CN111993725A - Method for improving electromagnetic shielding performance of MXene-based composite fabric material - Google Patents
Method for improving electromagnetic shielding performance of MXene-based composite fabric material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 87
- 239000004744 fabric Substances 0.000 title claims abstract description 85
- 239000002131 composite material Substances 0.000 title claims abstract description 48
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- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 238000005530 etching Methods 0.000 claims abstract description 6
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- 229910052751 metal Inorganic materials 0.000 claims description 3
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D—TEXTILES; PAPER
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Abstract
The invention relates to a method for improving the electromagnetic shielding performance of an MXene-based composite fabric material, which aims to overcome the defects of low absorption shielding efficiency, poor flexibility, complex preparation process and the like of the electromagnetic shielding material in the current market. The method is characterized in that a chemical etching method is used for etching MAX phase micron sheets to prepare a small-layer MXene dispersion liquid, then a fabric material is dip-coated, and a plurality of layers of MXene-coated fabric materials are arranged in a gradient mode according to MXene content and are compounded to obtain the MXene-based composite fabric material. The total electromagnetic shielding performance of the prepared composite fabric material can reach 91 dB, wherein the absorption and reflection shielding effectiveness can be adjusted through different gradient structures, and the electromagnetic shielding characteristic mainly based on absorption is realized.
Description
Technical Field
The invention relates to an electromagnetic shielding material, in particular to a method for improving the electromagnetic shielding performance of an MXene-based composite fabric material.
Background
From daily life to military facilities, when people use the convenient and efficient devices, the electromagnetic radiation generated by the devices not only affects the normal use of electronic and electrical equipment, but also harms the health of the people, and even threatens the life safety in serious cases. Therefore, in order to reduce the intensity of electromagnetic radiation, prevent the electromagnetic radiation from being damaged, and ensure the normal operation of electrical equipment, various electromagnetic shielding products are produced and developed rapidly, and the requirements for the performance of electromagnetic shielding materials also gradually tend to be lighter, more flexible and easier to process.
At present, electromagnetic wave shielding materials with conductivity, electromagnetic shielding performance, fabric softness, comfort and air permeability in the market are mainly divided into two types: one is to blend carbon fiber and some metal fiber with common yarn into woven and knitted fabric material by blending; the other method is to arrange nano-scale metal particles, conductive high polymer, ferrite and the like on the textile fibers in a manner of adding a coating so as to generate an electromagnetic shielding effect. At present, the electromagnetic shielding fabric is mainly applied to protective clothing, combat uniform, electromagnetic shielding curtains, outdoor electromagnetic shielding tents and the like.
MXene is a novel two-dimensional layered structure transition metal carbide or nitride, and has a structure similar to graphene. Obtaining MXene by selectively etching the A layer in the MAX phase, wherein the chemical formula of the MXene is Mn+1XnTxWherein M represents a transition metal, X represents carbon or nitrogen, TxRepresents a functional group (O, F, OH). MXene has excellent conductivity, mechanical property and electromagnetic shielding property.
Currently, some MXene-based electromagnetic shielding fabric materials appear, but the electromagnetic shielding materials have low shielding capability and poor mechanical properties, and the preparation process thereof is generally complex, so that a method which is simple and easy to operate and can effectively improve the electromagnetic shielding performance of the MXene-based electromagnetic shielding fabric materials is urgently needed to be developed.
Disclosure of Invention
In order to solve the problems of low absorption shielding energy, complex process and the like of the existing electromagnetic shielding material, the invention aims to provide a method for improving the electromagnetic shielding performance of an MXene-based composite fabric material.
A first object of the present invention is to provide a method for improving electromagnetic shielding performance of an MXene-based composite fabric material, comprising the steps of:
(1) providing multiple layers of fabric material coated with MXene, wherein the content of MXene on each layer of fabric material is different; MXene is obtained by selectively etching an Al layer in a metal conductive layered MAX phase;
(2) the MXene-coated fabric materials are arranged in a gradient manner according to the MXene content and compounded to obtain the MXene-based composite fabric material.
Further, the MAX phase includes Ti2AlC、Ti3AlC2Or Ta4AlC3And (4) phase(s). Preferably, the MAX phase is Ti3AlC2。
Further, in the step (1), the particle size of the MAX phase is 200-400 meshes.
