CN112831143A - Preparation method of compressible MXene/polymer electromagnetic shielding aerogel - Google Patents
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Abstract
The invention discloses a preparation method of a compressible MXene/polymer electromagnetic shielding aerogel, which comprises the following steps: preparing a few-layer or multi-layer MXene powder by etching delamination stripping, then preparing different polymer solutions, uniformly mixing according to a certain proportion, using MXene nanosheets as a framework material and a polymer as a nano connecting material through the interaction of a polymer phase and MXene, and preparing MXene aerogel with certain mechanical strength and elasticity by adopting a simple freeze drying method; on the basis of maintaining the MXene electromagnetic shielding performance, the mechanical property of the composite material is obviously improved, and the problems of poor toughness, poor environmental tolerance and difficulty in bearing a certain degree of processing deformation of the MXene material are solved; meanwhile, the invention can use multilayer MXene to prepare the aerogel, thereby obviously improving the utilization rate of MXene, and the prepared aerogel has simple process, environmental protection, low cost, high repeatability, is not easily influenced by environmental factors such as temperature, humidity and the like, and can be stored for a long time.
Description
Technical Field
The invention belongs to the technical field of material preparation, and relates to a preparation method of a compressible MXene/polymer electromagnetic shielding aerogel.
Background
In the field of high performance emi shielding, shielding materials that combine both excellent shielding effect and good mechanical flexibility have been urgently needed. In recent years, a new class of two-dimensional metal carbides and nitrides MXenes are widely used in the field of electromagnetic shielding due to their characteristics of large specific surface area, rich functional groups, metal conductivity, unique layered structure, and the like. With the development of flexible devices and wearable equipment, the aerogel material which is compressible, resilient and excellent in electromagnetic shielding performance has wide application prospect. However, the characteristics of easy stacking agglomeration and weak gelation limit the application of the three-dimensional aerogel material. Accordingly, designing aerogel materials based on MXenes that are lightweight, low density, mechanically good, and have excellent shielding properties has presented significant challenges.
It is known that the selection of the frame material and the design of its microstructure are the focus of research because the honeycomb-like structure composed of the nano-structured frame material and the micron-sized pores has low density, good flexibility, easy processability and good chemical stability. At present, the reported three-dimensional MXene aerogel synthesis methods mainly include a template method, a self-assembly method, electrostatic spinning, 3D printing and the like. However, the preparation process is complex and has high requirements on equipment. Inorganic substances such as graphene and carbon tubes containing carbon components are generally compounded, and few organic substances are contained. In addition, the volume properties of the aerogel are low due to the presence of abundant macropores. Reasonable mechanical compression and pore structure design are beneficial to eliminating pore space so as to improve the mechanical property of the composite material. Therefore, a preparation method of the three-dimensional MXene aerogel, which is simple to operate, green and environment-friendly, low in cost, and good in mechanical property and flexibility, needs to be found.
Disclosure of Invention
The invention aims to provide a preparation method of a compressible MXene/polymer electromagnetic shielding aerogel, and solves the problems of complex preparation process, high requirement on equipment and poor mechanical property caused by large pores in the prior art for preparing a three-dimensional MXene electromagnetic shielding aerogel.
The technical scheme adopted by the invention is that the preparation method of the compressible MXene/polymer electromagnetic shielding aerogel is characterized by comprising the following steps:
Mixing LiF and HCl solution in a certain mass ratio to obtain mixed solution 1, and mixing Ti3AlC2Adding the powder into the mixed solution 1 to obtain a mixed solution 2, placing the mixed solution 2 in an oil bath at the temperature of 30-45 ℃, magnetically stirring for 24-36 h, adding deionized water, centrifugally washing to weak acidity, collecting precipitate, and performing vacuum drying to obtain Ti3C2Performing ultrasonic dispersion on TxMXene powder for 10-30 min, performing centrifugal separation for three times, and collecting supernatant and precipitate respectively;
dissolving the polymer in deionized water under the condition of water bath at 40-90 ℃ to obtain a polymer solution, and mixing the Ti prepared in the step 13C2Dispersing TxMXene precipitated powder in a certain amount of deionized water to obtain Ti3C2Tx MXene dispersion, then mixing polymer solution and Ti according to a certain proportion3C2Uniformly mixing the Tx MXene dispersion liquid to obtain a mixed solution 3;
step 3, preparing MXene/polymer electromagnetic shielding aerogel;
placing the mixed solution 3 obtained in the step 2 in a freeze dryer, and freeze-drying for 48-72h to obtain Ti3C2TxThe/polymer composite aerogel, namely MXene/polymer electromagnetic shielding aerogel.
