CN114222493A - High-toughness Mxene composite electromagnetic shielding film and preparation method and application thereof - Google Patents
High-toughness Mxene composite electromagnetic shielding film and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of electromagnetic shielding materials, and provides a high-toughness Mxene composite electromagnetic shielding film, a preparation method and application thereof, in order to solve the problems of poor impedance matching performance and poor mechanical property of the traditional Mxene material3C2TxMxene; secondly, uniformly accumulating PEDOT molecular chains on two sides of the Mxene plane through the electrostatic action of the PEDOT molecular chains with positive charges and polar functional groups on the surface of the Mxene to prepare the compoundAnd obtaining the Mxene and PEDOT composite film. The film prepared by the method realizes higher shielding effect and elongation at break, the electromagnetic shielding effect reaches 80dB, the elongation at break is improved by 3 times, and the film can be applied to microwave darkroom and wearable electromagnetic protection.
Description
Technical Field
The invention relates to the field of electromagnetic shielding materials, in particular to a high-toughness Mxene composite electromagnetic shielding film, and a preparation method and application thereof.
Background
With the rapid development of electronic information, the gradual widespread use of wireless communication, radar instruments, mobile electronic devices, and the like, serious microwave radiation is caused, the normal life of people is disturbed, the speed and reliability of information transmission are seriously affected, and the human health may even be affected. In order to prevent unwanted microwave radiation, great efforts are made to pursue high-performance microwave absorbers by constructing specific structural units or integrating appropriate components. Among them, various conventional microwave absorbers, such as magnetic metals and metal oxides, are reported to have desirable absorption capacity. However, some inherent disadvantages, including high fill rates, poor chemical stability and high density, have hindered their engineering applications. In contrast, in addition to the widespread use of energy storage, carbonaceous materials are also considered to be the most promising candidate for microwave absorption due to their light weight, chemical inertness, abundant resources, ease of preparation, tunable dielectric properties, and low cost.
Commercialization of emerging highly integrated fifth generation (5G) wireless devices requires electromagnetic shielding materials with ease of fabrication, light weight, minimal thickness, and higher shielding efficiency. Generally, an effective electromagnetic shielding material is a material having high electrical conductivity. However, the most commonly used conductive and non-magnetic shielding materials, such as metal and carbon-based nanomaterials, including graphene and carbon nanotubes, hardly meet these requirements. There is a need for lightweight, ultra-thin, and flexible electromagnetic interference shielding materials to protect electronic circuits and portable telecommunications devices and to eliminate cross-talk between devices and device components.
Recently, Mxene and its composite material have demonstrated excellent electromagnetic shielding performance, Ti at a thickness of 20um in the X-band frequency range (8.2 to 12.4GHz)3C2TxThe electromagnetic shielding performance of the composite material is 58dB, and the composite material shows excellent prospect in intelligent application of electronic products. This shielding performance is attributed to the high conductivity, rich surface termination and lamination of the Mxene film。
The problems of the prior art are as follows: even though control of reflection and absorption has been demonstrated, the overall electromagnetic shielding performance is not substantially improved. This is fundamentally due to poor impedance matching performance. In conclusion, the conventional Mxene material has the problems of poor electromagnetic shielding performance and poor mechanical properties such as easy oxidation and brittleness.
Disclosure of Invention
Aiming at the defects of the existing Mxene material, the invention adopts an Mxene and polymer PEDOT to form a nano sheet by in-situ compounding, which can effectively relieve the problem of interface impedance mismatching, realize higher electromagnetic shielding performance and simultaneously have high-toughness mechanical properties.
A preparation method of a high-toughness Mxene composite electromagnetic shielding film comprises the following steps:
s1 preparation of Ti3C2Tx Mxene，
S2, uniformly accumulating PEDOT molecular chains on two sides of a Mxene plane through the electrostatic action of the PEDOT molecular chains with positive charges and polar functional groups on the surface of the Mxene to prepare the Mxene and PEDOT composite film.
