CN114520419A - Preparation method of cobalt-based metal organic framework derivative wave absorbing agent with nano composite structure - Google Patents
Preparation method of cobalt-based metal organic framework derivative wave absorbing agent with nano composite structure Download PDFInfo
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- CN114520419A CN114520419A CN202210106828.XA CN202210106828A CN114520419A CN 114520419 A CN114520419 A CN 114520419A CN 202210106828 A CN202210106828 A CN 202210106828A CN 114520419 A CN114520419 A CN 114520419A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
Abstract
The invention belongs to the field of materials, and particularly relates to a preparation method of a cobalt-based metal organic framework derivative wave absorbing agent with a nano composite structure, which solves the technical problem that the cobalt-based metal organic framework derivative is difficult to achieve high absorption bandwidth. Firstly, preparing a metal organic framework precursor by adopting a solvothermal method, dissolving cobalt nitrate hexahydrate, terephthalic acid and polyvinylpyrrolidone K30 in a mixed solution of deionized water, absolute ethyl alcohol and N, N-dimethylformamide, and stirring to obtain a uniform and stable solution. And then, sealing the solution in a polytetrafluoroethylene-lined stainless steel reaction kettle, carrying out solvent thermal reaction, cooling, collecting precipitate by centrifugation, washing with deionized water for several times, and drying. And finally, carbonizing at high temperature in a tube furnace under the protective atmosphere, and collecting and sintering the obtained product to obtain the cobalt-based metal organic framework derivative wave absorbing agent with the nano composite structure.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to a preparation method of a cobalt-based metal organic framework derivative wave absorbing agent with a nano composite structure.
Background
With the rapid development of information communication technology, various electronic devices, particularly fifth generation (5G) mobile communication devices, have greatly improved information exchange by providing extremely high data transmission rates and extremely low delays. As a medium for transmitting signals, electromagnetic waves received and generated have covered various scenes in social environments and sensitive electronic devices in industrial environments. High frequency electromagnetic waves have high energy density and pose a serious threat to the stable operation of sensitive devices and human health. Therefore, this difficulty has been a problem to be overcome, and the search for electromagnetic wave absorbing materials is urgent.
Carbon-based nanomaterials (carbon nanotubes and graphene) have been widely studied as candidates for electromagnetic wave absorbers due to their relatively low density and controllable dielectric parameters. However, due to their non-magnetic properties, their permeability is much lower than the imperfect impedance matching due to their dielectric constant, reducing absorption capacity. Recently, MXene is considered as a promising electromagnetic wave absorbent, but pure MXene has too high conductivity to be an excellent electromagnetic wave absorbent. Although the above materials exhibit electromagnetic wave absorption properties based on soft magnetic or dielectric properties, the coupling of magnetic and dielectric absorption is expected to be achieved by constructing a novel nanocomposite through a combination of magnetic and dielectric components. Therefore, the development of a new highly efficient electromagnetic wave absorbent is urgently required to meet this demand. At the same time, it is also expected that the fabrication of such nanocomposites with more porous structures would help to further tune the electromagnetic wave absorption.
Disclosure of Invention
The invention aims to provide a preparation method of a cobalt-based metal organic framework derivative wave absorbing agent with a nano composite structure, namely a method of solvothermal and high-temperature carbonization is adopted to prepare a multilayer composite structure loaded with nano particles, so that the technical problem that the cobalt-based metal organic framework derivative is difficult to achieve high absorption bandwidth is solved.
The technical scheme of the invention is as follows:
firstly, preparing a metal organic framework precursor by adopting a solvothermal method, dissolving cobalt nitrate hexahydrate, terephthalic acid and polyvinylpyrrolidone K30 in a mixed solution of deionized water, absolute ethyl alcohol and N, N-dimethylformamide, and stirring to obtain a uniform and stable solution; sealing the obtained solution in a polytetrafluoroethylene-lined stainless steel reaction kettle, carrying out solvent thermal reaction, cooling, collecting precipitate by centrifugation, washing with deionized water, and drying; and finally, carbonizing at high temperature in a tube furnace under the protective atmosphere, and collecting and sintering to obtain a product, namely the cobalt-based metal organic framework derivative wave absorbing agent with the nano composite structure.