The invention is also characterized in that:
LiF and Ti in step 13AlC2The mass ratio is 1:1, mass ratio of LiF to HCl 1: 12-20, and the concentration of HCl is 8-12M.
The rotating speed of centrifugal separation in the step 1 is 3000-4000 r/min, and the centrifugal separation time is 50-90 min.
The polymer in the step 2 is polyvinyl alcohol PVA or a water-based polyurethane film WPU.
The freeze-drying temperature in the step 3 is-70 to-50 ℃.
The invention has the beneficial effects that: the preparation method of the compressible MXene/polymer electromagnetic shielding aerogel comprises the steps of enabling polymer phases to interact with MXene, enabling MXene nanosheets to serve as a framework material and polymers to serve as nano connecting materials, and orderly connecting the MXene slices through mutual winding in a freeze drying process to obtain a novel elastic MXene aerogel; the groups on the main chain of the polymer can form compact hydrogen bonds with a large number of hydroxyl groups on the surface of MXene, so that the mechanical property of the composite material is further improved; meanwhile, the aerogel prepared by the invention is simple in process, green and environment-friendly, low in cost, high in repeatability, not easily influenced by environmental factors such as temperature and humidity, and capable of being stored for a long time.
Drawings
Fig. 1 is a scanning electron microscope image of a sample of example 3 of the preparation method of the compressible MXene/polymer electromagnetic shielding aerogel according to the present invention;
FIG. 2 is a scanning electron microscope image of a sample of example 9 of the preparation method of the compressible MXene/polymer electromagnetic shielding aerogel according to the present invention;
fig. 3 is a graph of compression modulus and electromagnetic shielding effectiveness of samples with different MXene/PVA mass ratios in an embodiment of the method for preparing a compressible MXene/polymer electromagnetic shielding aerogel according to the present invention;
fig. 4 is a graph of compression modulus and electromagnetic shielding effectiveness of samples with different MXene/WPU mass ratios in an embodiment of the method for preparing the compressible MXene/polymer electromagnetic shielding aerogel according to the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The preparation method of the compressible MXene/polymer electromagnetic shielding aerogel disclosed by the invention is implemented according to the following steps:
Mixing the components in a mass ratio of 1: mixing 12-20 parts of LiF and HCl solution to obtain mixed solution 1, wherein the concentration of HCl is 8-12M, and mixing Ti3AlC2Adding the powder into the mixed solution 1 to obtain a mixed solution 2, wherein LiF and Ti are3AlC2The mass ratio is 1:1, placing the mixed solution 2 in an oil bath at the temperature of 30-45 ℃, magnetically stirring for 24-36 h, adding deionized water, centrifugally washing to weak acidity, collecting precipitate, and performing vacuum drying to obtain Ti3C2TxCarrying out ultrasonic dispersion on MXene powder for 10-30 min, then carrying out centrifugal separation for three times, wherein the rotating speed of the centrifugal separation is 3000-4000 r/min, the centrifugal separation time is 50-90 min, and respectively collecting supernatant and precipitate
dissolving polymer polyvinyl alcohol PVA or waterborne polyurethane film WPU in deionized water under the condition of water bath at 40-90 ℃ to obtain polymer solution with the concentration of 50mg/mL, and adding Ti prepared in the step 13C2Tx MXene precipitated powder is dispersed in a certain amount of deionized water to obtain Ti with the concentration of 5-10 mg/mL3C2Tx MXene dispersion, and then mixing the polymer solution and Ti according to the mass ratio of 0.2-2.0: 13C2Uniformly mixing the Tx MXene dispersion liquid to obtain a mixed solution 3;
step 3, preparing MXene/polymer electromagnetic shielding aerogel;
placing the mixed solution 3 obtained in the step 2 into a freeze dryer, wherein the freeze drying temperature is-70 to-50 ℃, and the freeze drying time is 48 to 72 hours to obtain Ti3C2TxThe/polymer composite aerogel, namely MXene/polymer electromagnetic shielding aerogel.
