CN113823919B - Light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam and preparation method thereof - Google Patents
Light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam and preparation method thereof Download PDFInfo
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- CN113823919B CN113823919B CN202111121491.1A CN202111121491A CN113823919B CN 113823919 B CN113823919 B CN 113823919B CN 202111121491 A CN202111121491 A CN 202111121491A CN 113823919 B CN113823919 B CN 113823919B
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- 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
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- 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
- H01Q17/004—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems using non-directional dissipative particles, e.g. ferrite powders
Abstract
The invention discloses a light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam and a preparation method thereof. Carrying out hydrothermal reaction on the nickel complex solution to obtain a nickel/nickel oxide complex; mixing nickel with oxygenDispersing a nickel compound and a raw material containing graphene into an alcohol/water mixed solution to obtain a suspension; sequentially carrying out freezing solidification, freezing drying and thermal reduction treatment on the suspension to obtain light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam, wherein the nickel/nickel oxide composite is uniformly dispersed on graphene lamellar layers through electrostatic action in the wave-absorbing foam, and the graphene lamellar layers are stacked to form a foam structure; the wave-absorbing foam has excellent wave-absorbing performance in a low-frequency S wave band, and the density is as low as 0.001-1 g/cm 3 。
Description
Technical Field
The invention relates to a wave-absorbing material, particularly relates to a light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam material, and also relates to a preparation method of the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam material, belonging to the technical field of wave-absorbing materials.
Background
Along with the popularization of the electronic equipment driven by the development of science and technology, the electromagnetic pollution is brought when the life of people is facilitated. In daily life, low-frequency band (2-4 GHz) electromagnetic wave interference such as microwave ovens, radio frequency and microwave treatment equipment, electromagnetic communication and the like needs low-frequency wave-absorbing materials to reduce damage urgently. In the recent trend of portable development of devices and low frequency of electromagnetic application, a novel portable high-performance low-frequency absorption material has a great application demand.
Different from the traditional large-density ferrite wave-absorbing material, the new material graphite has high heat conductivity coefficient, high electron mobility, large specific surface area and high specific surface area due to the special two-dimensional structure of the new material graphiteDielectric constant, etc., making it potentially useful as a dielectric loss substrate. In the wave-absorbing application of graphene, the graphene is prepared by a freeze-drying method or a hydrothermal method, so that the porosity is improved, the structure of the graphene-based material is improved, and the wave-absorbing performance of the material is improved. In addition, magnetic metal, transition metal, their oxides, etc. are introduced to form a composite, such as Fe 3 O 4 /rGO、NiO/rGO、Co 3 O 4 The magnetic loss, the synergistic dielectric loss and the magnetic loss are introduced into the rGO and the like, and the method is an effective technical means for expanding the application frequency range and the application field of the graphene-based wave-absorbing material. The defect of electromagnetic matching of pure graphene can be overcome by compounding the magnetic substance with graphene, and the wave-absorbing performance of the composite material is improved by charge transfer between graphene interfaces and polarization relaxation of free carriers of graphene. However, the doped magnetic substance is easily agglomerated and unevenly distributed on the substrate, resulting in uneven material properties, and if the amount of the magnetic substance is increased for uniformity, the density may be increased due to an excessive amount of the filler, resulting in a subsequent process problem and loss of the original lightweight property. The wave-absorbing characteristic of the graphene-based composite material is mostly shown in that one or two strong absorption peaks exist in a higher frequency band such as 8-12 GHz or 12-18 GHz, so that the application range of the graphene-based composite material is limited.
Disclosure of Invention
Aiming at the defects of the graphene-based composite foam wave-absorbing material in the prior art, the invention aims to provide the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam, which has excellent wave-absorbing performance in a low-frequency S wave band and has the characteristic of light weight, and the density of the foam is as low as 0.001-1 g/cm 3 。
The second purpose of the invention is to provide a method for preparing the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam, which has the advantages of simple process flow and low cost.
