CN109054741A - Sandwich structure cobalt-nickel alloy particle/reduced graphene composite material preparation method - Google Patents
Sandwich structure cobalt-nickel alloy particle/reduced graphene composite material preparation method Download PDFInfo
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- CN109054741A CN109054741A CN201810695289.1A CN201810695289A CN109054741A CN 109054741 A CN109054741 A CN 109054741A CN 201810695289 A CN201810695289 A CN 201810695289A CN 109054741 A CN109054741 A CN 109054741A
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Abstract
The invention belongs to nano-functional material technical fields, specially sandwich structure cobalt-nickel alloy particle/reduced graphene composite material preparation method.The present invention selects graphene oxide as the carbon-based of cobalt nickel ion chelating growth, by changing chelating agent, PH regulator type and Concentration of precursor solution size, obtained size are distributed as 0.2 μm -- 1.2 μm of cobalt-nickel alloy particle, and chelate the surface for being scattered in reduced graphene；Again by subsequent freeze-drying process, the cobalt-nickel alloy with sandwich structure/reduced graphene composite material is obtained.The composite material shows excellent drain performance in field of microwave absorption, especially when the cobalt-nickel alloy particle mean size dispersed in compound 0.8 μm when, its maximum lossy microwave can reach -54.4dB (secondary microwave absorption peak is -45.4dB), bandwidth is up to 4 GHz, as the novel wave-absorbing material of microwave absorption, have broad application prospects.
Description
Technical field
The invention belongs to technical field of compound preparation, and in particular to a kind of adjustable cobalt nickel conjunction of the large scale of sandwich-like
Gold particle/reduced graphene compound preparation method and its application in field of microwave absorption.
Background technique
Since modern age, the information science of fast development facilitates the life of the mankind, while also promoting a large amount of electronic section
Birth of skill product, such as Web TV, mobile phone, 3G/4G, wireless network etc..It is raw that electromagnetic technique is already applied to human society
Every field in work, wherein mostly important is no more than its application in national defense safety, military project development field.But just
It is since it is extensive universal, they also bring very severe electromagnetic pollution problem[1].Electromagnetic wave is as a kind of high energy
Grain beam all generates serious influence to the health of the mankind and environment, electromagnetic interference phenomenon in our human societies already repeatly
See not fresh.Moreover, the appearance of stealth material has highly important strategic importance for the national defence of each country.Various reasons are compeled
So that global scientists have started the research boom of one absorbing material.Absorbing material refers to that those can absorb electricity
Magnetic wave simultaneously converts it into other forms energy (mainly thermal energy) and the unreflected material of milli[2].Nano material is due to its size
It is small arrived to a certain degree after, quantum size effect, tunnel-effect, small-size effect and Dielectric confinement effect etc. cause material
Expect the destruction of periodic boundary condition itself, so that nano material has much different from conventional material series characteristic and performance,
Such as: its physical property (acousto-optic electromagnetism and thermodynamic behaviour) occurs significantly to change with the reduction of size[3-5].Another party
Face, the specific surface area of the nanoparticle material 3-4 order of magnitude bigger than conventional coarse powder, also compares the absorptivity of infrared light and electromagnetic wave
Conventional material is much bigger, this allows for the reflected signal strength that infrared detector and radar obtain and is greatly lowered, therefore is difficult to send out
Now detection target plays the role of stealthy.Nano material has become one of most potential absorbing material[6-9]。
Generally, absorbing material can be divided into two classes: magnetic loss consumptive material to electromagnetic wave loss mechanism according to material by us
Material and dielectric loss material.Magnetic loss consumption material refers to transition metal (cobalt, iron, nickel) and its oxide, such as: four oxidations three
Iron, cobalt-nickel alloy etc.[10]；Dielectric material refers to carbon nanotube, molybdenum disulfide, titanium dioxide etc..They are to electromagnetic wave
Has good absorbability[11].It is pure but according to electric wire transmission principle it is found that due to being easier to be unsatisfactory for matching principle
Magnetic material or pure dielectric material bottleneck is always existed to the absorbent properties of electromagnetic wave: absorption intensity is small, absorb frequency
