CN113248725A - Preparation method of electromagnetic wave absorbing material based on MOF derivation and electromagnetic wave absorbing material - Google Patents
Preparation method of electromagnetic wave absorbing material based on MOF derivation and electromagnetic wave absorbing material Download PDFInfo
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- CN113248725A CN113248725A CN202110520635.4A CN202110520635A CN113248725A CN 113248725 A CN113248725 A CN 113248725A CN 202110520635 A CN202110520635 A CN 202110520635A CN 113248725 A CN113248725 A CN 113248725A
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Abstract
The invention relates to the technical field of electromagnetic wave absorbing materials, in particular to a preparation method of an electromagnetic wave absorbing material based on MOF derivation and an electromagnetic wave absorbing material. The preparation method comprises the following steps: step 1: and preparing a precursor. And mixing and stirring the metal salt aqueous solution and the 2-methylimidazole aqueous solution, fully reacting at room temperature, and centrifuging, washing and drying the obtained reactant to obtain the precursor with the MOFs structure. Step 2: and preparing the electromagnetic wave absorbing material. And (3) carrying out high-temperature heat treatment on the precursor in the step (1) under the protection of inert gas to obtain a spherical structure of the glutinous rice-like rice ball. The prepared electromagnetic wave absorbing material is a spherical structure similar to glutinous rice ball. The diameter of each single particle unit is 30-70 nm, and the diameter of each single electromagnetic wave absorption material is 400-800 nm. The invention has simple preparation process and low preparation cost, and does not produce environmental pollution in the preparation process. The electromagnetic wave absorbing material prepared by the invention has good wave absorbing performance, wide effective frequency width and small loading capacity.
Description
Technical Field
The invention relates to the technical field of electromagnetic wave absorbing materials, in particular to a preparation method of an electromagnetic wave absorbing material based on MOF derivation and an electromagnetic wave absorbing material.
Background
At present, with the rapid development of communication technology and electronic informatization, electromagnetic waves are widely applied to our living environment, which brings the continuous aggravation of electromagnetic wave pollution and threatens human health. Therefore, how to reduce or eliminate the harm of the increasingly worsening electromagnetic pollution to information, communication and the living and working environment of people is highly concerned by governments of various countries in the world, and is also a focus and hot point for research and discussion of expert and scholars of various countries.
Metal-organic frameworks (MOFs) are self-assembled from transition Metal ions and multifunctional organic ligands. The pore size and the shape of the catalyst can be controllably adjusted according to actual needs, and organic ligands with different lengths or different coordination numbers can be selected to prepare different pore sizes so as to meet the requirements of actual application. The composite material has the advantages of large specific surface area, ordered and adjustable pore channel structure, easy surface functionalization modification and the like, and is widely applied to the field of electromagnetic wave absorption in recent years.
At present, the MOFs-based electromagnetic wave absorbing material is prepared in the prior art, but the problems of complex preparation process, high preparation cost, waste liquid generated in the preparation process and environmental pollution, poor wave absorbing performance of the prepared electromagnetic wave absorbing material, narrow effective frequency bandwidth and large loading capacity still exist.
Therefore, there is an urgent need to develop an electromagnetic wave absorbing material with good wave absorbing performance, wide effective frequency bandwidth, small loading capacity, simple preparation process, low preparation cost and no waste liquid polluting the environment during the preparation process, and a preparation method thereof.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a preparation method of an electromagnetic wave absorbing material based on MOF derivation and the electromagnetic wave absorbing material.
The technical scheme of the invention is as follows:
a preparation method of an electromagnetic wave absorption material based on MOF derivation comprises the following steps:
step 1: preparation of the precursor
Dissolving a required amount of metal salt in deionized water, and dissolving a required amount of 2-methylimidazole in the deionized water; and mixing and stirring the metal salt aqueous solution and the 2-methylimidazole aqueous solution, fully reacting at room temperature, and centrifuging, washing and drying the obtained reactant to obtain the precursor with the MOFs structure.
Step 2: preparation of electromagnetic wave absorbing material
And (3) carrying out high-temperature heat treatment on the precursor prepared in the step (1) under the protection of inert gas to obtain a spherical structure of the glutinous rice ball-like rice ball.