In order to achieve the technical purpose, the invention provides a preparation method of light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam, which comprises the following steps:
1) Carrying out hydrothermal reaction on the nickel complex solution to obtain a nickel/nickel oxide complex;
2) Dispersing a nickel/nickel oxide compound and a raw material containing graphene into an alcohol/water mixed solution to obtain a suspension;
3) And sequentially carrying out freezing solidification, freezing drying and thermal reduction treatment on the suspension to obtain the composite material.
As a preferable embodiment, the nickel complex in the nickel complex solution is a complex formed by at least one of citric acid, citrate, ethylenediamine tetraacetic acid, ethylenediamine tetraacetate, glycine, glycinate, salicylic acid or salicylate and nickel ions. The concentration of nickel ions in the nickel complex solution is 1-50 g/L; the concentration of nickel ions in the nickel complex solution is preferably 20 to 40g/L. The nickel complex is obtained by reacting at least one complex of citric acid, sodium citrate, ethylene diamine tetraacetic acid, disodium ethylene diamine tetraacetic acid, glycine, sodium glycinate, salicylic acid and sodium salicylate with at least one nickel salt of nickel nitrate, nickel sulfate and nickel chloride according to the mass ratio of the complex to the nickel salt of 5-1.
As a preferred scheme, the conditions of the hydrothermal reaction are: reacting for 4-48 h at 120-240 ℃. The preferred hydrothermal reaction temperature is 150 to 210 ℃. The preferred hydrothermal reaction time is 8 to 18 hours.
As a preferable scheme, the raw material further comprises carbon nanotubes; the mass ratio of the carbon nanotubes to the graphene is (1). The mass ratio of the carbon nanotubes to the graphene is preferably 1. Preferred graphene is graphene oxide and/or reduced graphene oxide. Preferred carbon nanotubes are at least one of carboxylated or carbonylated carbon nanotubes, single-walled carbon nanotubes, or multi-walled carbon nanotubes. By introducing the carbon nano tubes, on one hand, the graphene composite foam structure can be better supported, and on the other hand, the dielectric property of the graphene composite foam is effectively enhanced by utilizing the lap joint formed by the slender carbon nano tubes between the lamellar graphene sheets. The amount and kind of the carbon nanotubes can be selected according to actual needs.
As a preferred scheme, the total mass ratio of the nickel/nickel oxide composite to the graphene and the carbon nanotubes is 5. The total mass ratio of the nickel/nickel oxide composite to the graphene and the carbon nanotube is preferably 2. If the mass ratio of the nickel/nickel oxide composite is too high, the formed foam is fragile, and if the mass ratio of the nickel/nickel oxide composite is too low, the suspension is liable to be delaminated, and it is difficult to obtain a uniform composite foam.
Preferably, the raw material further comprises an amine surfactant and/or a quaternary ammonium surfactant. The structural nickel/nickel oxide compound is subjected to surface treatment by using an amine surfactant and/or a quaternary ammonium surfactant, so that the surface of the structural nickel/nickel oxide compound is charged with cations, the dispersion of the structural nickel/nickel oxide compound is promoted, and the combination between the structural nickel/nickel oxide compound and graphene is strengthened.
As a preferable scheme, the mass of the amine surfactant and/or the quaternary ammonium surfactant is 1-5% of that of the structural nickel/nickel oxide composite; the amine surfactant is at least one of polyether amine and polyethyleneimine; the quaternary ammonium surfactant is at least one of polydiene dimethyl ammonium chloride and hexadecyl trimethyl ammonium bromide.
As a preferable scheme, the alcohol/water mixed solution is composed of an alcohol solvent and water according to a volume ratio of 30; the volume ratio of the alcohol solvent to water is 5; the alcohol solvent is at least one of methanol, ethanol, benzyl alcohol and glycol. When the volume ratio of the alcohol solvent to water is too low, the prepared nickel/nickel oxide assembled graphene-based composite foam is easy to crack; when the volume ratio of the alcohol solvent to water is too high, the prepared nickel/nickel oxide assembled graphene composite foam has large volume shrinkage.
As a preferred embodiment, the conditions for freezing and solidifying are as follows: the temperature is-86 ℃ to-48 ℃ and the time is 4-48 h.
