CN106479433A - A kind of Graphene composite wave-suction material and preparation method thereof - Google Patents
A kind of Graphene composite wave-suction material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to microwave absorption technique field is and in particular to a kind of Graphene composite wave-suction material and preparation method thereof, described Graphene composite wave-suction material is composited by carbonyl iron and graphene uniform.This preparation method prepares graphite oxide first with improving Hummers method, then graphite oxide is dispersed in carbonyl iron dispersion liquid；Then recycle ultrasonic reducing process that graphite oxide is reduced into Graphene, prepared Graphene composite wave-suction material., with respect to simple carbonyl iron and simple Graphene, its absorbing property is superior for the composite wave-suction material of the present invention, and suction intensity of wave is high, suction wave frequency bandwidth, density are less；It is also equipped with Modulatory character, realize the high-selenium corn under different frequency by adjusting Graphene with the mass ratio of carbonyl iron and thickness of composite material.
Description
Technical field
The present invention relates to microwave absorption technique field is and in particular to a kind of Graphene composite wave-suction material and its preparation side
Method.
Background technology
With the development of radar, microwave communication techniques, particularly wireless communication tool, internet and other communication equipments
Use in gigahertz range, people increasingly rise to the concern of electromagnetic interference and electromagnetic compatibility.Therefore, research has height
The demand of the electromagnetic shielding material of absorbability and broadband absorption is increasingly urgent.At present, absorbing material is not only extensively applied
In the stealthy field of military radar, and also there are a lot of applications in civil area, such as microwave dark room material, microwave attenuation unit device
Part, electromagnetic compatibility, microwave forming processing technology etc..Enter 21st century, with scientific and technological progress and innovation, and military war
The continuous improvement of the demand of omiting is it is desirable to new absorbing material has the characteristics that " thin, light, wide, strong ".
Magnetic metal material（As the metals such as Fe, Co, Ni and its alloy）, there is saturation magnetization height, pcrmeability and Jie
The advantages of electric constant is big, Curie temperature is high, temperature stability is good, is the important rubber-ferrite agent of a class.Inhale in magnetic metal
In wave material, because carbonyl iron dust has in microwave frequency band, pcrmeability is higher, pcrmeability real part, imaginary part Dispersion are good, low
Stronger absorbing property can be obtained under the conditions of matching thickness and be widely used.Magnetic metal absorbing material relies primarily on magnetic hysteresis
The mechanism such as loss, eddy-current loss, domain wall resonance and natural resonance are decaying and electromagnetic wave absorption.Typically can be by changing magnetic gold
Belong to structure（Lamellar, Fiber Aspect Ratio, needle-like whisker）Adjust its pcrmeability and dielectric constant, in wide frequency range, microwave is realized
High-selenium corn.Magnetic metal absorbing material there is also some shortcomings simultaneously, and such as electrical conductivity is high, corrosion resistance is low, density is big etc..
Graphene makes it have and is different from the special of other material with carbon elements as a kind of new carbon, unique single layer structure
Physicochemical properties, for study new carbon-based electromagnetic wave absorbent material bring new opportunities and challenges.Graphene has matter
The excellent properties such as gently, specific surface area is big, good conductivity and dielectric constant height.The graphenic surface of chemical method preparation exists a large amount of
Defect（Including marginality, topological defect, hole etc.）With the oxygen-containing functional group of residual, the localization of fermi level can be produced
State；There is the dielectric relaxor of outer-shell electron in the chemical bond energy simultaneously exposing to the open air on graphene sheet layer outside under electromagnetic field effect, from
And absorb and decay electromagnetic wave, in electromagnetic wave absorption field, there is potential using value.As other material with carbon elements, Graphene is made
It is that there is no magnetic and magnetic loss for the maximum shortcoming of electromagnetic wave absorbent material, but the huge specific surface area of Graphene is entered for it
Row functionalization is combined and provides unlimited possibility.
