CN111615320A - Cobalt-nickel-graphene composite wave-absorbing material and preparation method thereof - Google Patents
Cobalt-nickel-graphene composite wave-absorbing material and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 38
- 239000011358 absorbing material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 34
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000725 suspension Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001291 vacuum drying Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 230000007935 neutral effect Effects 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 claims abstract description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 6
- 239000012498 ultrapure water Substances 0.000 claims abstract description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 229910017052 cobalt Inorganic materials 0.000 claims description 13
- 239000010941 cobalt Substances 0.000 claims description 13
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 13
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 38
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 230000035699 permeability Effects 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229920000547 conjugated polymer Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 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
-
- 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
- C01B32/194—After-treatment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
Abstract
The invention provides a cobalt-nickel-graphene composite wave-absorbing material and a preparation method thereof, belonging to the field of wave-absorbing material preparation. The method provided by the invention comprises the following specific steps: s1, preparing a Co/Ni precursor: with Co (NO)3)2·6H2O、Ni(NO3)2·6H2O and Na4EDTA is used as a raw material, and a Co/Ni precursor is prepared by a hydrothermal method; s2, dissolving graphene and the Co/Ni precursor prepared in the step S2 in ultrapure water, performing ultrasonic dispersion for 2 hours to obtain a suspension, adding hydrazine hydrate, transferring the suspension into a high-pressure reaction kettle, putting the high-pressure reaction kettle into a vacuum drying oven, heating to 200 ℃, preserving heat for 24 hours, cooling to room temperature, repeatedly washing the suspension to be neutral by using deionized water and ethanol, and drying at 60 ℃ to obtain a Co/Ni @ GO composite material; s3, putting the Co/Ni @ GO composite material prepared in the step S2 into a tubular furnace, and N2And (3) heating to 700 ℃ in the atmosphere, and preserving the heat for 5-6h to obtain the Co/Ni @ rGO composite wave-absorbing material. The Co/Ni @ rGO composite wave-absorbing material provided by the invention has the advantages that the effective frequency band width is 12.2GHz, the maximum reflection loss can reach-46.3 dB (13.8GHz), the density is low, and the application prospect is good.
Description
Technical Field
The invention relates to the field of wave-absorbing material preparation, in particular to a cobalt-nickel-graphene composite wave-absorbing material and a preparation method thereof.
Background
With the development and application of radio network technology, a large amount of electromagnetic waves enter human living space, causing serious negative problems such as electromagnetic interference and electromagnetic radiation pollution. Different from the traditional electromagnetic shielding material, the wave-absorbing material can realize the effective absorption of electromagnetic waves without causing secondary radiation, but the existing wave-absorbing material has the defects of low absorption strength and narrow effective absorption bandwidth. The magnetic metal has high saturation magnetization and magnetic permeability and strong electromagnetic wave attenuation capability, but has poor chemical stability and corrosion resistance, high density, complex preparation method and low yield. In contrast, conjugated polymers and carbonaceous materials have the advantages of low density, low cost, corrosion resistance, and ease of preparation. Particularly, in the carbonaceous material, Graphene (GO) has a unique two-dimensional network structure, shows good electrical, thermal and mechanical properties, and can be used as an ideal substrate material of a light and efficient composite wave-absorbing material.
Disclosure of Invention
The first purpose of the invention is to provide a preparation method of a cobalt-nickel-graphene composite wave-absorbing material.
The second purpose of the invention is to provide a cobalt-nickel-graphene composite wave-absorbing material.
In order to achieve the first object, the preparation method of the cobalt-nickel-graphene composite wave-absorbing material provided by the invention comprises the following specific steps:
s1, preparing a Co/Ni precursor: with Co (NO)3)2·6H2O、Ni(NO3)2·6H2O and Na4EDTA is used as a raw material, and a Co/Ni precursor is prepared by a hydrothermal method;
the method specifically comprises the following steps: co (NO) in an amount of 0.024mol based on the total amount of the components3)2·6H2O、Ni(NO3)2·6H2Dissolving O and 0.012mol in 20mL of deionized water, adding 10mL of methanol, carrying out ultrasonic treatment for 30min to disperse uniformly, transferring to a reaction kettle, putting into a vacuum drying oven, heating to 200 ℃, keeping the temperature for 24h, cooling to room temperature, repeatedly washing with deionized water and ethanol to be neutral, and drying at 60 ℃ to obtain the Co/Ni precursor.
Wherein said Co (NO)3)2·6H2O and said Ni (NO)3)2·6H2The molar ratio of O is 1: 0.6-1.