As a preferred embodiment, the freeze-drying conditions are: the temperature is below minus 45 ℃, the vacuum degree is below 0.1Pa, and the time is 24-96 h;
as a preferable embodiment, the conditions of the thermal reduction treatment are: vacuum or nitrogen atmosphere is adopted, the temperature is 200-1000 ℃, and the time is 1-8 hours. The preferred temperature is 400 to 600 ℃. The preferred time is 2 to 4 hours.
The invention also provides the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam which is prepared by the preparation method.
As a preferred scheme, the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam has wave-absorbing performance in an S wave band, and the density is 0.001-1 g/cm 3 . The density of the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam is more preferably 0.01-0.1 g/cm 3 。
Compared with the prior art, the technical scheme of the invention has the following beneficial technical effects:
1) According to the light nickel/nickel oxide assembled graphene/carbon nanotube composite low-frequency wave-absorbing foam, nickel/nickel oxide in the graphene sheet layer is uniformly distributed and stacked to form a foam structure, so that anisotropy of the composite wave-absorbing foam material is effectively avoided. According to the invention, a proper amount of nickel/nickel oxide particles are doped into the graphene-based foam, so that the low-frequency wave-absorbing material meeting the requirements can be obtained.
2) The light nickel/nickel oxide assembled graphene/carbon nanotube composite low-frequency wave-absorbing foam has excellent wave-absorbing performance in a low-frequency S wave band, and the density is as low as 0.11g/cm 3 The following.
3) The preparation method of the light nickel/nickel oxide assembled graphene/carbon nanotube composite low-frequency wave-absorbing foam provided by the invention prevents magnetic particles from agglomerating by virtue of electrostatic action, realizes effective combination of nickel/nickel oxide particles and a graphene matrix, better maintains the density of the light composite wave-absorbing foam compared with metal particles, and produces a low-frequency wave-absorbing material as required by combining with a preparation process of composite foam.
4) The preparation process of the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam is simple in flow and low in cost, and is beneficial to large-scale production.
Drawings
Fig. 1 is an optical photograph of the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam.
Fig. 2 is an SEM electron micrograph of the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam.
Fig. 3 is an XRD of the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam.
Fig. 4 is a reflectivity curve of 2mm thickness of the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam prepared in example 1.
FIG. 5 is a reflectivity curve of 3.6mm in thickness of the lightweight nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam prepared in example 2.
Fig. 6 is a reflectivity curve of 3.6mm thickness of the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam prepared in example 3.
FIG. 7 is a reflectivity curve of 3.6mm thickness of the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam prepared in example 4.
FIG. 8 is a reflectivity curve of 3.6mm thickness of the lightweight nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam prepared in example 5.
Detailed Description
The following examples are intended to further illustrate the present disclosure, but not to limit the scope of the claims.
Example 1
1) 3.05g of disodium ethylene diamine tetraacetate, 5.25g of nickel nitrate hexahydrate, 15mL of methanol and 30mL of methanol aqueous solution of deionized water are mixed, and the mixture is subjected to high temperature and high pressure at 180 ℃ for 12 hours.
2) And (2) centrifuging, washing and vacuum drying the precipitate obtained in the step 1) at 60 ℃ for 12-18 h to obtain the nickel/nickel oxide compound.
3) And dispersing 400mg of graphene oxide and 400mg of nickel/nickel oxide compound into a mixed solution of 72mL of deionized water and 28mL of ethanol, carrying out ultrasonic treatment at 500W for 2.5h, and carrying out magnetic stirring for 2.5h to obtain a suspension.
4) The resulting suspension was poured into a quartz dish having an inner diameter of 190 × 10mm and a wall thickness of 2mm and four corners rounded off at φ =1mm, and the quartz dish was put into a refrigerator to be frozen and solidified at-85 ℃ for 12 hours, to obtain a frozen and solidified sample.
5) And putting the quartz capsule and the frozen and solidified sample into a freeze dryer, and carrying out freeze drying for 48 hours at the temperature of-60 ℃ and in the environment of 0.1Pa to obtain the nickel/nickel oxide assembled graphene oxide composite foam.
