CN112251193A - Composite wave-absorbing material based on MXene and metal organic framework and preparation method and application thereof - Google Patents
Composite wave-absorbing material based on MXene and metal organic framework and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a composite wave-absorbing material based on MXene and a metal organic framework, which is characterized in that the composite wave-absorbing material is based on layered nano-flake MXene matrix Ti3C2Loading metal nano-particles and TiO on a layered carbon skeleton obtained by compounding with a three-dimensional metal organic framework MOFs material2A composite of nanoparticles. The invention also discloses a preparation method of the composite wave-absorbing material and application of the composite wave-absorbing material in an electromagnetic wave absorbing material. The composite wave-absorbing material based on MXene and the metal organic framework and the preparation method thereof have the following beneficial effects: the composite wave-absorbing material based on MXene and the metal organic framework 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-51.8 dB when the thickness of a sample is 3.0 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 MXene and a metal organic framework, and a preparation method and application thereof.
Background
The increasing popularity of handheld and wearable devices has exacerbated the problem of electromagnetic radiation concealment and hazard on a large scale, directly affecting public health and the normal operation of electronic and telecommunications equipment. The inhibition of electromagnetic radiation damage is a hot research topic. Military personnel and weapons are protected from electromagnetic interference in the army, and the operational efficiency is improved. In the high-tech field, electromagnetic protection plays a crucial role in the development of precision instruments. Nowadays, the development of high-performance and light-weight electromagnetic absorption and electromagnetic shielding technology is one of the most feasible ways to eliminate the electromagnetic pollution hazard. Generally, electromagnetic wave absorbing materials are classified into two major types, an electrically lossy material and a magnetically lossy material, according to electromagnetic wave loss characteristics. Common materials such as MXene and derivatives thereof, magnetic metals, ferrite materials, etc. are widely used for manufacturing electromagnetic wave absorbing materials.
MXene(Ti3C2) The two-dimensional nano material is a novel two-dimensional material obtained by chemically etching ternary ceramic MAX phase with hydrofluoric acid (HF). MXene derivative TiO2@ C has made tremendous progress as a nanocomposite in many fields such as energy storage, catalysis, and electromagnetic wave absorption. MXene derivative TiO2@ C has the advantages of 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 wide application of the @ C in the field of electromagnetic wave absorption; meanwhile, magnetic materials such as Fe3O4 have various problems such as narrow absorption bandwidth, large thickness and large density, and practical application of the magnetic materials in the field of electromagnetic wave absorption is limited. And it is difficult to achieve excellent impedance matching and thus high electromagnetic wave absorption performance for a single dielectric material or magnetic material.
By designing a composite material of a magnetic material and a dielectric material, it is an effective solution to the above problems to utilize the synergistic effect between the two. E.g. Co complexed with graphene, Fe3O4Graphene-composited NiZn ferrite and stoneGraphene complexation, and the like. Although the electromagnetic wave absorption performance is substantially improved by compounding the magnetic material with the carbon material, how to prepare the high-performance electromagnetic wave absorption material by simple structure and optimization of components still has certain difficulty.
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 MXene and a metal organic framework and a preparation method thereof.
The invention aims to provide a composite wave-absorbing material based on MXene and a metal organic framework, wherein the composite wave-absorbing material is based on layered nanosheet MXene matrix Ti3C2Loading metal nano-particles and TiO on a layered carbon skeleton obtained by compounding with a three-dimensional metal organic framework MOFs material2A composite of nanoparticles.
As a preferred embodiment of the invention, the metal element in the three-dimensional metal-organic framework MOFs material is at least one selected from nickel, iron, cobalt and manganese.
It is a second object of the present invention to provide a method as described aboveA composite wave-absorbing material based on MXene and metal organic frame is prepared from layered nano-flake MXene matrix Ti3C2Carrying out in-situ reaction with a three-dimensional metal organic framework MOFs material in a microwave-assisted heating mode, and then carrying out heat treatment to obtain metal nanoparticles and TiO loaded on a layered carbon skeleton2A composite of nanoparticles.
As a preferred embodiment of the present invention, the temperature of the heat treatment is 600-800 ℃.
As a preferred embodiment of the present invention, the metal nanoparticles and TiO2The mass percentage of the nano particles in the composite material is more than 60%.