S2, dissolving graphene and the Co/Ni precursor prepared in the step S1 in ultrapure water, performing ultrasonic dispersion for 2 hours to obtain a suspension, adding hydrazine hydrate, transferring the suspension into a high-pressure reaction kettle, putting the high-pressure reaction kettle into a vacuum drying oven, heating to 200 ℃, preserving heat for 24 hours, cooling to room temperature, repeatedly washing the suspension to be neutral by using deionized water and ethanol, and drying at 60 ℃ to obtain a Co/Ni @ GO composite material;
wherein the mass ratio of the graphene to the Co/Ni precursor is 1: 0.8-1.2.
Wherein the heating rate is 1 ℃/min.
S3, putting the Co/Ni @ GO composite material prepared in the step S2 into a tubular furnace, and N2And (3) heating to 700 ℃ in the atmosphere, and preserving the heat for 5-6h to obtain the Co/Ni @ rGO composite wave-absorbing material.
Wherein the heating efficiency is 5 ℃/min.
The invention also discloses a cobalt nickel-graphene composite wave-absorbing material prepared by the preparation method of the cobalt nickel-graphene composite wave-absorbing material.
The invention has the beneficial effects that:
according to the invention, a Co/Ni precursor is prepared by a hydrothermal method, then the precursor is loaded on graphene, and a large amount of gas is released in the process of combining the Co/Ni precursor with the graphene through high-temperature pyrolysis, so that a large amount of gaps are formed in the Co/Ni precursor, and the Co/Ni and a two-dimensional network of the graphene are crosslinked to form a network microstructure in a molten state. The Co/Ni @ rGO composite wave-absorbing material provided by the invention has better absorption in a 3.9-16.1GHz band, the effective frequency band width is 12.2GHz, the maximum reflection loss can reach-46.3 dB (13.8GHz), the density is low, and the Co/Ni @ rGO composite wave-absorbing material has a good application prospect.
Detailed Description
In order to more clearly and completely describe the technical scheme of the invention, the invention is further described in detail by the specific embodiments, and it should be understood that the specific embodiments described herein are only used for explaining the invention, and are not used for limiting the invention, and various changes can be made within the scope defined by the claims of the invention.
Example 1
A preparation method of a cobalt nickel-graphene composite wave-absorbing material comprises the following specific steps:
s1, preparing a Co/Ni precursor: with Co (NO)3)2·6H2O、Ni(NO3)2·6H2O and Na4EDTA is used as a raw material, and a Co/Ni precursor is prepared by a hydrothermal method;
the method specifically comprises the following steps: co (NO) in an amount of 0.024mol based on the total amount of the components3)2·6H2O、Ni(NO3)2·6H2Dissolving O and 0.012mol in 20mL of deionized water, adding 10mL of methanol, carrying out ultrasonic treatment for 30min to disperse uniformly, transferring to a reaction kettle, putting into a vacuum drying oven, heating to 200 ℃, keeping the temperature for 24h, cooling to room temperature, repeatedly washing with deionized water and ethanol to be neutral, and drying at 60 ℃ to obtain the Co/Ni precursor.
Wherein said Co (NO)3)2·6H2O and said Ni (NO)3)2·6H2The molar ratio of O is 1: 0.8.
S2, dissolving graphene and the Co/Ni precursor prepared in the step S1 in ultrapure water, performing ultrasonic dispersion for 2 hours to obtain a suspension, adding hydrazine hydrate, transferring the suspension into a high-pressure reaction kettle, putting the high-pressure reaction kettle into a vacuum drying oven, heating to 200 ℃, preserving heat for 24 hours, cooling to room temperature, repeatedly washing the suspension to be neutral by using deionized water and ethanol, and drying at 60 ℃ to obtain a Co/Ni @ GO composite material;
wherein the mass ratio of the graphene to the Co/Ni precursor is 1:1.
Wherein the heating rate is 1 ℃/min.
S3, putting the Co/Ni @ GO composite material prepared in the step S2 into a tubular furnace, and N2And (3) heating to 700 ℃ in the atmosphere, and preserving the heat for 6 hours to obtain the Co/Ni @ rGO composite wave-absorbing material.
Wherein the heating efficiency is 5 ℃/min.