Preferably, in step 1, the metal salt is at least one of zinc salt, nickel salt, iron salt and cobalt salt.
Preferably, the metal salt is zinc salt and nickel salt, and the molar ratio of the zinc salt to the nickel salt is 1: 1-1: 20; the zinc salt is zinc nitrate or zinc acetate; the nickel salt is nickel nitrate or nickel acetate.
Preferably, the molar ratio of the zinc salt to the nickel salt is 1: 3.
Preferably, the metal salt is zinc salt and ferric salt, and the molar ratio of the zinc salt to the ferric salt is 1: 1-1: 20; the zinc salt is zinc nitrate or zinc acetate; the ferric salt is ferric nitrate or ferric acetate.
Preferably, the metal salt is zinc salt and cobalt salt, and the molar ratio of the zinc salt to the cobalt salt is 1: 1-1: 20; the zinc salt is zinc nitrate or zinc acetate; the cobalt salt is cobalt nitrate or cobalt acetate.
Preferably, in the step 1, the volume of the deionized water is 5-200 ml, and the mass of the 2-methylimidazole is 1-20 g.
Preferably, in the step 1, the mixing and stirring time is 1-48 h.
Preferably, in the step 2, the heating rate of the heat treatment is 1-30 ℃ min-1The heat treatment temperature is 300-800 ℃, during heat treatmentThe time is 1-15 h.
An electromagnetic wave absorbing material based on MOF derivation is prepared by the preparation method, and the single electromagnetic wave absorbing material is arranged into a spherical structure of a glutinous rice ball formed by agglomerating a plurality of particle units with spherical structures.
Furthermore, the diameter of the particle unit is 30-70 nm, and the diameter of the single electromagnetic wave absorption material is 400-800 nm.
The invention achieves the following beneficial effects:
the preparation method is simple, in the preparation process, the required sample is prepared by simple precipitation stirring, the reaction temperature is room temperature, and microwave-assisted heating and other modes are not carried out in the synthesis process. In addition, in the process of collecting the sample, the invention adopts simple centrifugal washing and drying without the steps of suction filtration washing and the like, thereby greatly simplifying the preparation process.
The preparation method has low preparation cost, and in the synthesis process, organic solvents such as N, N-dimethylformamide or methanol and the like are not used, and deionized water is used as a reaction solvent, so that the cost expenditure is reduced to a certain extent.
The preparation method does not produce waste liquid polluting the environment, the reaction solvent of the invention is deionized water, no waste liquid is produced, and no hazardous chemical is used, thus having no pollution to the environment.
The electromagnetic wave absorbing material optimizes the microstructure of the obtained sample according to the molar ratio of the metal salt, wherein N is the ratio of the metal salt to the metal salt2After pyrolysis, the conductivity of the material is further improved while the structure of the obtained porous carbon structure is optimized, and the magnetic metal and the porous carbon are ingeniously combined, so that the magnetic loss and the dielectric loss of a sample reach impedance matching to a certain extent, and the electromagnetic wave-absorbing performance of the material is further improved.
The Ni @ NC electromagnetic wave absorption material prepared by the preparation method has good electromagnetic wave absorption performance, the optimal reflection loss can reach-74.06 dB, the effective absorption bandwidth is 5.23GHz, and the Ni @ NC electromagnetic wave absorption material is obviously superior to the electromagnetic wave absorption material on the existing market.
Drawings
FIG. 1 is an XRD spectrum of the Ni @ NC electromagnetic wave absorption material prepared in example 1 of the present invention.
FIG. 2 is an SEM photograph of the Ni @ NC electromagnetic wave absorbing material prepared in example 1 of the present invention.
FIG. 3 is a graph of electromagnetic parameters (loading amount is 20 wt%) of a Ni @ NC electromagnetic wave absorption material produced in example 1 of the present invention.
FIG. 4 is a graph showing the reflection loss of the Ni @ NC electromagnetic wave absorbing material produced in example 1 of the present invention.
FIG. 5 is an XRD spectrum of the Ni @ NC electromagnetic wave absorption material prepared in example 2 of the present invention.
