CN112391143A - Synthesis and application of broadband efficient carbon-based metal cobalt wave-absorbing material - Google Patents
Synthesis and application of broadband efficient carbon-based metal cobalt wave-absorbing material Download PDFInfo
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- CN112391143A CN112391143A CN202011441894.XA CN202011441894A CN112391143A CN 112391143 A CN112391143 A CN 112391143A CN 202011441894 A CN202011441894 A CN 202011441894A CN 112391143 A CN112391143 A CN 112391143A
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Abstract
The invention discloses a preparation method and application of a broadband high-efficiency carbon-based metal cobalt wave-absorbing material, and belongs to the technical field of material preparation and microwave absorbing materials. The carbon-based metal cobalt is an organic metal complex which is synthesized by taking 2-methylimidazole, different cobalt salts and zinc salts as precursors under simple stirring at room temperature, and then the complex of the magnetic material and the carbon material is obtained through high-temperature pyrolysis. Compared with the traditional metal magnetic material, the carbon-based metal cobalt material prepared by the invention has good dispersity and small density, can exert the advantages of the magnetic material and the carbon material, and greatly improves the wave-absorbing performance of the material. Wherein, when the thickness is 2.7mm, the effective bandwidth reaches 6.96 GHz. The synthesis method is simple, the reaction condition is mild, the product is easy to separate, large-scale production can be realized, the actual production requirement is met, and the method has great application potential in the technical field of microwave absorption materials.
Description
Technical Field
The invention belongs to the technical field of microwave absorbing materials, and particularly relates to synthesis and related application of a broadband high-efficiency carbon-based metal cobalt wave-absorbing material.
Background
With the increasing progress of technology, electronic technology is also rapidly developed, but the electronic devices are used more and more commonly, which brings about a serious electromagnetic radiation pollution problem (listed as a fourth environmental pollution source by WHO). The harm of the pollution is mainly embodied in two aspects, namely, the harm is caused to the reproduction, the immunity and the nervous system of the human body, and the health of the human body is threatened; secondly, the normal operation of communication signals, precision instruments, electronic equipment and the like is seriously interfered, and the leakage of the electromagnetic signals is caused. Based on this, there is a need in real life for a material capable of effectively shielding and absorbing electromagnetic waves. In the military field, the materials are widely applied to stealth technology, and with the development of military technology, higher requirements are provided for the anti-detection capability and defense capability of weaponry. The wave-absorbing material can absorb electromagnetic waves incident to the surface of the equipment and reduce the energy of the reflected electromagnetic waves, so that the detectability of a target is reduced and the purpose of stealth is achieved. Therefore, the wave-absorbing material has wide application prospect in both military field and civil field.
The development requirement of the current wave-absorbing material meets the characteristics of thinness, lightness, width and strength, namely, the characteristics of thinness, lightness, wide effective absorption frequency band and strong absorption strength. At present, ferrite and magnetic metal are both widely researched and developed mature magnetic wave-absorbing materials, but have the following defects, such as: poor dispersion, high density, susceptibility to oxidation, susceptibility to corrosion, etc. limit further applications. To overcome these problems, the electromagnetic parameters can be controlled by compounding magnetic particles with a low density dielectric material. Carbon material is regarded as a good dielectric material due to its advantages of high conductivity, light weight, abundant content, low cost, etc. More and more researches are focused on the preparation of the composite wave-absorbing material of the magnetic particles and the carbon material, the composite wave-absorbing material can play the synergistic effect of the magnetic material and the carbon material, the magnetic loss and the dielectric loss are effectively combined, the wave-absorbing performance of the material is greatly improved, and the integral density of the material is reduced.
Disclosure of Invention
The invention aims to provide synthesis and application of a broadband high-efficiency carbon-based metal cobalt wave-absorbing material. The material has an obvious macroporous structure and good wave-absorbing performance, and the effective bandwidth can reach 6.96GHz when the thickness is 2.7 mm. The wave-absorbing performance of the material can be regulated and controlled by regulating the content of the precursor metal. The material has simple preparation process, good repeatability and low cost, and is beneficial to large-scale production.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention synthesizes the carbon material loaded with metallic cobalt. The material is synthesized by the following steps:
1) and (3) taking a clean beaker with the volume of 250mL, weighing 48mmol of 2-methylimidazole, dissolving in a mixed solution (the total volume is 80mL) of methanol and ethanol with the volume ratio of 0: 2-2: 0, and fully dissolving to obtain a solution A.
