CN112143460A - Composite wave-absorbing material based on metal organic framework material and preparation method and application thereof - Google Patents
Composite wave-absorbing material based on metal organic framework material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a composite wave-absorbing material based on a metal organic framework material, which is a nano composite material based on a metal organic framework MOFs material and formed by wrapping a porous carbon layer on the surface layer of metal nano particles. The invention also discloses a preparation method of the composite wave-absorbing material based on the metal organic framework material and application of the composite wave-absorbing material in an electromagnetic wave absorbing material. The composite wave-absorbing material based on the metal organic framework material has controllable, excellent and stable microwave absorption performance through an in-situ chemical synthesis method and a heat treatment process, and the maximum absorption strength can reach-82 dB when the thickness of a sample is 2.0 mm.
Description
Technical Field
The invention belongs to the technical field of composite wave-absorbing materials, and particularly relates to a composite wave-absorbing material based on a metal organic framework material, and a preparation method and application thereof.
Background
With the rapid development of wireless communication technology in the modern times, the harm caused by electromagnetic radiation and interference in daily life increasingly attracts the attention of global researchers. On one hand, electromagnetic radiation and interference threaten human health, and simultaneously cause interference to electromagnetic equipment, and bring a series of problems to the application of the electromagnetic equipment in the military field. To address these increasingly severe electromagnetic emissions and interferences, efforts have been made to develop efficient electromagnetic absorbing materials with thin matching thickness, wide absorption bandwidth, light weight, and strong absorption capacity. Electromagnetic absorbing materials can be classified into three major categories, namely, conductive materials, dielectric materials and magnetic materials, according to the loss characteristics of electromagnetic waves. Heretofore, carbon materials, magnetic metal materials, have been widely used for the production of electromagnetic absorbing materials.
Although there are a lot of reports on magnetic wave absorbing materials, the practical application of magnetic materials in the field of electromagnetic wave absorption is limited by various problems of narrow absorption bandwidth, large thickness, large density and the like of magnetic materials. On the other hand, carbon materials such as carbon nanotubes have the advantages of high hardness, small density, light weight, wide absorption bandwidth and the like, but impedance mismatch caused by relatively high complex dielectric constant and poor magnetic permeability severely limits the application of the carbon materials in the field of electromagnetic wave absorption. Therefore, it is difficult to achieve high electromagnetic wave absorption performance for a single conductive material or magnetic material. In order to overcome the above disadvantages, an effective method is to design a composite material of a magnetic material and a carbon material so as to utilize a synergistic effect between the two. Although the electromagnetic wave absorption performance is substantially improved by compounding the magnetic material and the carbon material, how to prepare the electromagnetic absorption material with high performance by a simple and convenient method still has certain difficulty.
Metal-Organic Frameworks (MOFs) are hybrid Organic-inorganic materials with intramolecular pores formed by self-assembly of Organic ligands and Metal ions or clusters through coordination bonds. Due to the characteristics of the nano-pores and the open channels, an ideal template can be provided for preparing the carbon material with the porous structure. Chinese patent CN108834389A discloses a preparation method of a bimetal organic framework derived porous carbon/multi-walled carbon nanotube nano composite wave-absorbing material, the composite wave-absorbing material takes a multi-walled carbon nanotube as a carrier, cobalt nitrate hexahydrate and zinc nitrate hexahydrate as metal salt precursors, 2-methylimidazole as an organic ligand, methanol and ethanol as a mixed solvent, and the composite wave-absorbing material consisting of the multi-walled carbon nanotube loaded Co/Zn bimetal nano porous carbon is prepared through a high-temperature pyrolysis method. The composite wave-absorbing material prepared by the patent has complex preparation process and components, the maximum absorption intensity is only-39.07 dB under the thickness of 3.0mm, and the electromagnetic wave absorption intensity is not enough.
Therefore, the development of the electromagnetic composite wave-absorbing material with simple preparation method and excellent performance has important significance for the development and production of the wave-absorbing material.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a composite wave-absorbing material based on a metal organic framework material and a preparation method thereof.
The invention aims to provide a composite wave-absorbing material based on a metal organic framework material, wherein the composite wave-absorbing material is a nano composite material which is based on a metal organic framework MOFs material and is formed by wrapping a porous carbon layer on the surface layer of metal nano particles.
As a preferred embodiment of the invention, the metal element in the MOFs material with metal-organic framework is selected from at least one of nickel, iron, cobalt and manganese.
The second purpose of the invention is to provide a preparation method of the composite wave-absorbing material based on the metal organic framework material, which comprises the steps of carrying out in-situ reaction on the metal organic framework MOFs material in a microwave-assisted heating mode, and then carrying out heat treatment to obtain the nano composite material with the porous carbon layer wrapped on the surface layer of the metal nano particles.