Example 1
0.75g of LiF and 9mL of HCl solution (12M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added3AlC2Slowly adding the powder into the mixed solution 1 to obtain a mixed solution 2, placing the mixed solution 2 in an oil bath at 30 ℃ for magnetic stirring for 24 hours, adding deionized water for centrifugal washing to be weakly acidic, collecting precipitates, carrying out vacuum drying to obtain MXene powder, carrying out ultrasonic dispersion for 10 minutes again, carrying out centrifugation for three times again, wherein the centrifugation speed is 3000r/min, the centrifugation time is 50 minutes, and respectively collecting supernatant and precipitates.
Under the condition of 90 ℃ water bath, 2g of PVA is dissolved in 40mL of deionized water to prepare PVA aqueous solution, 0.25g of MXene precipitated powder prepared in the step 1 is dispersed in 30mL of deionized water, and then 5.25g of PVA solution is added into the MXene solution and mixed uniformly to obtain mixed solution 3.
And (3) placing the mixed solution 3 prepared in the step 2 into a freeze dryer, and freeze-drying for 48 hours at-50 ℃. After the freezing is finished, taking out to obtain Ti3C2TxA polymer composite aerogel.
Example 2
0.75g of LiF and 15mL of HCl solution (8M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added3AlC2Slowly adding the powder into the mixed solution 1 to obtain a mixed solution 2, placing the mixed solution 2 in an oil bath at 45 ℃ for magnetic stirring for 36 hours, adding deionized water for centrifugal washing to be weakly acidic, collecting precipitates, carrying out vacuum drying to obtain MXene powder, carrying out ultrasonic dispersion for 30 minutes again, carrying out centrifugation for three times again, wherein the centrifugation speed is 4000r/min, the centrifugation time is 90 minutes, and respectively collecting supernatant and precipitates.
Under the condition of 90 ℃ water bath, 2g of PVA is dissolved in 40mL of deionized water to prepare PVA aqueous solution, 0.25g of MXene precipitated powder prepared in the step 1 is dispersed in 30mL of deionized water, and then 5.25g of PVA solution is added into the MXene solution and mixed uniformly to obtain mixed solution 3.
Placing the mixed solution 3 prepared in the step 2 in freeze-dryingFreeze-drying at-70 deg.C for 72h in a drier. After the freezing is finished, taking out to obtain Ti3C2TxA polymer composite aerogel.
Example 3
0.75g of LiF and 10mL of HCl solution (9M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added3AlC2Slowly adding the powder into the mixed solution 1 to obtain a mixed solution 2, placing the mixed solution 2 in an oil bath at 35 ℃ for magnetic stirring for 24 hours, adding deionized water for centrifugal washing to be weakly acidic, collecting precipitates, carrying out vacuum drying to obtain MXene powder, carrying out ultrasonic dispersion for 10 minutes again, carrying out centrifugation for three times again, wherein the centrifugation speed is 3500r/min, the centrifugation time is 60 minutes, and respectively collecting supernatant and precipitates.
Dissolving 2g of PVA in 40mL of deionized water at 90 ℃ in a water bath to prepare a PVA aqueous solution, dispersing 0.25g of MXene precipitated powder prepared in the step 1 in 30mL of deionized water, adding 5.25g of PVA solution into the MXene solution, and uniformly mixing to obtain a mixed solution 3.
