CN114539974A - Method for preparing magnetic metal @ graphene wave-absorbing material based on chemical vapor deposition method - Google Patents
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 39
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 35
- 239000011358 absorbing material Substances 0.000 title claims abstract description 29
- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 12
- 239000010941 cobalt Substances 0.000 claims abstract description 12
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 11
- 239000002105 nanoparticle Substances 0.000 claims abstract description 7
- 230000035484 reaction time Effects 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 10
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 8
- 239000005695 Ammonium acetate Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 229940043376 ammonium acetate Drugs 0.000 claims description 8
- 235000019257 ammonium acetate Nutrition 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 6
- 150000001868 cobalt Chemical class 0.000 claims description 6
- 229940011182 cobalt acetate Drugs 0.000 claims description 6
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 6
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 5
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 150000002505 iron Chemical class 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 43
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 14
- 239000002184 metal Substances 0.000 abstract description 10
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 229910003321 CoFe Inorganic materials 0.000 description 15
- 238000010521 absorption reaction Methods 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 229940032296 ferric chloride Drugs 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000000634 powder X-ray diffraction Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 229910002518 CoFe2O4 Inorganic materials 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 229910000531 Co alloy Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- QVYYOKWPCQYKEY-UHFFFAOYSA-N [Fe].[Co] Chemical compound [Fe].[Co] QVYYOKWPCQYKEY-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229940032950 ferric sulfate Drugs 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
A method for preparing a magnetic metal @ graphene wave-absorbing material based on a chemical vapor deposition method comprises the steps of placing cobalt ferrite nanoparticles in a methane atmosphere, carrying out chemical vapor deposition reaction at a high temperature, and cooling to obtain the magnetic metal @ graphene wave-absorbing material; the temperature of the chemical vapor deposition reaction is 800-1000 ℃, and the reaction time is 1-30 min. According to the invention, the magnetic metal @ graphene is synthesized in situ, so that not only can compact multilayer graphene be obtained to prevent oxidation of the magnetic metal, but also the dielectric loss of the material is effectively utilized, and the wave-absorbing material with wider application prospect can be prepared.
Description
Technical Field
The invention relates to the field of microwave absorbing materials, in particular to a method for preparing a magnetic metal @ graphene wave absorbing material based on a chemical vapor deposition method.
Background
The development and use of wave-absorbing materials are started in the military field at the earliest, and mainly aim to improve the survival capability of strategic weapons and avoid the search of radar. However, with the progress of science and technology, a large number of wireless communication devices enter the daily life of people, and a large amount of electromagnetic wave radiation and pollution exist while convenience is brought to the life. This makes it increasingly important to develop and develop superior microwave absorbing materials.
The wave absorbing mechanism of the wave absorbing material is that electromagnetic wave energy incident on the material is converted into heat energy or energy in other forms through dielectric loss or magnetic loss, but a single absorbing mechanism is difficult to meet the requirements of life and military affairs, so that the combination of the dielectric material and the magnetic material is an effective strategy, and the composite of the dielectric material and the magnetic material has dielectric loss and magnetic loss, is beneficial to improving impedance matching, improves the performance of a single material, and can widen the application range of the wave absorbing material. In the existing composite wave-absorbing material, the magnetic metal is easy to be oxidized, so that the application range of the wave-absorbing material is not wide, and the application of the wave-absorbing material is limited.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for preparing a magnetic metal @ graphene wave-absorbing material based on a chemical vapor deposition method, which can effectively prevent the oxidation of magnetic metal, is simple and convenient to operate, has high yield and has potential application prospects.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a magnetic metal @ graphene wave-absorbing material based on a chemical vapor deposition method comprises the steps of placing cobalt ferrite nanoparticles in a methane atmosphere, carrying out chemical vapor deposition reaction at a high temperature, and cooling to obtain the magnetic metal @ graphene wave-absorbing material; the temperature of the chemical vapor deposition reaction is 800-1000 ℃, and the reaction time is 1-30 min.
The size of the cobalt ferrite nano particles is 150-200 nm.
The cobalt ferrite nano-particles are prepared as follows: adding iron salt, cobalt salt and ammonium acetate into glycol solution for dissolving, then placing into a hydrothermal kettle for reaction, finally separating, washing and drying.
The iron salt is selected from at least one of ferric chloride and ferric sulfate, and the cobalt salt is selected from at least one of cobalt acetate and cobalt nitrate.
The molar ratio of the ferric salt to the cobalt salt to the ammonium acetate is 1:1: 6.5-2: 1: 13.
