CN116528576A - Magnetic carbon-based composite material, preparation method thereof and application thereof in electromagnetic wave absorption - Google Patents
Magnetic carbon-based composite material, preparation method thereof and application thereof in electromagnetic wave absorption Download PDFInfo
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- CN116528576A CN116528576A CN202310191870.0A CN202310191870A CN116528576A CN 116528576 A CN116528576 A CN 116528576A CN 202310191870 A CN202310191870 A CN 202310191870A CN 116528576 A CN116528576 A CN 116528576A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000010521 absorption reaction Methods 0.000 title abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 27
- 239000002243 precursor Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 33
- 239000012153 distilled water Substances 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 22
- 230000008569 process Effects 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000004140 cleaning Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 11
- 239000004202 carbamide Substances 0.000 claims description 11
- UCFIGPFUCRUDII-UHFFFAOYSA-N [Co](C#N)C#N.[K] Chemical compound [Co](C#N)C#N.[K] UCFIGPFUCRUDII-UHFFFAOYSA-N 0.000 claims description 9
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000001509 sodium citrate Substances 0.000 claims description 8
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 8
- 229940038773 trisodium citrate Drugs 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 7
- 229910001092 metal group alloy Inorganic materials 0.000 claims description 4
- 229910003321 CoFe Inorganic materials 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 150000002739 metals Chemical class 0.000 claims 1
- 239000011358 absorbing material Substances 0.000 description 10
- 229910017052 cobalt Inorganic materials 0.000 description 10
- 239000010941 cobalt Substances 0.000 description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 10
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 description 10
- 229960003351 prussian blue Drugs 0.000 description 10
- 239000013225 prussian blue Substances 0.000 description 10
- 239000012188 paraffin wax Substances 0.000 description 9
- 239000000945 filler Substances 0.000 description 8
- 230000005670 electromagnetic radiation Effects 0.000 description 5
- 238000011068 loading method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
Abstract
The invention discloses a magnetic carbon-based composite material, a preparation method thereof and application thereof in electromagnetic wave absorption, and belongs to the field of stealth materials. The composite material has the advantages of simple preparation process, high yield, high repeatability, low density, high magnetic component content and the like, and is pressed into rings to test the electromagnetic wave absorption performance. Because extra magnetic components are introduced into the precursor and etched, the composite material forms a hollow structure, the magnetic loss is enhanced, and the impedance matching is optimized, so that the attenuation capacity is improved, and the excellent electromagnetic wave absorption performance is obtained.
Description
Technical Field
The invention belongs to the technical field of stealth materials, and particularly relates to a magnetic carbon-based composite material, a preparation method thereof and application thereof in electromagnetic wave absorption.
Background
With the advent of the information age, advanced reconnaissance and precision striking technologies pose immeasurable threats to large weapons and detection equipment on modern battlefields. The application of stealth technology will play a critical role in order to achieve detection as well as anti-scout. The radar stealth technology mainly adopts the methods of radar wave-absorbing material design, appearance structure design, impedance loading design and the like, and is the most common and effective anti-detection technology at present. Compared with other two design methods, the radar wave absorbing material can be directly coated on the surface of a structure in any form and has stronger capability of reducing RCS, so that the radar wave absorbing material has been widely applied to the military field. Meanwhile, in life, the coming of the 5G age makes a large number of antenna devices generate electromagnetic radiation in the process of receiving and transmitting electromagnetic waves, and along with the increase of power, the electromagnetic radiation is also greatly enhanced. These electronic devices are also forcing people's living environment to be filled with a large number of electromagnetic radiation sources while bringing convenience to people's life. And a large amount of electromagnetic radiation can not only cause the aging and failure of precision instruments, but also cause harm to the social living environment and the life health safety of people. Therefore, how to reduce electromagnetic radiation and build a safe living environment has become a major research topic. Among them, designing and applying electromagnetic wave absorbing materials is one of the most dominant prevention and treatment means at present. Therefore, electromagnetic wave absorbing materials have raised research enthusiasts for researchers based on various aspects such as military and life. Meanwhile, compared with the traditional wave-absorbing material, the novel wave-absorbing material with the characteristics of strong absorption, wide bandwidth, thin thickness and low density is urgently required to be designed.