With narrow.Many scholars begin trying dielectric material and magnetic loss consumption material combining carry out matching impedance, using they
Synergistic effect is to reach the strong absorption to electromagnetic wave, for example, the Che Renchao seminar of Fudan University utilizes magnetic material ferroso-ferric oxide,
Cobalt-nickel alloy and various dielectric materials (titanium dioxide, manganese dioxide etc.), which combine, to be inhaled wave and has got very superior
Suction wave drain performance, solve the problems, such as that single component material wave-sucking performance is not strong.Although currently, having been reported that the cobalt nickel of small size
The problems such as alloy and graphene oxide, which chelate, carries out suction wave, but its dispersibility is poor, and absorbing property is general, and absorption band is narrow equal
It is seriously limited in the application in the field.Based on this, the present invention has a series of large scale cobalt-nickel alloys of sandwich structure
Particle/reduced graphene compound is made.By change magnetic-particle size, the saturation magnetization of compound,
Electromagnetic parameter and internal structure become adjustable, preferably absorb to reach to electromagnetic wave.Wherein, cobalt-nickel alloy provides strong magnetic
Loss (the effect of magnetic couplings caused by highdensity cobalt-nickel alloy particle；Irreversible domain motion；Magnetic resonance；Natural resonance；
Magnetoimpedance behavior etc. caused by magnetism), graphene provides dielectric loss, and (there is the different molecules of serial polarizability；Function
There are dipole polarizations for group's orientation；There are dipole relaxation processes for dipole；Interface is too many between cobalt nickel metal and graphene,
There are interfacial polarizations；There are built-in potentials to cause resistance loss, eddy-current loss for the electron accumulation state sequence of reduced graphene interlayer；
Simultaneously graphene due in reduction process existing defects can also cause dipole or resistance loss etc.).The compound is almost
Meet simultaneously and required greatly as the four of microwave absorbing material, and its synthesis is simple, cost is very low.
Summary of the invention
It is compound it is an object of the invention to make up reported extra small and single size cobalt-nickel alloy and graphene chelating
The defect that object is applied in field of microwave absorption, such as structure are at random[13], particle agglomeration[14], performance is poor[14]Deng providing one kind
Cobalt-nickel alloy particle/reduced graphene composite material preparation side of the adjustable submicron order of large scale with sandwich structure
Method.
Cobalt-nickel alloy particle/reduced graphene composite material preparation method of sandwich structure provided by the invention is led to
The type for changing simultaneously PH regulator, chelating agent is crossed, and adjusts Concentration of precursor solution, to change the cobalt-nickel alloy particle ruler of load
Very little, the average grain diameter of cobalt-nickel alloy is controlled at 0.2 ~ 1.2 μm in preparation-obtained composite material.Specific steps are as follows:
(1) firstly, by the graphene oxide ultrasonic disperse of 40 ± 3 mg in 20 ± 3 mL ethylene glycol, ultrasonic time is 30 ± 5
Min, is added the cobalt acetate of 0.05 ± 0.03 g, and stirring and dissolving adds the nickel acetate of 0.2 ± 0.08 g and stirring, keeps its molten
Solution obtains solution A；
(2) 20 ± 3 mL ethylene glycol solutions for having dissolved 0.12 ± 0.05 g citric acid are slowly added dropwise into solution A；Slowly drop
The speed of liquid feeding body is 8-15 seconds/drop, then by the above solution ultrasound 40 ± 5 minutes, obtains reaction solution；
(3) above-mentioned reaction solution is transferred in reaction kettle, is heated to 210 ± 10 DEG C, react 12-15 h；It is cooling to water heating kettle
Afterwards, it is washed for several times and is centrifugated with deionized water and dehydrated alcohol, it is compound to obtain thick cobalt nickel/reduced graphene
Object；
(4) compound obtained in step (3) is placed in the deionized water of 20 ± 10 mL, and cold dry using freeze drier
24 ± 1 h finally obtain cobalt-nickel alloy particle/reduced graphene compound with sandwich structure.
It generally, is 0.2-0.6 μm according to the average grain diameter of cobalt-nickel alloy particle in compound obtained by above step.
The present invention is further, step (2) is replaced are as follows: (2) be slowly added dropwise into solution A and dissolved 0.12 ± 0.05 g
20 ± 3 mL diglycol solution of sodium hydroxide；The speed that liquid is slowly added dropwise is 8-15 seconds/drop, then will be above molten
Liquid ultrasound 40 ± 5 minutes, obtain reaction solution, other steps are identical, finally obtain the cobalt-nickel alloy particle with sandwich structure/
Reduced graphene compound.
