CN115955834A - Preparation method of rhombus block-shaped powder with high microwave absorptivity by embedding CoPC/CNTs into MXene - Google Patents
Preparation method of rhombus block-shaped powder with high microwave absorptivity by embedding CoPC/CNTs into MXene Download PDFInfo
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Abstract
The invention discloses a preparation method of powder with high microwave absorptivity by embedding rhombic blocky CoPC/CNTs into MXene. The prepared composite powder has high microwave absorption performance and large specific surface area. The method is an effective process strategy for improving the electromagnetic wave absorption by constructing a complex multi-dimensional hierarchical structure and a controllable interface engineering among 0D porous carbon-supported Co nanoparticles (CoPC), 1D CNTs and 2D MXene sheets.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, and particularly relates to a preparation method of powder with high microwave absorptivity by embedding rhombic block CoPC/CNTs into MXene.
Background
With the rapid development of the 5G network communication technology, the electromagnetic wave pollution not only influences the normal operation of precision instruments, but also causes harm to human health. Therefore, the research on the electromagnetic wave absorbing material has important significance for reducing the electromagnetic wave pollution. However, the conventional electromagnetic wave absorbent has limited practical applications due to its disadvantages of heavy weight, high density, poor impedance matching, low absorption capacity, etc. Therefore, it is important to research a novel electromagnetic wave absorbing material with ultra-thin thickness, light weight and strong absorption capacity, wherein electromagnetic waves can be converted into heat or energy in other forms through multiple reflection and conductive transmission among structures in the material. The excellent electromagnetic wave absorbing material mainly depends on the composition and the design of the internal microstructure, which are two most important factors for designing and manufacturing the electromagnetic wave absorbing material.
Ti 3 C 2 T x MXene is a novel transition metal carbide material with a two-dimensional layered structure, and has the characteristics of low density, high conductivity, high specific surface area, adjustable terminal groups and the like. A large number of polar groups (-OH, -F and the like) on the surface of MXene can be used as active sites of other phases such as magnetic units, polymers and the like, and the polarization behavior of the MXene is improved. However, the electromagnetic wave attenuation mechanism inherent to pure dielectric absorbers is limited. In addition, MXene has a single dielectric loss, making it difficult to achieve effective impedance matching, resulting in low Reflection Loss (RL) and narrow Effective Absorption Bandwidth (EAB).
Disclosure of Invention
The invention aims to provide a preparation method of powder with high microwave absorbability by embedding rhombic block CoPC/CNTs into MXene, which has high microwave absorbability and large specific surface area.
The technical scheme adopted by the invention is that the preparation method of the powder with high microwave absorptivity by embedding rhombic block CoPC/CNTs into MXene is implemented according to the following steps:
and 3, adding the rhombic block-shaped CoPC/CNTs powder into CTAB and deionized water, performing ultrasonic treatment to obtain a mixed solution F, adding the mixed solution F into the MXene suspension, continuously oscillating for 6-24h, and performing freeze drying to obtain powder with high microwave absorption performance of CoPC/CNTs @ MXene.
The invention is also characterized in that:
zn (NO) in step 1 3 ) 2 -6H 2 O、Co(NO 3 ) 2 -6H 2 The mass ratio of O to methanol is 1:2-4:81.
in the step 1, the mass ratio of the 2-Melm to the methanol is 1:10.
in the step 1, the mass ratio of the mixed solution A to the methanol in the mixed solution B is 2.4:1.
in the step 1, the conditions for annealing the CoPC/CNTs precursor in a vacuum tube furnace are as follows: heating at 500-1100 deg.C under argon atmosphere for 1-6h.
LiF and Ti in step 2 3 AIC 2 The mass ratio of the powder is 1:1, the mass ratio of LiF to HCI is 1:10-20, wherein the concentration of HCI is 6-8M.
The rotation speed of the centrifugation in the step 2 is 2500-4000rmp, and the centrifugation time is 30-90min.