Traditional single absorbing material（Ferrite, carbon-based material, ultra-fine magnetic metallic powder, ceramic material etc.）Although inhaling
Wave energy power is strong, but density is generally large or absorption band is narrow it is difficult to have both simultaneously strong absorption, density little with wide suction wave frequency
The advantages of band, is it is impossible to meet use demand.Additionally, existing major part absorbing material preparation process is complicated, the response time is long, becomes
This higher it is difficult to realize large-scale production.Therefore study and prepare novel wave-absorbing material electromagnetic wave absorption, for minimizing electromagnetism spoke
Penetrate, improve human lives' condition and improve national military strength, have very important significance.
Content of the invention
In order to overcome shortcoming and defect present in prior art, it is an object of the invention to provide a kind of Graphene is combined
Absorbing material, this composite wave-suction material absorbing property is superior, and suction intensity of wave is high, suction wave frequency bandwidth, density are less；It is also equipped with adjustable
Control property, realizes the high-selenium corn under different frequency by adjusting Graphene with the mass ratio of carbonyl iron and thickness of composite material.
Another object of the present invention is to providing a kind of preparation method of Graphene composite wave-suction material, this preparation method system
Standby process is simple, and less using equipment, the response time is short, and environmental protection is pollution-free, it is possible to achieve large-scale production.
The purpose of the present invention is achieved through the following technical solutions：A kind of Graphene composite wave-suction material, described Graphene is multiple
Close absorbing material to be composited by carbonyl iron and graphene uniform.
The Graphene composite wave-suction material of the present invention is composited by carbonyl iron and graphene uniform, this composite wave-suction material
With respect to simple carbonyl iron and simple Graphene, its absorbing property is superior, inhales intensity of wave height, inhales wave frequency bandwidth, density relatively
Little；It is also equipped with Modulatory character, realize different frequency by adjusting Graphene with the mass ratio of carbonyl iron and thickness of composite material
Under high-selenium corn.
Preferably, the weight that described carbonyl iron and described Graphene are combined ratio is for 10-20：1-2.The present invention passes through carbonyl
The weight ratio that ferrum and Graphene are combined controls in 10-20：, so that carbonyl iron and Graphene can uniformly be combined, prepared is compound for 1-2
Absorbing material has excellent absorbing property.
Preferably, described carbonyl iron be spherical carbonyl iron, at least one in lamellar carbonyl iron and fibrous carbonyl iron.
Typically can be by changing the structure of magnetic metal carbonyl iron（As lamellar, threadiness etc.）, to adjust its pcrmeability and
Dielectric constant, using its high magnetic loss, realizes the strong absorption to microwave in wide frequency range.Fibrous carbonyl iron has obvious shape
Shape anisotropy, its axial pcrmeability is more than radial direction pcrmeability, and axial dielectric constant is more than radial direction dielectric constant.Lamellar carbonyl iron
Due to its magnetic anisotropy, its pcrmeability is substantially better than spherical carbonyl iron, has higher magnetic loss, and absorbing property is better than spherical
Carbonyl iron.Therefore, lamellar, fibrous carbonyl iron/Graphene composite wave-suction material and spherical carbonyl iron/Graphene composite wave-absorbing material
Material is compared, and its absorbing property more preferably, inhales wave frequency section wider.
Preferably, described carbonyl iron is spherical carbonyl iron, a diameter of 0.5-5 μm of spherical carbonyl iron.The present invention passes through to adopt
With a diameter of 0.5-5 μm of spherical carbonyl iron, prepared spherical carbonyl iron/Graphene composite wave-suction material has excellent suction ripple
Performance, not only inhales intensity of wave greatly, and it is wide to inhale wave frequency section.
Another preferably described carbonyl iron is lamellar carbonyl iron, and lamellar carbonyl iron is area at 1-25 μm2, thickness is in 20-
The irregularly shaped thin slice of 30nm.The present invention passes through using area at 1-25 μm2, thickness 20-30nm lamellar carbonyl iron, system
Lamellar carbonyl iron/Graphene the composite wave-suction material obtaining has excellent absorbing property, not only inhales intensity of wave greatly, and inhales wave frequency
Duan Kuan.
