CN113597252B - Preparation method of carbon/magneto-electromagnetic wave absorbing material with sandwich structure - Google Patents
Preparation method of carbon/magneto-electromagnetic wave absorbing material with sandwich structure Download PDFInfo
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- CN113597252B CN113597252B CN202111038277.XA CN202111038277A CN113597252B CN 113597252 B CN113597252 B CN 113597252B CN 202111038277 A CN202111038277 A CN 202111038277A CN 113597252 B CN113597252 B CN 113597252B
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Abstract
The invention discloses a carbon/magnetic electromagnetic wave absorbing material with a sandwich structure and a preparation method thereof, wherein ferric salt is used for preparing flaky ferroferric oxide; 5-10g of flaky material obtained by coating polydopamine with flaky ferroferric oxide, then placing the flaky material coated with polydopamine into a nitrogen atmosphere at 450-600 ℃ for carbonization treatment for 1 hour to obtain a material, adding the material into 100ml of distilled water, then adding 5g of ferric chloride and ferrous chloride blend with the molar ratio of 2:1, stirring and dissolving, gradually dripping 8ml of ammonia water, reacting in a water bath at 50 ℃ for 1 hour, and cleaning. The sandwich-structure carbon/magneto-electromagnetic wave absorbing material has the structure that ferroferric oxide is used as an inner layer, a middle layer is used as a carbon layer, and an outermost layer is nano ferroferric oxide particles, so that the electromagnetic wave absorbing performance of the material can be obviously improved, the material has dielectric loss and magnetic loss performance, and the material is light in weight and has a very wide application prospect.
Description
Technical Field
The invention belongs to the technical field of electromagnetic materials, and particularly relates to a carbon/magneto-electromagnetic wave absorbing material with a sandwich structure and a preparation method thereof.
Background
With the rapid development of electronic and electric technologies, the electromagnetic energy utilization range is continuously expanded, and electromagnetic radiation pollution is caused. The problem of electromagnetic pollution has become the 5 th major nuisance following wastewater, exhaust gas, solid waste and noise, and reports on this century suggest that electromagnetic pollution will replace noise pollution to become one of the major 5 major physical pollution. Currently, the use of electromagnetic wave absorbing materials to attenuate or eliminate electromagnetic wave pollution is an effective approach.
Ferrite or carbon materials are currently widely used in the market as electromagnetic wave absorbing materials. The ferroferric oxide, carbonyl iron and magnetic electromagnetic wave absorbing materials are heavy in weight, and the prepared materials are thick and heavy, so that the application range of the materials is limited. On the other hand, the carbon-based electromagnetic wave absorbing material has the advantages of light weight, adjustable frequency range and good compatibility with the organic/inorganic phase interface of the matrix. The graphite powder, carbon black, carbon nano tube, chopped carbon fiber and activated carbon fiber are all reported as carbon-based electromagnetic wave protection functional fillers. However, the main factor that determines the wave absorbing characteristics of the carbon material is resistance, but the conductivity is high, and electromagnetic waves are easily reflected, which affects the absorption efficiency. For this reason, many researchers have improved electromagnetic wave absorption performance of materials by loading magnetic particles on carbon materials, including graphite powder nickel plating, carbon nanotube nickel plating, and nano ferrite particles, and have improved electromagnetic wave absorption materials by coating a dielectric loss material, a magnetic loss material, and the like. Patent CN109936974B, CN110028931a proposes a method for preparing an electromagnetic wave absorbing material with a sandwich structure, but the preparation process has certain defects, not an obvious multilayer structure, but a hybrid material, and the control of the layer number cannot be freely performed, so that the electromagnetic wave absorbing performance cannot be regulated and controlled automatically.
Disclosure of Invention
In order to solve the problems of heavy product quality, difficult molding, single electromagnetic wave loss mechanism and the like of the electromagnetic wave absorbing material in the prior art, the invention prepares the carbon/electromagnetic wave absorbing material with a sandwich structure, and micron sheet-shaped particles with a carbon layer, a magnetic layer and other multilayer structures are formed in an in-situ hybridization mode, so that the carbon/electromagnetic wave absorbing material can effectively absorb electromagnetic waves and has a very wide application prospect.
In order to achieve the above purpose, the present invention provides the technical scheme: the sandwich-structure carbon/magneto-electromagnetic wave absorbing material comprises an inner layer of ferroferric oxide, a middle layer of carbon layer and an outermost layer of nano ferroferric oxide particles.
Preferably, the inner layer is ferroferric oxide, the middle layer is a carbon layer, the outer layer is nano ferroferric oxide particles and is a combined layer, and the sandwich-structure carbon/magnetic electromagnetic wave absorbing material is provided with at least 2 combined layers.