In the step 3, the mass ratio of the rhombic block-shaped CoPC/CNTs powder to CTAB to deionized water is 2:1:10.
the mass ratio of the MXene suspension to the mixed solution F in the step 3 is 0.5-3:2.
the conditions of freeze drying in step 3 are: placing the solution after continuous oscillation in a freeze dryer, pre-freezing at-40 deg.C for 2-4h, cooling to-60 deg.C, and freeze drying for 24-48h.
The invention has the beneficial effects that:
CoPC/CNTs samples with a novel layered structure, which are composed of Carbon Nanotubes (CNTs) grafted onto Porous Carbon (PC) -supported cobalt nanoparticles, were initially prepared by pyrolysis of bimetallic ZnCo-MOF. The prepared composite powder has high microwave absorption performance and large specific surface area. The construction of a complex multi-dimensional hierarchical structure and controllable interface engineering among 0D porous carbon Co-loaded nanoparticles (CoPC), 1D CNTs and 2D MXene sheets is an effective process strategy for improving the electromagnetic wave absorption, wherein D represents the dimension.
Drawings
FIG. 1 is a scanning electron microscope image of the composite microwave absorbing powder with embedded MXene nanosheets of CoPC/CNTs prepared in example 5;
FIG. 2 is a scanning electron microscope cross-section of the composite microwave absorbing powder with embedded MXene nanosheets of CoPC/CNTs prepared in example 6;
FIG. 3 is a graph of the microwave absorption efficiency of samples at different mass ratios of CoPC/CNTs and MXene suspensions in the examples.
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 powder with high microwave absorptivity by embedding MXene into rhombic block CoPC/CNTs is implemented according to the following steps:
zn (NO) 3 ) 2 -6H 2 O and Co (NO) 3 ) 2 -6H 2 O is dissolved in methanol, in which Zn (NO) is present 3 ) 2 -6H 2 O、Co(NO 3 ) 2 -6H 2 The mass ratio of O to methanol is 1:2-4:81, magnetically stirring for 10-30min to obtain a mixed solution A; dissolving 2-Melm in methanol, wherein the mass ratio of the 2-Melm to the methanol is 1:10, preparing a mixed solution B, and adding the mixed solution B into the mixed solution A, wherein the mass ratio of the mixed solution A to the methanol in the mixed solution B is 2.4:1, continuously stirring for 0.5-2h at room temperature, and standing for 10-24h to obtain a mixed solution C; washing the mixed solution C with methanol for 3 times, centrifuging and collecting a product, and drying the collected product in a vacuum drying oven to obtain ZnCo-MOF powder; putting ZnCo-MOF powder into a vacuum tube furnace for annealing and annealingThe fire conditions were: under the condition of argon atmosphere, heating at 500-1100 ℃ for 1-6h to obtain rhombus block-shaped CoPC/CNTs powder;
mixing LiF and HCI solution to prepare mixed solution D, and mixing Ti 3 AIC 2 Adding the powder into the mixed solution D, placing the mixed solution into a water bath at 25-45 ℃, and stirring the mixed solution for 18-26h to obtain a mixed solution E, wherein LiF and Ti 3 AIC 2 The mass ratio of the powder is 1:1, the mass ratio of LiF to HCI is 1:10-20, wherein the concentration of HCI is 6-8M, washing with deionized water until ph =7, centrifuging at the rotating speed of 2500-4000rmp for 30-90min, and taking out supernatant to obtain Mxene suspension;
adding the rhombic CoPC/CNTs powder into CTAB and deionized water, wherein the mass ratio of the rhombic CoPC/CNTs powder to the CTAB to the deionized water is 2:1:10, obtaining a mixed solution F after ultrasonic treatment, and adding the mixed solution F into an MXene suspension, wherein the mass ratio of the MXene suspension to the mixed solution F is (0.5-3): continuously shaking for 6-24h, and freeze-drying under the following conditions: placing the solution after continuous oscillation in a freeze dryer, pre-freezing for 2-4h at-40 ℃, and then freeze-drying for 24-48h; the powder with high microwave absorption performance of CoPC/CNTs @ MXene is obtained.