The reaction temperature of the hydrothermal kettle is 180-200 ℃, and the reaction time is 20-24 h. When the reaction temperature is lower than 180 ℃, cobalt ferrite particles cannot be synthesized, and when the reaction temperature is higher than 200 ℃, the uniformity of the particles is reduced. When the reaction time is shorter than 20h, cobalt ferrite particles cannot be synthesized, and when the reaction time is longer than 24h, the uniformity of the particles is reduced.
The separation can be performed by adopting a magnet, and the washing is performed by adopting water and ethanol.
The atmosphere of the chemical vapor deposition reaction is methane or mixed gas of methane and argon, and the gas flow is 10-50 ml/min.
In the mixed gas of methane and argon, the volume ratio of argon is not higher than 50%.
The temperature rise time of the chemical vapor deposition reaction is 50-65 min. The heating time is determined by the fastest heating rate of the tube furnace, if the heating time is too long, the final magnetic metal particles are seriously agglomerated, and the absorption of electromagnetic waves is not facilitated.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
1. the magnetic metal @ graphene material prepared by the invention is different from other magnetic metal/graphene materials, the graphene grows in situ, is not externally added, is tightly combined with a magnetic metal kernel, can fully protect the kernel from being oxidized, and has a good application prospect in construction of novel functional devices or materials;
2. the magnetic metal @ graphene material prepared by the invention adopts highly dispersed metal oxide as a magnetic metal source, effectively ensures the proportion of the magnetic metal, and is beneficial to the application of the material in the field of microwave absorption. And the cobalt ferrite can be replaced by other metal oxides containing iron, cobalt and nickel elements.
3. The preparation method of the invention has the advantages of simple operation, strong operability, good reproducibility and high yield up to 90%.
Drawings
FIG. 1 is CoFe prepared in example 12@ SEM picture of graphene material.
FIG. 2 is CoFe prepared in example 12X-ray powder diffraction patterns of @ graphene materials.
FIG. 3 is CoFe prepared in example 12@ raman shift plot of graphene material.
FIG. 4 is CoFe prepared in example 12@ graphene materials microwave absorption performance plots.
Figure 5 is an SEM image of the CoFe @ graphene material prepared in example 2.
FIG. 6 is an X-ray powder diffraction pattern of the CoFe @ graphene material prepared in example 2.
Fig. 7 is a raman shift plot of the CoFe @ graphene material prepared in example 2.
Fig. 8 is a graph of the microwave absorption performance of the CoFe @ graphene material prepared in example 2.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects of the present invention clearer and clearer, the present invention is further described in detail below with reference to the accompanying drawings and embodiments.
Example 1
This example is CoFe2The preparation method of the @ graphene material comprises the following steps:
(1) in 100ml of polytetrafluoroethylene lining, ferric chloride, cobalt acetate and ammonium acetate are added into 60ml of ethylene glycol and stirred to be dissolved, the mass ratio of the ferric chloride to the cobalt acetate is 2:1, the ferric chloride can adopt ferric chloride hexahydrate or ferric chloride hexahydrate, the addition amount is 540mg when the ferric chloride hexahydrate is adopted, and the addition amount is 324mg when anhydrous ferric chloride is adopted, wherein the addition amount of the ammonium acetate is 500 mg. The mixed solution was stirred at room temperature for 3h to ensure complete dissolution and uniform mixing. Putting the polytetrafluoroethylene lining into a reaction kettle, screwing, and finally putting the reaction kettle into an oven to react for 20 hours at a constant temperature of 200 ℃.
(2) After the reaction is finished, cooling the reaction solution to room temperature, separating the product by using a magnet, washing the obtained product by using water, ultrasonically washing the product by using ethanol for multiple times, and drying the product in vacuum to obtain the CoFe2O4And (3) powder.
(3) 100mg of CoFe2O4The powder was placed on a porcelain boat and placed in a tubular furnace for reaction in methane with a gas flow of 25 ml/min. Set up to heat upThe time is 60min, the heat preservation time is 10min, the temperature reduction time is 5h, and the reaction temperature is 1000 ℃.
(4) After the reaction is finished, taking out a sample to obtain CoFe2@ graphene material.
As can be seen from FIG. 1, CoFe prepared according to the examples2@ graphene material, the metal outer layer is coated with carbon. FIG. 2 is CoFe2X-ray powder diffraction pattern of @ graphene material, as can be seen in fig. 2: diffraction angles of 44.79 °,65.07 ° and 82.30 ° with face-centered cubic Co3Fe7(JCPDS No. 48-1817) or Fe (JCPDS No. 06-0696) (110), (200) and (211) crystal faces correspond to each other, and the inner core of the material is iron-cobalt alloy; the diffraction angle of 22.64 degrees corresponds to the (111) crystal face of graphitized carbon (JCPDS No. 75-2078), which indicates that the surface of the material has carbon. FIG. 3 is CoFe2The Raman shift diagram of the @ graphene material shows that the surface of the material is multilayer graphene. The above results confirm that the material is a magnetic metal @ graphene material. FIG. 4 is CoFe2The absorption energy diagram of the material for electromagnetic waves under different thicknesses indicates that the material has 90% energy loss for the electromagnetic wave energy when the reflection loss is-10 dB, so that the material has better microwave absorption capacity.