2) And taking another clean beaker with the volume of 250mL, weighing 0 mmol-12 mmol of zinc nitrate and 0 mmol-12 mmol of cobalt nitrate, simultaneously putting the zinc nitrate and the cobalt nitrate into the beaker, dissolving the beaker in a mixed solution (the total volume is 80mL) of methanol and ethanol with the volume ratio of 0: 2-2: 0, and fully stirring to form a transparent solution B.
3) And slowly dripping the solution B into the solution A, continuously stirring for 6-36 h, centrifuging, washing with ethanol for 3 times, drying at the temperature of 60-100 ℃ in vacuum for 12-24 h, and grinding to obtain powder.
4) Taking 100-300 mg of the powder obtained in the step 3), carrying out heat treatment for 1-3 h at 500-1000 ℃, and controlling the temperature rise speed to be 1-5 ℃/min, N2And (5) protecting the atmosphere (the flow rate is 30-50 sccm), and naturally cooling to room temperature to obtain a black sample.
The prepared material is applied to the wave-absorbing performance test, and the experimental conditions are as follows:
mixing powder to be measured with paraffin according to a certain mass ratio, melting the paraffin and the powder mixture to be measured on a constant-temperature heating magnetic stirrer, cooling, then pouring into a coaxial ring mold, compacting by external force, wherein the inner diameter of a coaxial ring sample is 3.04mm, the outer diameter of the coaxial ring sample is 7.00mm, and the thickness of the coaxial ring sample is 2-3 mm, and then placing the annular sample into a coaxial clamp for measurement. The Agilent N5230A vector network analyzer is a testing instrument, the testing frequency range is 2-18 GHz, and the testing temperature is room temperature.
The invention has the following effects and advantages:
1) the invention adopts a simple synthesis method to obtain the pyrolysis precursor, has simple operation and high purity of the target product, and can realize mass synthesis.
2) According to the invention, the black magnetic sample obtained by annealing the precursor at different temperatures is applied to the wave-absorbing performance test, and the experimental result shows that the effective bandwidth of the material is 6.96GHz when the test thickness is 2.7 mm.
3) Experiments prove that the wave absorbing performance of the material can be effectively regulated and controlled by controlling the content of the Co source in the precursor.
4) The synthesis method is simple, and the obtained material is easy to apply and is beneficial to popularization in industrial application.
Drawings
FIG. 1 shows XRD spectra of materials prepared in examples 1 and 2 of the present invention
Fig. 2 shows Raman spectra of materials prepared in examples 1 and 2 of the present invention.
FIG. 3 shows the real part of the dielectric constant (ε') of the electromagnetic parameter (a) of the wave-absorbing material prepared in examples 1 and 2 of the present invention; (b) imaginary part of dielectric constant (. epsilon. "); (c) real part of magnetic permeability (μ'); (d) graph of imaginary permeability (. mu.').
FIG. 4 is a wave-absorbing reflection loss chart of the wave-absorbing material prepared in embodiments 1 and 2 of the present invention, wherein the thickness of the wave-absorbing material is 2.7 mm.
Detailed Description
In order to make the aforementioned features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below, but the present invention is not limited thereto. In addition, it will be apparent to those skilled in the art that modifications or improvements may be made in the components and amounts of the materials used in the embodiments without departing from the spirit and scope of the invention as defined in the appended claims.