According to the preparation method of the cobalt-based metal organic framework derivative wave absorbing agent with the nano composite structure, the purity of cobalt nitrate hexahydrate is more than or equal to 98.5 wt%, the purity of terephthalic acid is more than or equal to 99 wt%, polyvinylpyrrolidone K30 is super grade pure, deionized water is analytically pure, the purity of absolute ethyl alcohol is more than or equal to 99.7 wt%, and the purity of N, N-dimethylformamide is more than or equal to 99.5 wt%.
According to the preparation method of the cobalt-based metal organic framework derivative wave absorbing agent with the nano composite structure, the amount of cobalt nitrate hexahydrate is 1.748g, the amount of terephthalic acid is 0.6g, the amount of polyvinylpyrrolidone K30 is 4.0g, and the amounts of deionized water, absolute ethyl alcohol and N, N-dimethylformamide are 40mL respectively.
According to the preparation method of the cobalt-based metal organic framework derivative wave absorbing agent with the nano composite structure, the stirring time is 20-40 min, and the temperature of the solvothermal reaction is kept at 180-220 ℃ for 10-15 hours.
The preparation method of the cobalt-based metal organic framework derivative wave absorbing agent with the nano composite structure comprises the step of drying for 6-10 hours in vacuum at the temperature of 50-70 ℃.
The cobalt-based metal with the nano composite structureThe preparation method of the organic framework derivative wave absorbing agent comprises the following process parameters of high-temperature carbonization in a tubular furnace: the heating rate is 8-12 ℃/min, the heat preservation temperature is 700 +/-10 ℃, and the heat preservation time is 4-6 hours; the protective atmosphere is 95 percent of Ar and 5 percent of H in percentage by volume2The mixed gas of (1).
The preparation method of the cobalt-based metal organic framework derivative wave absorbing agent with the nano composite structure is characterized in that: more than two layers of composite structures loaded with nano-particles.
According to the preparation method of the cobalt-based metal organic framework derivative wave absorbing agent with the nano composite structure, the basic framework of the cobalt-based metal organic framework derivative is in a typical fan-shaped form, the overall size of the cobalt-based metal organic framework derivative is 50-100 mu m, the surface of each single-layer sheet is covered with nano particles, and the material of the nano particles is simple substance cobalt.
The cobalt-based metal organic framework derivative wave-absorbing agent with the nano composite structure is applied, and the cobalt-based metal organic framework derivative is used as a wave-absorbing material with a frequency band of 11-18 GHz.
The cobalt-based metal organic framework derivative wave-absorbing agent with the nano composite structure is applied by mixing the cobalt-based metal organic framework derivative with a medium for absorbing electromagnetic waves to serve as a wave-absorbing material; according to the mass percentage, the cobalt-based metal organic framework derivative accounts for 30-60 wt%, and the balance is a medium for absorbing electromagnetic waves.
The design idea of the invention is as follows:
at present, the effective bandwidth of the pure cobalt-based metal organic framework derivative is lower and is lower than 6GHz, so that the wide application of the pure cobalt-based metal organic framework derivative is limited. Firstly, preparing a metal organic framework precursor by adopting a solvothermal method, dissolving cobalt nitrate hexahydrate, terephthalic acid and polyvinylpyrrolidone K30 in a mixed solution of deionized water, absolute ethyl alcohol and N, N-dimethylformamide, and stirring to obtain a uniform and stable solution; sealing the obtained solution in a polytetrafluoroethylene-lined stainless steel reaction kettle, carrying out solvent thermal reaction, cooling, collecting precipitate by centrifugation, washing with deionized water, and drying; and finally, carbonizing at high temperature in a tube furnace under the protective atmosphere, and collecting and sintering to obtain a product, namely the cobalt-based metal organic framework derivative wave absorbing agent with the nano composite structure.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention adopts a simple solvothermal method to prepare a metal organic framework precursor, synthesizes a novel cobalt-based metal organic framework derivative through solvothermal and sintering processes, and the composite material has a layered porous layered structure, is loaded with nano particles on a layer sheet and can be used in the field of electromagnetic wave absorption.
2. The preparation method has the advantages of simple preparation process, convenient operation, low cost, safety, reliability and high repeatability.
3. The invention improves the current situation that the effective bandwidth of the pure cobalt-based metal organic framework derivative is lower than 6GHz, and widens the application prospect of the pure cobalt-based metal organic framework derivative.
Drawings
FIG. 1 is an X-ray diffraction spectrum of a cobalt-based metal organic framework derivative wave-absorbing agent of a nanocomposite structure in an embodiment; in the figure, the abscissa 2 θ (degree) is the diffraction angle, and the ordinate Intensity (a.u.) is the relative Intensity.