Up to now, researchers have studied various electromagnetic wave absorbing materials including carbon materials, magnetic materials, composite materials, and the like. Compared with a single-component wave absorber, the composite material with multiple components is easier to obtain good wave absorbing performance. The magnetic carbon-based composite material derived from the metal organic framework has dielectric loss and magnetic loss, and has adjustable morphology and components, thereby attracting the attention of researchers. However, the problems of single component, unstable structure, small content of magnetic component, etc. remain the main reasons for limiting the application thereof. In order to solve the above problems, from the viewpoint of improving the magnetic loss of the material, a wave-absorbing material having characteristics of high performance, light weight, etc. is prepared by introducing additional magnetic components and constructing a hollow or porous structure. The additional magnetic component is introduced, so that more interfaces can be introduced to improve the interface polarization loss, alloy can be formed, and the magnetic loss is improved; the hollow structure can prevent the phenomenon that the density of the material is greatly increased due to the introduction of more metal elements, and is beneficial to optimizing impedance matching and improving the performance of the material. Therefore, based on cobalt-based Prussian blue material, the cobalt-based Prussian blue material is subjected to ion exchange and etching, and extra magnetic elements are introduced, so that the magnetic loss capacity of the cobalt-based Prussian blue material is enhanced after high-temperature pyrolysis, and the magnetic carbon-based composite material with good dielectric loss, magnetic loss and impedance matching characteristics is prepared.
Disclosure of Invention
The invention provides a magnetic carbon-based composite material, a preparation method thereof and application thereof in electromagnetic wave absorption, the prepared magnetic/carbon composite material has the advantages of simple preparation method, high yield and repetition rate, higher magnetic component content, metal alloy formation, material magnetic loss enhancement and interface polarization loss optimization; meanwhile, due to the hollow structure, the density of the material can be reduced, the reflection and scattering of electromagnetic waves are promoted, the attenuation process is prolonged, and excellent electromagnetic wave absorption performance is facilitated to be obtained.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a magnetic carbon-based composite material, wherein the material is of a hollow cube structure, metal components (Co/CoFe) are wrapped in carbon in the material, and the dimension of the hollow cube is 0.5-1 mu m; the metal, the metal alloy and the carbon component interact to form an interface, so that the interface polarization loss is enhanced; the introduction of additional magnetic components improves the magnetic loss capacity of the material and reduces the conductive loss, thereby promoting the attenuation of electromagnetic waves and optimizing the impedance matching characteristic.
The preparation method of the magnetic carbon-based composite material comprises the following steps:
1) 580mg of CoCl 2 ·6H 2 O was dissolved in distilled water, and 1.06g of lemon was addedTrisodium citrate;
2) 532mg of potassium cobalt cyanide was dissolved in distilled water;
3) Slowly adding the solution in the step 2) into the solution in the step 1) in the stirring process, uniformly stirring, standing for 24 hours, centrifugally cleaning, drying and collecting;
4) Putting the precursor in the step 3) with a certain mass into a 100mL sealed bottle, adding 100mL distilled water, and performing ultrasonic dispersion;
5) Sequentially adding FeCl with a certain molar mass into the solution in the step 4) in the continuous stirring process 2 ·4H 2 O and urea with a certain mass, and continuously stirring after sealing;
6) Setting the temperature of the water bath kettle and heating to 80 ℃;
7) Placing the sealed bottle in the step 5) in the water bath pot in the step 6), and continuously stirring for a certain time at a certain rotating speed;
8) Standing the solution reacted in the step 7) for 6 hours at room temperature, centrifugally cleaning, drying and collecting;
9) And (3) carrying out heat treatment at 600 ℃ on the powder in the step (8) in a nitrogen atmosphere, wherein the heating rate is 2 ℃/min, and the time is 2h, so as to obtain the hollow magnetic/carbon composite material.