FIG. 6 is a graph of electromagnetic parameters (loading amount is 20 wt%) of Ni @ NC electromagnetic wave absorbing material prepared in example 2 of the present invention.
Detailed Description
To facilitate an understanding of the present invention by those skilled in the art, specific embodiments thereof are described below with reference to the accompanying drawings.
Example 1
The preparation method of the Ni @ NC electromagnetic wave absorption material specifically comprises the following steps:
step 1: 0.2975g of zinc nitrate and 0.873g of nickel nitrate (molar ratio of zinc nitrate to nickel nitrate is 1: 3) were dissolved in 30ml of deionized water, and 2.602g of 2-methylimidazole were dissolved in 5ml of deionized water, and they were mixed and stirred at room temperature for 12 hours. And centrifuging the product after reaction for 5min at the rotating speed of 8000r/min, centrifuging and washing for 3-5 times, and finally drying in an oven at 55 ℃ to obtain a precursor NiZn-ZIF-L.
Step 2: adding precursor powder into N2Under protection, at 1 ℃ for min-1And heating to 700 ℃, preserving the heat for 2h, and naturally cooling to room temperature to obtain the Ni @ NC electromagnetic wave absorbing material.
From FIG. 1, it is found that the respective crystal planes of C (002) and Ni (111), (200) and (202) are obtained, and the diffraction peak intensity is high, indicating that the crystallinity is high.
As can be seen from FIG. 2, the diameter of the small particles was about 50nm, and the diameter of the spheres obtained by polymerization was about 500 nm. And it can be clearly seen that the small particles are agglomerated into a spherical structure.
As can be seen from FIG. 3, the real part of the complex dielectric constant is in the range of 6 to 8, and the imaginary part is in the range of 2 to 3, which indicates that the sample has high dielectric properties. Meanwhile, the initial permeability is close to 1 and higher than that of most of the electromagnetic wave absorbing agents of the same type, and the main reason is that the sample has extremely strong magnetism.
As can be seen from FIG. 4, when the impedance matching thickness is 1.91mm, the Ni @ NC electromagnetic wave absorption material achieves the maximum absorption strength of-74.06 dB at 15.63GHz, and effectively absorbs the broadband of 5.23 GHz.
Example 2
The preparation method of the Ni @ NC electromagnetic wave absorption material specifically comprises the following steps:
step 1: 0.2975g of zinc nitrate and 0.291g of nickel nitrate (molar ratio of zinc nitrate to nickel nitrate is 1: 1) were dissolved in 30ml of deionized water, and 2.602g of 2-methylimidazole was dissolved in 5ml of deionized water, and the two were mixed and stirred at room temperature for 12 hours. And centrifuging the product after reaction for 5min at the rotating speed of 8000r/min, centrifuging and washing for 3-5 times, and finally drying in an oven at 55 ℃ to obtain a precursor NiZn-ZIF-L.
Step 2: adding precursor powder into N2Under protection, at 1 ℃ for min-1And heating to 700 ℃, preserving the heat for 2h, and naturally cooling to room temperature to obtain the Ni @ NC electromagnetic wave absorbing material.
From FIG. 5, it can be found that the crystal planes corresponding to C (002) and Ni (111), (200) and (202), respectively, have higher diffraction peak intensities, indicating that the crystallinity is higher. But the strength was reduced compared to example 1.
As can be seen from fig. 6, the real part of the complex dielectric constant fluctuates around 3, and the imaginary part fluctuates around 1, and compared with the Ni @ NC electromagnetic wave absorbing material prepared in example 1, the main reason for the reduction of the complex dielectric constant of the material prepared in example 2 is the reduction of the nickel content, and the pores after the particle agglomeration are fewer, so that the conductive network is difficult to construct, the complex permeability is significantly reduced, and the magnetic property of the sample is also weakened.