Example 1
2.36g of Zn (NO) 3 ) 2 -6H 2 O and 4.72g of Co (NO) 3 ) 2 -6H 2 And mixing the solution A and the solution O, adding 240mL of methanol solution, and magnetically stirring for 20min to prepare a mixed solution A. Then, 7.88g of 2-Melm was dissolved in 100mL of a methanol solution to prepare a mixed solution B, which was then added to the mixed solution A, stirred at room temperature for 1 hour, and left to stand for 24 hours to obtain a mixed solution C. The resulting mixed solution C was washed 3 times with a methanol solution and centrifuged to collect the product. And (3) drying the collected product in a vacuum drying oven at the drying temperature of 60 ℃ for 10h to obtain purple ZnCo-MOF powder, namely a CoPC/CNTs precursor. Finally, placing the CoPC/CNTs precursor in a vacuum tube furnace in argon gasAnd under the atmosphere condition, the heating temperature is 800 ℃, and the heating time is 2h, so that the rhombic block-shaped CoPC/CNTs powder is finally obtained.
1g of LiF and 15mL of HCI solution were mixed to obtain a mixed solution B, and 1g of Ti was added 3 AIC 2 The powder was added to the mixed solution B and placed in a 25 ℃ water bath and stirred for 18h to give a mixed solution C, which was washed with deionized water to ph =7. And (3) ultrasonically dispersing for 5min, centrifuging the mixed solution C by using a high-speed centrifuge (the rotating speed is 2500rmp, the centrifuging time is 30 min) for 3 times, and collecting a solution intermediate to obtain the MXene suspension.
Dissolving 2mg of CTAB in 100mL of deionized water, taking 100mg of CoPC/CNTs powder, dissolving the powder in 5mL of prepared CTAB solution, and mixing and performing ultrasonic treatment for 1h to obtain a mixed solution F, namely the CoPC/CNTs with positive electricity. 10mg of positively charged CoPC/CNTs powder was then taken and added to 20mL of MXene suspension and shaking continued for 8h. Finally, the mixed solution F is placed in a freeze dryer for pre-freezing for 3h at the temperature of minus 40 ℃, cooling to the temperature of minus 60 ℃, and then freeze-drying for 48h. The CoPC/CNTs @ Mxene composite microwave absorbing powder is obtained.
Example 2
2.36g of Zn (NO) 3 ) 2 -6H 2 O and 4.72g of Co (NO) 3 ) 2 -6H 2 And mixing the solution A and the solution O, adding 240mL of methanol solution, and magnetically stirring for 20min to prepare a mixed solution A. Then, 7.88g of 2-Melm was dissolved in 100mL of a methanol solution to prepare a mixed solution B, which was then added to the mixed solution A, stirred at room temperature for 1 hour, and left to stand for 24 hours to obtain a mixed solution C. The resulting mixed solution C was washed 3 times with a methanol solution and centrifuged to collect the product. And (3) drying the collected product in a vacuum drying oven at the drying temperature of 60 ℃ for 11h to obtain purple ZnCo-MOF powder, namely a CoPC/CNTs precursor. And finally, placing the CoPC/CNTs precursor in a vacuum tube furnace, heating at 800 ℃ for 2 hours under the argon atmosphere condition, and finally obtaining the rhombic block-shaped CoPC/CNTs powder.
1g of LiF and 17mL of HCI solution were mixed to obtain a mixed solution B, and 1g of Ti was added 3 AIC 2 Adding the powder into the mixed solution B, placing the mixed solution in a water bath at the temperature of 30 ℃, stirring the mixed solution for 20 hours to obtain a mixed solution C, washing the mixed solution C to p by using deionized waterh =7, ultrasonically dispersing for 10min, repeatedly centrifuging the mixed solution C by using a high-speed centrifuge (the rotating speed is 3000rmp, the centrifuging time is 40 min) for 3 times, and collecting a solution intermediate to obtain the MXene suspension.