Example 2
A preparation method of a cobalt nickel-graphene composite wave-absorbing material comprises the following specific steps:
s1, preparing a Co/Ni precursor: with Co (NO)3)2·6H2O、Ni(NO3)2·6H2O and Na4EDTA is used as a raw material, and a Co/Ni precursor is prepared by a hydrothermal method;
the method specifically comprises the following steps: co (NO) in an amount of 0.024mol based on the total amount of the components3)2·6H2O、Ni(NO3)2·6H2Dissolving O and 0.012mol in 20mL of deionized water, adding 10mL of methanol, carrying out ultrasonic treatment for 30min to disperse uniformly, transferring to a reaction kettle, putting into a vacuum drying oven, heating to 200 ℃, keeping the temperature for 24h, cooling to room temperature, repeatedly washing with deionized water and ethanol to be neutral, and drying at 60 ℃ to obtain the Co/Ni precursor.
Wherein said Co (NO)3)2·6H2O and said Ni (NO)3)2·6H2The molar ratio of O is 1: 0.6.
S2, dissolving graphene and the Co/Ni precursor prepared in the step S1 in ultrapure water, performing ultrasonic dispersion for 2 hours to obtain a suspension, adding hydrazine hydrate, transferring the suspension into a high-pressure reaction kettle, putting the high-pressure reaction kettle into a vacuum drying oven, heating to 200 ℃, preserving heat for 24 hours, cooling to room temperature, repeatedly washing the suspension to be neutral by using deionized water and ethanol, and drying at 60 ℃ to obtain a Co/Ni @ GO composite material;
wherein the mass ratio of the graphene to the Co/Ni precursor is 1: 0.8.
Wherein the heating rate is 1 ℃/min.
S3, putting the Co/Ni @ GO composite material prepared in the step S2 into a tubular furnace, and N2And (3) heating to 700 ℃ in the atmosphere, and preserving the heat for 6 hours to obtain the Co/Ni @ rGO composite wave-absorbing material.
Wherein the heating efficiency is 5 ℃/min.
Example 3
A preparation method of a cobalt nickel-graphene composite wave-absorbing material comprises the following specific steps:
s1, preparing a Co/Ni precursor: with Co (NO)3)2·6H2O、Ni(NO3)2·6H2O and Na4EDTA is used as a raw material, and a Co/Ni precursor is prepared by a hydrothermal method;
the method specifically comprises the following steps: co (NO) in an amount of 0.024mol based on the total amount of the components3)2·6H2O、Ni(NO3)2·6H2Dissolving O and 0.012mol in 20mL deionized water, adding 10mL methanol, performing ultrasonic treatment for 30min to disperse uniformly, transferring to a reaction kettle, placing into a vacuum drying oven, heating to 200 deg.C, maintaining the temperature for 24h, cooling to room temperature, and repeatedly washing with deionized water and ethanolWashing to neutrality, drying at 60 deg.c to obtain Co/Ni precursor.
Wherein, Co (NO)3)2·6H2O and Ni (NO)3)2·6H2The molar ratio of O is 1:1.
S2, dissolving graphene and the Co/Ni precursor prepared in the step S1 in ultrapure water, performing ultrasonic dispersion for 2 hours to obtain a suspension, adding hydrazine hydrate, transferring the suspension into a high-pressure reaction kettle, putting the high-pressure reaction kettle into a vacuum drying oven, heating to 200 ℃, preserving heat for 24 hours, cooling to room temperature, repeatedly washing the suspension to be neutral by using deionized water and ethanol, and drying at 60 ℃ to obtain a Co/Ni @ GO composite material;
wherein the mass ratio of the graphene to the Co/Ni precursor is 1: 1.2.
Wherein the heating rate is 1 ℃/min.
S3, putting the Co/Ni @ GO composite material prepared in the step S2 into a tubular furnace, and N2And (3) heating to 700 ℃ in the atmosphere, and preserving the heat for 6 hours to obtain the Co/Ni @ rGO composite wave-absorbing material.
Wherein the heating efficiency is 5 ℃/min.
Comparative example 1
Wherein, Co (NO)3)2·6H2O and Ni (NO)3)2·6H2The molar ratio of O was 1:2, as in example 1.
Comparative example 2
The mass ratio of graphene to the Co/Ni precursor was 1:2, and the rest was the same as in example 1.