Example 3
The preparation method of the Ni @ NC electromagnetic wave absorption material specifically comprises the following steps:
step 1: 0.873g of nickel nitrate (zinc nitrate/nickel nitrate molar ratio of 0:1) was dissolved in 30ml of deionized water, and 2.602g of 2-methylimidazole was dissolved in 5ml of deionized water, and the two were mixed and stirred at room temperature for 12 hours. And centrifuging the product after reaction for 5min at the rotating speed of 8000r/min, centrifuging and washing for 3-5 times, and finally drying in an oven at 55 ℃ to obtain a precursor Ni-ZIF-L.
Step 2: adding precursor powder into N2Under protection, at 1 ℃ for min-1And heating to 700 ℃, preserving the heat for 2h, and naturally cooling to room temperature to obtain the Ni @ NC electromagnetic wave absorbing material. The diameter of the Ni @ NC electromagnetic wave absorption material is 400nm, the maximum absorption intensity is-55.1 dB, and the broadband is effectively absorbed by 3.63 GHz.
Example 4
The preparation method of the NC electromagnetic wave absorption material specifically comprises the following steps:
step 1: 0.2975g of zinc nitrate (molar ratio of zinc nitrate to nickel nitrate: 1: 0) was dissolved in 30ml of deionized water, and 2.602g of 2-methylimidazole was dissolved in 5ml of deionized water, and the two were mixed and stirred at room temperature for 12 hours. And centrifuging the product after reaction for 5min at the rotating speed of 8000r/min, centrifuging and washing for 3-5 times, and finally drying in an oven at 55 ℃ to obtain a precursor Zn-ZIF-L.
Step 2: adding precursor powder into N2Under protection, at 1 ℃ for min-1And heating to 700 ℃, preserving the heat for 2h, and naturally cooling to room temperature to obtain the NC electromagnetic wave absorbing material. The diameter of the NC electromagnetic wave absorption material is 800nm, the maximum absorption intensity is-1.75 dB, and the NC electromagnetic wave absorption material can effectively absorb 0GHz of a broadband.
Example 5
The preparation method of the Fe @ NC electromagnetic wave absorption material specifically comprises the following steps:
step 1: 0.2975g of zinc nitrate and 1.212g of iron nitrate (molar ratio of zinc nitrate to iron nitrate is 1: 3) were dissolved in 30ml of deionized water, and 2.602g of 2-methylimidazole were dissolved in 5ml of deionized water, and they were mixed and stirred at room temperature for 12 hours. And centrifuging the product after reaction for 5min at the rotating speed of 8000r/min, centrifuging and washing for 3-5 times, and finally drying in an oven at 55 ℃ to obtain a precursor FeZn-ZIF-L.
Step 2: adding precursor powder into N2Under protection, at 1 ℃ for min-1And heating to 700 ℃, preserving the heat for 2h, and naturally cooling to room temperature to obtain the Fe @ NC electromagnetic wave absorbing material. The diameter of the Fe @ NC electromagnetic wave absorption material is 1 mu m, and the maximum absorption intensity is-45.04 dB, so that the broadband is effectively absorbed at 4.65 GHz.
Example 6
The preparation method of the Co @ NC electromagnetic wave absorption material specifically comprises the following steps:
step 1: 0.2975g of zinc nitrate and 0.873g of cobalt nitrate (the molar ratio of the zinc nitrate to the cobalt nitrate is 1: 3) are dissolved in 30ml of deionized water, 2.602g of 2-methylimidazole is dissolved in 5ml of deionized water, and the two are mixed and stirred at room temperature for 12 hours; and centrifuging the product after reaction for 5min at the rotating speed of 8000r/min, centrifuging and washing for 3-5 times, and finally drying in an oven at 55 ℃ to obtain a precursor CoZn-ZIF-L.
Step 2: adding precursor powder into N2Under protection, at 1 ℃ for min-1And heating to 700 ℃, preserving the heat for 2h, and naturally cooling to room temperature to obtain the Co @ NC electromagnetic wave absorbing material. The diameter of the Co @ NC electromagnetic wave absorption material is 4 mu m, the maximum absorption intensity is 44.3dB, and the broadband is effectively absorbed by 2 GHz.
The invention further prepares the spherical structure of the glutinous rice ball by taking the specific metal organic framework as the precursor, and the prepared electromagnetic wave absorbing material has high dielectric constant and strong electromagnetic wave loss capability and plays a role in promoting the synthesis and development of metal electromagnetic materials.