In the step, the mass of the precursor in the step 4) is 50-200 mg;
0 as described in step 5)<FeCl 2 ·4H 2 The mass of the O substance is less than or equal to 4mmol, and the mass range of the urea is 0-2.4 g;
the rotating speed range of the water bath pot in the step 7) is 100-300 r/min, and the stirring time range is 3-24 h;
the magnetic carbon-based composite material and paraffin are mixed and pressed into a ring with the internal-external diameter ratio of 3.0/7.0, the filler ratio of the material and the paraffin is regulated to be 15-40 wt%, and electromagnetic wave absorption performance is tested and calculated.
The beneficial effects are that: the invention provides a magnetic carbon-based composite material and a preparation method thereof and application thereof in electromagnetic wave absorption, the magnetic carbon-based composite material is prepared by coprecipitation, etching, ion exchange and one-step heat treatment, the invention researches the influence of different shapes, magnetism and carbon component content on the electromagnetic performance of the material after heat treatment by adjusting the content of reactants and reaction conditions added in the etching and ion exchange processes, and discovers that the composite material with balanced dielectric loss and magnetic loss shows more excellent absorption performance, mainly because metal oxide is generated on the surface of a precursor after ion exchange and additional magnetic components are introduced, the carbon component is used for reducing metal ions and metal oxide into metal simple substances after carbonization, thereby not only improving the magnetic loss energy consumption of the material, but also greatly reducing the conductive loss of the material, improving the interface polarization loss and optimizing the impedance matching, thereby improving the electromagnetic performance of the material; in addition, the hollow structure promotes multiple scattering and diffraction of electromagnetic waves, prolongs the reaction path, reduces the density, and provides a new idea and direction for obtaining a light and efficient electromagnetic wave absorbing material.
Drawings
FIG. 1 is a scanning electron microscope image of a magnetic carbon-based composite material prepared in example 1 of the present invention
FIG. 2 is a transmission electron micrograph of a magnetic carbon-based composite material prepared according to example 1 of the present invention
FIG. 3 is a graph showing the reflection loss of the magnetic carbon-based composite material prepared in example 1 of the present invention at a loading of 25%
FIG. 4 is an XRD pattern of a magnetic carbon-based composite material prepared in example 2 of the present invention
FIG. 5 is a graph showing the reflection loss of the magnetic carbon-based composite material prepared in example 2 of the present invention at a loading of 25%
FIG. 6 is a scanning electron microscope image of a magnetic carbon-based composite material prepared in example 3 of the present invention
FIG. 7 is a graph showing the reflection loss of the magnetic carbon-based composite material prepared in example 3 of the present invention at a loading of 25%
Detailed Description
The invention is further described with reference to the drawings and the specific embodiments below:
example 1
The preparation method of the magnetic carbon-based composite material comprises the following steps:
580mg of CoCl 2 ·6H 2 O and 1.06g of trisodium citrate were dissolved in 80mL of distilled water to form a clear solution A; 532mg of potassium cobalt cyanide was dissolved in 80mL of distilled water to form a clear solution B; slowly adding the solution B into the solution A in the continuous stirring process, uniformly stirring, standing for 24 hours, centrifugally cleaning, drying and collecting to obtain a cobalt-based Prussian blue precursor; taking 100mg of precursor in a 100mL sealed bottle, adding 100mL of distilled water, and performing ultrasonic dispersion; in the continuous stirring process of the solution, 2mmol FeCl is added in sequence 2 ·4H 2 O and 0.3g of urea are stirred and dispersed uniformly and then are placed in a water bath kettle which is heated to 80 ℃, stirred for 6 hours at the rotating speed of 100r/min, then kept stand for 6 hours at room temperature, centrifugally cleaned, dried and collected; then carrying out heat treatment on the powder at 600 ℃ for 2 hours at 2 ℃/min under the nitrogen atmosphere to obtain a magnetic/carbon composite material; it was then mixed with paraffin wax at a 25% filler ratio and tested for electromagnetic parameters.