6) Putting the nickel/nickel oxide assembled graphene oxide composite foam into a box-type atmosphere furnace in N 2 Raising the temperature from room temperature to 600 ℃ at a speed of 5 ℃/min under protection, keeping the temperature at 600 ℃ for 2h, and then cooling to room temperature along with the furnace to obtain the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam as shown in figure 1, wherein figures 2 and 3 are SEM electron micrographs and XRD patterns of the obtained samples respectively, and the density of the samples is 0.084g/cm 3 。
The light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam prepared in the embodiment is mixed with 85% paraffin to prepare an annular mixture sample with an outer diameter of 7mm and an inner diameter of 3.04 mm. The coaxial method is adopted for testing, the vector network analyzer is used for measuring the electromagnetic parameters of the sample in the range of 2-18 GHz, and CST software is used for calculating the reflection loss condition of the composite wave-absorbing foam as shown in figure 4.
Example 2
1) 2.5g of sodium citrate, 5.8g of nickel nitrate hexahydrate, 30mL of ethanol and 30mL of deionized water are mixed, and hydrothermal reaction is carried out at 180 ℃ for 12h.
2) And (2) centrifugally washing the precipitate obtained in the step 1), and drying for 12-18 h at 60 ℃ in vacuum to obtain the nickel/nickel oxide compound.
3) And dispersing 400mg of graphene oxide and 400mg of nickel/nickel oxide compound into a mixed solution of 72mL of deionized water and 28mL of ethylene glycol, carrying out ultrasonic treatment at 500W for 2.5h, and carrying out magnetic stirring for 2.5h to obtain a suspension.
4) The resulting suspension was poured into a quartz dish having an inner diameter of 190 × 10mm and a wall thickness of 2mm, with four corners rounded off at phi =1mm, and the quartz dish was placed in a refrigerator and freeze-cured at-85 ℃ for 12 hours to obtain a freeze-cured sample.
5) And putting the quartz capsule and the frozen and solidified sample into a freeze dryer, and carrying out freeze drying for 48 hours at the temperature of-60 ℃ and in the environment of 0.1Pa to obtain the nickel/nickel oxide assembled graphene oxide composite foam.
6) Putting the nickel/nickel oxide assembled graphene oxide composite foam into a box-type atmosphere furnace in N 2 Rising from room temperature to 450 ℃ at a speed of 5 ℃/min under protection, andkeeping the temperature at 450 ℃ for 2h, and then cooling the mixture to room temperature along with the furnace to obtain the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam with the density of 0.098g/cm 3 。
The light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam prepared in the embodiment is mixed with 85% paraffin to prepare an annular mixture sample with an outer diameter of 7mm and an inner diameter of 3.04 mm. The coaxial method is adopted for testing, the vector network analyzer is used for measuring the electromagnetic parameters of the sample in the range of 2-18 GHz, and CST software is used for calculating the reflection loss condition of the composite wave-absorbing foam as shown in figure 5.
Example 3
1) 3.05g of disodium ethylene diamine tetraacetate, 5.25g of nickel nitrate hexahydrate, 15mL of methanol and 30mL of methanol aqueous solution of deionized water are mixed, and the mixture is subjected to high temperature and high pressure at 200 ℃ for 24 hours.
2) And (2) centrifugally washing the precipitate obtained in the step 1), and drying for 12-18 h at 60 ℃ in vacuum to obtain the nickel/nickel oxide compound.
3) Dissolving 1mg of polydiene dimethyl ammonium chloride into a mixed solution of 72mL of deionized water and 28mL of ethanol, taking 400mg of graphene oxide and 400mg of the nickel/nickel oxide compound obtained in the preparation step 2), dispersing the graphene oxide and the nickel/nickel oxide compound into the solution, carrying out ultrasonic treatment at 500W for 2.5h, and carrying out magnetic stirring for 2.5h to obtain a suspension.
4) The resulting suspension was poured into a quartz dish having an inner diameter of 190 × 10mm and a wall thickness of 2mm, with four corners rounded off at phi =1mm, and the quartz dish was placed in a refrigerator and freeze-cured at-85 ℃ for 12 hours to obtain a freeze-cured sample.
