CN115612181A - Composite aerogel for electromagnetic interference shielding and preparation method thereof - Google Patents
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Abstract
The invention discloses a composite aerogel for shielding electromagnetic interference and a preparation method thereof. The polypyrrole-modified cellulose nanofiber is used as a gel matrix to prepare the aerogel, so that an interconnected conductive network structure is provided, the dispersion of a conductive filler is facilitated, and the agglomeration of the conductive filler is prevented; MXene and polyvinylpyrrolidone modified copper nanowires are used as conductive fillers, so that the electromagnetic interference shielding capability of the aerogel is improved. Therefore, the multi-component composite aerogel is constructed and can be used for realizing electromagnetic interference shielding.
Description
Technical Field
The disclosure relates to the technical field of new materials, in particular to a composite aerogel for shielding electromagnetic interference and a preparation method thereof.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
With the development of wireless communication technology, rapid transmission of information can facilitate life, but also causes a great deal of electromagnetic pollution, which not only interferes with the operation of precise electronic equipment and instruments and threatens information security, but also causes harm to human health, so that an efficient electromagnetic interference shielding material is urgently needed to avoid unnecessary electromagnetic interference. At present, traditional metal and metal matrix composite materials are widely used for electromagnetic interference shielding, but the traditional metal and metal matrix composite materials have the limitations of easy corrosion, large volume, large density, serious secondary electromagnetic pollution and the like. Therefore, in order to realize the performance advantages of easy processing, corrosion resistance, low cost and adjustable performance, the conductive polymer composite material containing the conductive filler is widely concerned. In addition, in special fields such as aerospace, intelligent electronic devices, wireless telecommunications and the like, low-density performance is required for electromagnetic interference shielding materials, so the conductive polymer composite aerogel attracts wide attention because the conductive polymer composite aerogel has the advantages of ultralow density, good conductivity, large specific surface area, high porosity, three-dimensional structure and the like, can be used as a framework of an electromagnetic interference shielding material to construct a continuous conductive network, and is favorable for realizing dissipation of incident electromagnetic waves.
The copper nanowire (CuNW) has metal conductivity as a metal nanowire, and thus is advantageous for electromagnetic interference shielding. But because the surface of the conductive network lacks functional groups capable of interacting, the conductive network is easy to agglomerate, and the construction of the conductive network is influenced.
The two-dimensional transition metal carbo/nitride (MXene) has the formula M n+1 X n T x Having excellent metalloid conductivity and two-dimensional layered structure compared to conventional metals, wherein Ti 3 C 2 T x The product has good conductivity due to mature synthesis conditions, and strong electromagnetic wave absorption and reflection ability, and is suitable for useUsed as electromagnetic interference shielding material. However, it is difficult to assemble MXene nanoplatelets directly into aerogel structures due to their relatively poor interlayer bonding capability.
Cellulose Nanofiber (CNF) is rich in source and light, and is helpful for forming a three-dimensional network structure and preventing conductive fillers from being stacked, but the insulation property of the cellulose nanofiber can hinder the transmission of electrons in the three-dimensional structure of the aerogel, and the cellulose nanofiber is not beneficial to electromagnetic interference shielding.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a composite aerogel for shielding electromagnetic interference and a preparation method thereof.
In order to realize the purpose, the invention is realized by the following technical scheme:
in a first aspect, the invention provides a preparation method of an electromagnetic interference shielding aerogel, which comprises the steps of uniformly dispersing polypyrrole-modified cellulose nanofibers, polyvinylpyrrolidone-modified copper nanowires and MXene in water according to a proportion, directionally freezing by using liquid nitrogen, and freeze-drying to obtain the composite aerogel.
In a second aspect, the present disclosure provides an electromagnetic interference shielding aerogel prepared by the preparation method.
The beneficial effects achieved by one or more of the embodiments of the invention are as follows:
1) The method takes the polypyrrole-modified cellulose nanofiber as a gel matrix to prepare the aerogel, provides an interconnected conductive network structure, contributes to dispersion of the conductive filler, and prevents agglomeration of the conductive filler; MXene and polyvinylpyrrolidone modified copper nanowires are used as conductive fillers, and the electromagnetic interference shielding capacity of the aerogel is improved. Therefore, the multi-component composite aerogel is constructed and can be used for realizing electromagnetic interference shielding.