As can be seen from FIG. 1, the magnetic carbon-based composite material prepared in example 1 has a cubic structure as a whole and a size of about 0.5 to 1 μm, and it can be confirmed that the interior of the material has a hollow structure by combining FIG. 2. The reflection loss diagram of the material at the filling amount of 25% is shown as 3, and the reflection loss of the material at 1.75mm is minus 20.11dB, and meanwhile, the effective absorption bandwidth can reach 6GHz, and the frequency range is 12-18 GHz.
Example 2
The preparation method of the magnetic carbon-based composite material comprises the following steps:
580mg of CoCl 2 ·6H 2 O and 1.06g of trisodium citrate were dissolved in 80mL of distilled water to form a clear solution A; 532mg of potassium cobalt cyanide was dissolved in 80mL of distilled water to form a clear solution B; slowly adding the solution B into the solution A in the continuous stirring process, uniformly stirring, standing for 24 hours, centrifugally cleaning, drying and collecting to obtain a cobalt-based Prussian blue precursor; 200mg of precursor is taken in a 100mL sealed bottle, 100mL of distilled water is added, and ultrasonic dispersion is carried out; in the continuous stirring process of the solution, 2mmol FeCl is added in sequence 2 ·4H 2 O and 0.6g of urea are stirred and dispersed uniformly and then are placed at the temperature of 80 DEG CStirring in a water bath kettle at 200r/min for 12h, standing at room temperature for 6h, centrifugally cleaning, drying and collecting; then carrying out heat treatment on the powder at 600 ℃ for 2 hours at 2 ℃/min under the nitrogen atmosphere to obtain a magnetic carbon-based composite material; it was then mixed with paraffin wax at a 25% filler ratio and tested for electromagnetic parameters.
The magnetic carbon-based composite material has various magnetic components; fig. 4 is an XRD pattern of the prepared magnetic carbon-based composite material, and diffraction peaks of Co and CoFe alloys after calcination can be observed, demonstrating successful introduction of Fe additional magnetic components and formation of metal alloys. The reflection loss graph at 25% of the material loading is shown in fig. 5, and it can be seen that the minimum reflection loss of the material at 2mm is-55.11 dB, and at 1.95mm thickness, the effective absorption bandwidth is 5.98GHz, and the specific frequency range is 11.72-17.70 GHz.
Example 3
The preparation method of the magnetic carbon-based composite material comprises the following steps:
580mg of CoCl 2 ·6H 2 O and 1.06g of trisodium citrate were dissolved in 80mL of distilled water to form a clear solution A; 532mg of potassium cobalt cyanide was dissolved in 80mL of distilled water to form a clear solution B; slowly adding the solution B into the solution A in the continuous stirring process, uniformly stirring, standing for 24 hours, centrifugally cleaning, drying and collecting to obtain a cobalt-based Prussian blue precursor; 150mg of precursor is taken in a 100mL sealed bottle, 100mL of distilled water is added, and ultrasonic dispersion is carried out; in the continuous stirring process of the solution, 3mmol FeCl is added in sequence 2 ·4H 2 O and 1.2g of urea are stirred and dispersed uniformly and then are placed in a water bath kettle which is heated to 80 ℃, stirred for 18 hours at the rotating speed of 200r/min, then kept stand for 6 hours at room temperature, centrifugally cleaned, dried and collected; then carrying out heat treatment on the powder at 600 ℃ for 2 hours at 2 ℃/min under the nitrogen atmosphere to obtain a magnetic/carbon composite material; it was then mixed with paraffin wax at a 25% filler ratio and tested for electromagnetic parameters.
As can be seen from fig. 6, the magnetic/carbon composite material prepared in example 3 has a cubic structure as a whole, but the overall structure is collapsed to some extent due to the enhanced etching degree in the precursor. The reflection loss graph of the material at 25% of the filling amount is shown as 7, and it can be seen that the reflection loss of the material can reach-22.92 dB at 1.9mm, and the effective absorption bandwidth is 5.6GHz.