Preferably, S1 therein prepares Ti3C2TxThe Mxene step specifically comprises the following steps:
s11, adding LiF and HCl into the reaction kettle;
s12, mixing Ti3AlC2Adding the mixture into a reaction kettle one by one, and reacting under a stirring state;
s13, centrifuging the product after the reaction is finished, adding the bottom sediment after centrifugation into HCl, and stirring to obtain slurry;
s14, centrifuging the slurry to obtain viscous precipitate and upper liquid with black color;
s15, taking the viscous precipitate, adding deionized water into the viscous precipitate, performing ultrasonic treatment under the protection of inert atmosphere, and performing centrifugal treatment after ultrasonic treatment to obtain dark green dispersion liquid and obtain Ti3C2TxMxene gel solution.
S16, the gel solutionFiltering with water system filter membrane, vacuum drying, grinding into powder, and weighing Ti3C2TxConcentration of Mxene gel solution.
Preferably, the step S2 specifically includes the following steps:
s21, mixing PEDOT: aqueous PSS solution and Ti3C2TxThe Mxene gel solutions were mixed and,
s22, carrying out suction filtration on the mixed gel to prepare a film,
and S23, washing the film with deionized water.
Preferably, the process for preparing the high-toughness Mxene composite electromagnetic shielding film per unit comprises the following steps:
said S1 preparing Ti3C2TxThe specific process of the Mxene comprises the following steps:
s11, adding 1.56g of LiF and 20mL of 9mol/l HCL solution into a polytetrafluoroethylene kettle, and reacting at 30 ℃ for 2h to ensure that LiF is fully reacted;
s12, weighing 1g Ti3AlC2Slowly adding the mixture into a polytetrafluoroethylene kettle for several times within 10min, adjusting the rotating speed of the reactor to 500rpm, and reacting for 24 hours at 30 ℃;
s13, centrifuging the product after the reaction is finished, pouring out the upper liquid, adding the bottom sediment into 2mol/l HCL solution, and stirring for 2h to obtain slurry;
s14, centrifuging the slurry at 5000rpm for 5min until viscous precipitate and upper layer liquid turn black, stopping centrifuging, and pouring out the upper layer liquid;
s15, adding 50mL of deionized water into the viscous precipitate, performing ultrasonic treatment for 1.5h under the protection of inert atmosphere, and after the ultrasonic treatment is finished, performing centrifugal treatment at 2500rpm for 30min to obtain dark green dispersion liquid and obtain Ti3C2TxMxene gel solution;
s16, filtering the gel solution with 0.22 micron water-based filter membrane, drying, vacuum drying at 40 deg.C, drying, grinding into powder to obtain Ti3C2TxThe solubility of the Mxene gel solution is5mg/mL；
The S2 specifically includes the following steps:
s21, PEDOT: PSS aqueous solution with solid content of 6% and Ti3C2TxMxene gel solution, mixed in a volume ratio of 1:3,
s22, carrying out suction filtration on the mixture to prepare a film,
and S23, washing the film with deionized water to fully wash away the PSS component, and finally obtaining the Mxene and PEDOT composite film.
The invention also discloses the high-toughness Mxene composite electromagnetic shielding film prepared by the preparation method of the high-toughness Mxene composite electromagnetic shielding film, wherein the Mxene and PEDOT are compounded in situ to form a micron-sized sheet.
Preferably, the nano-scale flakes comprise PEDOT in an amount of 30% by weight.
Preferably, the molecular chain of the PEDOT is positively charged, and the positively charged PEDOT molecular chain and the Mxene surface polar functional group are uniformly accumulated on two sides of the Mxene plane through electrostatic interaction.
The invention also discloses application of the high-toughness Mxene composite electromagnetic shielding film prepared by the method, in particular application in the aspects of microwave darkrooms and wearable electromagnetic protection.
The Mxene @ PEDOT composite film provided by the invention has the beneficial effect of high electromagnetic shielding, and the principle is as follows: PEDOT is doped into Mxene to obviously weaken the polar functional group on the surface of the Mxene, so that an ultrathin film with higher conductivity is directly formed, and the electromagnetic shielding performance is improved. Meanwhile, the research result shows that compared with a pure Mxene sheet, the Mxene @ PEDOT composite material containing 30 wt% of PEDOT shows excellent mechanical property, and the elongation at break of the Mxene @ PEDOT composite material is improved by more than 3 times.
The Mxene @ PEDOT composite material has a two-dimensional planar structure which is very similar to that of Mxene, and the shielding performance of the Mxene @ PEDOT composite material is realized through electrostatic interaction of PEDOT and Mxene surface polar functional groups. The electrostatic interaction of the positively charged PEDOT molecular chain and the polar functional group on the surface of the Mxene is uniformly accumulated on two sides of the plane of the Mxene. Due to the exceptionally high electromagnetic wave absorption in the layered structure, the 20um thick Mxene @ PEDOT composite film showed an electromagnetic shielding performance of 80dB, which is greater than 58dB for a pure Mxene film measured 20um thick.