2) Cellulose nanofibers are subjected to in-situ polymerization modification by pyrrole to form a conductive network, so that the conductivity is enhanced, a charge transmission channel is opened, and the electron transmission is promoted;
the copper nanowire is subjected to in-situ modification by polyvinylpyrrolidone, so that surface functional groups of the copper nanowire are enriched, dispersion is favorably realized, and agglomeration is prevented.
MXene, copper nanowires and cellulose nanofibers are selected as building elements to build the aerogel, and the aerogel can be applied to electromagnetic interference shielding.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Fig. 1 is a morphology map (fig. 1 a) and XPS characterization (fig. 1 b) of MXene prepared in example 1 of the present disclosure;
fig. 2 is a topography of polyvinylpyrrolidone coated copper nanowires (CuNW @ pvp) prepared in example 2 of the present disclosure (fig. 2a is CuNW, fig. 2b, c are CuNW @ pvp);
FIG. 3 is a topographical map of polypyrrole-modified cellulose nanofibers (CNF @ PPy) prepared in example 3 of the present disclosure (CNF is shown in FIG. 3a, PPy is shown in FIG. 3b, and CNF @ PPy is shown in FIG. 3 c);
fig. 4 is a scanning electron microscopy topographic map (fig. 4 a), a fourier infrared spectrum (fig. 4 b), and an electromagnetic interference shielding performance test chart (fig. 4c, d) of the aerogel prepared in example 4 of the present disclosure.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
In a first aspect, the invention provides a preparation method of an electromagnetic interference shielding aerogel, which comprises the steps of uniformly dispersing polypyrrole-modified cellulose nanofibers, polyvinylpyrrolidone-modified copper nanowires and MXene in water according to a proportion, directionally freezing by using liquid nitrogen, and freeze-drying to obtain the composite aerogel.
In some embodiments, the mass ratio of polypyrrole-modified cellulose nanofibers, polyvinylpyrrolidone-modified copper nanowires, MXene, and water is 0.8-1.2:0.8-1.2:0.8-1.2:100.
in some embodiments, the polypyrrole-modified cellulose nanofibers are prepared by:
dripping hydrochloric acid solution of pyrrole into cellulose nanofiber aqueous solution, and stirring for the first time for set time; hydrochloric acid may promote the polymerization of pyrrole.
And adding a hydrochloric acid solution of ferric chloride into the solution, stirring for a set time for the second time, reacting, and after the reaction is finished, washing, and freeze-drying to obtain the ferric chloride. Ferric chloride is used as an oxidant to initiate polymerization of pyrrole monomers.
Preferably, the time for the second stirring reaction is 20-40min.
Preferably, the mass ratio of the pyrrole to the cellulose nano-fiber to the ferric chloride is 0.3-0.5:1:2.5-3.
In some embodiments, the polyvinylpyrrolidone modified copper nanowires are prepared by a method comprising: and (2) uniformly mixing the alkali liquor, the soluble copper salt solution and the polyvinylpyrrolidone solution, adding ethylenediamine and hydrazine hydrate, stirring for reaction, and then carrying out solid-liquid separation, washing and drying to obtain the catalyst. Hydrazine hydrate acts to reduce copper ions, which are directionally controlled by ethylenediamine to control their length and diameter growth.
Preferably, the alkali liquor is sodium hydroxide or potassium hydroxide, and the copper salt is copper nitrate. The stability and solubility of copper nitrate are good.
Preferably, the mass ratio of the soluble copper salt to the polyvinylpyrrolidone is 60-65.
In a second aspect, the present disclosure provides an electromagnetic interference shielding aerogel prepared by the preparation method.
The present invention will be further described with reference to the following examples.