Example 4
The preparation method of the magnetic carbon-based composite material comprises the following steps:
580mg of CoCl 2 ·6H 2 O and 1.06g of trisodium citrate were dissolved in 80mL of distilled water to form a clear solution A; 532mg of potassium cobalt cyanide was dissolved in 80mL of distilled water to form a clear solution B; slowly adding the solution B into the solution A in the continuous stirring process, uniformly stirring, standing for 24 hours, centrifugally cleaning, drying and collecting to obtain a cobalt-based Prussian blue precursor; 200mg of precursor is taken in a 100mL sealed bottle, 100mL of distilled water is added, and ultrasonic dispersion is carried out; in the continuous stirring process of the solution, 4mmol FeCl is added in sequence 2 ·4H 2 O and 2.4g of urea are stirred and dispersed uniformly and then are placed in a water bath kettle which is heated to 80 ℃, stirred for 12 hours at the rotating speed of 300r/min, then kept stand for 6 hours at room temperature, centrifugally cleaned, dried and collected; then carrying out heat treatment on the powder at 600 ℃ for 2 hours at 2 ℃/min under the nitrogen atmosphere to obtain a magnetic/carbon composite material; it was then mixed with paraffin wax at a 25% filler ratio and tested for electromagnetic parameters.
Example 5
The preparation method of the magnetic carbon-based composite material comprises the following steps:
580mg of CoCl 2 ·6H 2 O and 1.06g of trisodium citrate were dissolved in 80mL of distilled water to form a clear solution A; 532mg of potassium cobalt cyanide was dissolved in 80mL of distilled water to form a clear solution B; slowly adding the solution B into the solution A in the continuous stirring process, uniformly stirring, standing for 24 hours, centrifugally cleaning, drying and collecting to obtain a cobalt-based Prussian blue precursor; 200mg of precursor is taken in a 100mL sealed bottle, 100mL of distilled water is added, and ultrasonic dispersion is carried out; in the continuous stirring process of the solution, 0mmol FeCl is added in sequence 2 ·4H 2 O and 0g of urea are stirred and dispersed uniformly and then are placed in a water bath kettle which is heated to 80 ℃, stirred for 12 hours at the rotating speed of 200r/min, then are kept stand for 6 hours at room temperature, centrifugally cleaned and driedDrying and collecting; then carrying out heat treatment on the powder at 600 ℃ for 2 hours at 2 ℃/min under the nitrogen atmosphere to obtain a magnetic/carbon composite material; it was then mixed with paraffin wax at a 25% filler ratio and tested for electromagnetic parameters.
Example 6
The preparation method of the magnetic carbon-based composite material comprises the following steps:
580mg of CoCl 2 ·6H 2 O and 1.06g of trisodium citrate were dissolved in 80mL of distilled water to form a clear solution A; 532mg of potassium cobalt cyanide was dissolved in 80mL of distilled water to form a clear solution B; slowly adding the solution B into the solution A in the continuous stirring process, uniformly stirring, standing for 24 hours, centrifugally cleaning, drying and collecting to obtain a cobalt-based Prussian blue precursor; taking 100mg of precursor in a 100mL sealed bottle, adding 100mL of distilled water, and performing ultrasonic dispersion; in the continuous stirring process of the solution, 4mmol FeCl is added in sequence 2 ·4H 2 O and 2.4g of urea are stirred and dispersed uniformly and then are placed in a water bath kettle which is heated to 80 ℃, stirred for 24 hours at the rotating speed of 300r/min, then are kept stand for 6 hours at room temperature, centrifugally cleaned, dried and collected; then carrying out heat treatment on the powder at 600 ℃ for 2 hours at 2 ℃/min under the nitrogen atmosphere to obtain a magnetic/carbon composite material; it was then mixed with paraffin wax at a 25% filler ratio and tested for electromagnetic parameters.