Drawings
Some specific embodiments of the invention will be described in detail hereinafter, by way of illustration and not limitation, with reference to the accompanying drawings. The same reference numbers in the drawings identify the same or similar elements or components. Those skilled in the art will appreciate that the drawings are not necessarily drawn to scale. In the drawings:
FIG. 1 is an SEM image of a Mxene @ PBTz-SO3Na thin film.
FIG. 2 is an SEM image of a Mxene @ PEDOT film.
FIG. 3 is XPS of Mxene @ PEDOT film.
FIG. 4 is electromagnetic shielding performance data for Mxene and Mxene @ PEDOT films.
FIG. 5 is a plot of pure Mxene, Mxene @ PBTz-SO3Na, and Mxene @ PEDOT sheet resistance over time.
Detailed Description
The first step is as follows: preparation of Ti3C2Tx Mxene
1. 1.56g LiF and 20mL 9M HCl are added into a polytetrafluoroethylene (100mL) kettle and reacted for 2h at 30 ℃ (LiF is fully reacted);
2. weigh 1g of Ti3AlC2Slowly adding the mixture into the kettle in small amount one by one (about 10min), adjusting the rotating speed of the reactor to 500rpm, and reacting for 24h at 30 ℃;
3. after the reaction is finished, pouring the product into a50 mL centrifuge tube for centrifugation, pouring out the upper liquid, adding the lower bottom precipitate into 2MHCl, and stirring for 2 h;
4. after the reaction is finished, pouring the slurry into two 50mL centrifuge tubes respectively, centrifuging for 7-8 times under the condition of 5min at 5000rpm until viscous precipitates and upper layer liquid are blackened, stopping centrifuging, and pouring the upper layer liquid;
5. and respectively adding 50mL of deionized water into the centrifuge tubes, pouring the mixture into a three-opening round-bottom flask, introducing inert gas into one opening, fixing a support into the other opening, and plugging the opening after the atmosphere is introduced into the last opening. Placing the above device in the containerAnd (5) carrying out ultrasonic treatment for 1.5h in an ultrasonic machine of the ice bag. And after the ultrasonic treatment is finished, pouring the liquid into a centrifugal tube, and centrifuging at 2500rpm for 30min to finally obtain the dark green dispersion liquid. The precipitate can be obtained by vacuum filtering with 0.22 μm water-based filter membrane, drying, standing in 40 deg.C vacuum drying oven for 2 hr, taking out, grinding into powder, and storing in a drier to obtain Mxene (Ti)3C2Tx) The solubility of the gel solution was 5 mg/mL.
The second step is that: and uniformly accumulating PEDOT molecular chains on two sides of the plane of the Mxene by the electrostatic action of the PEDOT molecular chains with positive charges and polar functional groups on the surface of the Mxene to prepare the Mxene and PEDOT composite membrane.
Poly (3, 4-ethylenedioxythiophene): aqueous solutions of poly (styrene sulfonate) (PEDOT: PSS) (i.e., Clevios P VP 4083 with 1.0-1.3% solids) were purchased from Heraeus, Germany, and prepared by mixing the following ingredients, PEDOT: and mixing the PSS aqueous solution and the Mxene gel at a ratio of 1:3(v/v), carrying out suction filtration to prepare a film, washing the film by using deionized water, and washing away the PSS component dissolved in water to finally obtain the Mxene @ PEDOT composite film.
It is believed that the blend of Mxene with other polymers will have reduced electromagnetic shielding properties and reduced conductivity as demonstrated by the discussion of a. iqbal, f. shahzad, et al, but that the blend of Mxene with PEDOSS in this embodiment has improved both properties.