Dissolving 2mg of CTAB in 100mL of deionized water, taking 100mg of CoPC/CNTs powder, dissolving the powder in 5mL of prepared CTAB, and mixing and performing ultrasonic treatment for 1h to obtain a mixed solution F, namely the CoPC/CNTs with positive electricity. 10mg of positively charged CoPC/CNTs powder was then added to 20mL of MXene suspension and shaken for 10h. Finally, the mixed solution F is placed in a freeze dryer for pre-freezing for 3h at the temperature of minus 40 ℃, cooling to the temperature of minus 60 ℃, and then freeze-drying for 48h. The CoPC/CNTs @ Mxene composite microwave absorbing powder is obtained.
Example 3
2.36g of Zn (NO) 3 ) 2 -6H 2 O and 4.72g of Co (NO) 3 ) 2 -6H 2 And mixing the solution A and the solution O, adding 240mL of methanol solution, and magnetically stirring for 20min to prepare a mixed solution A. Then, 7.88g of 2-Melm was dissolved in 100mL of a methanol solution to prepare a mixed solution B, which was then added to the mixed solution A, stirred at room temperature for 1 hour, and left to stand for 24 hours to obtain a mixed solution C. The resulting mixed solution C was washed 3 times with a methanol solution and centrifuged to collect the product. And (3) drying the collected product in a vacuum drying oven at the drying temperature of 60 ℃ for 12h to obtain purple ZnCo-MOF powder, namely a CoPC/CNTs precursor. And finally, placing the CoPC/CNTs precursor in a vacuum tube furnace, heating at 800 ℃ for 2 hours under the argon atmosphere condition, and finally obtaining the rhombic block-shaped CoPC/CNTs powder.
1g of LiF and 20mL of HCI solution were mixed to obtain a mixed solution B, and 1g of Ti was added 3 AIC 2 Adding the powder into the mixed solution B, placing the mixed solution B in a 35 ℃ water bath, stirring for 22h to obtain a mixed solution C, washing with deionized water until ph =7, performing ultrasonic dispersion for 16min, repeating the centrifugation of the mixed solution C for 3 times by using a high-speed centrifuge (the rotation speed is 3500rmp, and the centrifugation time is 60 min), and collecting a solution intermediate to obtain the MXene suspension.
Dissolving 2mg of CTAB in 100mL of deionized water, taking 100mg of CoPC/CNTs powder, dissolving in 5mL of prepared CTAB, and performing ultrasonic mixing for 1h to obtain a mixed solution F, namely the positively charged CoPC/CNTs. 10mg of the positively charged CoPC/CNTs powder was then added to 20mL of MXene suspension prepared in step 2, and shaking continued for 12h. Finally, the mixed solution F is placed in a freeze dryer for pre-freezing for 2 to 4 hours at the temperature of minus 40 ℃, and then is frozen and dried for 48 hours after being cooled to the temperature of minus 60 ℃. The CoPC/CNTs @ Mxene composite microwave absorbing powder is obtained.
Example 4
2.36g of Zn (NO) 3 ) 2 -6H 2 O and 4.72g of Co (NO) 3 ) 2 -6H 2 And mixing the solution A and the solution O, adding 240mL of methanol solution, and magnetically stirring for 20min to prepare a mixed solution A. Then, 7.88g of 2-Melm was dissolved in 100mL of methanol solution to prepare a mixed solution B, which was then added to the mixed solution A, stirred at room temperature for 1 hour, and left to stand for 24 hours to obtain a mixed solution C. The resulting mixed solution C was washed 3 times with a methanol solution and centrifuged to collect the product. And (3) drying the collected product in a vacuum drying oven at the drying temperature of 60 ℃ for 10-12h to obtain purple ZnCo-MOF powder, namely a CoPC/CNTs precursor. And finally, placing the CoPC/CNTs precursor in a vacuum tube furnace, heating at 800 ℃ for 2h under the argon atmosphere, and finally obtaining the rhombic block-shaped CoPC/CNTs powder.