Generally, thus the average grain diameter of cobalt-nickel alloy particle is 0.3-0.6 μm in gained compound.
The present invention is further, step (2) is replaced are as follows: (2) be slowly added dropwise into solution A and dissolved 0.12 ± 0.05 g
20 ± 3 mL ethylene glycol solutions；The speed that liquid is slowly added dropwise is 8-15 seconds/drop, then by 40 ± 5 points of the above solution ultrasound
Clock obtains reaction solution, other steps are identical, and it is multiple to finally obtain cobalt-nickel alloy particle/reduced graphene with sandwich structure
Close object.
Generally, thus the average grain diameter of cobalt-nickel alloy particle is 0.8 ~ 1.2 μm in gained compound.
Preparation method of the present invention obtains the cobalt-nickel alloy particle/reduced graphene composite material with sandwich structure, bears
The cobalt-nickel alloy particle size of load is adjustable.By changing PH regulator citric acid, chelating agent diglycol and variation forerunner
Liquid concentration, the average grain diameter for preparing resulting cobalt-nickel alloy is 0.2 μm -- 1.2 μm (such as respectively 0.2 μm, 0.5 μm, 0.8
μm, 1.2 μm).
The present invention can make the saturation magnetization of compound by changing the size of magnetic-particle, electromagnetic parameter and
Internal structure becomes adjustable, preferably absorbs to reach to electromagnetic wave.Wherein, it is (highly dense to provide strong magnetic loss for cobalt-nickel alloy
The effect of magnetic couplings caused by the cobalt-nickel alloy particle of degree；Irreversible domain motion；Magnetic resonance；Natural resonance；Magnetism causes
Magnetoimpedance behavior etc.), graphene provides dielectric loss, and (there is the different molecules of serial polarizability；Arrangement side of functional group
To there are dipole polarizations；There are dipole relaxation processes for dipole；Interface is too many between cobalt nickel metal and graphene, and there are interfaces
Polarization；There are built-in potentials to cause resistance loss, eddy-current loss for the electron accumulation state sequence of reduced graphene interlayer；Graphite simultaneously
Alkene due in reduction process existing defects can also cause dipole or resistance loss etc.).The compound almost meets simultaneously
Four as microwave absorbing material require greatly, and its synthesis is simple, and cost is very low.
In particular, when the cobalt-nickel alloy particle mean size dispersed in compound 0.8 μm when, maximum microwave damage
Consumption can reach -54.4 dB (secondary microwave absorption peak is -45.4 dB), and bandwidth is up to 4 GHz, the suction wave material as microwave absorption
Material, effect are more preferable.
The cobalt-nickel alloy of sandwich structure prepared by the present invention/reduced graphene composite material can be used for microwave absorption, tool
Body step are as follows: by adjustable large scale cobalt-nickel alloy particle/reduced graphene compound with 1:6(compound: paraffin) quality point
Number is dispersed in paraffin, is subsequently poured into aluminum template, and being pressed into interior is 3 mm, and outer diameter is sample of 7 mm with a thickness of 2 mm,
It is put into the reflection loss that sample is measured in network vector instrument later.
It is characterized using scanning electron microscope (1 kV of SEM, Hitachi FE-SEM S-4800 operated at)
Its morphology and size；Utilize transmitted electron Electronic Speculum (200 kV of TEM, JEOL JEM-2100F operated at), constituency electricity
Sub- diffraction (SAED), energy loss spectroscopy (EDS) and Microstructure Information characterization.X- difraction spectrum is in Bruker D8 X-
ray diffractometer (Germany) with Ni-filtere Cu KR radiation operated at 40
It is measured on kV and40 mA.
A series of size adjustable cobalt-nickel alloy particles with sandwich structure of the invention/reduced graphene compound is used
It is good absorption effect, at low cost in microwave absorption or electromagnetic shielding device.
Detailed description of the invention
Fig. 1 a-d is that graphene oxide other conditions are being not added under the same conditions, is by what one step hydro thermal method synthesized
Arrange the cobalt-nickel alloy low power SEM figure of different size distributions.
