtain a colloidal aramid nano-fiber sheet; mixing Ti3C2TxAdding the MXene/silver nanowire dispersion liquid, and continuously performing suction filtration to obtain the colloidal double-layer structure Ti3C2TxMXene/silver nanowire-aramid nanofiber sheet; the obtained colloidal bilayer structure Ti3C2TxHot-pressing and drying the MXene/silver nanowire-aramid nanofiber sheet at the temperature of 60 ℃ for 24 hours at the hot-pressing pressure of 5MPa to obtain Ti3C2TxThe mass fraction of MXene/silver nanowire is 80 percent and the Ti content is3C2TxFlexible high-strength double-layer structure Ti with MXene/silver nanowire mass ratio of 10:13C2TxMXene/silver nanowire-aramid nanofiber electromagnetic shielding composite film. Obtained Ti3C2TxThe MXene-based electromagnetic shielding composite film has the conductivity of 3705.6S/cm, the tensile strength of 79.7MPa, the tensile modulus of 2.4GPa and the electromagnetic shielding effectiveness of 79.8dB in an X-wave band (8.2-12.4 GHz).
Double-layer structure Ti obtained in examples 1 to 53C2TxThe schematic microstructure of the MXene/silver nanowire-aramid nanofiber composite film is shown in FIG. 4.
Comparative example 1
A flexible aramid nano-fiber film is composed of aramid nano-fibers, silver-free nano-wires and Ti3C2TxMXene; the aramid nano-fiber is prepared from para-aramid chopped fibers serving as raw materials in a potassium hydroxide and dimethyl sulfoxide mixed solution system, and the diameter of the aramid nano-fiber is 5-20 nm, and the length of the aramid nano-fiber is 5-20 microns; hot-pressing pressure of flexible aramid nano-fiber filmIs 5 MPa.
A preparation method of a flexible high-strength flexible aramid nanofiber film comprises the following steps: adding para-aramid fibers into a potassium hydroxide and dimethyl sulfoxide solution system, controlling the proportion of the para-aramid fibers to be 1g:1.5g:500mL, stirring at room temperature for 7 days, and adding deionized water to obtain a deep red aramid nanofiber dispersion liquid with the concentration of 0.5mg/mL, wherein the diameter of the aramid nanofibers is 5-20 nm, and the length of the aramid nanofibers is 5-20 microns; carrying out vacuum-assisted suction filtration on the aramid nano-fiber dispersion liquid through a nylon filter membrane with the aperture of 0.22 mu m to obtain a wet aramid nano-fiber film; and (3) carrying out hot-pressing drying on the obtained wet aramid nano-fiber film at the temperature of 80 ℃ for 24 hours to obtain the aramid nano-fiber film. The obtained aramid nano-fiber film is an insulating material and has the tensile strength of 154.4 MPa.
Comparative example 2
MXene-based electromagnetic shielding composite film, Ti3C2TxThe MXene-based electromagnetic shielding film is made of Ti3C2TxMXene; ti3C2TxThe size of the MXene lamella is 100-300 nm; ti3C2TxThe hot pressing pressure of the MXene-based electromagnetic shielding material is 0.5 MPa.
A preparation method of an MXene-based electromagnetic shielding composite film comprises the following steps: adding 400-mesh MAX ceramic powder into hydrochloric acid for neutralizing a lithium fluoride system, controlling the proportion of the three to be 1g:1g:20mL, and stirring for one day at 35 ℃ to obtain black Ti3C2TxCentrifuging MXene solution with 3500r/min deionized water to obtain dark green Ti3C2TxMXene dispersion liquid, wherein the size of the prepared MXene lamella is 100-300 nm; mixing Ti3C2TxThe MXene dispersion liquid is subjected to vacuum-assisted suction filtration by a cellulose filter membrane with the aperture of 0.45 mu m to obtain colloidal Ti3C2TxMXene flakes; hot-pressing and drying the obtained wet MXene film at the temperature of 80 ℃ for 24h to obtain Ti3C2TxThe MXene film has the tensile strength of 14MPa, the tensile modulus of 0.79GPa and the electromagnetic shielding effectiveness of 51dB in an X wave band (8.2-12.4 GHz).