1g of LiF and 20mL of HCI solution were mixed to obtain a mixed solution B, and 1g of Ti was added 3 AIC 2 Adding the powder into the mixed solution B, placing the mixed solution B in a water bath at 42 ℃, stirring the mixed solution for 24-26h to obtain a mixed solution C, adjusting the pH to be =7 by using deionized water, performing ultrasonic dispersion for 22min, repeating the centrifugation of the mixed solution C for 3 times by using a high-speed centrifuge (the rotation speed is 3500rmp, and the centrifugation time is 90 min), and collecting a solution intermediate to obtain the MXene suspension.
Dissolving 2mg of CTAB in 100mL of deionized water, taking 100mg of CoPC/CNTs powder, dissolving in 5mL of prepared CTAB, and performing ultrasonic mixing for 1h to obtain a mixed solution F, namely the positively charged CoPC/CNTs. 10mg of positively charged CoPC/CNTs powder was then taken and added to 20mL of MXene suspension and shaking continued for 24h. Finally, the mixed solution F is placed in a freeze dryer for pre-freezing for 3h at the temperature of minus 40 ℃, cooling to the temperature of minus 60 ℃, and then freeze-drying for 48h. The CoPC/CNTs @ Mxene composite microwave absorbing powder is obtained.
Example 5
2.36g of Zn (NO) 3 ) 2 -6H 2 O and 4.72g of Co (NO) 3 ) 2 -6H 2 And mixing the solution A and the solution O, adding 240mL of methanol solution, and magnetically stirring for 20min to prepare a mixed solution A. Then, 7.88g of 2-Melm was dissolved in 100mL of a methanol solution to prepare a mixed solution B, which was then added to the mixed solution A, stirred at room temperature for 1 hour, and left to stand for 24 hours to obtain a mixed solution C. The resulting mixed solution C was washed 3 times with a methanol solution and centrifuged to collect the product. And (3) drying the collected product in a vacuum drying oven at the drying temperature of 60 ℃ for 12h to obtain purple ZnCo-MOF powder, namely a CoPC/CNTs precursor. And finally, placing the CoPC/CNTs precursor in a vacuum tube furnace, heating at 800 ℃ for 2 hours under the argon atmosphere condition, and finally obtaining the rhombic block-shaped CoPC/CNTs powder.
1g of LiF and 20mL of HCI solution were mixed to obtain a mixed solution B, and 1g of Ti was added 3 AIC 2 Adding the powder into the mixed solution B, placing the mixed solution B in a 38 ℃ water bath, stirring for 23h to obtain a mixed solution C, adjusting the pH to be =7 by using deionized water, performing ultrasonic dispersion for 19min, centrifuging for 60min at the rotation speed of 3500rpm, repeating for 3 times, and collecting a solution intermediate to obtain an MXene suspension.
Dissolving 2mg of CTAB in 100mL of deionized water, taking 100mg of CoPC/CNTs powder, dissolving in 5mL of prepared CTAB, and performing ultrasonic mixing for 1h to obtain a mixed solution F, namely the positively charged CoPC/CNTs. Then 20mg of the positively charged CoPC/CNTs powder was added to 20mL of MXene suspension and shaking continued for 12h. And finally, placing the mixed solution F in a freeze dryer, pre-freezing for 2 hours at the temperature of minus 40 ℃, cooling to the temperature of minus 60 ℃, and then freeze-drying for 48 hours. The CoPC/CNTs @ Mxene composite microwave absorbing powder is obtained. The specific surface area of the obtained unit mass material is 1,695.9m 2 G, the mesoporous diameter is 1.6nm, and the pore volume is 0.68cm 3 /g。
FIG. 1 is a scanning electron micrograph of CoPC/CNTs @ Mxene composite powder obtained in example 5. As can be seen from fig. 1, it is clearly observed that the CoPC/CNTs are uniformly embedded in the MXene nanosheets in the composite powder prepared in example 5 at a mass ratio of 1.