Example 1
1) Synthesis of MXene Ti 3 C 2 T x ：
Lithium fluoride (1 g) and hydrochloric acid (9 mol/L) (20 mL) were put in a 50mL polytetrafluoroethylene beaker, stirred for 30 minutes, and after complete dissolution, MAX (Ti) was added within 5 minutes 3 AlC 2 ) (1 g), stirring in a constant-temperature water bath at 35 ℃ for 24 hours, centrifuging and washing repeatedly at 3500rpm by using deionized water, and ultrasonically separating the upper black liquid for 1 hour by using an ice water bathThe layer was centrifuged at 3500rpm, and the supernatant liquid was freeze-dried to obtain MXene.
TEM images confirmed a size around 600nm, as shown in FIG. 1a, and XPS confirmed the introduction of oxygen-containing functional groups, as shown in FIG. 1 b.
2) Synthesis of polyvinylpyrrolidone coated copper nanowires (cunnw @ pvp):
preparing sodium hydroxide into an aqueous solution with the concentration of 15mmol/mL, preparing copper nitrate into an aqueous solution with the concentration of 0.24g/mL, preparing polyvinylpyrrolidone into an aqueous solution with the concentration of 0.025g/mL, mixing 640mL of an aqueous solution of sodium hydroxide, 32mL of an aqueous solution of copper nitrate and 5mL of an aqueous solution of polyvinylpyrrolidone, adding 4.8mL of ethylenediamine and 0.33mL of hydrazine hydrate, stirring for 5 minutes, carrying out constant-temperature water bath at 60 ℃ for 4 hours, centrifuging and washing with deionized water and acetone, and carrying out freeze drying to obtain CuNW @ PVP. SEM demonstrated successful coating of PVP on the CuNW surface, as shown in fig. 2a, b, and TEM demonstrated the presence of a PVP shell layer around 50nm thick on the CuNW surface, as shown in fig. 2 c.
3) Synthesizing polypyrrole-modified cellulose nanofiber (CNF @ PPy):
preparing cellulose nano-fibers into an aqueous solution with the concentration of 5 mg/mL;
mixing 0.335mL of pyrrole and 20mL of 0.5mol/L of hydrochloric acid, dropwise adding the mixed solution into 20mL of cellulose nanofiber aqueous solution, and stirring for 5 minutes;
adopting 0.5mol/L hydrochloric acid as a solvent to prepare 20mL of 0.146mg/mL ferric chloride hexahydrate solution, adding the solution, stirring for 30 minutes, centrifugally washing by deionized water, and freeze-drying to obtain CNF @ PPy. TEM proves the modification of the granular polypyrrole on the surface of the cellulose nanofiber, as shown in FIGS. 3a, b and c.
4) The preparation method of the electromagnetic interference shielding aerogel comprises the following steps:
mixing and dispersing the components obtained in the steps 1), 2) and 3) in different proportions to prepare aqueous solution with the concentration of 10mg/mL, putting the aqueous solution on an iron plate, directionally freezing the aqueous solution by liquid nitrogen, and freezing and drying the aqueous solution to obtain the composite aerogel.
In FIG. 4, c is a mass ratio meter, M 2 C 1 C 1 MXene: cunw @ pvp: cnf @ ppy is 2;
M 1 C 1 C 2 MXene: cunw @ pvp: cnf @ ppy is 1;
M 1 C 0 C 1 MXene: cunw @ pvp: cnf @ ppy is 1;
M 1 C 2 C 1 MXene: cunw @ pvp: cnf @ ppy is 1;
M 1 C 1 C 0 MXene: cunw @ pvp: cnf @ ppy is 1;
M 1 C 1 C 1 MXene: cunw @ pvp: CNF @ PPy is 1.
The directional aperture of the aerogel is about 20 micrometers, as shown in fig. 4a, infrared tests prove that the aerogel has characteristic peaks of all components, and prove that the aerogel is successfully combined, as shown in fig. 4b, the aerogel is cut into fixed sizes, and electromagnetic interference shielding performance tests are carried out on the aerogel through a vector network analyzer, wherein the electromagnetic interference shielding performance tests exceed the current commercial level by 20dB, and the specific electromagnetic interference shielding efficiency can reach 1000dB cm 3 g -1 The shielding mechanism is mainly the absorbing mechanism, as shown in fig. 4c and d.