Example 7
580mg of CoCl 2 ·6H 2 O and 1.06g of trisodium citrate were dissolved in 80mL of distilled water to form a clear solution A; 532mg of potassium cobalt cyanide was dissolved in 80mL of distilled water to form a clear solution B; slowly adding the solution B into the solution A in the continuous stirring process, uniformly stirring, standing for 24 hours, centrifugally cleaning, drying and collecting to obtain a cobalt-based Prussian blue precursor; taking 50mg of precursor in a 100mL sealed bottle, adding 100mL of distilled water, and performing ultrasonic dispersion; in the continuous stirring process of the solution, 0mmol FeCl is added in sequence 2 ·4H 2 O and 2.4g of urea are stirred and dispersed uniformly and then are placed in a water bath kettle which is heated to 80 ℃, stirred for 24 hours at the rotating speed of 100r/min, then are kept stand for 6 hours at room temperature, centrifugally cleaned, dried and collected; the powder is then treated in nitrogen atmosphere at 2 DEG CCarrying out heat treatment at 600 ℃ for 2 hours per min to obtain the magnetic carbon-based composite material; it was then mixed with paraffin wax at a 25% filler ratio and tested for electromagnetic parameters.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Those skilled in the art can make improvements and modifications to these embodiments and realize them in other embodiments without changing the technical principle of the present invention, and these improvements and modifications are also within the scope of the present invention. All other forms of substitution or modification made according to the technical principles of the present invention are also within the scope of the present invention.
Claims (7)
1. The magnetic carbon-based composite material is characterized in that the material is of a hollow cube structure, and carbon in the material wraps metal components; the simple metals, metal alloys and carbon components interact to form an interface.
2. The magnetic carbon-based composite material according to claim 1, wherein the hollow cube size is 0.5-1 μm.
3. The magnetic carbon-based composite material according to claim 1 or 2, wherein the metal components are Co elemental metal and CoFe alloy.
4. The preparation method of the magnetic carbon-based composite material is characterized by comprising the following steps of:
1) 580mg of CoCl 2 ·6H 2 O was dissolved in distilled water, and 1.06g of trisodium citrate was added;
2) 532mg of potassium cobalt cyanide was dissolved in distilled water;
3) Slowly adding the solution in the step 2) into the solution in the step 1) in the stirring process, uniformly stirring, standing for 24 hours, centrifugally cleaning, drying and collecting;
4) Putting the precursor in the step 3) with a certain mass into a 100mL sealed bottle, adding 100mL distilled water, and performing ultrasonic dispersion;
5) Sequentially adding FeCl with a certain molar mass into the solution in the step 4) in the continuous stirring process 2 ·4H 2 O and urea with a certain mass, and continuously stirring after sealing;
6) Setting the temperature of the water bath kettle and heating to 80 ℃;
7) Placing the sealed bottle in the step 5) in the water bath pot in the step 6), and continuously stirring for a certain time at a certain rotating speed;
8) Standing the solution reacted in the step 7) for 6 hours at room temperature, centrifugally cleaning, drying and collecting;
9) And (3) carrying out heat treatment at 600 ℃ on the powder in the step (8) in a nitrogen atmosphere, wherein the heating rate is 2 ℃/min, and the time is 2h, so as to obtain the hollow magnetic carbon-based composite material.
5. The method for producing a magnetic carbon-based composite material according to claim 4, wherein the mass of the precursor in step 4) is 50 to 200mg.
6. The method for producing a magnetic carbon-based composite material according to claim 4, wherein the 0 in step 5)<FeCl 2 ·4H 2 The mass of the O substance is less than or equal to 4mmol, and the mass range of the urea is 0-2.4 g.
7. The method for producing a magnetic carbon-based composite material according to claim 4, wherein the rotation speed of the water bath in step 7) is in the range of 100 to 300r/min and the stirring time is in the range of 3 to 24 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310191870.0A CN116528576A (en) | 2023-03-02 | 2023-03-02 | Magnetic carbon-based composite material, preparation method thereof and application thereof in electromagnetic wave absorption |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310191870.0A CN116528576A (en) | 2023-03-02 | 2023-03-02 | Magnetic carbon-based composite material, preparation method thereof and application thereof in electromagnetic wave absorption |
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| CN116528576A true CN116528576A (en) | 2023-08-01 |
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| CN202310191870.0A Pending CN116528576A (en) | 2023-03-02 | 2023-03-02 | Magnetic carbon-based composite material, preparation method thereof and application thereof in electromagnetic wave absorption |
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| Country | Link |
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