As a preferred embodiment of the present invention, the temperature of the heat treatment is 500-700 ℃.
As a preferred embodiment of the invention, the specific surface area of the nanocomposite is greater than 70m2/g。
As a preferred embodiment of the present invention, the preparation method comprises the steps of:
step (1), mixing metal salt, organic ligand, sodium hydroxide, N-dimethylformamide and water to obtain uniform mixed liquor;
step (2), heating the uniform mixed solution obtained in the step (1) to 100-150 ℃ in a microwave-assisted heating manner, preserving the heat for 5-30min, and then cooling to room temperature;
step (3), centrifugally separating, cleaning and drying the product obtained in the step (2) to obtain a composite material precursor; and
and (4) performing heat treatment on the composite material precursor obtained in the step (3) in inert gas, wherein the heat treatment temperature is 500-700 ℃, the heat preservation time is 60-180min, and the heating rate is 5-10 ℃/min.
As a preferred embodiment of the present invention, the metal salt is at least one of chloride, nitrate and acetate of nickel, iron, cobalt and manganese; the organic ligand is at least one selected from terephthalic acid and 2-amino terephthalic acid.
As a preferred embodiment of the present invention, the molar ratio of the metal salt, the organic ligand, sodium hydroxide and N, N-dimethylformamide is 1: (1-3): (2-3): (400-1200).
As a preferred embodiment of the present invention, the inert gas is a hydrogen/nitrogen gas mixture or a hydrogen/argon gas mixture.
The third purpose of the invention is to provide the application of the composite wave-absorbing material based on the metal organic framework material in the electromagnetic wave absorbing material.
Compared with the prior art, the composite wave-absorbing material based on the metal organic framework material and the preparation method thereof have the following beneficial effects: the composite wave-absorbing material based on the metal organic framework material has controllable, excellent and stable microwave absorption performance through an in-situ chemical synthesis method and a heat treatment process, and the maximum absorption strength can reach-82 dB when the thickness of a sample is 2.0 mm.
Drawings
FIG. 1 is an XRD (X-ray diffraction) spectrum of composite wave-absorbing materials obtained in example 1, example 2, example 3 and a comparative example of the invention;
FIG. 2 is a hysteresis loop of composite wave-absorbing materials obtained in examples 1, 2, 3 and comparative examples of the present invention;
FIG. 3 is SEM (top) and TEM (bottom) images of example 2 of the present invention;
FIG. 4 shows specific surface areas of examples 1, 2 and 3 according to the present invention;
FIG. 5-1 is a wave-absorbing property diagram of example 1 of the present invention;
FIG. 5-2 is a wave-absorbing property diagram of example 2 of the present invention;
FIG. 5-3 is a wave-absorbing property diagram of example 3 of the present invention;
fig. 5-4 are wave-absorbing performance graphs of comparative examples of the present invention.
Detailed Description
The present invention will be further described with reference to the following specific examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.
Examples 1 to 6:
a composite wave-absorbing material based on a metal organic framework material is a nano composite material which is based on a metal organic framework MOFs material and is formed by wrapping a porous carbon layer on the surface layer of metal nano particles. Preferably, the metal element in the metal-organic framework MOFs material is selected from at least one of nickel, iron, cobalt and manganese. In this embodiment, the three-dimensional metal-organic framework MOFs material is exemplified by Ni-MOFs.
A preparation method of the composite wave-absorbing material based on Ni-MOFs comprises the following steps:
sequentially adding A g of nickel nitrate hexahydrate and B g of terephthalic acid into 50ml of N, N-dimethylformamide, and stirring at the temperature of about 25 ℃ for about 60 minutes to fully dissolve and uniformly mix;
step (2), slowly dropwise adding C ml of sodium hydroxide (0.4M) into the solution obtained in the step (1), and stirring at the temperature of about 25 ℃ for about 60 minutes to fully dissolve and uniformly mix the solution;
transferring the solution obtained in the step (1) into a three-neck flask, exhausting gas for 1 hour, and carrying out in-situ synthesis by adopting a microwave-assisted heating method, wherein the reaction power is 3kw, the reaction temperature is D ℃, and the heat preservation time is E minutes; centrifugally separating the prepared sample, washing the sample for three times by using N, N-dimethylformamide and deionized water, placing the sample in an oven at about 60 ℃, and drying the sample for about 24 hours;
and (4) carrying out heat treatment on the sample prepared in the step (3) in an inert gas F atmosphere, wherein the heating rate is 5 ℃/min, the heat treatment temperature is M ℃, the heat preservation time is N minutes, and the sample is cooled to the room temperature along with the furnace.