And (3) placing the mixed solution 3 prepared in the step 2 into a freeze dryer, and freeze-drying for 72 hours at-65 ℃. After the freezing is finished, taking out to obtain Ti3C2TxA polymer composite aerogel.
Example 4
0.75g of LiF and 10mL of HCl solution (9M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added3AlC2Slowly adding the powder into the mixed solution 1 to obtain a mixed solution 2, placing the mixed solution 2 in an oil bath at 35 ℃ for magnetic stirring for 24 hours, adding deionized water for centrifugal washing to be weakly acidic, collecting precipitates, carrying out vacuum drying to obtain MXene powder, carrying out ultrasonic dispersion for 10 minutes again, carrying out centrifugation for three times again, wherein the centrifugation speed is 3500r/min, the centrifugation time is 60 minutes, and respectively collecting supernatant and precipitates.
Under the condition of 90 ℃ water bath, 2g of PVA is dissolved in 40mL of deionized water to prepare PVA aqueous solution, 0.15g of MXene precipitated powder prepared in the step 1 is dispersed in 30mL of deionized water, and then 5.25g of PVA solution is added into the MXene solution and mixed uniformly to obtain mixed solution 3.
And (3) placing the mixed solution 3 prepared in the step 2 into a freeze dryer, and freeze-drying for 72 hours at-65 ℃. After the freezing is finished, taking out to obtain Ti3C2TxA polymer composite aerogel.
Example 5
0.75g of LiF and 10mL of HCl solution (9M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added3AlC2Slowly adding the powder into the mixed solution 1 to obtain a mixed solution 2, placing the mixed solution 2 in an oil bath at 35 ℃ for magnetic stirring for 24 hours, adding deionized water for centrifugal washing to be weakly acidic, collecting precipitates, carrying out vacuum drying to obtain MXene powder, carrying out ultrasonic dispersion for 10 minutes again, carrying out centrifugation for three times again, wherein the centrifugation speed is 3500r/min, the centrifugation time is 60 minutes, and respectively collecting supernatant and precipitates.
Under the condition of 90 ℃ water bath, 2g of PVA is dissolved in 40mL of deionized water to prepare PVA aqueous solution, 0.35g of MXene precipitated powder prepared in the step 1 is dispersed in 30mL of deionized water, and then 5.25g of PVA solution is added into the MXene solution and mixed uniformly to obtain mixed solution 3.
And (3) placing the mixed solution 3 prepared in the step 2 into a freeze dryer, and freeze-drying for 72 hours at-65 ℃. After the freezing is finished, taking out to obtain Ti3C2TxA polymer composite aerogel.
Example 6
0.75g of LiF and 10mL of HCl solution (9M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added3AlC2Slowly adding the powder into the mixed solution 1 to obtain a mixed solution 2, placing the mixed solution 2 in an oil bath at 35 ℃ for magnetic stirring for 24 hours, adding deionized water for centrifugal washing to be weakly acidic, collecting precipitates, carrying out vacuum drying to obtain MXene powder, carrying out ultrasonic dispersion for 10 minutes again, carrying out centrifugation for three times again, wherein the centrifugation speed is 3500r/min, the centrifugation time is 60 minutes, and respectively collecting supernatant and precipitates.
Under the condition of 60 ℃ water bath, 2g of WPU is dissolved in 40mL of deionized water to prepare a WPU aqueous solution, 0.25g of MXene precipitated starch powder prepared in the step 1 is dispersed in 30mL of deionized water, and then 5.25g of WPU solution is added into the MXene solution and mixed uniformly to obtain a mixed solution 3.
And (3) placing the mixed solution 3 prepared in the step 2 into a freeze dryer, and freeze-drying for 72 hours at-65 ℃. After the freezing is finished, taking out to obtain Ti3C2TxA polymer composite aerogel.