Further, in step (1), the fabric material is a thermoplastic material, such as polypropylene, polyethylene, polyvinyl chloride, polystyrene, polyamide or acrylic thermoplastic material. Preferably, the textile material is a polypropylene nonwoven.
Further, in the step (1), the preparation method of MXene comprises the following steps:
etching the MAX phase by using a mixed aqueous solution of lithium fluoride, hydrochloric acid and nitric acid, wherein the mass ratio of the lithium fluoride to the hydrochloric acid to the MAX phase is 1 to5: 10-15: 1-5: 10 to 15. The mixed aqueous solution contains chloride ions, fluoride ions and hydrogen ions, and Ti is etched by the above method3AlC2And the Al in the phase enables the surface texture of the obtained MXene to be more uniform and the conductivity to be better.
Further, MXene comprises Ti2C、Ti3C2Or Ta4C3. Preferably MXene is Ti3C2。
Preferably, the preparation method of MXene comprises the following steps:
uniformly mixing lithium fluoride phase powder, a hydrochloric acid aqueous solution and a nitric acid aqueous solution to obtain a mixed aqueous solution; adding the MAX phase into the mixed aqueous solution, stirring and reacting for 24-48 hours at 35-40 ℃, centrifuging and washing for multiple times until the pH value of the centrifugate is greater than 6. And under the protection of argon, performing ultrasonic treatment for 45-60 minutes in an ice bath environment to obtain the aqueous dispersion of the small-layer MXene. Preferably, the concentration of MXene in the aqueous dispersion is 5-60 mg/ml.
Further, in the step (1), the content of MXene on the fabric material is 0.01-0.4 g/cm2。
Further, in the step (1), the MXene-coated fabric material is provided with four layers, wherein the content of MXene on the fabric material is 0.01-0.1 g/cm2、0.1~0.2g/cm2、0.2~0.3g/cm2、0.3~0.4g/cm2。
Further, the method for preparing the MXene-coated fabric material comprises the following steps:
and (3) dipping the aqueous dispersion of MXene on the fabric, and carrying out vacuum drying for 5-10 hours at the drying temperature of 45-60 ℃ to obtain the fabric material coated with MXene.
Further, in the step (2), compounding by adopting a hot pressing method, wherein the hot pressing temperature is 160-220 ℃. The hot pressing method is adopted for compounding the fabric material, the process is simple, the cost is lower, the operation is easy, and the method is suitable for large-scale production.
A second object of the present invention is to provide an MXene-based composite fabric material prepared by the above method, which comprises a plurality of layers of MXene-coated fabric material, wherein the MXene content is arranged in a gradient manner along the thickness direction of the composite fabric material.
The MXene-based composite fabric material has a multilayer MXene gradient structure, so that the composite fabric material has good flexibility and shielding performance, and the comfort of the fabric is not influenced.
A third object of the invention is to disclose the use of MXene based composite fabric material for electromagnetic shielding.
Further, the MXene content in the MXene-based composite fabric material is arranged from low to high in a gradient manner along the radiation direction of the electromagnetic waves. When the MXene content is arranged in a gradient manner from low to high, the absorption loss and the reflection loss of the MXene content are continuously reduced, meanwhile, the low-concentration part generates a barrier-like effect, the electromagnetic waves are almost completely consumed in the material, the secondary electromagnetic radiation damage caused by the reverse direction of the electromagnetic waves is prevented, the shielding efficiency of the composite fabric material can reach more than 90 decibels, and the composite fabric material has excellent electromagnetic shielding performance.
By the scheme, the invention at least has the following advantages:
the invention provides a method for improving the electromagnetic shielding performance of an MXene-based composite fabric material. The multi-layer gradient structure of MXene in the composite fabric material effectively reduces the surface reflection of incident electromagnetic waves, and effectively dissipates the electromagnetic waves along with the increase of the incident depth of the electromagnetic waves, so that the skin effect of the material is reduced. In addition, MXene has high intrinsic conductivity and polarized surface, so that the composite fabric material has excellent electromagnetic shielding performance.