As another aspect of the present invention, the present invention provides a method for preparing a sandwich-structured carbon/magneto-electromagnetic wave absorbing material, comprising the steps of (1) dissolving an iron salt into diethylene glycol to prepare a metal salt solution S1 having a mass fraction of 8% -10%; (2) Adding a buffering agent into the solution S1, stirring and dissolving, and standing for 5 minutes to prepare a solution S2; (3) Transferring the S2 solution into an autoclave, introducing protective gas, keeping the temperature at 200 ℃ for 8 hours, vibrating for 1 time every 30 minutes to prevent agglomeration of particles, taking out, washing with deionized water, and drying to obtain flaky ferroferric oxide; (4) Preparing 1-2g/L dopamine hydrochloride and adjusting pH to 8.5 to prepare solution S3; (5) Putting the flaky ferroferric oxide prepared in the step (3) into a solution S3, wherein the mass fraction of the flaky ferroferric oxide is 9-11%, and then carrying out oscillation reaction for 10-24 hours in a water bath at 30 ℃ to obtain a flaky material coated with polydopamine; (6) The sheet material coated with polydopamine is placed into a nitrogen atmosphere with the temperature of 450-600 ℃ for carbonization treatment for 1 hour to obtain a material S4; (7) Adding 10g of material S4 into 100ml of distilled water, adding 5g of ferric chloride and ferrous chloride blend with the molar ratio of 2:1, stirring and dissolving, gradually dripping 8ml of ammonia water, reacting in a water bath at 50 ℃ for 1 hour, and cleaning.
Preferably, the iron salt is selected from the group consisting of ferric sulfate and ferric chloride.
Preferably, the sandwich-structured carbon/magneto-electromagnetic wave absorbing material has an inner layer of ferroferric oxide, an intermediate layer of carbon and an outer layer of nano ferroferric oxide particles.
Preferably, the steps (4) to (7) are repeated, and a multilayered electromagnetic wave absorbing material can be prepared.
The beneficial effects of the invention are as follows:
the flaky carbon/magneto-electromagnetic wave absorbing material with the sandwich structure prepared by cross hybridization molding of the ferroferric oxide and the carbon can obviously improve the electromagnetic wave absorbing performance of the material, has both dielectric loss and magnetic loss performance, has light weight, can be used as an electromagnetic wave absorbent to be compounded with textiles, high polymer adhesives and the like to prepare a light and soft electromagnetic wave absorbing composite material, and has very wide application prospect.
Drawings
FIG. 1 is an SEM image of a carbon-magnetic electromagnetic wave absorbing material of a sandwich structure prepared according to the present invention;
FIG. 2 is a graph showing electromagnetic wave absorption performance of the carbon-magnetic electromagnetic wave absorption material with a sandwich structure prepared in example 1 of the present invention;
FIG. 3 is a graph showing electromagnetic wave absorption performance of the carbon-magnetic electromagnetic wave absorbing material with a sandwich structure according to the embodiment 2 of the present invention;
fig. 4 is an electromagnetic wave absorption performance diagram of the carbon-magnetic electromagnetic wave absorption material with the sandwich structure prepared in example 3 of the present invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Example 1:
(1) 2g of anhydrous ferric chloride is dissolved in 20ml of diethylene glycol to prepare a metal salt solution;
(2) Adding 2g of citric acid-sodium citrate buffer (pH=10) into the solution in the step 1, stirring and dissolving, and standing for 5 minutes to prepare a solution;
(3) Transferring the solution prepared in the step 2 into a stainless steel autoclave with a Teflon lining, keeping the temperature at 200 ℃ for 8 hours, introducing nitrogen to protect ferroferric oxide from oxidation in the reaction process, and vibrating for 1 time every 30 minutes to prevent agglomeration of particles; then taking out, washing and drying with deionized water to obtain flaky ferroferric oxide;
(4) Preparing 1g/L dopamine hydrochloride, and regulating the pH value of the solution to 8.5 by using a citric acid-sodium citrate buffer;
(5) Putting 5g of flaky ferroferric oxide into 50ml of the solution prepared in the step 4, and then carrying out oscillation reaction in a water bath at 30 ℃ for 10 hours to obtain a flaky material coated with polydopamine, wherein the thickness of polydopamine is 5nm;
(6) Carbonizing the material prepared in the step 5 in nitrogen atmosphere at 450 ℃ for 1 hour, and then taking out;
(7) Adding 10g of the material prepared in the step 6 into 100ml of distilled water, then adding 5g of ferric chloride and ferrous chloride blend with the molar ratio of 2:1, stirring and dissolving, gradually dripping 8ml of ammonia water, reacting in a water bath at 50 ℃ for 1 hour, and then washing for later use;
(8) The prepared material is prepared by taking ferroferric oxide as an inner layer, a middle layer as a carbon layer, and an outermost layer as nano ferroferric oxide particles, wherein the conductivity is 0.2S/cm, and the special sandwich structure has certain electromagnetic wave absorption performance, as shown in the following figure 2.