And (3) testing conditions are as follows:
material characterization Ti was studied by scanning electron microscopy (SEM, aspect F50, FEI, USA)3C2TxAnd Ti3C2TxStructure and morphology of @ PEDOT film. SEM was also used to verify the thickness measurements originally made on a high precision length gauge (tolerance factor of ± 0.1 μm) of a Heidenhain instrument (germany). Chemical structural changes were examined using X-ray photoelectron spectroscopy (XPS, PHI 5000VersaProbe, Ulvac-PHI, japan) with Al K α as the X-ray source with a power of 25W. The EMI shielding efficiency of all samples was measured after standard calibration (using short offset, short circuit and load on both ports) using a WR-90 rectangular waveguide using a 2-port network analyzer (ENA5071C, Agilent technologies, USA) in the following frequency rangeThe amount of 8.2-12.4GHz (X band). The original and annealed samples were cut to 25X 12mm2Is slightly larger than the size of the opening of the sample rack by 22.84 multiplied by 10.14mm2. Before the final measurement is performed, the sample is carefully mounted to avoid any leakage at the waveguide edge and tightened. The force electric sensor is used for testing the breaking elongation of the film, and the film is stretched at the speed of 0.02 cm/s.
Ti3C2TxThe action with positive ions is stronger than that of other ions, and PEDOT molecular chains with positive charges and Mxene surface polar functional groups are uniformly accumulated on two sides of an Mxene plane through electrostatic action.
As shown in FIG. 1, from Mxene @ PBTz-SO3The element analysis of the Na film shows that PBTz-SO3Na of Na+The ion is substantially coincident with the element of Mxene, and PBtz-SO3 -S element of (a) is hardly visible.
As shown in fig. 2, from elemental analysis of the Mxene @ PEDOT film, it can be seen that the S element of the positively charged PEDOT substantially coincides with the element of Mxene, further demonstrating that Mxene is more prone to interact with positively charged groups.
As shown in FIG. 3, XPS data shows that the oxygen element of Mxene has a coupling effect with the oxygen element of PEDOT, indicating that Mxene has an assembly effect with PEDOT having positive charge characteristics.
Ti3C2TxThe high-toughness electromagnetic shielding film formed by compounding with a conductive PEDOT molecular chain can realize excellent electromagnetic shielding performance, and the electromagnetic shielding performance reaches a value of 80dB as shown in figure 4.
Ti3C2TxThe high-toughness electromagnetic shielding film formed by compounding the high-toughness electromagnetic shielding film with a high polymer material PEDOT can realize excellent mechanical property, and effectively solves the problem of the traditional Ti3C2TxThe problem of oxidation brittleness of the film. As shown in FIG. 4, the electromagnetic shielding performance reaches a value of 80 dB.
The high-toughness Mxene composite electromagnetic shielding film has good electromagnetic shielding effect when used in a microwave anechoic chamber, and can be used for directly forming a cavity to form the microwave anechoic chamber without using a pasting mode for operation, so that the electromagnetic shielding effect is prevented from being reduced due to untight connection at a joint.
The high-toughness Mxene composite electromagnetic shielding film provided by the invention can be applied to wearable electromagnetic protection. The high-toughness Mxene composite electromagnetic shielding film provided by the invention has the characteristics of good electromagnetic shielding effect, high toughness and the like, can be used for wearable electromagnetic protection, and can achieve the effects of improving the comfort and prolonging the service life.
The above description is only a part of the embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (9)
1. The preparation method of the high-toughness Mxene composite electromagnetic shielding film is characterized by comprising the following steps of:
s1 preparation of Ti3C2Tx Mxene，
S2, uniformly accumulating PEDOT molecular chains on two sides of a Mxene plane through the electrostatic action of the PEDOT molecular chains with positive charges and polar functional groups on the surface of the Mxene to prepare the Mxene and PEDOT composite film.
2. The method for preparing the high-toughness Mxene composite electromagnetic shielding film according to claim 1, wherein the S1 specifically comprises the following steps:
s11, adding LiF and HCl into the reaction kettle;
s12, mixing Ti3AlC2Adding the mixture into a reaction kettle one by one, and reacting under a stirring state;
s13, centrifuging the product after the reaction is finished, adding the bottom sediment after centrifugation into HCl, and stirring to obtain slurry;
s14, centrifuging the slurry to obtain viscous precipitate and upper liquid with black color;
s15, taking the viscous precipitate, adding deionized water into the viscous precipitate, performing ultrasonic treatment under the protection of inert atmosphere, and performing centrifugal treatment after ultrasonic treatment to obtain dark green dispersion liquid and obtain Ti3C2TxMxene gel solution.