Example 7
0.75g of LiF and 10mL of HCl solution (9M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added3AlC2Slowly adding the powder into the mixed solution 1 to obtain a mixed solution 2, placing the mixed solution 2 in an oil bath at 35 ℃ for magnetic stirring for 24 hours, adding deionized water for centrifugal washing to be weakly acidic, collecting precipitates, carrying out vacuum drying to obtain MXene powder, carrying out ultrasonic dispersion for 10 minutes again, carrying out centrifugation for three times again, wherein the centrifugation speed is 3500r/min, the centrifugation time is 60 minutes, and respectively collecting supernatant and precipitates.
Under the condition of 60 ℃ water bath, 2g of WPU is dissolved in 40mL of deionized water to prepare a WPU aqueous solution, 0.15g of MXene precipitated starch powder prepared in the step 1 is dispersed in 30mL of deionized water, and then 3.15g of WPU solution is added into the MXene solution and uniformly mixed to obtain a mixed solution 3.
And (3) placing the mixed solution 3 prepared in the step 2 into a freeze dryer, and freeze-drying for 72 hours at-65 ℃. After the freezing is finished, taking out to obtain Ti3C2TxA polymer composite aerogel.
Example 8
0.75g of LiF and 10mL of HCl solution (9M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added3AlC2Slowly adding the powder into the mixed solution 1 to obtain a mixed solution 2, placing the mixed solution 2 in an oil bath at 35 ℃ for magnetic stirring for 24 hours, adding deionized water for centrifugal washing to be weakly acidic, collecting precipitates, carrying out vacuum drying to obtain MXene powder, carrying out ultrasonic dispersion for 10 minutes again, carrying out centrifugation for three times again, wherein the centrifugation speed is 3500r/min, the centrifugation time is 60 minutes, and respectively collecting supernatant and precipitates.
Under the condition of 60 ℃ water bath, 2g of WPU is dissolved in 40mL of deionized water to prepare a WPU aqueous solution, 0.15g of MXene precipitated starch powder prepared in the step 1 is dispersed in 30mL of deionized water, and then 9.45g of WPU solution is added into the MXene solution and mixed uniformly to obtain a mixed solution 3.
And (3) placing the mixed solution 3 prepared in the step 2 into a freeze dryer, and freeze-drying for 72 hours at-65 ℃. After the freezing is finished, taking out to obtain Ti3C2TxA polymer composite aerogel.
Example 9
0.75g of LiF and 10mL of HCl solution (9M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added3AlC2Slowly adding the powder into the mixed solution 1 to obtain a mixed solution 2, placing the mixed solution 2 in an oil bath at 35 ℃ for magnetic stirring for 24 hours, adding deionized water for centrifugal washing to be weakly acidic, collecting precipitates, carrying out vacuum drying to obtain MXene powder, carrying out ultrasonic dispersion for 10 minutes again, carrying out centrifugation for three times again, wherein the centrifugation speed is 3500r/min, the centrifugation time is 60 minutes, and respectively collecting supernatant and precipitates.
Under the condition of 60 ℃ water bath, 2g of WPU is dissolved in 40mL of deionized water to prepare a WPU aqueous solution, 0.15g of MXene precipitated starch powder prepared in the step 1 is dispersed in 30mL of deionized water, and then 15.75g of WPU solution is added into the MXene solution and mixed uniformly to obtain a mixed solution 3.
And (3) placing the mixed solution 3 prepared in the step 2 into a freeze dryer, and freeze-drying for 72 hours at-65 ℃. After the freezing is finished, taking out to obtain Ti3C2TxA polymer composite aerogel.
Example 10
0.75g of LiF and 10mL of HCl solution (9M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added3AlC2Slowly adding the powder into the mixed solution 1 to obtain a mixed solution 2, placing the mixed solution 2 in an oil bath at 35 ℃ for magnetic stirring for 24 hours, adding deionized water for centrifugal washing to be weakly acidic, collecting precipitates, carrying out vacuum drying to obtain MXene powder, carrying out ultrasonic dispersion for 10 minutes again, carrying out centrifugation for three times again, wherein the centrifugation speed is 3500r/min, the centrifugation time is 60 minutes, and respectively collecting supernatant and precipitates.