Example 2
1) Synthesis of MXene Ti 3 C 2 T x ：
Lithium fluoride (1 g) and hydrochloric acid (10 mol/L) (20 mL) were put in a 50mL polytetrafluoroethylene beaker, stirred for 40 minutes, and after complete dissolution, MAX (Ti) was added within 4 minutes 3 AlC 2 ) (1.2 g), stirring in a constant-temperature water bath at 37 ℃ for 24 hours, centrifuging and washing with deionized water at 3500rpm for multiple times, carrying out ultrasonic demixing on the black liquid at the upper layer for 1 hour through an ice water bath, centrifuging at 4000rpm, and carrying out freeze drying on the liquid at the upper layer to obtain MXene.
2) Synthesis of polyvinylpyrrolidone coated copper nanowires (cunnw @ pvp):
preparing sodium hydroxide into an aqueous solution with the concentration of 15mmol/mL, preparing copper nitrate into an aqueous solution with the concentration of 0.24g/mL, preparing polyvinylpyrrolidone into an aqueous solution with the concentration of 0.025g/mL, mixing 640mL of an aqueous solution of sodium hydroxide, 32mL of an aqueous solution of copper nitrate and 5mL of an aqueous solution of polyvinylpyrrolidone, adding 4.8mL of ethylenediamine and 0.33mL of hydrazine hydrate, stirring for 5 minutes, carrying out constant-temperature water bath at 60 ℃ for 4 hours, centrifuging and washing with deionized water and acetone, and carrying out freeze drying to obtain CuNW @ PVP.
3) Synthetic polypyrrole-modified cellulose nanofibers (cnf @ ppy):
preparing cellulose nano-fibers into an aqueous solution with the concentration of 8 mg/mL;
0.4mL of pyrrole is mixed with 20mL0.5 mol/L of hydrochloric acid, the mixed solution is dropwise added into the cellulose nanofiber aqueous solution, and the mixture is stirred for 5 minutes;
0.5mol/L hydrochloric acid is used as a solvent to prepare 0.157mg/mL ferric chloride hexahydrate solution, the solution is added and stirred for 30 minutes, deionized water is used for centrifugal washing, and the CNF @ PPy is obtained by freeze drying. The mass ratio of the pyrrole to the cellulose nano-fiber to the ferric chloride is 0.5:1:3.
4) The preparation method of the electromagnetic interference shielding aerogel comprises the following steps:
the method comprises the following steps of 1), 2) and 3) obtaining the polypyrrole-modified cellulose nanofiber, the polyvinylpyrrolidone-modified copper nanowire and MXene according to the mass ratio of 0.8:1.2: and 1.2, dispersing the aerogel into water to prepare a water solution with the concentration of 10mg/mL, putting the water solution on an iron plate, directionally freezing the solution through liquid nitrogen, and freeze-drying the solution to obtain the composite aerogel.
Example 3
1) Synthesis of MXene Ti 3 C 2 T x ：
Lithium fluoride (1.2 g) and hydrochloric acid (6 mol/L) (30 mL) were put in a 50mL polytetrafluoroethylene beaker, stirred for 50 minutes, and after complete dissolution, MAX (Ti) was added within 5 minutes 3 AlC 2 ) (1.5 g), stirring in a constant-temperature water bath at 35 ℃ for 28 hours, centrifuging and washing with deionized water for multiple times at 4000rpm, carrying out ultrasonic demixing on the upper layer black liquid for 1 hour by using an ice water bath, centrifuging at 3500rpm, and carrying out freeze drying on the upper layer black liquid to obtain MXene.
2) Synthesis of polyvinylpyrrolidone coated copper nanowires (cunnw @ pvp):
preparing sodium hydroxide into an aqueous solution with the concentration of 20mmol/mL, preparing copper nitrate into an aqueous solution with the concentration of 0.31g/mL, preparing polyvinylpyrrolidone into an aqueous solution with the concentration of 0.034g/mL, mixing 600mL of the sodium hydroxide aqueous solution, 30mL of the copper nitrate aqueous solution and 5mL of the polyvinylpyrrolidone aqueous solution, adding 4.2mL of ethylenediamine and 0.35mL of hydrazine hydrate, stirring for 5 minutes, carrying out constant-temperature water bath at 60 ℃ for 5 hours, carrying out centrifugal washing on deionized water and acetone, and carrying out freeze drying to obtain CuNW@PVP.