Another preferred, described carbonyl iron is fibrous carbonyl iron, a diameter of 0.01nm-1 μm of fibrous carbonyl iron, long
Spend for 20-100 μm.The present invention passes through using a diameter of 0.01nm-1 μm, and length is 20-100 μm of fibrous carbonyl iron, is obtained
Fibrous carbonyl iron/Graphene composite wave-suction material there is excellent absorbing property, it is big not only to inhale intensity of wave, and inhales wave frequency
Duan Kuan.
Another object of the present invention is achieved through the following technical solutions：A kind of preparation side of Graphene composite wave-suction material
Method, prepares graphite oxide first with improving Hummers method, then graphite oxide is dispersed in carbonyl iron dispersion liquid；So
After recycle ultrasonic reducing process that graphite oxide is reduced into Graphene, prepared Graphene composite wave-suction material.
Preferably, comprise the steps：
（1）With natural flake graphite as raw material, prepare graphite oxide using improving Hummers method；
（2）The graphite oxide being obtained is added in deionized water, ultrasonic disperse 0.5-1h, obtains graphite oxide dispersion；
（3）Carbonyl iron is added in ethylene glycol, ultrasonic disperse 0.5-1h, obtains carbonyl iron dispersion liquid；
（4）Graphite oxide dispersion is mixed with carbonyl iron homogeneous dispersion, ultrasonic and mechanical agitation 0.5-1h, obtain mixing molten
Liquid；
（5）Add concentrated hydrochloric acid, then ultrasonic and mechanical agitation 1-3h in mixed solution, obtain reactant liquor；
（6）By reactant liquor sucking filtration, wash, be dried, prepared Graphene composite wave-suction material.
The present invention pass through first will be uniform to graphite oxide and the abundant ultrasonic agitation of carbonyl iron after, add hydrochloric acid, can be by oxygen
Graphite is fully reduced into Graphene, and dispersed in the composite, prepared composite wave-suction material has excellent
Absorbing property.With existing be initially charged hydrochloric acid compared with, hydrochloric acid has begun to react with graphite oxide, visually visible generation lamella relatively
Thick carbonaceous products, antedating response is not reduced into Graphene.Ultimately result in be reduced into Graphene amount considerably less, Duo Shuoshi
Carbonyl, and mix uneven.
Preferably, described step（2）In, the concentration of graphite oxide dispersion is 1-2mg/mL.The present invention passes through to aoxidize
The concentration of graphite dispersing solution controls in 1-2mg/mL, and its dispersion effect is good so that carbonyl iron and Graphene can uniformly be combined, and is obtained
Composite wave-suction material there is excellent absorbing property.
Described step（3）In, the concentration of carbonyl iron dispersion liquid is 10-20mg/mL.The present invention passes through carbonyl iron dispersion liquid
Concentration control in 10-20mg/mL, its dispersion effect is good so that carbonyl iron and Graphene can uniformly be combined, prepared compound suction
Wave material has excellent absorbing property.
Described step（5）In, the addition of concentrated hydrochloric acid is the 0.5 ‰ -2.5 ‰ of mixed liquor volume.Specifically, work as mixing
When the volume of solution is 200mL, the addition of concentrated hydrochloric acid is 0.1-0.5mL.The present invention passes through to control the addition of concentrated hydrochloric acid
The 0.5 ‰ -2.5 ‰ of mixed liquor volume, graphite oxide fully can be reduced into Graphene, and be dispersed in compound
In absorbing material, prepared composite wave-suction material has excellent absorbing property.
Preferably, described step（4）With described step（5）In, churned mechanically rotating speed is 300-500rpm/min.This
Bright by churned mechanically rotating speed is controlled in 300-500rpm/min, its dispersion effect good so that carbonyl iron and Graphene energy
Uniformly it is combined, prepared composite wave-suction material has excellent absorbing property.
Described step（6）In, washing is colourless to filtrate using deionized water and absolute ethanol washing product, is dried and adopts
40-80 DEG C of forced air drying 12-24h.The present invention is by being washed deionized water and dehydrated alcohol, and controls the baking temperature to be
40-80 DEG C, drying time is 12-24h, and product purity is high, and prepared composite wave-suction material has excellent absorbing property.