TABLE 1Shown as preparing Ti3C2TxThe embodiment and the comparative example of the MXene-based electromagnetic shielding composite film are compared with the conductivity, the electromagnetic shielding performance and the tensile performance of the prepared electromagnetic shielding composite film.
TABLE 1
As can be seen from Table 1, examples 1 to 5 are two-dimensional Ti with high conductivity3C2TxMXene nanosheet layer and high-length-diameter-ratio one-dimensional silver nanowire are used as conductive materials to construct a three-dimensional conductive network structure, flexible high-strength aramid nanofiber is used as a high-performance polymer reinforcing layer, and vacuum-assisted suction filtration and hot-pressing treatment are carried out to obtain flexible high-strength double-layer structure Ti3C2TxMXene/silver nanowire-aramid nanofiber electromagnetic shielding composite film. Comparative example 1 without Ti addition3C2TxMXene pure aramid nanofiber film, comparative example 2 pure Ti3C2TxMXene film. Compared with the pure aramid fiber nano-fiber film in the comparative example 1 and the pure Ti in the comparative example 23C2TxMXene electromagnetic shielding films, two-layer structure Ti in examples 1 to 53C2TxThe MXene/silver nanowire-aramid nanofiber electromagnetic shielding composite film has good flexibility, high tensile strength and modulus and excellent broadband electromagnetic shielding performance.
Claims (10)
1. The flexible high-strength MXene-based electromagnetic shielding composite film is characterized in that: comprising an electrically conductive layer Ti3C2TxMXene/silver nanowire and polymer reinforced layer aramid nanofiber, Ti3C2TxThe mass fraction of the MXene/silver nanowire conducting layer is 10-80%; ti3C2TxThe mass ratio of MXene to the silver nanowires is 10: 0.5-10: 1.5.
2. The flexible high-strength MXene-based electromagnetic shielding composite film according to claim 1, wherein: the Ti3C2TxMXene is prepared from MAX-phase ceramic with 200-400 meshes as a raw material in a mixed solution of hydrochloric acid and lithium fluoride, and the size of a lamella is 100-300 nm.
3. The flexible high-strength MXene-based electromagnetic shielding composite film according to claim 1, wherein: the silver nanowires have the diameter of 20-50 nm and the length-diameter ratio of 500-1000.
4. The flexible high-strength MXene-based electromagnetic shielding composite film according to claim 1, wherein: the aramid nano-fiber is prepared from one of para-aramid yarn fiber, para-aramid chopped fiber and para-aramid fabric fiber serving as a raw material in a potassium hydroxide and dimethyl sulfoxide mixed solution system, and is 5-20 nm in diameter and 5-20 microns in length.
5. The flexible high-strength MXene-based electromagnetic shielding composite film according to claim 1, wherein: the hot-pressing pressure of the flexible high-strength MXene-based electromagnetic shielding composite film is 0.5-5 MPa, and the hot-pressing temperature is 50-80 ℃.
6. The preparation method of the flexible high-strength MXene-based electromagnetic shielding composite film is characterized by comprising the following steps of:
step 1, adding para-aramid fibers into a potassium hydroxide and dimethyl sulfoxide mixed solution, and stirring at room temperature to obtain a deep red aramid nanofiber dispersion liquid;
step 2, adding MAX ceramic powder into a mixed solution of hydrochloric acid and lithium fluoride, stirring at 35 ℃ to obtain a black solution, and centrifugally cleaning to obtain blackish green Ti3C2TxMXene dispersion liquid;
step 3, dispersing silver nanowires with the diameter of 20-50 nm and the length-diameter ratio of 500-1000 into deionized water, and performing ultrasonic dispersion to obtain a silver nanowire dispersion liquid;
step 4, Ti obtained in the step 23C2TxMixing MXene dispersion liquid with the silver nanowire dispersion liquid obtained in the step 3, and performing ultrasonic dispersion to obtain Ti3C2TxMXene/silver nanowire mixed dispersion liquid;
step 5, carrying out vacuum-assisted suction filtration on the aramid nano-fiber dispersion liquid obtained in the step 1 through an organic filter membrane with the aperture of 0.22-0.45 mu m to obtain a colloidal aramid nano-fiber sheet;
step 6, the Ti obtained in the step 4 is treated3C2TxAdding the MXene/silver nanowire mixed dispersion liquid, and continuously performing vacuum-assisted suction filtration to obtain the colloid Ti with the double-layer structure3C2TxMXene/silver nanowire-aramid nanofiber sheet;
step 7, the colloidal double-layer structure Ti obtained in the step 6 is processed3C2TxCarrying out vacuum hot-pressing drying on the MXene/silver nanowire-aramid nanofiber sheet at the temperature of 50-80 ℃ for 24h to obtain the Ti with the flexible high-strength double-layer structure3C2TxMXene/silver nanowire-aramid nanofiber electromagnetic shielding composite film.