FIG. 2 is a scanning electron microscope (topographical map) of a cobalt-based metal organic framework derivative absorber of the nanocomposite structure in an example.
FIG. 3 shows magnetization curves of cobalt-based MOFs absorber of nanocomposite structure at 300K (room temperature); in the figure, the abscissa H (kOe) represents the magnetic field intensity, and the ordinate M (emu/g) represents the magnetization.
FIG. 4 shows the variation of electromagnetic parameters with frequency of cobalt-based metal organic framework derivative wave-absorbers of the nanocomposite structure. Wherein, (a) the change relation of a real part epsilon 'of the dielectric constant with the frequency, (b) the change relation of an imaginary part epsilon' of the dielectric constant with the frequency, (c) the change relation of a real part mu 'of the magnetic permeability with the frequency, and (d) the change relation of an imaginary part mu' of the magnetic permeability with the frequency; in the figure, the abscissa frequency (GHz) is the frequency.
The reflection loss of the cobalt-based metal organic framework derivative absorber of the nanocomposite structure in the example of fig. 5 varies with frequency. Wherein (a)30 wt.% of the cobalt-based metal organic framework derivative absorber of the nanocomposite structure has a reflection loss as a function of frequency, (b)40 wt.% of the cobalt-based metal organic framework derivative absorber of the nanocomposite structure has a reflection loss as a function of frequency, (c)50 wt.% of the cobalt-based metal organic framework derivative absorber of the nanocomposite structure has a reflection loss as a function of frequency, (d)60 wt.% of the cobalt-based metal organic framework derivative absorber of the nanocomposite structure has a reflection loss as a function of frequency; in the figure, frequency (GHz) is the abscissa, and reflection loss (dB) is the ordinate RL (dB).
Detailed Description
In the specific implementation process, the preparation method of the cobalt-based metal organic framework derivative wave absorbing agent with the nano composite structure comprises the following steps: firstly, preparing a metal organic framework precursor by adopting a solvothermal method, dissolving cobalt nitrate hexahydrate, terephthalic acid and polyvinylpyrrolidone K30 in a mixed solution of deionized water, absolute ethyl alcohol and N, N-dimethylformamide, and stirring to obtain a uniform and stable solution. And then sealing the obtained solution in a polytetrafluoroethylene-lined stainless steel reaction kettle, carrying out solvent thermal reaction, cooling, collecting precipitates by centrifugation, washing with deionized water for 2-6 times, and drying. And finally, carbonizing at high temperature in a tube furnace under the protective atmosphere, and collecting a product obtained by sintering.
The present invention will be explained in further detail below by way of examples and figures.
Examples
In this embodiment, the preparation method of the cobalt-based metal organic framework derivative wave-absorbing agent with the nano composite structure is as follows:
first, 1.748g of cobalt nitrate hexahydrate, 0.6g of terephthalic acid and 4.0g of polyvinylpyrrolidone K30 were dissolved in a mixed solution containing 40ml of deionized water, 40ml of anhydrous ethanol and 40ml of N, N-dimethylformamideIn the solution, stirring was carried out for 30 minutes to obtain a uniform and stable solution. Next, the resulting solution was sealed in a teflon lined stainless steel reaction kettle and incubated at 200 ℃ for 12 hours. Then, the resulting pink precipitate was washed 3 times with deionized water and dried under vacuum at 60 ℃ for 8 hours. Finally, in a tube furnace at a volume percentage of Ar (95%)/H2(5%) heating the obtained product at the speed of 10 ℃/min under the protective atmosphere, wherein the heat preservation temperature is 700 ℃, and the heat preservation time is 5 hours. Collecting the product obtained by sintering to obtain the multilayer composite structure of the cobalt-based metal organic framework derivative loaded with the nano particles.
As shown in FIG. 1, the main phase of the obtained multilayer composite structure of the cobalt-based metal organic framework derivative supporting the nanoparticles is simple substance cobalt.
As shown in fig. 2, the obtained cobalt-based metal organic framework derivative multilayer composite structure loaded with nanoparticles has the structural characteristics that: a multilayer composite structure loaded with nanoparticles. The basic skeleton is a typical fan-shaped form, the overall size of the basic skeleton is about 80 mu m, the surface of each single-layer sheet is covered with nanoscale spherical particles, and the nanoscale spherical particles are made of simple substance cobalt.