The Co/Ni @ rGO composite wave-absorbing material powder prepared in the embodiment is mixed with paraffin according to the filling amount of 30 wt% and placed into a mortar, a small amount of petroleum ether is added, the grinding is continued until the petroleum ether is completely volatilized, and a coaxial test piece with the inner diameter of 3mm, the outer diameter of 7mm and the thickness of 2mm is pressed by using a special mold. And (3) testing the complex dielectric constant and the complex magnetic permeability by adopting a vector network analyzer, and finally calculating the reflection loss of the complex dielectric constant and the complex magnetic permeability to the electromagnetic wave by utilizing a transmission line theory. The results are shown in the following table:
TABLE 1
As can be seen from Table 1, the Co/Ni @ rGO composite wave-absorbing material prepared by the embodiment of the invention has better wave-absorbing performance. Wherein, the molar ratio of cobalt to nickel is 1:0.8, the mass ratio of cobalt to nickel to graphene is 1:1, the maximum effective bandwidth of example 1 is 12.2GHz, and the maximum reflection loss value is-46.3 dB at 13.8 GHz. By comparing the comparative example 1, the comparative example 2 and the example 1, the mol ratio of cobalt and nickel and the mass ratio of cobalt and nickel and graphene can affect the wave-absorbing performance of the wave-absorbing material.
Finally, it should be emphasized that the above-described preferred embodiments of the present invention are merely examples of implementations, rather than limitations, and that many variations and modifications of the invention are possible to those skilled in the art, without departing from the spirit and scope of the invention.
Claims (7)
1. A preparation method of a cobalt nickel-graphene composite wave-absorbing material is characterized by comprising the following specific steps:
s1, preparing a Co/Ni precursor: with Co (NO)3)2·6H2O、Ni(NO3)2·6H2O and Na4EDTA is used as a raw material, and a Co/Ni precursor is prepared by a hydrothermal method;
s2, dissolving graphene and the Co/Ni precursor prepared in the step S1 in ultrapure water, performing ultrasonic dispersion for 2 hours to obtain a suspension, adding hydrazine hydrate, transferring the suspension into a high-pressure reaction kettle, putting the high-pressure reaction kettle into a vacuum drying oven, heating to 200 ℃, preserving heat for 24 hours, cooling to room temperature, repeatedly washing the suspension to be neutral by using deionized water and ethanol, and drying at 60 ℃ to obtain a Co/Ni @ GO composite material;
s3, putting the Co/Ni @ GO composite material prepared in the step S2 into a tubular furnace, and N2And (3) heating to 700 ℃ in the atmosphere, and preserving the heat for 5-6h to obtain the Co/Ni @ rGO composite wave-absorbing material.
2. The method for preparing a cobalt-nickel-graphene composite wave-absorbing material according to claim 1, wherein the preparation of the Co/Ni precursor in step S1 specifically comprises the following steps:
co (NO) in an amount of 0.024mol based on the total amount of the components3)2·6H2O、Ni(NO3)2·6H2Dissolving O and 0.012mol in 20mL of deionized water, adding 10mL of methanol, carrying out ultrasonic treatment for 30min to disperse uniformly, transferring to a reaction kettle, putting into a vacuum drying oven, heating to 200 ℃, keeping the temperature for 24h, cooling to room temperature, repeatedly washing with deionized water and ethanol to be neutral, and drying at 60 ℃ to obtain the Co/Ni precursor.
3. The method for preparing cobalt nickel-graphene composite wave-absorbing material according to claim 2, wherein Co (NO) is used3)2·6H2O and said Ni (NO)3)2·6H2The molar ratio of O is 1: 0.6-1.
4. The method for preparing the cobalt-nickel-graphene composite wave-absorbing material according to claim 1, wherein the mass ratio of the graphene to the Co/Ni precursor in the step S2 is 1: 0.8-1.2.
5. The method for preparing the cobalt-nickel-graphene composite wave-absorbing material according to claim 1, wherein the temperature rise rate of the temperature rise in the step S2 is 1 ℃/min.
6. The method for preparing the cobalt-nickel-graphene composite wave-absorbing material according to claim 1, wherein the temperature rise rate of the temperature rise in the step S3 is 5 ℃/min.
7. The cobalt nickel-graphene composite wave-absorbing material prepared by the preparation method of the cobalt nickel-graphene composite wave-absorbing material of any one of claims 1 to 6.
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| CN113088252A (en) * | 2021-04-01 | 2021-07-09 | 安徽理工大学 | Iron-cobalt-nickel alloy/carbon/graphene ultrathin wave-absorbing material and preparation method thereof |
| CN113328262A (en) * | 2021-05-31 | 2021-08-31 | 青岛科技大学 | Preparation method of manganese oxide @ Ni-Co/graphite carbon nanocomposite |
| CN114276782A (en) * | 2021-09-27 | 2022-04-05 | 哈尔滨工业大学 | Preparation method of frequency-adjustable (SnO2/Sn/rGO) composite wave-absorbing material |
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Application publication date: 20200901 |