Fig. 2 a-d is the size adjustable cobalt-nickel alloy particle/reduced graphene compound rGO/ with sandwich structure
CN4The low power electron scanning photo (SEM) of-x, it can be seen that serial compound has graphene/CoNi4/ graphene/CoNi4It is more
Layer arranges laminating sandwich structure.
Fig. 3 is size adjustable cobalt-nickel alloy particle/reduced graphene compound rGO/CN with sandwich structure4- x's
X-ray diffraction (XRD) figure, more can accurately reflect the information such as the crystal phase, purity, crystallinity of product.
Fig. 4 is size adjustable cobalt-nickel alloy particle/reduced graphene compound rGO/CN with sandwich structure4- x exists
The characterization of magnetic property when 300 K.It can reflect fully aware ofly: with the increase of cobalt-nickel alloy particle size, he
Magnetic property also accordingly changed.
Fig. 5 is size adjustable cobalt-nickel alloy particle/reduced graphene compound rGO/CN with sandwich structure4- x exists
Maximum reflection loss curve, abscissa represent wave frequency under respective thickness, and ordinate represents reflection loss.
Specific embodiment
Embodiment 1:
(1) with size adjustable cobalt-nickel alloy particle/reduced graphene compound rGO/CN of sandwich structure4- 0.2:
Firstly, at room temperature, by the graphene oxide ultrasonic disperse of 40 mg in 20 mL ethylene glycol, ultrasonic time 30
Then min is separately added into the cobalt acetate of 0.05 g and the nickel acetate of 0.2 g in order and dissolves respectively, is slowly added dropwise later molten
The 20 mL ethylene glycol (the aobvious acidity of PH) of the citric acid of 0.125 g are solved, rate of addition is 10 seconds/drop.The above solution is poured into instead
It answers in kettle, is heated to 210 DEG C, react 13 h；
After water heating kettle is cooling, after being washed for several times with deionized water and dehydrated alcohol, centrifuge separation, later in freeze drier
It is done for 24 hours cold, finally obtaining the particle mean size with sandwich structure is 0.2 μm of cobalt-nickel alloy particle/reduced graphene
Compound rGO/CN4-0.2。
Embodiment 2:
(2) with size adjustable cobalt-nickel alloy particle/reduced graphene compound rGO/CN of sandwich structure4- 0.5 conjunction
At:
Firstly, at room temperature, by the graphene oxide ultrasonic disperse of 40 mg in mono- contracting second two of 10 mL ethylene glycol and 10 mL
In alcohol, ultrasonic time is 30 min, is then separately added into the cobalt acetate of 0.05 g and the nickel acetate of 0.2 g in order and difference is molten
Solution, is slowly added dropwise the 10 mL ethylene glycol for having dissolved 0.12 g sodium hydroxide and 10 mL diethylene glycol mixed solution (PH later
Aobvious alkalinity), rate of addition is 10 seconds/drop.The above solution is poured into reaction kettle, is heated to 210 DEG C, reacts 13 h；
After water heating kettle is cooling, after being washed for several times with deionized water and dehydrated alcohol, centrifuge separation, later in freeze drier
In cold dry 24 h, the average particle size particle size with sandwich structure is finally obtained about in 0.5 μm or so of cobalt-nickel alloy
Grain/reduced graphene compound rGO/CN4- 0.5 compound.