The values of the various parameters of the above example are listed in table 1.
TABLE 1
Comparative example:
in this example, the material produced was Ti3C2A material.
Ti of the example3C2The preparation method of the material comprises the following steps:
adding 0.24g of nickel nitrate hexahydrate and 0.42g of terephthalic acid into 50ml of N, N-dimethylformamide sequentially, and stirring at the temperature of about 25 ℃ for about 60 minutes to fully dissolve and uniformly mix;
step (b), slowly dripping 5ml of sodium hydroxide solution (0.4M) into the solution obtained in the step (a), and stirring for about 60 minutes at the temperature of about 25 ℃ to fully dissolve and uniformly mix the sodium hydroxide solution;
transferring the solution obtained in the step (b) into a three-neck flask, exhausting gas for 1 hour, and carrying out in-situ synthesis by adopting a microwave-assisted heating method, wherein the reaction power is 3kw, the reaction temperature is 100 ℃, and the heat preservation time is 10 minutes; and (3) centrifugally separating the prepared sample, washing the sample for three times by using N, N-dimethylformamide and deionized water, and drying the sample in an oven at about 60 ℃ for about 24 hours.
And (3) performance testing:
(1) respectively adopting irradiation source as Cu-Ka
X-ray diffraction (abbreviated as XRD) of the sample to determine the crystal structure of the sample.
(2) The magnetic properties of the product were obtained by a physical property measurement system (manufactured by quantum design, ltd.).
(3) And respectively observing the appearance of the sample by adopting a Scanning Electron Microscope (SEM), a Transmission Electron Microscope (TEM) and a high-resolution transmission electron microscope (HRTEM).
(4) The nitrogen adsorption-release curves of the samples were recorded using a Quad-rasorb-SI instrument, respectively, and the specific surface areas of the samples were measured by the Brunauer-Emmett-teller (bet) method.
(5) And measuring the electromagnetic parameters of the complex dielectric constant and the complex permeability of the electromagnetic parameters by a Siamese 3672B-S vector network analyzer in a frequency range of 2-18GHz by using a coaxial line method. Preparation of a test sample: the product was prepared by uniformly dispersing it in paraffin wax, 25% by weight, and then pressing into annular parts (7.0 mm outside diameter, 3.04 mm inside diameter).
The phase change of the materials obtained in examples 1, 2 and 3 and comparative example is shown in FIG. 1, and the magnetic properties thereof are shown in FIG. 2. The microstructure of the material prepared in example 2 is shown in fig. 3, and the change in specific surface area is shown in fig. 4. The wave absorption properties of the materials prepared in examples 1, 2, 3 and comparative example are shown in table 2 below, and the results are shown in fig. 5.
Table 2 table of wave-absorbing properties of examples 1, 2 and 3 and comparative example
In Table 2, RL is reflection loss, RLminIs the minimum reflection loss.
Phase analysis:
as can be seen from fig. 1, the composite materials prepared in examples 1, 2, 3 consist of two phases of Ni and carbon after heat treatment.
And (3) magnetic property analysis:
as can be seen from fig. 2, the Ni-based metal-organic framework nanocomposite obtained in the comparative example has no typical hysteresis behavior, mainly due to the lack of ferromagnetic components in its composition; the products obtained in examples 1, 2 and 3 all have relatively obvious hysteresis behavior, and the saturation magnetization of the product obtained in example 3 is obviously higher than that of the product obtained in example 1, mainly because the magnetic content of the Ni-porous carbon in example 3 is higher than that of the Ni-porous carbon in the product obtained in example 1 after heat treatment.
And (3) analyzing the change of the morphology and the specific surface area:
as can be seen from FIG. 3, the heat treatment resulted in the product of example 2, which in SEM images had a layered structure containing a large number of particles, and which was spectrally analyzed to be composed of Ni and C. It contains porous carbon and a large number of Ni nanoparticles (-30 nm) by TEM image analysis. In addition, the high-resolution TEM further discovers that a crystallized carbon layer with the thickness of 5nm is wrapped on the surface layer of the Ni nano-particles to form a Ni @ C core-shell structure. As shown in fig. 4, the specific surface area of the products obtained in examples 1, 2 and 3 is continuously reduced with the progress of the heat treatment, the particles are collapsed mainly due to the thermal decomposition of the organic matter, and the oxide particles grow up with the rise of the temperature, and the prepared nanocomposite has a higher specific surface area, which is beneficial to improving the electromagnetic wave absorption performance of the composite.