3) Synthetic polypyrrole-modified cellulose nanofibers (cnf @ ppy):
preparing cellulose nano-fibers into an aqueous solution with the concentration of 8 mg/mL;
0.413mL of pyrrole is mixed with 20mL of 0.6mol/L hydrochloric acid, and the mixed solution is dropwise added into the cellulose nanofiber aqueous solution and stirred for 5 minutes;
0.5mol/L hydrochloric acid is used as a solvent to prepare 0.141mg/mL ferric chloride hexahydrate solution, the solution is added and stirred for 30 minutes, deionized water is used for centrifugal washing, and the CNF @ PPy is obtained by freeze drying. The mass ratio of the pyrrole to the cellulose nano-fiber to the ferric chloride is 0.3:1:2.5.
4) The preparation method of the electromagnetic interference shielding aerogel comprises the following steps:
the method comprises the following steps of 1), 2) and 3) obtaining the polypyrrole-modified cellulose nanofiber, the polyvinylpyrrolidone-modified copper nanowire and MXene according to the mass ratio of 1.2:1.2:1, dispersing in water to prepare a water solution with the concentration of 10mg/mL, putting the water solution on an iron plate, directionally freezing the solution by liquid nitrogen, and freeze-drying the solution to obtain the composite aerogel.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of an electromagnetic interference shielding aerogel is characterized by comprising the following steps: uniformly dispersing the polypyrrole-modified cellulose nanofiber, the polyvinylpyrrolidone-modified copper nanowire and MXene in water according to a ratio, directionally freezing by using liquid nitrogen, and freeze-drying to obtain the composite aerogel.
2. The method for preparing an electromagnetic interference shielding aerogel according to claim 1, wherein: the mass ratio of the polypyrrole-modified cellulose nanofiber to the polyvinylpyrrolidone-modified copper nanowire to the MXene to water is 0.8-1.2:0.8-1.2:0.8-1.2:100.
3. the method for preparing an electromagnetic interference shielding aerogel according to claim 1, wherein: the preparation method of the polypyrrole-modified cellulose nanofiber comprises the following steps:
dripping a hydrochloric acid solution of pyrrole into a cellulose nano-fiber aqueous solution, and stirring for the first time for set time;
and adding a hydrochloric acid solution of ferric chloride into the solution, stirring for a set time for the second time, reacting, and after the reaction is finished, washing, and freeze-drying to obtain the ferric chloride.
4. The method for preparing an electromagnetic interference shielding aerogel according to claim 3, wherein: the time of the second stirring reaction is 20-40min.
5. The method for preparing an electromagnetic interference shielding aerogel according to claim 3, wherein: the mass ratio of the pyrrole to the cellulose nano-fiber to the ferric chloride is 0.3-0.5:1:2.5-3.
6. The method for preparing an electromagnetic interference shielding aerogel according to claim 1, wherein: the preparation method of the copper nanowire modified by the polyvinylpyrrolidone comprises the following steps: and (2) uniformly mixing the alkali liquor, the soluble copper salt solution and the polyvinylpyrrolidone solution, adding ethylenediamine and hydrazine hydrate, stirring for reaction, and then carrying out solid-liquid separation, washing and drying to obtain the catalyst.
7. The method for preparing an electromagnetic interference shielding aerogel according to claim 6, wherein: the alkali liquor is sodium hydroxide or potassium hydroxide.
8. The method for preparing an electromagnetic interference shielding aerogel according to claim 6, wherein: the copper salt is copper nitrate.
9. The method for preparing an electromagnetic interference shielding aerogel according to claim 6, wherein: the mass ratio of the soluble copper salt to the polyvinylpyrrolidone is 60-65.
10. An electromagnetic interference shielding aerogel, comprising: prepared by the preparation method of any one of claims 1 to 9.
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