Example 2:
(1) 10g of anhydrous ferric chloride is dissolved in 80ml of diethylene glycol to prepare a metal salt solution;
(2) Adding 5g of citric acid-sodium citrate buffer (pH=10) into the solution in the step 1, stirring and dissolving, and standing for 5 minutes to prepare a solution;
(3) Transferring the solution prepared in the step 2 into a stainless steel autoclave with a Teflon lining, keeping the temperature at 200 ℃ for 8 hours, introducing nitrogen to protect ferroferric oxide from oxidation in the reaction process, and vibrating for 1 time every 30 minutes to prevent agglomeration of particles; then taking out, washing and drying with deionized water to obtain flaky ferroferric oxide;
(4) Preparing 2g/L dopamine hydrochloride, and regulating the pH value of the solution to 8.5 by using a citric acid-sodium citrate buffer;
(5) Putting 10g of flaky ferroferric oxide into 80ml of the solution prepared in the step 4, and then carrying out oscillation reaction for 24 hours in a water bath at 30 ℃ to obtain a flaky material coated with polydopamine, wherein the thickness of polydopamine is 10nm;
(6) The material prepared in the step 5 is placed into a nitrogen atmosphere at 600 ℃ for carbonization treatment for 1 hour, and then is taken out;
(7) Adding 10g of the material prepared in the step 6 into 100ml of distilled water, then adding 5g of ferric chloride and ferrous chloride blend with the molar ratio of 2:1, stirring and dissolving, gradually dripping 8ml of ammonia water, reacting in a water bath at 50 ℃ for 1 hour, and then washing for later use;
(8) The prepared material is characterized in that ferroferric oxide is used as an inner layer, a middle layer is used as a carbon layer, the outermost layer is nano ferroferric oxide particles, the conductivity is 0.8S/cm, a special sandwich structure has good electromagnetic wave absorption performance, the carbonization temperature of dopamine is controlled, and the electromagnetic wave absorption performance of the material can be effectively improved, as shown in the following figure 3.
Example 3:
(1) 10g of anhydrous ferric chloride is dissolved in 80ml of diethylene glycol to prepare a metal salt solution;
(2) Adding 5g of citric acid-sodium citrate buffer (pH=10) into the solution in the step 1, stirring and dissolving, and standing for 5 minutes to prepare a solution;
(3) Transferring the solution prepared in the step 2 into a stainless steel autoclave with a Teflon lining, keeping the temperature at 200 ℃ for 8 hours, introducing nitrogen to protect ferroferric oxide from oxidation in the reaction process, and vibrating for 1 time every 30 minutes to prevent agglomeration of particles; then taking out, washing and drying with deionized water to obtain flaky ferroferric oxide;
(4) Preparing 2g/L dopamine hydrochloride, and regulating the pH value of the solution to 8.5 by using a citric acid-sodium citrate buffer;
(5) Putting 10g of flaky ferroferric oxide into 80ml of the solution prepared in the step 4, and then carrying out oscillation reaction for 24 hours in a water bath at 30 ℃ to obtain a flaky material coated with polydopamine, wherein the thickness of polydopamine is 10nm;
(6) The material prepared in the step 5 is placed into a nitrogen atmosphere at 600 ℃ for carbonization treatment for 1 hour, and then is taken out;
(7) Adding 10g of the material prepared in the step 6 into 100ml of distilled water, then adding 5g of ferric chloride and ferrous chloride blend with the molar ratio of 2:1, stirring and dissolving, gradually dripping 8ml of ammonia water, reacting in a water bath at 50 ℃ for 1 hour, and then washing for later use;
(8) Repeating the steps 4-7 for 1 time, and coating polydopamine, carbonizing and loading the outermost ferroferric oxide;
(9) The prepared material is characterized in that ferroferric oxide is used as an inner layer, a carbon layer and a nano ferroferric oxide particle layer are used for alternately loading, the conductivity is 0.85S/cm, a special sandwich structure of multiple layers has excellent electromagnetic wave absorption performance, the electromagnetic wave absorption performance of the material is found to be strong, the minimum loss reaches-19 dB, and the bandwidth of effective loss (< -10 dB) in the range of 2-18GHz is 12GHz, as shown in the following figure 4.