5) And putting the quartz capsule and the frozen and solidified sample into a freeze dryer, and carrying out freeze drying for 48 hours at the temperature of-60 ℃ and in the environment of 0.1Pa to obtain the nickel/nickel oxide assembled graphene oxide composite foam.
6) Putting the nickel/nickel oxide assembled graphene oxide composite foam into a box-type atmosphere furnace in N 2 Raising the temperature from room temperature to 600 ℃ at a speed of 5 ℃/min under protection, keeping the temperature at 600 ℃ for 4h, and then cooling to room temperature along with a furnace to obtain the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam with the density of 0.081g/cm 3 。
The light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam prepared in the embodiment is mixed with 85% paraffin to prepare an annular mixture sample with an outer diameter of 7mm and an inner diameter of 3.04 mm. The coaxial method is adopted for testing, the electromagnetic parameters of the sample in the range of 2-18 GHz are measured by a vector network analyzer, and the reflection loss condition of the composite wave-absorbing foam is calculated by using CST software and is shown in figure 6.
Example 4
1) 3.05g of disodium ethylene diamine tetraacetate, 5.25g of nickel nitrate hexahydrate, 15mL of methanol and 30mL of methanol aqueous solution of deionized water are mixed, and the mixture is subjected to high temperature and high pressure at 200 ℃ for 24 hours.
2) And (2) centrifugally washing the precipitate obtained in the step 1), and drying for 12-18 h at 60 ℃ in vacuum to obtain the nickel/nickel oxide compound.
3) And (3) dissolving 400mg of graphene oxide, 82mg of carboxylated multi-walled carbon nanotubes and 400mg of the nickel/nickel oxide compound obtained in the step 2) into a mixed solution of 72mL of deionized water and 28mL of absolute ethyl alcohol, carrying out 500W ultrasonic treatment for 2.5h, and carrying out magnetic stirring for 2.5h to obtain a suspension.
4) The resulting suspension was poured into a quartz dish having an inner diameter of 190 × 10mm and a wall thickness of 2mm, with four corners rounded off at phi =1mm, and the quartz dish was placed in a refrigerator and freeze-cured at-85 ℃ for 12 hours to obtain a freeze-cured sample.
5) And putting the quartz capsule and the frozen and solidified sample into a freeze dryer, and freeze-drying for 48 hours at-60 ℃ under the environment of 0.1Pa to obtain the nickel/nickel oxide assembled graphene oxide/carbon nano tube composite foam.
6) Putting the nickel/nickel oxide assembled graphene oxide/carbon nano tube composite foam into a box-type atmosphere furnace in N 2 Raising the temperature from room temperature to 600 ℃ at a speed of 5 ℃/min under protection, keeping the temperature at 600 ℃ for 2h, and then cooling to room temperature along with a furnace to obtain the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam with the density of 0.101g/cm 3 。
The light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam prepared in the embodiment is mixed with 85% paraffin to prepare an annular mixture sample with an outer diameter of 7mm and an inner diameter of 3.04 mm. The coaxial method is adopted for testing, the vector network analyzer is used for measuring the electromagnetic parameters of the sample in the range of 2-18 GHz, and CST software is used for calculating the reflection loss condition of the composite wave-absorbing foam, wherein the reflection loss is shown in figure 7.
Example 5
1) 3.05g of disodium ethylenediamine tetraacetate, 5.25g of nickel nitrate hexahydrate and 15mL of methanol are mixed with 30mL of methanol aqueous solution of deionized water, and the mixture is subjected to high temperature and high pressure at 200 ℃ for 24 hours.
2) And (2) centrifugally washing the precipitate obtained in the step 1), and drying for 12-18 h at 60 ℃ in vacuum to obtain the nickel/nickel oxide compound.
3) Dissolving 1mg of polydiene dimethyl ammonium chloride into a mixed solution of 72mL of deionized water and 28mL of absolute ethyl alcohol, taking 400mg of reduced graphene oxide, 82mg of single-walled carbon nanotube and 400mg of nickel/nickel oxide compound obtained in the preparation step 2), dispersing into the solution, carrying out ultrasonic treatment for 2.5h at 500W, and carrying out ball milling and mixing for 2.5h to obtain a suspension.