As shown in FIG. 3, the cobalt-based metal organic framework derivative wave-absorbing agent having a nanocomposite structure had a saturation magnetization of 134.93emu/g, and showed strong magnetic properties.
As shown in FIG. 4, 30 wt.%, 40 wt.%, 50 wt.%, and 60 wt.% cobalt-based metal organic framework derivative absorbent samples with nanocomposite structures are mixed with 70 wt.%, 60 wt.%, 50 wt.%, and 40 wt.% paraffin (medium for absorbing electromagnetic waves), respectively, and the electromagnetic properties measured at room temperature have a real part of dielectric constant ε 'ranging from 5 to 35 in the range of 2 to 18GHz, an imaginary part of dielectric constant ε "ranging from 5 to 55 in the range of 2 to 18GHz, a real part of complex permeability μ' ranging from 0.7 to 1.35 in the range of 2 to 18GHz, and an imaginary part of complex permeability μ" ranging from 0 to 0.25 in the range of 2 to 18 GHz.
As shown in fig. 5, by mass percentage, curves of the change of reflection loss of cobalt-based metal organic framework derivative absorbent samples with a nanocomposite structure with frequency are given, and the curves show that, when the content of the samples is measured from 30 wt.% to 60 wt.%, the samples have good wave absorbing performance in a high frequency range (11 to 18GHz) when the content of the samples reaches 30 wt.%, the reflection loss approaches-32.92 dB (> 99.99% absorption), and the effective bandwidth of 6.9GHz when d is 2.5mm, which in sum up has strong wave absorbing performance in a high frequency range of 11 to 18 GHz.
Comparative example 1
In this comparative example, 1.748g of cobalt nitrate hexahydrate, 0.6g of terephthalic acid and 4.0g of polyvinylpyrrolidone K30 were dissolved in a mixed solution containing 40ml of deionized water, 40ml of anhydrous ethanol and 40ml of N, N-dimethylformamide, and stirred for 30 minutes to obtain a uniform and stable solution. Next, the mixed solution was sealed in a teflon-lined stainless steel reaction vessel and incubated at 200 ℃ for 12 hours. Then, the resulting pink precipitate was washed 3 times with deionized water and dried under vacuum at 60 ℃ for 8 hours. Finally, in a tube furnace at a volume percentage of Ar (95%)/H2(5%) heating the obtained product at the speed of 10 ℃/min under the protective atmosphere, keeping the temperature at 600 ℃, and keeping the temperature for 5 hours to obtain the cobalt-based metal organic framework derivative multilayer composite structure loaded with the nano particles. But because the heating temperature in the tube furnace is insufficient, the electromagnetic matching is poor, the wave absorbing performance is poor, and the performance indexes are as follows: the optimal reflection loss at 13.7GHz is-6.9 dB, and no effective bandwidth exists.
Comparative example 2
In this comparative example, 1.748g of cobalt nitrate hexahydrate, 0.6g of terephthalic acid and 4.0g of polyvinylpyrrolidone K30 were dissolved in a mixed solution containing 40ml of deionized water, 40ml of anhydrous ethanol and 40ml of N, N-dimethylformamide, and stirred for 30 minutes to obtain a uniform and stable solution. Next, the mixed solution was sealed in a teflon-lined stainless steel reaction vessel and incubated at 200 ℃ for 12 hours. Then, the resulting pink precipitate was washed 3 times with deionized water and dried under vacuum at 60 ℃ for 8 hours. Finally, in a tube furnace at a volume percentage of Ar (95%)/H2(5%) heating the obtained product at a speed of 10 ℃/min under a protective atmosphere, keeping the temperature at 800 ℃ and keeping the temperature atAnd (5) heating for 5 hours to obtain the cobalt-based metal organic framework derivative multilayer composite structure loaded with the nano particles. However, the electromagnetic matching is poor due to the over-high heating temperature in the tube furnace, so the wave absorbing performance is poor, and the performance refers to the following: the optimal reflection loss at 14.6GHz is-14.99 dB, and the maximum effective bandwidth is 5.9 GHz.