Example 2
The preparation method of the CoFe @ graphene material in the embodiment is as follows:
(1) in a 100ml polytetrafluoroethylene lining, ferric sulfate, cobalt acetate and ammonium acetate are added into 60ml ethylene glycol and stirred to be dissolved, the mass ratio of the ferric sulfate to the cobalt acetate is 1:1, wherein the adding amount of the ferric sulfate is 400mg, and the adding amount of the ammonium acetate is 500 mg. The mixed solution was stirred at room temperature for 3h to ensure complete dissolution and uniform mixing. Putting the polytetrafluoroethylene lining into a reaction kettle, screwing, and finally putting the reaction kettle into an oven to perform constant temperature reaction for 20 hours at 200 ℃.
(2) After the reaction is finished, cooling the reaction solution to room temperature, separating the product by using a magnet, washing the obtained product by using water, ultrasonically washing the product by using ethanol for multiple times, and drying the product in vacuum to obtain the cobalt ferrite powder.
3) 100mg of CoFe2O4The powder is placed in the porcelainThe boat is placed in a tubular furnace with the volume ratio of methane to argon being 1:0.5 for reaction, and the gas flow is 50 ml/min. Setting the temperature rise time to be 55min, the heat preservation time to be 30min, the temperature reduction time to be 10h and the reaction temperature to be 900 ℃.
(4) And after the reaction is finished, taking out a sample to obtain the CoFe @ graphene material.
As can be seen from fig. 5, the metal outer layer of the CoFe @ graphene material prepared according to the example was coated with carbon. Fig. 6 is an X-ray powder diffraction pattern of CoFe @ graphene material, as can be seen in fig. 6: diffraction angles 44.80 °,65.08 ° and 82.30 ° with face-centered cubic Co3Fe7(JCPDS No. 48-1817) or Fe (JCPDS No. 06-0696) (110), (200) and (211) crystal faces correspond to each other, and the inner core of the material is iron-cobalt alloy; the diffraction angle of 22.64 degrees corresponds to the (111) crystal face of graphitized carbon (JCPDS No. 75-2078), which indicates that the surface of the material has carbon. Fig. 7 is a raman shift graph of a CoFe @ graphene material, which shows that the surface of the material is multi-layer graphene. The above results confirm that the material is a magnetic metal @ graphene material. FIG. 8 is an absorption energy diagram of CoFe @ graphene material for electromagnetic waves at different thicknesses, and when the reflection loss is-10 dB, the material has 90% energy loss for the electromagnetic wave energy, so that the material is seen to have better microwave absorption capacity.
According to the invention, the magnetic metal @ graphene is synthesized in situ, so that not only can compact multilayer graphene be obtained to prevent oxidation of the magnetic metal, but also the dielectric loss of the material is effectively utilized, and the wave-absorbing material with wider application prospect can be prepared.
Claims (10)
1. A method for preparing a magnetic metal @ graphene wave-absorbing material based on a chemical vapor deposition method is characterized by comprising the following steps of: placing cobalt ferrite nano particles in a methane atmosphere, carrying out chemical vapor deposition reaction at high temperature, and cooling to obtain a magnetic metal @ graphene wave-absorbing material; the temperature of the chemical vapor deposition reaction is 800-1000 ℃, and the reaction time is 1-30 min.
2. The method for preparing the magnetic metal @ graphene wave-absorbing material based on the chemical vapor deposition method as claimed in claim 1, wherein the method comprises the following steps: the size of the cobalt ferrite nano particles is 150-200 nm.
3. The method for preparing the magnetic metal @ graphene wave-absorbing material based on the chemical vapor deposition method according to claim 2, wherein the cobalt ferrite nanoparticles are prepared as follows: adding iron salt, cobalt salt and ammonium acetate into glycol solution for dissolving, then placing into a hydrothermal kettle for reaction, finally separating, washing and drying.
4. The method for preparing the magnetic metal @ graphene wave-absorbing material based on the chemical vapor deposition method as claimed in claim 3, wherein the method comprises the following steps: the iron salt is selected from at least one of ferric chloride and ferric sulfate, and the cobalt salt is selected from at least one of cobalt acetate and cobalt nitrate.
5. The method for preparing the magnetic metal @ graphene wave-absorbing material based on the chemical vapor deposition method as claimed in claim 3, wherein the method comprises the following steps: the molar ratio of the ferric salt to the cobalt salt to the ammonium acetate is 1:1: 6.5-2: 1: 13.