As a preferred embodiment of the present invention, the preparation method comprises the steps of:
step (1) of adding Ti3C2Mixing the material with metal salt, organic ligand, sodium hydroxide, dimethyl formamide and water to obtain uniform mixed solution;
step (2), heating the uniform mixed solution obtained in the step (1) to 90-120 ℃ in a microwave-assisted heating mode, preserving the temperature for 30-60 seconds, and then cooling to room temperature;
step (3), 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 a mixed gas of hydrogen and argon, wherein the heat treatment temperature is 600-800 ℃, the heat preservation time is 100-150min, 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 Ti3C2The molar ratio of the material, the metal salt and the organic ligand is 1: (0.5-3): (0.5-3).
As a preferred embodiment of the present invention, the Ti3C2The preparation method of the material isThe chemical etching method comprises the following steps:
step (a) of adding Ti3AlC2Mixing with hydrofluoric acid;
step (b), heating the solution obtained in the step (a) to 40-50 ℃, preserving heat for 20-24 hours, and then cooling to room temperature;
and (c) centrifugally separating the product obtained in the step (b) to obtain a precipitate, washing the precipitate until the pH value of the centrifugal upper layer liquid is more than 5, and then washing and vacuum drying.
The third purpose of the invention is to provide an application of the composite wave-absorbing material based on MXene and the metal organic framework in an electromagnetic wave absorbing material.
Compared with the prior art, the composite wave-absorbing material based on MXene and the metal organic framework and the preparation method thereof have the following beneficial effects: the composite wave-absorbing material based on MXene and the metal organic framework 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-51.8 dB when the thickness of a sample is 3.0 mm.
Drawings
FIG. 1 is an XRD (X-ray diffraction) spectrum of the composite wave-absorbing material obtained in example 1, example 2 and example 3;
FIG. 2 is a hysteresis loop of composite wave-absorbing materials obtained in example 1, example 2 and comparative example of the present invention;
FIG. 3 is SEM (top) and TEM (bottom) images of comparative example, example 1, example 2 and example 3, respectively, from left to right;
FIG. 4-1 is a wave-absorbing property diagram of the composite wave-absorbing material obtained in the comparative example of the present invention;
FIG. 4-2 is a wave-absorbing property diagram of the composite wave-absorbing material obtained in example 1 of the present invention;
FIG. 4-3 is a wave-absorbing property diagram of the composite wave-absorbing material obtained in example 2 of the present invention;
fig. 4-4 are wave-absorbing performance diagrams of the composite wave-absorbing material obtained in example 3 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:
an MXene and metal organic framework-based composite wave-absorbing material is a layered nano-flake MXene matrix Ti3C2Loading metal nano-particles and TiO on a layered carbon skeleton obtained by compounding with a three-dimensional metal organic framework MOFs material2A composite of nanoparticles. Preferably, the metal element in the three-dimensional 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 Fe-MOFs.
A preparation method of the composite wave-absorbing material based on MXene and Fe-MOFs comprises the following steps:
(1) MXene matrix Ti3C2Preparation of the material:
step (1.1), 0.5 g of Ti3AlC2Adding into 10 ml concentrated hydrochloric acid solution containing 0.5 g lithium fluoride, and stirring at 25 deg.C for 5 min;
step (1.2), transferring the solution obtained in the step (1.1) into an oil bath pan, preserving the heat for 24 hours at the temperature of 40-50 ℃, cooling to room temperature, and then carrying out centrifugal separation on the liquid to obtain a centrifuged precipitate;
step (1.3), washing the product obtained in step (1.2) with deionized water until the pH value of the centrifugal upper layer liquid is more than 5, and then washing with alcohol liquid for 3 times;
and (1.4) drying the product obtained in the step (1.3) under vacuum.
(2)Ti3C2Preparation of the/Fe-MOFs composite material:
step (2.1), adding A g of the material prepared in the step (1) into a solution containing B g of ferric trichloride hexahydrate, C g of terephthalic acid, D g of sodium hydroxide, E ml of water and F ml (mass concentration is more than 99.8%) of dimethylformamide, heating to about 100 ℃ in a microwave-assisted heating mode, preserving heat for about 40 seconds, and then cooling to room temperature;
step (2.2), washing the product obtained in step (2.1) with deionized water for 3 times, and then washing with alcohol liquid for 3 times;
and (2.3) drying the product obtained in the step (2.2) under vacuum.
(3)Fe&TiO2The preparation method of the @ C composite wave-absorbing material comprises the following steps:
and (3) carrying out heat treatment on the material obtained in the step (2) in a hydrogen and argon mixed gas, wherein the heat treatment temperature is M ℃, the heat preservation time is N minutes, and the heating rate is 5-10 ℃/min.