4) The resulting suspension was poured into a quartz dish having an inner diameter of 190 × 10mm and a wall thickness of 2mm, with four corners rounded off at phi =1mm, and the quartz dish was placed in a refrigerator and freeze-cured at-85 ℃ for 12 hours to obtain a freeze-cured sample.
5) And putting the quartz capsule and the frozen and solidified sample into a freeze dryer, and freeze-drying for 48 hours at-60 ℃ under the environment of 0.1Pa to obtain the nickel/nickel oxide assembled graphene oxide/carbon nano tube composite foam.
6) Putting the nickel/nickel oxide assembled graphene oxide/carbon nano tube composite foam into a box-type atmosphere furnace in N 2 Raising the temperature from room temperature to 600 ℃ at a speed of 5 ℃/min under protection, keeping the temperature at 600 ℃ for 2h, and then cooling to room temperature along with the furnace to obtain the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam with the density of 0.110g/cm 3 。
The light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam prepared in the embodiment is mixed with 85% paraffin to prepare an annular mixture sample with an outer diameter of 7mm and an inner diameter of 3.04 mm. The coaxial method is adopted for testing, the vector network analyzer is used for measuring the electromagnetic parameters of the sample in the range of 2-18 GHz, and CST software is used for calculating the reflection loss condition of the composite wave-absorbing foam as shown in figure 8.
Claims (8)
1. A preparation method of light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam is characterized by comprising the following steps: the method comprises the following steps:
1) Carrying out hydrothermal reaction on the nickel complex solution to obtain a nickel/nickel oxide compound;
2) Dispersing a nickel/nickel oxide compound and a raw material containing graphene into an alcohol/water mixed solution to obtain a suspension;
3) Sequentially carrying out freezing solidification, freeze drying and thermal reduction treatment on the suspension to obtain the material;
the raw material also comprises carbon nano tubes;
the mass ratio of the carbon nanotube to the graphene is 1;
the total mass ratio of the structural nickel/nickel oxide compound to the graphene and the carbon nanotube is (2);
the raw material also comprises an amine surfactant and/or a quaternary ammonium surfactant;
the alcohol/water mixed solution consists of an alcohol solvent and water according to a volume ratio of 30-1;
the freezing and solidifying conditions are as follows: the temperature is-86 ℃ to-48 ℃, and the time is 4-48 h.
2. The preparation method of the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam according to claim 1, characterized by comprising the following steps: the nickel complex in the nickel complex solution is a complex formed by at least one of citric acid, citrate, ethylenediamine tetraacetic acid salt, glycine, glycinate, salicylic acid or salicylate and nickel ions.
3. The preparation method of the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam according to claim 1, characterized by comprising the following steps: the conditions of the hydrothermal reaction are as follows: reacting for 4-48 h at 120-240 ℃.
4. The preparation method of the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam according to claim 1, characterized by comprising the following steps: the mass of the amine surfactant and/or the quaternary ammonium surfactant is 1-5% of that of the structural nickel/nickel oxide composite; the amine surfactant is at least one of polyether amine and polyethyleneimine; the quaternary ammonium surfactant is at least one of polydiene dimethyl ammonium chloride and hexadecyl trimethyl ammonium bromide.
5. The preparation method of the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam according to claim 1, characterized by comprising the following steps: the alcohol solvent is at least one of methanol, ethanol, benzyl alcohol and glycol.
6. The preparation method of the light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam according to claim 1, characterized by comprising the following steps:
the conditions of freeze drying are as follows: the temperature is below minus 45 ℃, the vacuum degree is below 0.1Pa, and the time is 24-96 h;
the conditions of the thermal reduction treatment are as follows: vacuum or nitrogen atmosphere is adopted, the temperature is 200-1000 ℃, and the time is 1-5 hours.
7. A light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam is characterized in that: obtained by the production method according to any one of claims 1 to 6.
8. The light nickel/nickel oxide assembled graphene-based composite low-frequency wave-absorbing foam obtained according to claim 7 is characterized in that: has wave absorbing performance in S wave band and density of 0.001-1 g/cm 3 。
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