6. The method for preparing the magnetic metal @ graphene wave-absorbing material based on the chemical vapor deposition method as claimed in claim 3, wherein the method comprises the following steps: the reaction temperature of the hydrothermal kettle is 180-200 ℃, and the reaction time is 20-24 h.
7. The method for preparing the magnetic metal @ graphene wave-absorbing material based on the chemical vapor deposition method as claimed in claim 3, wherein the method comprises the following steps: the separation can be performed by adopting a magnet, and the washing is performed by adopting water and ethanol.
8. The method for preparing the magnetic metal @ graphene wave-absorbing material based on the chemical vapor deposition method as claimed in claim 1, wherein the method comprises the following steps: the atmosphere of the chemical vapor deposition reaction is methane or mixed gas of methane and argon, and the gas flow is 10-50 ml/min.
9. The method for preparing the magnetic metal @ graphene wave-absorbing material based on the chemical vapor deposition method according to claim 8, is characterized in that: in the mixed gas of methane and argon, the volume ratio of argon is not higher than 50%.
10. The method for preparing the magnetic metal @ graphene wave-absorbing material based on the chemical vapor deposition method as claimed in claim 1 or 8, wherein the method comprises the following steps: the temperature rise time of the chemical vapor deposition reaction is 50-65 min.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101710512A (en) * | 2009-11-20 | 2010-05-19 | 哈尔滨工程大学 | Composite material of graphene and carbon-encapsulated ferromagnetic nano metal and preparation method thereof |
| WO2013011250A1 (en) * | 2011-07-21 | 2013-01-24 | Arkema France | Graphene-based conductive composite fibres |
| WO2013093350A1 (en) * | 2011-12-20 | 2013-06-27 | Institut National Polytechnique De Toulouse | Graphene production method and graphene obtained by said method |
| WO2014060686A1 (en) * | 2012-10-19 | 2014-04-24 | Arkema France | Drilling fluid containing graphene |
| WO2014060685A1 (en) * | 2012-10-19 | 2014-04-24 | Arkema France | Method for producing a graphene-based thermosetting composite material |
| CN104692367A (en) * | 2015-01-30 | 2015-06-10 | 东南大学 | Preparation method of metallic graphene |
| CN106191804A (en) * | 2016-06-06 | 2016-12-07 | 重庆大学 | A kind of preparation method of magnetic graphene nano belt/graphene composite film |
| CN106587030A (en) * | 2017-01-11 | 2017-04-26 | 重庆大学 | Method for preparing graphene thin film by chemical vapor deposition at normal pressure and low temperature |
| CN109936974A (en) * | 2019-04-03 | 2019-06-25 | 厦门大学 | A kind of synthetic method of sandwich structure CoFe@C/ graphene electromagnetic wave absorbent material |
| CN110258106A (en) * | 2019-07-19 | 2019-09-20 | 中南林业科技大学 | A kind of preparation method of the sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene |
-
2022
- 2022-02-21 CN CN202210159163.9A patent/CN114539974A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101710512A (en) * | 2009-11-20 | 2010-05-19 | 哈尔滨工程大学 | Composite material of graphene and carbon-encapsulated ferromagnetic nano metal and preparation method thereof |
| WO2013011250A1 (en) * | 2011-07-21 | 2013-01-24 | Arkema France | Graphene-based conductive composite fibres |
| WO2013093350A1 (en) * | 2011-12-20 | 2013-06-27 | Institut National Polytechnique De Toulouse | Graphene production method and graphene obtained by said method |
| WO2014060686A1 (en) * | 2012-10-19 | 2014-04-24 | Arkema France | Drilling fluid containing graphene |
| WO2014060685A1 (en) * | 2012-10-19 | 2014-04-24 | Arkema France | Method for producing a graphene-based thermosetting composite material |
| CN104692367A (en) * | 2015-01-30 | 2015-06-10 | 东南大学 | Preparation method of metallic graphene |
| CN106191804A (en) * | 2016-06-06 | 2016-12-07 | 重庆大学 | A kind of preparation method of magnetic graphene nano belt/graphene composite film |
| CN106587030A (en) * | 2017-01-11 | 2017-04-26 | 重庆大学 | Method for preparing graphene thin film by chemical vapor deposition at normal pressure and low temperature |
| CN109936974A (en) * | 2019-04-03 | 2019-06-25 | 厦门大学 | A kind of synthetic method of sandwich structure CoFe@C/ graphene electromagnetic wave absorbent material |
| CN110258106A (en) * | 2019-07-19 | 2019-09-20 | 中南林业科技大学 | A kind of preparation method of the sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene |
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