The above-described embodiments of the present invention do not limit the scope of the present invention. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (10)
1. A preparation method of an electromagnetic wave absorbing material based on MOF derivation is characterized by comprising the following steps:
step 1: preparation of the precursor
Dissolving a required amount of metal salt in deionized water, and dissolving a required amount of 2-methylimidazole in the deionized water; mixing and stirring a metal salt aqueous solution and a 2-methylimidazole aqueous solution, fully reacting at room temperature, and centrifuging, washing and drying the obtained reactant to obtain a precursor with an MOFs structure;
step 2: preparation of electromagnetic wave absorbing material
And (3) carrying out high-temperature heat treatment on the precursor prepared in the step (1) under the protection of inert gas to obtain a spherical structure of the glutinous rice ball-like rice ball.
2. The method for preparing the electromagnetic wave absorbing material based on the MOF derivation according to the claim 1, wherein: in the step 1, the metal salt is at least one of zinc salt, nickel salt, iron salt and cobalt salt.
3. The method for preparing the electromagnetic wave absorbing material based on the MOF derivation according to the claim 2, wherein: the metal salt is zinc salt and nickel salt, and the molar ratio of the zinc salt to the nickel salt is 1: 1-1: 20; the zinc salt is zinc nitrate or zinc acetate; the nickel salt is nickel nitrate or nickel acetate.
4. The method for preparing the electromagnetic wave absorbing material based on the MOF derivation according to the claim 3, wherein: the molar ratio of the zinc salt to the nickel salt is 1: 3.
5. The method for preparing the electromagnetic wave absorbing material based on the MOF derivation according to the claim 2, wherein: the metal salt is zinc salt and ferric salt, and the molar ratio of the zinc salt to the ferric salt is 1: 1-1: 20; the zinc salt is zinc nitrate or zinc acetate; the ferric salt is ferric nitrate or ferric acetate.
6. The method for preparing the electromagnetic wave absorbing material based on the MOF derivation according to the claim 2, wherein: the metal salt is zinc salt and cobalt salt, and the molar ratio of the zinc salt to the cobalt salt is 1: 1-1: 20; the zinc salt is zinc nitrate or zinc acetate; the cobalt salt is cobalt nitrate or cobalt acetate.
7. The method for preparing the electromagnetic wave absorbing material based on the MOF derivation according to the claim 1, wherein: in the step 1, the volume of the deionized water is 5-200 ml, and the mass of the 2-methylimidazole is 1-20 g.
8. The method for preparing the electromagnetic wave absorbing material based on the MOF derivation according to the claim 1, wherein: in the step 1, the mixing and stirring time is 1-48 h.
9. The method for preparing the electromagnetic wave absorbing material based on the MOF derivation according to the claim 1, wherein: in the step 2, the heating rate of the heat treatment is 1-30 ℃ per minute-1The heat treatment temperature is 300-800 ℃, and the heat treatment time is 1-15 h.
10. An electromagnetic wave absorbing material based on MOF derivation, characterized in that: the production method according to any one of claims 1 to 9, wherein the single electromagnetic wave absorbing material is provided in a spherical structure of a glutinous rice ball-like mass agglomerated from a plurality of spherical-structured particle units; the diameter of the particle unit is 30-70 nm, and the diameter of the single electromagnetic wave absorption material is 400-800 nm.
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| CN114907574A (en) * | 2022-06-14 | 2022-08-16 | 浙江理工大学 | Shape-controllable metal-organic framework material and preparation method and application thereof |
| CN115029711A (en) * | 2022-06-20 | 2022-09-09 | 陕西科技大学 | Carbon-coated ultra-small Fe 3 C nano particle electrocatalyst and its preparing method |
| CN115028847A (en) * | 2022-05-09 | 2022-09-09 | 复旦大学 | CoNi alloy MOF porous material and preparation and application thereof |
| 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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| CN115029711A (en) * | 2022-06-20 | 2022-09-09 | 陕西科技大学 | Carbon-coated ultra-small Fe 3 C nano particle electrocatalyst and its preparing method |
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