According to the preparation process of coating, carbonization and the like, the carbon layer is generated on the surface of the flaky ferroferric oxide in situ, the structure of the produced product is more stable, the carbonization rate of dopamine is controlled through carbonization temperature, and the number of layers can be controlled through the preparation process, so that the maximum absorption performance under different electromagnetic wave frequency bands is achieved. Compared with the blending and hybridization of various materials by other technologies, the preparation method has the advantages that the dispersion rule of various materials is irregular and the stability is poor, the preparation method is carried out layer by layer, the thickness of each layer is controllable, and the prepared materials are stable in performance. The carbon layer has a large influence on the material performance, and the preparation of the carbon layer with different conductivity is performed by using the dopamine cladding and carbonization technology to control the overall electromagnetic wave impedance matching and the cooperative electromagnetic wave loss of the material.
The foregoing is only a preferred embodiment of the invention, it being noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (4)
1. A preparation method of a sandwich-structured carbon/magneto-electromagnetic wave absorbing material is characterized by comprising the following steps of: comprises the steps of,
(1) Dissolving ferric salt into diethylene glycol to prepare a metal salt solution S1 with the mass fraction of 8% -10%;
(2) Adding a buffering agent into the solution S1, stirring and dissolving, and standing for 5 minutes to prepare a solution S2;
(3) Transferring the solution S2 into an autoclave, introducing protective gas, keeping at 200 ℃ for 8 hours, vibrating for 1 time every 30min to prevent agglomeration of particles, taking out, washing with deionized water, and drying to obtain flaky ferroferric oxide;
(4) Preparing 1-2g/L dopamine hydrochloride and adjusting the pH value to 8.5 to prepare a solution S3;
(5) Putting the flaky ferroferric oxide prepared in the step (3) into a solution S3, wherein the mass fraction of the flaky ferroferric oxide is 9-11%, and then carrying out oscillation reaction for 10-24 hours in a water bath at 30 ℃ to obtain a flaky material coated with polydopamine;
(6) The sheet material coated with polydopamine is placed into a nitrogen atmosphere with the temperature of 450-600 ℃ for carbonization treatment for 1 hour to obtain a material S4;
(7) Adding 10g of material S4 into 100ml of distilled water, adding 5g of ferric chloride and ferrous chloride blend with the molar ratio of 2:1, stirring and dissolving, gradually dripping 8ml of ammonia water, reacting in a water bath at 50 ℃ for 1 hour, and cleaning to obtain the carbon/magneto-electromagnetic wave absorbing material with the sandwich structure.
2. The method for preparing the sandwich-structured carbon/magneto-electromagnetic wave absorbing material according to claim 1, wherein the method comprises the following steps: the ferric salt in the step (1) is selected from ferric sulfate and ferric chloride.
3. The method for preparing the sandwich-structured carbon/magneto-electromagnetic wave absorbing material according to claim 1, wherein the method comprises the following steps: the sandwich structure carbon/magneto-electromagnetic wave absorbing material obtained in the step (7) is characterized in that the inner layer is ferroferric oxide, the middle layer is a carbon layer, and the outer layer is nano ferroferric oxide particles.
4. A method for preparing a sandwich-structured carbon/magneto-electromagnetic wave absorbing material as defined in claim 3, wherein: and (3) repeating the steps (4) - (7) to prepare the multi-layer electromagnetic wave absorbing material.
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| PCT/CN2022/091932 WO2023029564A1 (en) | 2021-09-06 | 2022-05-10 | Carbon/magnetic electromagnetic wave absorbing material having sandwich structure, and preparation method therefor |
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| US11202398B2 (en) * | 2017-09-28 | 2021-12-14 | Murata Manufacturing Co., Ltd. | Electromagnetic shielding material and method for producing the same |
| CN110712400B (en) * | 2019-09-06 | 2021-10-08 | 天津大学 | Method for preparing layered carbon fiber electromagnetic shielding composite material by using three-dimensional carbon/ferroferric oxide Koch layered layer |
| CN113597252B (en) * | 2021-09-06 | 2023-08-22 | 南通大学 | Preparation method of carbon/magneto-electromagnetic wave absorbing material with sandwich structure |
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| CN107761364A (en) * | 2017-11-03 | 2018-03-06 | 西北工业大学 | A kind of ferroso-ferric oxide/molybdenum disulfide/carbon fiber composite wave-suction material and the preparation method for passing through two-step reaction |
| CN109503858A (en) * | 2019-01-17 | 2019-03-22 | 南京大学 | A kind of magnetism sandwich structure metal-organic framework materials and preparation method |
| CN111040729A (en) * | 2019-11-15 | 2020-04-21 | 中国人民解放军陆军工程大学 | Preparation method and application of silicon carbide-based nano composite wave-absorbing material |
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