Example 6
2.36g of Zn (NO) 3 ) 2 -6H 2 O and 4.72g of Co (NO) 3 ) 2 -6H 2 And mixing the solution A and the solution B, adding 240mL of methanol solution, and magnetically stirring for 20min to prepare a mixed solution A. Then, 7.88g of 2-Melm was dissolved in 100mL of a methanol solution to prepare a mixed solution B, which was then added to the mixed solution A, stirred at room temperature for 1 hour, and left to stand for 24 hours to obtain a mixed solution C. The resulting mixed solution C was washed 3 times with a methanol solution and centrifuged to collect the product. And (3) drying the collected product in a vacuum drying oven at the drying temperature of 60 ℃ for 12h to obtain purple ZnCo-MOF powder, namely a CoPC/CNTs precursor. And finally, placing the CoPC/CNTs precursor in a vacuum tube furnace, heating at 800 ℃ for 2h under the argon atmosphere, and finally obtaining the rhombic block-shaped CoPC/CNTs powder.
1g of LiF and 20mL of HCI solution were mixed to obtain a mixed solution B, and 1g of Ti was added 3 AIC 2 Adding the powder into the mixed solution B, placing the mixed solution B in a water bath at 40 ℃ and stirring the mixed solution C for 24h to obtain a mixed solution C, adjusting the pH to be =7 by using deionized water, ultrasonically dispersing the mixed solution C for 20min, centrifuging the mixed solution C for 60min at the rotating speed of 3000-3500rpm, repeating the steps for 3 times, and collecting a solution intermediate to obtain MXene suspension.
Dissolving 2mg of CTAB in 100mL of deionized water, taking 100mg of CoPC/CNTs powder, dissolving in 5mL of prepared CTAB, and performing ultrasonic mixing for 1h to obtain a mixed solution F, namely the positively charged CoPC/CNTs. 30mg of positively charged CoPC/CNTs powder was then added to 20mL of MXene suspension and shaken for 12h. Finally, the mixed solution F is placed in a freeze dryer for pre-freezing for 4h at the temperature of minus 40 ℃, cooling to the temperature of minus 60 ℃, and then freeze-drying for 48h. The CoPC/CNTs @ Mxene composite microwave absorbing powder is obtained. FIG. 2 is a scanning electron micrograph of the CoPC/CNTs @ Mxene composite powder obtained in example 6, and it can be clearly observed from FIG. 2 that CoPC/CNTs are distributed on MXene nanosheets.
The composite powder obtained in the embodiment 1-4 of the invention is obtained in different experimental environments under the condition that the mass ratio of CoPC/CNTs to MXene is 1. The experimental conditions of example 3 are preferably obtained by experimental control. Examples 5-6 different qualities of CoPC/CNTs and MXene under the same experimental environmentThe composite films are 1. The connection performance, the specific surface area and the microwave absorption efficiency of the composite sample can be effectively regulated and controlled by adjusting the content of CoPC/CNTs. The specific surface area of the CoPC/CNTs @ Mxene composite powder obtained by the method in unit mass is 1690.2-1671.3cm 2 G, the mesoporous aperture is 1.53-1.65nm, and the pore volume is 0.65-0.71cm 3 The/g is 4 times higher than that of pure MOF. As shown in FIG. 3, the composite powder with the mass ratio of 1 is that the microwave absorption performance reaches-54.2 dB, and the effective absorption bandwidth is 3.9GHz, so that the obtained CoPC/CNTs @ Mxene composite powder material has excellent microwave absorption efficiency and high specific surface area.
Through the mode, the preparation method of the powder with the high microwave absorption performance, which is obtained by embedding the rhombic block CoPC/CNTs into the MXene nanosheet layer, has the advantages of simple preparation process, easiness in control and low manufacturing cost; the CoPC/CNTs @ Mxene composite powder has the advantages of large specific surface area, abundant mesopores on the surface and excellent microwave absorption performance. The powder provides more possibilities for the preparation of MXene-based composite materials.