7. The preparation method of the flexible high-strength MXene-based electromagnetic shielding composite film according to claim 6, wherein the aramid nanofibers in step 1 are prepared from one of para-aramid yarn fibers, para-aramid chopped fibers and para-aramid fabric fibers as a raw material in a potassium hydroxide and dimethyl sulfoxide mixed solution system, and the proportion of the para-aramid fibers, the potassium hydroxide and the dimethyl sulfoxide is 0.5-1.5 g: 1-2 g: 100-1000 mL.
8. The preparation method of the flexible high-strength MXene-based electromagnetic shielding composite film according to claim 6, wherein the aramid nanofiber dispersion liquid in the step 1 can be uniformly dispersed in water, the diameter of the aramid nanofiber is 5-20 nm, the length of the aramid nanofiber is 5-20 μm, the concentration of the aramid nanofiber is 0.2-2 mg/mL, the stirring speed is 500-1000 r/min, and the stirring time is 3-7 days.
9. The method for preparing the flexible high-strength MXene-based electromagnetic shielding composite film as claimed in claim 6, wherein Ti in the step 23C2TxMXene is prepared by taking MAX-phase ceramic with 200-400 meshes as a raw material in a mixed solution of hydrochloric acid and lithium fluoride, wherein the ratio of MAX-phase ceramic to lithium fluoride to hydrochloric acid is 1-2 g: 20-40 mL, and Ti3C2TxThe size of the MXene lamella is 100-300 nm;
in the step 2, the stirring speed is 500-1000 r/min, the stirring time is 20-24 h, the centrifugal speed is 3000-4000 r/min, and the centrifugal time is 50-80 min;
in the step 3, the concentration of the silver nanowires in the silver nanowire dispersion liquid is 0.5-5 mg/mL, and the ultrasonic power is 200-300W.
10. The method for preparing the flexible high-strength MXene-based electromagnetic shielding composite film according to claim 6, wherein the hot-pressing pressure in the step 7 is 0.5-5 MPa.
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| CN114150496B (en) * | 2021-11-15 | 2023-07-28 | 吉林大学 | Flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing performances and preparation method thereof |
| CN114369284A (en) * | 2021-12-15 | 2022-04-19 | 西安理工大学 | Preparation method of CNF-MXene/silver nanowire porous composite film |
| CN114305339A (en) * | 2022-01-07 | 2022-04-12 | 吉林大学 | Degradable pressure sensor and preparation method thereof |
| CN114854199A (en) * | 2022-05-13 | 2022-08-05 | 青岛科技大学 | Sawtooth-shaped conductive silicone rubber nanocomposite and preparation method and application thereof |
| CN114854199B (en) * | 2022-05-13 | 2023-06-20 | 青岛科技大学 | Sawtooth-shaped conductive silicone rubber nanocomposite and preparation method and application thereof |
| CN115322430A (en) * | 2022-07-25 | 2022-11-11 | 成都飞机工业（集团）有限责任公司 | Wave-absorbing aerogel composite material and preparation method thereof |
| CN115322430B (en) * | 2022-07-25 | 2023-10-03 | 成都飞机工业（集团）有限责任公司 | Wave-absorbing aerogel composite material and preparation method thereof |
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