Wave-absorbing performance analysis:
as can be seen from Table 2 and FIG. 5, the RL values of the Ni-based metal-organic framework nanocomposite obtained in the comparative example are all greater than-10 dB in the measured frequency range, i.e. the Ni-based metal-organic framework nanocomposite does not have good wave-absorbing performance. The Ni-porous carbon sample of the product obtained in the example 1 has the thickness range of 2.0-5.0mm and the wave-absorbing bandwidth (RL)<-10dB) of 5.0 to 18.0GHz and RL at a specimen thickness of 3.5mmminIs-28 dB. The thickness range of the Ni-porous carbon particle sample of the product obtained in the embodiment 2 is 1.5-5mm, and the wave-absorbing bandwidth (RL) of the Ni-porous carbon particle sample<-10dB) of 4.2 to 18GHz, RL at a frequency of 15.3GHz and a specimen thickness of 2.0mmminIs-82 dB. The thickness range of the Ni-porous carbon particle sample of the product obtained in the embodiment 3 is 1.5-2.5mm, and the wave-absorbing bandwidth (RL) of the sample is wide<-10dB) of 9.5 to 18GHz and RL at a specimen thickness of 1.5mmminIs-13 dB. Therefore, the product obtained in example 2 shows excellent wave-absorbing performance in the range of C-Ku frequency band (4-18GHz), and has great application potential.
In conclusion, the nano composite material with excellent wave absorption performance and the porous carbon layer wrapped on the surface layer of the metal nano particle can be prepared by simple microwave-assisted heating reaction and heat treatment technology, particularly, the phase composition and microstructure of the nano particle of the nano composite material can be effectively adjusted in the technological process, the performance of the nano composite material is finally adjusted, the nano composite material is beneficial to promoting industrial production, and the nano composite material has important significance for wide application and development of the wave absorbing material.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (10)
1. The composite wave-absorbing material based on the metal organic framework material is characterized by being a nano composite material which is based on the metal organic framework MOFs material and is formed by wrapping a porous carbon layer on the surface layer of metal nano particles.
2. The composite wave-absorbing material based on the metal-organic framework material as claimed in claim 1, wherein the metal element in the metal-organic framework MOFs material is at least one selected from nickel, iron, cobalt and manganese.
3. The method for preparing the composite wave-absorbing material based on the metal organic framework material according to claim 1, wherein the metal organic framework MOFs material is subjected to in-situ reaction in a microwave-assisted heating mode, and then is subjected to heat treatment to obtain the nano composite material with the porous carbon layer wrapped on the surface layer of the metal nano particles.
4. The method as claimed in claim 3, wherein the temperature of the heat treatment is 500-700 ℃.
5. The method according to claim 3, wherein the nanocomposite material has a specific surface area of more than 70m2/g。
6. The method of manufacturing according to claim 3, comprising the steps of:
step (1), mixing metal salt, organic ligand, sodium hydroxide, N-dimethylformamide and water to obtain uniform mixed liquor;
step (2), heating the uniform mixed solution obtained in the step (1) to 100-150 ℃ in a microwave-assisted heating manner, preserving the heat for 5-30min, and then cooling to room temperature;
step (3), centrifugally separating, cleaning and drying the product obtained in the step (2) to obtain a composite material precursor; and
and (4) performing heat treatment on the composite material precursor obtained in the step (3) in inert gas, wherein the heat treatment temperature is 500-700 ℃, the heat preservation time is 60-180min, and the heating rate is 5-10 ℃/min.
7. The method according to claim 6, wherein the metal salt is at least one of chloride, nitrate and acetate of nickel, iron, cobalt and manganese; the organic ligand is at least one selected from terephthalic acid and 2-amino terephthalic acid.
8. The method according to claim 6, wherein the molar ratio of the metal salt, the organic ligand, the sodium hydroxide and the N, N-dimethylformamide is 1: (1-3): (2-3): (400-1200).
9. The method according to claim 6, wherein the inert gas is a hydrogen/nitrogen gas mixture or a hydrogen/argon gas mixture.
10. The composite wave-absorbing material based on the metal organic framework material as claimed in claim 1, which is applied to an electromagnetic wave absorbing material.
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| CN113285243A (en) * | 2021-05-14 | 2021-08-20 | 同济大学 | Covalent organic framework composite material and preparation method and application thereof |
| CN113620349A (en) * | 2021-09-01 | 2021-11-09 | 合肥工业大学 | One-dimensional iron-based wave-absorbing material derived from metal organic framework and preparation method thereof |
| CN114479762A (en) * | 2022-03-01 | 2022-05-13 | 同济大学 | Magnetic metal/metal oxide/carbon nano composite material, preparation method and application thereof |
| 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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| 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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