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:
step (a), 0.5 g of Ti3AlC2Adding into 10 ml concentrated hydrochloric acid solution containing 0.5 g lithium fluoride, and stirring at 25 deg.C for 5 min;
transferring the solution obtained in the step (a) into an oil bath pan, preserving the temperature for 24 hours at about 50 ℃, cooling to room temperature, and then carrying out centrifugal separation on the liquid to obtain a centrifuged precipitate;
washing the product obtained in the step (b) with deionized water until the pH value of the centrifugal upper layer liquid is more than 5, and washing with alcohol liquid for 3 times;
and (d) drying the product obtained in the step (c) under vacuum.
And (3) performance testing:
(1) and respectively adopting a Transmission Electron Microscope (TEM) and a Scanning Electron Microscope (SEM) to observe the appearance of the sample.
(2) Respectively using radiation sources of
X-ray diffraction (abbreviated as XRD) of the sample to determine the crystal structure of the sample.
(3) The complex permittivity and complex permeability of the electromagnetic parameters were determined by means of the coaxial line method by means of an Agilent N5224A vector network analyzer in the frequency range of 2-18 GHz. Preparation of a test sample: the product was prepared by uniformly dispersing it in paraffin wax, which was 40% by weight, and then pressing into an annular member (7.0 mm outer diameter, 3.04 mm inner diameter).
The phase change of the materials prepared in examples 1, 2 and 3 and comparative example is shown in fig. 1, and the magnetic properties thereof are shown in table 2 below, and the results are shown in fig. 2.
TABLE 2 magnetic Properties of examples 1, 2 and 3 and comparative examples
In Table 2, Ms is the saturation magnetization, and Hc is the coercive force.
The shapes of the materials prepared in examples 1, 2 and 3 and the comparative example under a transmission electron microscope are shown in FIG. 3, and the changes of the specific surface area are shown in FIG. 4.
The wave absorption properties of the materials prepared in examples 1, 2, 3 and comparative example are shown in table 3 below.
Table 3 table of wave-absorbing properties of examples 1, 2 and 3 and comparative example
TABLE 3, where RL is the reflection loss, RLminIs the minimum reflection loss.
Phase analysis:
as can be seen from FIG. 1, the comparative example is typical of Ti3C2Material derivativePeak shooting, the product obtained by compounding Fe-MOFs material and proper heat treatment mainly contains Fe nano-particles and TiO2And (3) nanoparticles.
And (3) morphology analysis:
as can be seen from FIG. 3, the comparative example still maintains a layered structure without significant particles on the surface of the sheet layer since it is not compounded with Fe-MOFs and has not been heat-treated. The product of example 1, in TEM and SEM images, showed smaller nanoparticle roughness between the lamellae, but the shape of the lamellae remained complete. The product of example 2, with smaller nanoparticles appearing between the lamellae in the TEM and SEM images, still has the morphology characteristics of the comparative example in the overall morphology of the lamellar structure. The product of example 3, in TEM and SEM images, the size of the nano-particles between the sheets is obviously increased, and the surface of the sheet structure becomes rough, mainly because the Fe and TiO precipitated by the product is caused by the increase of the heat treatment temperature2The nanoparticles grow rapidly.
Wave-absorbing performance analysis:
as can be seen from Table 3 and FIG. 4, the product Ti obtained in the comparative example3C2The absorption bandwidth (RL) of a material sample with a thickness of 1-5mm and a sample thickness of 1.6mm<-10dB) is 3.5 GHz. The product obtained in example 1 had a sample thickness in the range of 1 to 5mm, a frequency of 6.6GHz and a sample thickness of 3.0mm, RLminIs-51.8 dB; absorption Bandwidth (RL) of a specimen thickness of 1.6mm<-10dB) is 6.5 GHz. The thickness range of the sample of the product obtained in the example 2 is 1-5mm, the wave absorption performance in the measured range is poor, and the RL values are all larger than-10 dB. Absorption Bandwidth (RL) of a specimen thickness of 1.6mm<-10dB) is 6.5 GHz. The product obtained in example 3 has a sample thickness in the range of 1-5mm, and an absorption bandwidth of 5GHz can be achieved when the sample thickness is 1.6 mm. Therefore, the product obtained in example 1 shows excellent wave-absorbing performance in a wider frequency range (11.5-18GHz), and has great application potential.
In conclusion, the method can prepare the metal nano-particles and TiO loaded on the layered carbon skeleton with excellent wave absorption performance by simple chemical etching, microwave-assisted heating reaction and heat treatment technology2Composite adsorption of nano particlesThe wave material and the parameter performance of the process are stable and efficient, which is beneficial to promoting the industrialized production and has important significance for the 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 MXene and metal organic framework is characterized in that the composite wave-absorbing material is based on layered nano-flake MXene matrix Ti3C2Loading metal nano-particles and TiO on a layered carbon skeleton obtained by compounding with a three-dimensional metal organic framework MOFs material2A composite of nanoparticles.