Claims (10)
1. The preparation method of the powder with high microwave absorptivity, in which rhombus block CoPC/CNTs are embedded into MXene, is characterized by comprising the following steps:
step 1, adding Zn (NO) 3 ) 2 -6H 2 O and Co (NO) 3 ) 2 -6H 2 Dissolving O in methanol, and magnetically stirring for 10-30min to obtain a mixed solution A; dissolving 2-Melm in methanol to prepare a mixed solution B, adding the mixed solution B into the mixed solution A, continuously stirring for 0.5-2h at room temperature, and standing for 10-24h to obtain a mixed solution C; washing the mixed solution C with methanol for 3 times, centrifuging and collecting a product, and drying the collected product in a vacuum drying oven to obtain ZnCo-MOF powder; putting the ZnCo-MOF powder into a vacuum tube furnace for annealing to obtain diamond-shaped block-shaped CoPC/CNTs powder;
step 2, mixing LiF and HCI solution to prepare mixed solution D, and mixing Ti 3 AIC 2 Adding the powder into the mixed solution D, stirring in 25-45 deg.C water bath to obtain mixed solution E, and removingWashing the daughter water until ph =7, centrifuging and taking out a supernatant to obtain an Mxene suspension;
and 3, adding the rhombic block-shaped CoPC/CNTs powder into CTAB and deionized water, performing ultrasonic treatment to obtain a mixed solution F, adding the mixed solution F into the MXene suspension, continuously oscillating for 6-24h, and performing freeze drying to obtain powder with high microwave absorption performance of CoPC/CNTs @ MXene.
2. The method for preparing MXene-embedded rhombohedral CoPC/CNTs powder with high microwave absorptivity as claimed in claim 1, wherein the Zn (NO) is added in step 1 3 ) 2 -6H 2 O、Co(NO 3 ) 2 -6H 2 The mass ratio of O to methanol is 1:2-4:81.
3. the method for preparing the diamond-shaped block-shaped CoPC/CNTs embedded MXene powder with high microwave absorptivity according to claim 1, wherein the mass ratio of 2-Melm to methanol in step 1 is 1:10.
4. the method for preparing the powder with high microwave absorptivity by embedding MXene into the rhombic CoPC/CNTs in the claim 1 is characterized in that the mass ratio of methanol in the mixed solution A to methanol in the mixed solution B in the step 1 is 2.4:1.
5. the method for preparing MXene-embedded rhombic CoPC/CNTs powder with high microwave absorptivity according to claim 1, wherein the conditions for annealing CoPC/CNTs precursor in the vacuum tube furnace in the step 1 are as follows: heating at 500-1100 deg.C under argon atmosphere for 1-6h.
6. The method of claim 1, wherein the step 2 of preparing the LiF and Ti powders with high microwave absorptivity by embedding the rhombohedral CoPC/CNTs into MXene comprises 3 AIC 2 The mass ratio of the powder is 1:1, the mass ratio of LiF to HCI is 1:10-20, wherein the concentration of HCI is 6-8M.
7. The method for preparing MXene-embedded rhombic CoPC/CNTs powder with high microwave absorptivity according to claim 1, wherein the rotation speed of the centrifugation in step 2 is 2500-4000rmp, and the centrifugation time is 30-90min.
8. The method for preparing MXene-embedded rhombic CoPC/CNTs powder with high microwave absorptivity according to claim 1, wherein the mass ratio of the rhombic CoPC/CNTs powder to the CTAB to the deionized water in step 3 is 2:1:10.
9. the method for preparing MXene-embedded rhombic CoPC/CNTs powder with high microwave absorptivity according to claim 1, wherein the mass ratio of the MXene suspension to the mixed solution F in step 3 is 0.5-3:2.
10. the method for preparing MXene-embedded rhombohedral CoPC/CNTs powder with high microwave absorptivity according to claim 1, wherein the conditions of freeze-drying in step 3 are as follows: placing the solution after continuous oscillation in a freeze dryer, pre-freezing at-40 deg.C for 2-4h, cooling to-60 deg.C, and freeze drying for 24-48h.
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