The MXene-based composite fabric material prepared by the method has the effective electromagnetic shielding effectiveness as high as 91 dB, wherein the absorption and reflection shielding effectiveness can be adjusted by adjusting the MXene content of each layer of MXene-coated fabric material, so that the electromagnetic shielding characteristic mainly based on absorption is realized. The invention solves the defects of low absorption and shielding efficiency, low flexibility, complex preparation process and the like of the existing porous electromagnetic shielding material.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following description is made with reference to the preferred embodiments of the present invention and the accompanying detailed drawings.
Drawings
Fig. 1 is an electron microscope picture of MXene;
fig. 2 is a cross-sectional electron microscope picture of the MXene-based composite fabric material prepared in example 5;
fig. 3 is a surface electron microscope picture of the MXene-based composite fabric material prepared in example 5;
FIG. 4 shows the results of the electromagnetic shielding performance test of MXene-based composite fabric materials prepared in examples 1 to 5 in X band;
FIG. 5 shows the results of the electromagnetic shielding performance test at 8.2GHz of MXene-based composite fabric materials prepared in examples 1-5;
figure 6 illustrates the flexibility of the MXene-based composite fabric material prepared in example 5.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the following examples of the invention, the preparation of the aqueous dispersion of small layer MXene used is as follows:
weighing 1.0 g of lithium fluoride, adding the lithium fluoride into a mixed aqueous solution of 100 ml of hydrochloric acid (36 mass percent) and 100 ml of nitric acid (65 mass percent), and stirring for 5-30 minutes until the lithium fluoride is dissolved to obtain a mixed solution. 0.8-1 g of MAX phase Ti is weighed3AlC2Slowly adding the powder (MAX phase purity is 98% and particle size is about 38 microns) into the mixed solution, stirring and reacting at 35-40 ℃ for 24-48 hours, centrifuging at 3500 rpm, cleaning with distilled water, centrifuging at 8000 rpm, repeating for multiple times until pH value is reached>6. And under the protection of argon, performing ultrasonic treatment for 45-60 minutes in an ice bath environment to obtain the small-layer MXene aqueous dispersion. According to the different quality of the added MAX phase, MXene concentrate is obtained respectivelyAqueous MXene dispersions at 15 mg/ml, 30 mg/ml, 45 mg/ml and 60 mg/ml.
Fig. 1 is an electron microscope image of MXene, from which it can be seen that its surface morphology is relatively uniform.
Example 1
(1) Carrying out ultrasonic pretreatment on the polypropylene non-woven fabric by using acetone to remove oil stains and impurities on the surface of the fabric, and cleaning and drying the fabric by using distilled water;
(2) dipping 15 mg/ml of MXene aqueous dispersion on the pretreated fabric, and carrying out vacuum drying for 5-10 hours at the drying temperature of 45-60 ℃ to obtain MXene coated polypropylene non-woven fabric; wherein the content of MXene on the dried fabric is 0.06g/cm2;
(3) And (3) orderly stacking the four layers of MXene coated polypropylene non-woven fabrics prepared in the step (2), and then carrying out hot-pressing compounding at the temperature of 160-200 ℃ to obtain the MXene-based composite fabric material.
The MXene-based composite fabric material prepared in this example was tested for electromagnetic shielding performance, as shown in fig. 4-5, the shielding performance was up to 42 db, wherein the absorption shielding performance was up to 32 db.
Example 2
An MXene-based composite web material was prepared as in example 1 except that in step (2) a 30 mg/ml aqueous MXene dispersion was dip coated onto the pre-treated web and after drying the MXene content of the web was 0.14g/cm2。
The MXene-based composite fabric material prepared in this example was tested for electromagnetic shielding performance, as shown in fig. 4-5, the shielding performance was 53 db, wherein the absorption shielding performance was 41 db.
Example 3
An MXene-based composite web material was prepared as in example 1 except that in step (2) a 45 mg/ml aqueous MXene dispersion was dip coated onto the pre-treated web and after drying the MXene content of the web was 0.25g/cm2。
The MXene-based composite fabric material prepared in this example was tested for electromagnetic shielding performance, as shown in fig. 4-5, the shielding performance was up to 66 db, wherein the absorption shielding performance was up to 53 db.
Example 4
An MXene-based composite web material was prepared as in example 1 except that in step (2) a 60 mg/ml aqueous MXene dispersion was dip coated onto the pre-treated web and after drying the MXene content of the web was 0.32g/cm2。
The MXene-based composite fabric material prepared in this example was tested for electromagnetic shielding performance, as shown in fig. 4-5, the shielding performance was up to 75 db, wherein the absorption shielding performance was up to 62 db.