Embodiment 3:
(3) with size adjustable cobalt-nickel alloy particle/reduced graphene compound rGO/CN of sandwich structure4- 0.8 conjunction
At:
Firstly, at room temperature, by the graphene oxide ultrasonic disperse of 40 mg in 20 mL ethylene glycol, ultrasonic time 30
Then min is separately added into the cobalt acetate of 0.02 g and the nickel acetate of 0.08 g in order and dissolves respectively, is slowly added dropwise later molten
The 20 mL ethylene glycol (the aobvious alkalinity of PH) of the sodium hydroxide of 0.12 g are solved, rate of addition is 10 seconds/drop.The above solution is poured into
In reaction kettle, 210 DEG C are heated to, reacts 13 h；
After water heating kettle is cooling, after being washed for several times with deionized water and dehydrated alcohol, centrifuge separation, later in freeze drier
In cold dry 24 h, the average particle size particle size with sandwich structure is finally obtained about in 0.8 μm of cobalt-nickel alloy particle/reduction
Graphene complex rGO/CN4-0.8。
Embodiment 4:
(3) with size adjustable cobalt-nickel alloy particle/reduced graphene compound rGO/CN of sandwich structure4- 1.2 conjunction
At:
Firstly, at room temperature, by the graphene oxide ultrasonic disperse of 40 mg in 20 mL ethylene glycol, ultrasonic time 30
Then min is separately added into the cobalt acetate of 0.05 g and the nickel acetate of 0.2 g in order and dissolves respectively, is slowly added dropwise later molten
The 20 mL ethylene glycol (the aobvious alkalinity of PH) of the sodium hydroxide of 0.12 g are solved, rate of addition is 10 seconds/drop.The above solution is poured into
In reaction kettle, 210 DEG C are heated to, reacts 13 h；
After water heating kettle is cooling, after being washed for several times with deionized water and dehydrated alcohol, centrifuge separation, later in freeze drier
In cold dry 24 h, cobalt-nickel alloy particle/reduced graphene of the particle size with sandwich structure about at 1.2 μm is compound
Object rGO/CN4-1.2。
Size adjustable cobalt-nickel alloy particle/reduced graphene compound rGO/CN with sandwich structure4The synthesis of-x
Morphology and size be by scanning electron microscope (1 kV of SEM, Hitachi FE-SEM S-4800 operated at)
It is directly the sample powder of drying to be sprinkled upon on conducting resinl to make come what is characterized.The selective electron diffraction of compound series
(SAED), energy loss spectroscopy (EDS) and Microstructure Information are by transmitted electron Electronic Speculum (TEM, JEOL JEM-2100F
200 kV of operated at) come what is characterized, the sample of transmission electron microscope is by graphene/CoNi4/ graphene/CoNi4@stone
The laminated composites that black alkene multilayer arrangement is covered are dispersed in ethanol solution, are then added dropwise on 6 μ L solution to carbon support copper mesh
Production.X- difraction spectrum is in BrukerD8 X-ray diffractometer (Germany) with Ni-filtere
It is measured on 40 kV and of Cu KR radiation operated at, 40 mA.
Fig. 1 a-d be by one step hydro thermal method synthesize serial cobalt nickel particle size low power SEM figure, wherein a figure be for
It is the cobalt nickel particle of PH regulator hydrothermal synthesis using citric acid, average-size is 0.2 μm or so；If added with half
Reduction solvent is diglycol, and the cobalt nickel that uniform particle sizes are distributed in 0.5 μm or so can be synthesized by us, such as schemes b；Accordingly
0.8 μm or so of cobalt nickel also can be obtained in the content of reduction cobalt acetate and nickel acetate, such as schemes c；D figure is cobalt acetate and nickel acetate is
0.05:0.2 when, 1.2 μm or so of cobalt nickel being synthesized using ethylene glycol as solvent.From a-d figure, it can be seen that closing
The CoNi being distributed at different sizes4Alloying pellet is uniform in size, and size distribution is preferable.
Fig. 2 is size adjustable cobalt-nickel alloy particle/reduced graphene compound low power SEM with sandwich structure
Figure.Wherein, (a) can be seen that, in rGO/CN4In -0.2 compound, 0.2 μm or so of cobalt-nickel alloy particle is fully wrapped up
The inside of reduced graphene layer, particle diameter distribution is preferable, but clustering phenomena is serious.The marginal portion of compound is buckle condition
Graphene, surface curve is more, and this structure can increase the scattering of electromagnetic wave, is conducive to the absorption of electromagnetic wave；(b) multiple in
Close object rGO/CN4- 0.5 pattern, it preferably illustrates the sandwich structure of compound: being specially the cobalt nickel of 0.5 μ m in size
For even particulate dispersion in fold graphene, layer and layer distribution are apparent；(c) compound rGO/CN is then illustrated4-0.8
Microscopic appearance, show with size increase its sandwich the available intact reservation of structure；But work as alloying pellet
When size increases to 1.2 μm, due to its strong magnetic action, special sandwich structure can be by partial destruction, and alloying pellet
Start to reunite on the surface layer of reduced graphene (such as figure D compound rGO/CN4- 1.2 pattern is shown).