Under the condition of 60 ℃ water bath, 2g of WPU is dissolved in 40mL of deionized water to prepare a WPU aqueous solution, 0.25g of MXene precipitated starch powder prepared in the step 1 is dispersed in 30mL of deionized water, and then 2.63g of WPU solution is added into the MXene solution and mixed uniformly to obtain a mixed solution 3.
And (3) placing the mixed solution 3 prepared in the step 2 into a freeze dryer, and freeze-drying for 72 hours at-65 ℃. After the freezing is finished, taking out to obtain Ti3C2TxA polymer composite aerogel.
FIG. 1 is a scanning electron microscope image of MXene/PVA aerogel prepared in example 3. Examples 1-3 are composites obtained under different experimental conditions with a 1:1 ratio by mass of MXene to PVA. The experimental conditions in example 3 are preferred as controlled by experimental controls. Examples 3 to 5 are composite materials obtained under the same experimental conditions with MXene to PVA mass ratios of 1:1, 0.6:1 and 1.4:1, respectively. The experimental result shows that the composite aerogel sample prepared in the embodiment 3 with the mass ratio of 1:1 has the best appearance and the best mechanical property within the range of 0.6:1-1.4:1, the composite aerogel has a three-dimensional pore structure as shown in fig. 1, the pores of the composite aerogel are uniform, and the compression strength, the electrical property and the electromagnetic shielding effect of the composite aerogel can be effectively regulated and controlled by adjusting the content of PVA. As shown in FIG. 3, by adding 50 wt% of PVA, the compression modulus of the composite aerogel can reach 12.1kPa, which is 4 times higher than that of the existing pure MXene aerogel, and the electromagnetic shielding effectiveness can reach-69 dB, so that the light-weight firm high-performance electromagnetic shielding aerogel can be prepared. However, excessive PVA inevitably reduces the electrical conductivity and reduces the amount of charge carrier soft aerogel, which will impair its EMI shielding effect to some extent. The aerogel can provide high EMI shielding performance even under low PVA content due to interaction of PVA and MXene, but the MXene/PVA composite aerogel is prepared by taking the mass ratio of MXene to PVA as the optimal content when the mass ratio of MXene to PVA is 1:1 respectively in consideration of the compressive strength and the electromagnetic shielding effect.
FIG. 2 is a scanning electron microscope image of MXene/WPU aerogel prepared in example 9. Examples 6 to 10 are composites obtained with MXene to WPU mass ratios of 1:1, 1:1, 0.33:1, 0.2:1 and 2:1, respectively, under the same experimental conditions. The experimental result shows that the composite aerogel sample prepared in example 9 with the mass ratio of 0.2:1 to 0.2:1 has the best appearance, no surface crack and the best mechanical property within the range of 0.2:1 to 2:1, and has a layered pore structure as shown in fig. 2, uniform lamellar pores and certain compressibility elasticity. The compressive strength, the electrical property and the electromagnetic shielding effect of the composite aerogel can be effectively regulated and controlled by adjusting the WPU content. With the gradual increase of the WPU content, the prepared composite aerogel has better macroscopic performance, and the surface flaw and crack are gradually reduced. As shown in FIG. 4, when 83.3 wt% of WPU is added, the compression modulus of the composite aerogel can reach 9.9kPa, which is 3 times higher than that of pure MXene aerogel, the composite aerogel has high elasticity and compressibility of 70%, can be circularly compressed for more than 1000 times, the electromagnetic shielding efficiency can reach-78 dB, and the aerogel with adjustable electromagnetic shielding efficiency, light weight, compressibility and rebound can be prepared. Excessive WPU inevitably reduces the conductivity and impairs its electromagnetic shielding effect to some extent. However, in the experiment, the electromagnetic shielding performance of the sample is not obviously reduced along with the gradual increase of the WPU content. This is because the aerogel pore channels formed by the WPU and the MXene can be used for multi-stage reflection of electromagnetic waves, thereby achieving an energy loss goal. The MXene/WPU composite aerogel is prepared by taking the mass ratio of MXene to WPU of 0.2:1 as the optimal content in consideration of the compressive strength and the electromagnetic shielding effect.