The above-described embodiments are merely illustrative of the present invention and are not to be construed as limiting the scope of the invention or as limiting the structure of the invention in any way. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (10)
1. A preparation method of a cobalt-based metal organic framework derivative wave absorbing agent with a nano composite structure is characterized by comprising the following steps of firstly, preparing a metal organic framework precursor by a solvothermal method, dissolving cobalt nitrate hexahydrate, terephthalic acid and polyvinylpyrrolidone K30 in a mixed solution of deionized water, absolute ethyl alcohol and N, N-dimethylformamide, and stirring to obtain a uniform and stable solution; sealing the obtained solution in a polytetrafluoroethylene-lined stainless steel reaction kettle, carrying out solvent thermal reaction, cooling, collecting precipitate by centrifugation, washing with deionized water, and drying; and finally, carbonizing at high temperature in a tube furnace under the protective atmosphere, and collecting and sintering to obtain a product, namely the cobalt-based metal organic framework derivative wave absorbing agent with the nano composite structure.
2. The method for preparing a cobalt-based metal organic framework derivative wave-absorbing agent with a nanocomposite structure according to claim 1, wherein the purity of cobalt nitrate hexahydrate is greater than or equal to 98.5 wt%, the purity of terephthalic acid is greater than or equal to 99 wt%, polyvinylpyrrolidone K30 is super grade pure, deionized water is analytically pure, the purity of absolute ethyl alcohol is greater than or equal to 99.7 wt%, and the purity of N, N-dimethylformamide is greater than or equal to 99.5 wt%.
3. The method for preparing a cobalt-based metal organic framework derivative wave absorber having a nanocomposite structure according to claim 1, wherein the amount of cobalt nitrate hexahydrate is 1.748g, the amount of terephthalic acid is 0.6g, the amount of polyvinylpyrrolidone K30 is 4.0g, and the amounts of deionized water, absolute ethyl alcohol and N, N-dimethylformamide are 40mL, respectively.
4. The preparation method of the cobalt-based metal organic framework derivative wave-absorbing agent with the nano-composite structure as claimed in claim 1, wherein the stirring time is 20-40 min, and the temperature of the solvothermal reaction is kept at 180-220 ℃ for 10-15 hours.
5. The method for preparing a cobalt-based metal organic framework derivative wave-absorbing agent with a nanocomposite structure according to claim 1, wherein the drying condition is vacuum drying at 50-70 ℃ for 6-10 hours.
6. The method for preparing a cobalt-based metal organic framework derivative wave-absorbing agent with a nano-composite structure as claimed in claim 1, wherein the technological parameters of high-temperature carbonization in a tube furnace are as follows: the heating rate is 8-12 ℃/min, the heat preservation temperature is 700 +/-10 ℃, and the heat preservation time is 4-6 hours; the protective atmosphere is 95 percent of Ar and 5 percent of H in percentage by volume2The mixed gas of (1).
7. The method for preparing a cobalt-based metal organic framework derivative wave-absorbing agent having a nanocomposite structure of claim 1, wherein the cobalt-based metal organic framework derivative has a structural characteristic of: more than two layers of composite structures loaded with nano-particles.
8. The method for preparing a cobalt-based metal organic framework derivative wave absorber with a nanocomposite structure as claimed in claim 7, wherein the basic skeleton of the cobalt-based metal organic framework derivative is typically fan-shaped, the overall size of the cobalt-based metal organic framework derivative is 50-100 μm, the surface of each single-layer sheet is covered with nanoparticles, and the material of the nanoparticles is elemental cobalt.
9. Use of the cobalt-based metal organic framework derivative wave-absorbing agent with the nano-composite structure as defined in any one of claims 1 to 8, wherein the cobalt-based metal organic framework derivative is used as a wave-absorbing material in a frequency band of 11-18 GHz.
10. The use of the cobalt-based metal organic framework derivative wave absorber having a nanocomposite structure according to claim 9, wherein the cobalt-based metal organic framework derivative is mixed with an electromagnetic wave absorbing medium to serve as a wave absorbing material; according to the mass percentage, the cobalt-based metal organic framework derivative accounts for 30-60 wt%, and the balance is a medium for absorbing electromagnetic waves.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115322744A (en) * | 2022-09-14 | 2022-11-11 | 中国海洋大学 | Nickel-carbon composite material for absorbing electromagnetic waves and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115322744A (en) * | 2022-09-14 | 2022-11-11 | 中国海洋大学 | Nickel-carbon composite material for absorbing electromagnetic waves and preparation method thereof |
| CN115322744B (en) * | 2022-09-14 | 2024-03-22 | 中国海洋大学 | Nickel-carbon composite material for absorbing electromagnetic waves and preparation method thereof |
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