Fig. 3 is size adjustable cobalt-nickel alloy particle/reduced graphene compound X-ray diffraction with sandwich structure
(XRD) figure.XDR more can accurately reflect the information such as the crystal phase, purity, crystallinity of product.Respectively with serial face in figure
The curve of color presents cobalt-nickel alloy, graphene oxide, adjustable large scale cobalt-nickel alloy particle/reduction with sandwich structure
The XRD curve of graphene complex.Then it can be seen that adjustable large scale cobalt-nickel alloy particle/reduction with sandwich structure
Graphene complex is 44.5o, 51.8o, 76.7oOccurring three strongest peak respectively, the XRD diffraction maximum of this and cobalt-nickel alloy is consistent,
Its (111) for corresponding respectively to face-centred cubic structure cobalt-nickel alloy, (200), (220) face.Since the peak of pure graphene is located at
10.2o, the peak of pure reduced graphene is located at 27.6o, however, combination product has occurred faint therebetween intensity peak, this
It demonstrates only to be partially reduced with radical oxidation graphene and becomes reduced graphene, order is only broken by part
Bad, order degree is retained.Moreover, we can with it is conjectured that: during the reaction, Co2+And Ni2+It can be with oxidation stone
Catalysis reaction occurs for black alkene, can also to be that degree of graphitization is higher.Generally speaking, XRD diagram is demonstrating compound substance just
True property, and and have the generation of impurity.
Fig. 4 is size adjustable cobalt-nickel alloy particle/reduced graphene compound rGO/CN with sandwich structure4- x exists
The characterization of magnetic property when 300 K.The rGO/CN it can be seen from (c)4The hysteresis loop of-x series all shows the shape of S,
This illustrates that cobalt-nickel alloy successfully loads so that compound has the corresponding ferromagnetic characteristic of cobalt-nickel alloy.Moreover, from (d)
(local magnetic field strength enlarged drawing) is as can be seen that rGO/CN4The hysteresis loop of the compound of-x series has different areas,
And the increase of the size with cobalt-nickel alloy particle, saturation magnetization are sequentially increased.Since the change of particle size causes
Compound has a different Dielectric behaviors, Magnetic behavior and possesses different structure features, because the series compound shows
Very excellent adjustable microwave absorbing property is gone out.It is compound to carry out controllable adjustment by the size of alloying pellet size for this explanation
The microwave absorbing property of object material.
Fig. 5 is size adjustable cobalt-nickel alloy particle/reduced graphene compound rGO/CN with sandwich structure4- x exists
Reflection loss curve under respective thickness.Wherein, compound rGO/CN4- 0.2 when with a thickness of 2 mm its maximum reflection damage
Losing is -15.04 dB；Compound rGO/CN4- 0.5 in 2.5 mm of thickness of sample, and maximum reflection loss is -34.98 dB；
Compound rGO/CN4- 0.8 in 3.5 mm of thickness of sample, and maximum reflection loss is -54.44 dB；Compound rGO/CN4-
1.2 in 2.5 mm of thickness of sample, and maximum reflection loss is -24.38 dB.With pure graphene or pure CoNi4Alloy
The maximum reflection loss of particle is compared, compound rGO/CN4- x series meets low thickness simultaneously, and wideband is strong to absorb, and density is low
Etc. require.Moreover, compound rGO/CN4- 0.8 in 3.5 mm of thickness of sample, and maximum reflection loss is -54.44 dB,
Ability to electromagnetic wave loss is several times of many conventional absorbing materials.
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Claims (5)
1. a kind of cobalt-nickel alloy particle/reduced graphene composite material preparation method of sandwich structure, which is characterized in that logical
The type for changing simultaneously PH regulator, chelating agent is crossed, and adjusts Concentration of precursor solution, to change the cobalt-nickel alloy particle ruler of load
It is very little；The specific steps of preparation are as follows:
(1) firstly, by the graphene oxide ultrasonic disperse of 40 ± 3 mg in 20 ± 3 mL ethylene glycol, ultrasonic time is 30 ± 5
Min, is added the cobalt acetate of 0.05 ± 0.03 g, and stirring and dissolving adds the nickel acetate of 0.2 ± 0.08 g and stirring, keeps its molten
Solution obtains solution A；
(2) 20 ± 3 mL ethylene glycol solutions for having dissolved 0.12 ± 0.05 g citric acid are added dropwise into solution A；Liquid is added dropwise
Speed is 8-15 seconds/drop, then by the above solution ultrasound 40 ± 5 minutes, obtains reaction solution；
(3) above-mentioned reaction solution is transferred in reaction kettle, is heated to 210 ± 10 DEG C, react 12-15 h；It is cooling to water heating kettle
Afterwards, it is washed for several times and is centrifugated with deionized water and dehydrated alcohol, it is compound to obtain thick cobalt nickel/reduced graphene
Object；
(4) compound obtained in step (3) is placed in the deionized water of 20 ± 10 mL, and cold dry using freeze drier
24 ± 1 h finally obtain cobalt-nickel alloy particle/reduced graphene compound with sandwich structure.