It can be seen from examples 6 and 7 that, under the same experimental conditions and with the same MXene/WPU mass ratio of 1:1, the density of the prepared aerogel has a great influence on the mechanical properties and electromagnetic shielding properties of the aerogel, and therefore, the density of the aerogel is optimized in the preparation process, so that the aerogel has excellent appearance, mechanical properties and electromagnetic shielding properties.
In conclusion, the composite aerogel is prepared by adopting multiple layers of MXene, PVA and WPU respectively and regulating and controlling the ratio of different components and experimental conditions. The preparation method not only improves the utilization rate of MXene, but also provides experimental guidance and practical application values for preparation and performance application of the MXene-based polymer aerogel.
Claims (7)
1. The preparation method of the compressible MXene/polymer electromagnetic shielding aerogel is characterized by comprising the following steps:
step 1, synthesizing Ti3C2Tx MXene；
Mixing LiF and HCl solution in a certain mass ratio to obtain mixed solution 1, and mixing Ti3AlC2Adding the powder into the mixed solution 1 to obtain a mixed solution 2, placing the mixed solution 2 in an oil bath at the temperature of 30-45 ℃, magnetically stirring for 24-36 h, adding deionized water, centrifugally washing to weak acidity, collecting precipitate, and performing vacuum drying to obtain Ti3C2Performing ultrasonic dispersion on TxMXene powder for 10-30 min, performing centrifugal separation for three times, and collecting supernatant and precipitate respectively;
step 2, preparing Ti3C2Tx MXene/polymer mixed solution;
dissolving the polymer in deionized water under the condition of water bath at 40-90 ℃ to obtain a polymer solution, and mixing the Ti prepared in the step 13C2Dispersing TxMXene precipitated powder in a certain amount of deionized water to obtain Ti3C2Tx MXene dispersion, then mixing polymer solution and Ti according to a certain proportion3C2Uniformly mixing the Tx MXene dispersion liquid to obtain a mixed solution 3;
step 3, preparing MXene/polymer electromagnetic shielding aerogel;
placing the mixed solution 3 obtained in the step 2 in a freeze dryer, and freeze-drying for 48-72h to obtain Ti3C2TxThe/polymer composite aerogel, namely MXene/polymer electromagnetic shielding aerogel.
2. The method for preparing the compressible MXene/polymer electromagnetic shielding aerogel according to claim 1, wherein LiF and Ti in step 13AlC2The mass ratio is 1:1, mass ratio of LiF to HCl 1: 12-20, and the concentration of HCl is 8-12M.
3. The method for preparing the compressible MXene/polymer electromagnetic shielding aerogel according to claim 1, wherein the rotation speed of the centrifugal separation in the step 1 is 3000-4000 r/min, and the centrifugal separation time is 50-90 min.
4. The method for preparing the compressible MXene/polymer electromagnetic shielding aerogel according to claim 1, wherein the Ti in the step 23C2The concentration of the Tx MXene dispersion liquid is 5-10 mg/mL, and the concentration of the polymer solution is 50 mg/mL.
5. The method for preparing the compressible MXene/polymer electromagnetic shielding aerogel according to claim 1, wherein the polymer in the step 2 is polyvinyl alcohol PVA or aqueous polyurethane film WPU.
6. The method for preparing the compressible MXene/polymer electromagnetic shielding aerogel according to claim 1, wherein the Ti in the step 23C2The mass ratio of the Tx MXene solution to the polymer solution is 0.2-2.0: 1.
7. The method for preparing the compressible MXene/polymer electromagnetic shielding aerogel according to claim 1, wherein the freeze-drying temperature in the step 3 is-70 to-50 ℃.
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