The beneficial effects of the present invention is：The composite wave-suction material of the present invention is with respect to simple carbonyl iron and simple stone
Black alkene, its absorbing property is superior, and suction intensity of wave is high, suction wave frequency bandwidth, density are less；It is also equipped with Modulatory character, by adjusting stone
Black alkene realizes the high-selenium corn under different frequency with the mass ratio of carbonyl iron and thickness of composite material.
Graphite oxide is reduced into Graphene using ultrasonic reducing process by the preparation method of the present invention, strong with other without high temperature
Reducing agent, the response time is shorter, simple and fast.
The preparation method of the present invention is passed through to be combined suction using improvement Hummers method and ultrasonic reducing process two step synthesizing graphite alkene
Wave material, preparation process is simple, and less using equipment, the response time is short, it is possible to achieve large-scale production.
The preparation method environmental protection of the present invention, pollution-free, and material is also a kind of environmentally friendly cleaning material in itself.
Brief description
Fig. 1 is the SEM figure of the different carbonyl iron of three kinds of patterns and graphite oxide；Wherein,（a）SEM figure for spherical carbonyl iron；
（b）SEM figure for lamellar carbonyl iron；（c）SEM figure for fibrous carbonyl iron；（d）SEM figure for graphite oxide.
Fig. 2 is the SEM figure of the different carbonyl iron/Graphene of three kinds of patterns in embodiment 1-3；Wherein,（a）For embodiment 1 also
The SEM figure of the spherical carbonyl iron/Graphene of former rear product；（b）SEM for product lamellar carbonyl iron/Graphene after embodiment 2 reduction
Figure；（c）SEM figure for product threadiness carbonyl iron/Graphene after embodiment 3 reduction.
Fig. 3 is graphite oxide and spherical carbonyl iron/Graphene in embodiment 1（SCI/RGO）Infrared spectrogram.
Fig. 4 is spherical carbonyl iron/Graphene composite wave-suction material in embodiment 1（SCI/RGO）Absorbing property figure.
Fig. 5 is lamellar carbonyl iron/Graphene composite wave-suction material in embodiment 2（FCI/RGO）Absorbing property figure.
Fig. 6 is fibrous carbonyl iron/Graphene composite wave-suction material in embodiment 3（FI/RGO）Absorbing property figure.
Specific embodiment
For the ease of the understanding of those skilled in the art, with reference to embodiment and accompanying drawing 1-6, the present invention is made further
Explanation, the content that embodiment refers to not limitation of the invention.
Embodiment 1
A kind of preparation method of Graphene composite wave-suction material, comprises the steps：
（1）With natural flake graphite as raw material, prepare graphite oxide using improving Hummers method；
（2）The graphite oxide being obtained is added in deionized water, ultrasonic disperse 1h, the graphite oxide obtaining concentration 1mg/mL divides
Dispersion liquid；
（3）Spherical carbonyl iron is added in ethylene glycol, ultrasonic disperse 1h, the spherical carbonyl iron obtaining concentration 6.67mg/mL divides
Dispersion liquid；
（4）Graphite oxide dispersion is mixed with spherical carbonyl iron homogeneous dispersion, ultrasonic and mechanical agitation 1h, control rotating speed is
500rpm/min, obtains mixed solution；
（5）Take 200mL mixed solution, add the concentrated hydrochloric acid of 0.2mL, then ultrasonic and mechanical agitation 1h, control rotating speed is
500rpm/min；
（6）After reaction terminates, sucking filtration, colourless to filtrate using deionized water and absolute ethanol washing product respectively, using 40 DEG C
Forced air drying 24h, the black powder obtaining is and absorbs by force wide band spherical carbonyl iron/Graphene composite wave-suction material.
In embodiment 1, the SEM figure of raw material ball shape carbonyl iron is shown in Fig. 1（a）, improve Hummers method and prepare graphite oxide and see
Fig. 1（d）.In embodiment 1, the SEM figure of the spherical carbonyl iron of product/Graphene composite wave-suction material is shown in Fig. 2（a）It is seen that spherical carbonyl
Ferrum is mixed with graphene uniform.