2. preparation method according to claim 1, which is characterized in that replace step (2) are as follows: be added dropwise into solution A molten
20 ± 3 mL diglycol solution of 0.12 ± 0.05 g sodium hydroxide are solved；Be added dropwise liquid speed be 8-15 seconds/
Drop obtains reaction solution then by the above solution ultrasound 40 ± 5 minutes；Other steps are identical, finally obtain with sandwich structure
Cobalt-nickel alloy particle/reduced graphene compound.
3. preparation method according to claim 1, which is characterized in that replace step (2) are as follows: be added dropwise into solution A molten
20 ± 3 mL ethylene glycol solutions of 0.12 ± 0.05 g are solved；The speed that liquid is added dropwise is 8-15 seconds/drop, then will be above molten
Liquid ultrasound 40 ± 5 minutes, reaction solution is obtained, other steps are identical, finally obtain the cobalt nickel Nanoalloy with sandwich structure
Particle/reduced graphene compound.
4. the cobalt-nickel alloy particle/reduced graphene for the sandwich structure that the preparation method as described in one of claim 1-3 obtains
Composite material.
5. cobalt-nickel alloy particle/reduced graphene composite material with sandwich structure is in microwave as claimed in claim 4
Application in absorption field.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN113015422A (en) * | 2021-02-22 | 2021-06-22 | 山东大学 | Cobalt-nickel alloy/reduced graphene oxide nanocomposite for shielding high-frequency electromagnetic waves, and preparation method and application thereof |
| CN114032067A (en) * | 2021-12-03 | 2022-02-11 | 中国海洋大学 | CoFe @ C/rGO electromagnetic wave absorption composite material and preparation method thereof |
| CN114957855A (en) * | 2022-06-10 | 2022-08-30 | 南京航空航天大学 | Wave-absorbing heat-conducting thermoplastic composite material and preparation method thereof |
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| CN103117389A (en) * | 2013-01-25 | 2013-05-22 | 浙江大学 | Nickel-cobalt oxide/graphene composite material as well as preparation method and application thereof |
| CN105295832A (en) * | 2014-07-25 | 2016-02-03 | 南京理工大学 | Preparation method for reduced graphene oxide/Ni-Co ternary composite wave-absorbing material |
| CN105390676A (en) * | 2015-11-02 | 2016-03-09 | 北京师范大学 | Quick preparation method for graphene base metal or metal oxide with sandwich structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103117389A (en) * | 2013-01-25 | 2013-05-22 | 浙江大学 | Nickel-cobalt oxide/graphene composite material as well as preparation method and application thereof |
| CN105295832A (en) * | 2014-07-25 | 2016-02-03 | 南京理工大学 | Preparation method for reduced graphene oxide/Ni-Co ternary composite wave-absorbing material |
| CN105390676A (en) * | 2015-11-02 | 2016-03-09 | 北京师范大学 | Quick preparation method for graphene base metal or metal oxide with sandwich structure |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113015422A (en) * | 2021-02-22 | 2021-06-22 | 山东大学 | Cobalt-nickel alloy/reduced graphene oxide nanocomposite for shielding high-frequency electromagnetic waves, and preparation method and application thereof |
| CN114032067A (en) * | 2021-12-03 | 2022-02-11 | 中国海洋大学 | CoFe @ C/rGO electromagnetic wave absorption composite material and preparation method thereof |
| CN114957855A (en) * | 2022-06-10 | 2022-08-30 | 南京航空航天大学 | Wave-absorbing heat-conducting thermoplastic composite material and preparation method thereof |
| CN114957855B (en) * | 2022-06-10 | 2023-02-03 | 南京航空航天大学 | Wave-absorbing heat-conducting thermoplastic composite material and preparation method thereof |
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