Example 1
Preparing the broadband high-efficiency carbon-based metal cobalt: dissolving 48mmol of 2-methylimidazole in 80mL of mixed solution of methanol and ethanol, wherein the volume ratio of the methanol to the ethanol is 1:1 to form solution A; and dissolving 11.4mmol of zinc nitrate and 0.6mmol of cobalt nitrate in 80mL of mixed solution of methanol and ethanol, wherein the volume ratio of the methanol to the ethanol is 1:1, and stirring to form a transparent uniform solution B. And slowly dripping the solution B into the solution A, continuously stirring at room temperature for 24h, centrifuging, washing with ethanol for 3 times, drying at 60 ℃ in vacuum for 12h, taking out and grinding to obtain powder. Then carrying out heat treatment on the obtained powder for 2h at 910 ℃, controlling the temperature rise speed to be 5 ℃/min, and controlling N2And (3) protecting the atmosphere (with the flow rate of 50sccm), naturally cooling to room temperature, and finally obtaining the carbon-based metal cobalt material, wherein the content of the metal cobalt is low, so that XRD and Raman have no obvious characteristic signal peak of cobalt, but the existence of carbon can be verified.
Example 2
Preparing the broadband high-efficiency carbon-based metal cobalt: dissolving 48mmol of 2-methylimidazole in 80mL of mixed solution of methanol and ethanol, wherein the volume ratio of the methanol to the ethanol is 1:1 to form solution A; and dissolving 9mmol of zinc nitrate and 3mmol of cobalt nitrate in 80mL of mixed solution of methanol and ethanol, wherein the volume ratio of the methanol to the ethanol is 1:1, and stirring to form a transparent and uniform solution B. And slowly dripping the solution B into the solution A, continuously stirring at room temperature for 24h, centrifuging, washing with ethanol for 3 times, drying at 60 ℃ in vacuum for 12h, taking out and grinding to obtain powder. Then carrying out heat treatment on the obtained powder for 2h at 910 ℃, controlling the temperature rise speed to be 5 ℃/min, and controlling N2And (4) protecting the atmosphere (with the flow rate of 50sccm), naturally cooling to room temperature to obtain the carbon-based metal cobalt material, and verifying the existence of cobalt and graphitized carbon by XRD and Raman.
The material obtained by the invention is applied to wave-absorbing tests.
The above-described reactions are preferred embodiments of the present invention, and all equivalent changes and modifications within the scope of the claims should be considered as included in the present invention.
Claims (3)
1. A broadband high-efficiency carbon-based metal cobalt wave-absorbing material is characterized in that: the carbon-based metal cobalt has good wave-absorbing performance, and the effective bandwidth is 6.96GHz when the thickness is 2.7 mm.
2. A method for preparing the broadband high-efficiency carbon-based metal cobalt wave-absorbing material as claimed in claim 1, is characterized in that:
1) weighing 48mmol of 2-methylimidazole, dissolving in a mixed solution (the total volume is 80mL) of methanol and ethanol in a volume ratio of 0: 2-2: 0, and fully dissolving to obtain a solution A.
2) Weighing 0 mmol-12 mmol of zinc nitrate and 0 mmol-12 mmol of cobalt nitrate, dissolving in a mixed solution (the total volume is 80mL) of methanol and ethanol with the volume ratio of 0: 2-2: 0, and fully stirring to form a transparent solution B.
3) And slowly dripping the solution B into the solution A, continuously stirring for 6-36 h, centrifuging, washing with ethanol for 3 times, drying at the temperature of 60-100 ℃ in vacuum for 12-24 h, and grinding to obtain powder.
4) Taking 100-300 mg of the powder, carrying out heat treatment for 1-3 h at 500-1000 ℃, controlling the temperature rise speed to be 1-5 ℃/min, and controlling N2And (5) protecting the atmosphere (the flow rate is 30-50 sccm), and naturally cooling to room temperature to obtain a black sample.
3. The application of the broadband high-efficiency carbon-based metal cobalt wave-absorbing material as claimed in claim 1, wherein: the carbon-based metal cobalt is applied to microwave absorption.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114914710A (en) * | 2022-05-18 | 2022-08-16 | 山东大学 | Electromagnetic wave absorbing material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114914710A (en) * | 2022-05-18 | 2022-08-16 | 山东大学 | Electromagnetic wave absorbing material and preparation method and application thereof |
| CN114914710B (en) * | 2022-05-18 | 2023-06-27 | 山东大学 | Electromagnetic wave absorbing material and preparation method and application thereof |
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