Example 5
(1) Carrying out ultrasonic pretreatment on four pieces of polypropylene non-woven fabric by using acetone to remove oil stains and impurities on the surface of the fabric, and cleaning and drying the fabric by using distilled water;
(2) respectively dipping and coating 15 mg/ml, 30 mg/ml, 45 mg/ml and 60 mg/ml MXene aqueous dispersion on a piece of pretreated fabric, and carrying out vacuum drying for 5-10 hours at the drying temperature of 45-60 ℃ to obtain polypropylene non-woven fabrics coated with different contents of MXene; wherein the content of MXene on the dried fabric is 0.04g/cm respectively2、0.17g/cm2、0.26g/cm2、0.34g/cm2。
(3) And (3) orderly stacking four layers of MXene coated polypropylene non-woven fabrics prepared in the step (2) according to the sequence of MXene content from low to high, and then carrying out hot-pressing compounding at the temperature of 200 ℃ to obtain the MXene-based composite fabric material.
The MXene-based composite fabric material prepared in this example was tested for electromagnetic shielding performance, and electromagnetic waves were irradiated to the composite fabric material from the side of the fabric material with lower MXene content, as shown in fig. 4-5, the shielding performance was up to 91 db, wherein the absorption shielding performance was up to 76 db.
Fig. 2-3 are cross-sectional and surface electron microscope images of the composite fabric material based on MXene prepared in this example, and it can be seen from the images that the smooth and flat surface of the fabric material surface is uniformly covered with MXene material, and in the cross-sectional images, it can be seen that the gaps in the fabric material after hot pressing are uniform, and MXene is uniformly distributed around the fiber material.
When the MXene-based composite fabric material prepared in this example is manually bent, as shown in fig. 6, the composite fabric material can be easily bent without breaking, and during the bending process, the surface of the composite fabric material still remains flat without cracks and powder falling, which indicates that the MXene-based composite fabric material prepared in the present invention has good flexibility.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for improving the electromagnetic shielding performance of an MXene-based composite fabric material is characterized by comprising the following steps:
(1) providing multiple layers of fabric material coated with MXene, wherein the content of MXene on each layer of fabric material is different; MXene is obtained by selectively etching an Al layer in a metal conductive layered MAX phase;
(2) the MXene-coated fabric materials are arranged in a gradient manner according to the MXene content and compounded to obtain the MXene-based composite fabric material.
2. The method of claim 1, wherein: in step (1), the MAX phase includes Ti2AlC、Ti3AlC2Or Ta4AlC3Phase (1); the particle size of the MAX phase is 200-400 meshes.
3. The method of claim 1, wherein: in the step (1), the fabric material is a thermoplastic material.
4. The method of claim 1, wherein: in the step (1), the preparation method of MXene comprises the following steps:
etching the MAX phase by using a mixed aqueous solution of lithium fluoride, hydrochloric acid and nitric acid, wherein the mass ratio of the lithium fluoride to the hydrochloric acid to the nitric acid to the MAX phase is 1-5: 10-15: 1-5: 10 to 15.
5. The method of claim 1, wherein: in the step (1), the content of MXene on the fabric material is 0.01-0.4 g/cm2。
6. The method of claim 1, wherein: in the step (1), the MXene-coated fabric material is divided into four layers, wherein the MXene content of the fabric material is 0.01-0.1 g/cm2、0.1~0.2g/cm2、0.2~0.3g/cm2、0.3~0.4g/cm2。
7. The method of claim 1, wherein: in the step (2), compounding by adopting a hot pressing method, wherein the hot pressing temperature is 160-220 ℃.
8. An MXene-based composite fabric material prepared according to the method of any one of claims 1 to 7, characterized by: comprises a plurality of layers of fabric materials coated with MXene, and the MXene content is arranged in a gradient manner along the thickness direction of the composite fabric material.
9. Use of the MXene-based composite fabric material of claim 8 in electromagnetic shielding.
10. Use according to claim 9, characterized in that: the MXene content in the MXene-based composite fabric material is arranged from low to high in a gradient manner along the radiation direction of electromagnetic waves.
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