2. The composite wave-absorbing material based on MXene and metal organic framework as claimed in claim 1, wherein the metal element in the three-dimensional metal organic framework MOFs material is selected from at least one of nickel, iron, cobalt and manganese.
3. The method for preparing the composite wave-absorbing material based on MXene and the metal organic framework as claimed in claim 1, wherein the layered nano-flake MXene matrix Ti is prepared by3C2Carrying out in-situ reaction with a three-dimensional metal organic framework MOFs material in a microwave-assisted heating mode, and then carrying out heat treatment to obtain metal nanoparticles and TiO loaded on a layered carbon skeleton2A composite of nanoparticles.
4. The method as claimed in claim 3, wherein the temperature of the heat treatment is 600-800 ℃.
5. According toThe method of claim 3, wherein the metal nanoparticles and TiO are mixed2The mass percentage of the nano particles in the composite material is more than 60%.
6. The method of manufacturing according to claim 3, comprising the steps of:
step (1) of adding Ti3C2Mixing the material with metal salt, organic ligand, sodium hydroxide, dimethyl formamide and water to obtain uniform mixed solution;
step (2), heating the uniform mixed solution obtained in the step (1) to 90-120 ℃ in a microwave-assisted heating mode, preserving the temperature for 30-60 seconds, and then cooling to room temperature;
step (3), 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 a mixed gas of hydrogen and argon, wherein the heat treatment temperature is 600-800 ℃, the heat preservation time is 100-150min, 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 Ti is3C2The molar ratio of the material, the metal salt and the organic ligand is 1: (0.5-3): (0.5-3).
9. The method according to claim 6, wherein the Ti is3C2The preparation method of the material is a chemical etching method, and comprises the following steps:
step (a) of adding Ti3AlC2Mixing with hydrofluoric acid;
step (b), heating the solution obtained in the step (a) to 40-50 ℃, preserving heat for 20-24 hours, and then cooling to room temperature;
and (c) centrifugally separating the product obtained in the step (b) to obtain a precipitate, washing the precipitate until the pH value of the centrifugal upper layer liquid is more than 5, and then washing and vacuum drying.
10. The use of the composite wave absorbing material based on MXene and metal organic framework according to claim 1 in an electromagnetic wave absorbing material.
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| CN113817195A (en) * | 2021-11-02 | 2021-12-21 | 浙江优可丽新材料有限公司 | Chitin @ MXene @ Ni chain thin film material and preparation method and application thereof |
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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 |
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| CN113316379A (en) * | 2021-05-26 | 2021-08-27 | 湖南工程学院 | Nano composite structure wave absorber material, preparation method and application |
| CN113316379B (en) * | 2021-05-26 | 2022-09-02 | 湖南工程学院 | Nano composite structure wave absorber material, preparation method and application |
| WO2022259775A1 (en) * | 2021-06-10 | 2022-12-15 | 株式会社村田製作所 | Magnetic material, electromagnetic component, and method for manufacturing magnetic material |
| CN115843172B (en) * | 2021-09-18 | 2024-01-09 | 安徽璜峪电磁技术有限公司 | Hollow carbon supported metal nickel particles, preparation method and application of microwave absorption |
| CN115843172A (en) * | 2021-09-18 | 2023-03-24 | 安徽璜峪电磁技术有限公司 | Hollow carbon-loaded metal nickel particle, preparation method and application of microwave absorption |
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| CN113950236B (en) * | 2021-11-01 | 2022-09-30 | 北京航空航天大学 | MXene-based composite material and preparation method and application thereof |
| CN113817195A (en) * | 2021-11-02 | 2021-12-21 | 浙江优可丽新材料有限公司 | Chitin @ MXene @ Ni chain thin film material and preparation method and application thereof |
| CN113817195B (en) * | 2021-11-02 | 2023-11-03 | 浙江优可丽新材料有限公司 | chitin@MXene@Ni chain film material and preparation method and application thereof |
| CN114985011B (en) * | 2022-05-18 | 2023-12-22 | 东南大学 | TiO (titanium dioxide) 2 MXene/MOFs photocatalytic material and preparation method thereof |
| CN114985011A (en) * | 2022-05-18 | 2022-09-02 | 东南大学 | TiO 2 2 Mxene/MOFs photocatalytic material and preparation method thereof |
| CN115093677A (en) * | 2022-07-13 | 2022-09-23 | 哈尔滨工业大学 | Preparation method of MOF @ MXene reinforced resin matrix composite material |
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