S16, filtering the gel solution with a water-based filter membrane, drying, vacuum drying, grinding into powder, and weighing Ti3C2TxConcentration of Mxene gel solution.
3. The method for preparing the high-toughness Mxene composite electromagnetic shielding film according to claim 2, wherein the S2 specifically comprises the following steps:
s21, mixing PEDOT: aqueous PSS solution and Ti3C2TxThe Mxene gel solutions were mixed and,
s22, carrying out suction filtration on the mixed gel to prepare a film,
and S23, washing the film with deionized water.
4. The method for preparing the high-toughness Mxene composite electromagnetic shielding film according to claim 1, wherein the process for preparing each unit of the high-toughness Mxene composite electromagnetic shielding film is as follows:
said S1 preparing Ti3C2TxThe specific process of the Mxene comprises the following steps:
s11, adding 1.56g of LiF and 20mL of 9mol/l HCL solution into a polytetrafluoroethylene kettle, and reacting at 30 ℃ for 2h to ensure that LiF is fully reacted;
s12, weighing 1g Ti3AlC2Slowly adding the mixture into a polytetrafluoroethylene kettle for several times within 10min, adjusting the rotating speed of the reactor to 500rpm, and reacting for 24 hours at 30 ℃;
s13, centrifuging the product after the reaction is finished, pouring out the upper liquid, adding the bottom sediment into 2mol/l HCL solution, and stirring for 2h to obtain slurry;
s14, centrifuging the slurry at 5000rpm for 5min until viscous precipitate and upper layer liquid turn black, stopping centrifuging, and pouring out the upper layer liquid;
s15, adding 50mL of deionized water into the viscous precipitate, performing ultrasonic treatment for 1.5h under the protection of inert atmosphere, and after the ultrasonic treatment is finished, performing centrifugal treatment at 2500rpm for 30min to obtain dark green dispersion liquid and obtain Ti3C2TxMxene gel solution;
s16, filtering the gel solution with 0.22 micron water-based filter membrane, drying, vacuum drying at 40 deg.C, drying, grinding into powder to obtain Ti3C2TxThe solubility of the Mxene gel solution is 5 mg/mL;
the S2 specifically includes the following steps:
s21, PEDOT: PSS aqueous solution with solid content of 6% and Ti3C2TxMxene gel solution, mixed in a volume ratio of 1:3,
s22, carrying out suction filtration on the mixture to prepare a film,
and S23, washing the film with deionized water to fully wash away the PSS component, and finally obtaining the Mxene and PEDOT composite film.
5. The high-toughness Mxene composite electromagnetic shielding film prepared by the preparation method of the high-toughness Mxene composite electromagnetic shielding film according to claim 4,
and the Mxene and PEDOT are compounded in situ to form a sheet with the thickness of micron order.
6. The high tenacity Mxene composite electromagnetic shielding film according to claim 5,
in the nanoscale flakes, PEDOT accounts for 30% by weight.
7. A high toughness Mxene composite electromagnetic shielding film according to claim 6, wherein the PEDOT molecular chain is positively charged, and the positively charged PEDOT molecular chain and the Mxene surface polar functional group are uniformly accumulated on both sides of the Mxene plane through electrostatic interaction.
8. The use of the high toughness Mxene composite electromagnetic shielding film according to any one of claims 5 to 7, which is applied to a microwave darkroom.
9. The use of a high toughness Mxene composite electromagnetic shielding film according to any of the claims 5 to 7, which is applied to wearable electromagnetic protection.
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| CN115260692A (en) * | 2022-08-16 | 2022-11-01 | 北京航空航天大学 | Composite hydrogel, preparation method, electromagnetic shielding device and displacement sensor |
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| CN111341497A (en) * | 2020-03-13 | 2020-06-26 | 浙江大学 | Preparation method of silver nanowire-MXene composite transparent conductive film |
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| CN113224231A (en) * | 2021-04-27 | 2021-08-06 | 上海应用技术大学 | Preparation method of flexible Mxene/PEDOT/PSS composite thermoelectric material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115260692A (en) * | 2022-08-16 | 2022-11-01 | 北京航空航天大学 | Composite hydrogel, preparation method, electromagnetic shielding device and displacement sensor |
| CN115260692B (en) * | 2022-08-16 | 2023-10-24 | 北京航空航天大学 | Composite hydrogel, preparation method, electromagnetic shielding device and displacement sensor |
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