In embodiment 1, the infrared spectrogram of the spherical carbonyl iron of product/Graphene composite wave-suction material is shown in Fig. 3 it is seen that passing through
After ultrasonic reduction, the substantial amounts of oxygen-containing functional group of graphite oxide disappears, and illustrates that graphite oxide is successfully reduced into Graphene.
By the black powder product in embodiment 1 with hard paraffin according to mass ratio 60%：40% uniformly mixes, in die for special purpose
It is pressed into the coaxial annulus sample of external diameter 7.00mm, internal diameter 3.04mm, thickness about 3mm, with model Keysight N5242A in tool
Vector network analyzer tests its absorbing property, and test frequency is 2-18GHz.The suction of spherical carbonyl iron/Graphene composite sample
Ripple performance is as shown in figure 4, when the matching thickness of this composite sample is 1.5mm, at 14.25GHz, absorbing property preferably reaches
Arrive -41.83dB, the effective Absorber Bandwidth being wherein less than -10dB is 4.04GHz（12.57-16.61GHz）, less than the suction of -20dB
The a width of 1.0GHz of take-up（13.70-14.70GHz）.
Embodiment 2
A kind of preparation method of Graphene composite wave-suction material, comprises the steps：
（1）With natural flake graphite as raw material, prepare graphite oxide using improving Hummers method；
（2）The graphite oxide being obtained is added in deionized water, ultrasonic disperse 1h, the graphite oxide obtaining concentration 1mg/mL divides
Dispersion liquid；
（3）Lamellar carbonyl iron is added in ethylene glycol, ultrasonic disperse 1h, obtains the lamellar carbonyl iron dispersion of concentration 10mg/mL
Liquid；
（4）Graphite oxide dispersion is mixed with lamellar carbonyl iron homogeneous dispersion, ultrasonic and mechanical agitation 1h, control rotating speed is
500rpm/min, obtains mixed solution；
（5）Take 200mL mixed solution, add the concentrated hydrochloric acid of 0.2mL, then ultrasonic and mechanical agitation 1h, control rotating speed is
500rpm/min；
（6）After reaction terminates, sucking filtration, colourless to filtrate using deionized water and absolute ethanol washing product respectively, using 40 DEG C
Forced air drying 24h, the black powder obtaining is and absorbs by force wide band lamellar carbonyl iron/Graphene composite wave-suction material.
In embodiment 2, the SEM figure of material piece shape carbonyl iron is shown in Fig. 1（b）.Product lamellar carbonyl iron/Graphene in embodiment 2
SEM figure see Fig. 2（b）It is seen that lamellar carbonyl iron is mixed with graphene uniform.
By the black powder product in embodiment 2 with hard paraffin according to mass ratio 60%：40% uniformly mixes, in die for special purpose
It is pressed into the coaxial annulus sample of external diameter 7.00mm, internal diameter 3.04mm, thickness about 3mm, with model Keysight N5242A in tool
Vector network analyzer tests its absorbing property, and test frequency is 2-18GHz.The suction of lamellar carbonyl iron/Graphene composite sample
As shown in figure 5, the thickness working as this composite sample is 2.0mm, at 9.18GHz, absorbing property can reach -33.1dB to ripple performance,
The effective Absorber Bandwidth being wherein less than -10dB is 4.99GHz（6.91-11.90GHz）, the Absorber Bandwidth less than -20dB is
1.51GHz（8.37-9.88GHz）.When the matching thickness of this composite sample is 1.5mm, at 13.69GHz, absorbing property can reach
Arrive -21.49dB, the effective Absorber Bandwidth being wherein less than -10dB is 7.30GHz（10.15-17.45GHz）, less than the suction of -20dB
The a width of 1.23GHz of take-up（13.03-14.26GHz）.
Embodiment 3
A kind of preparation method of Graphene composite wave-suction material, comprises the steps：
（1）With natural flake graphite as raw material, prepare graphite oxide using improving Hummers method；
（2）The graphite oxide being obtained is added in deionized water, ultrasonic disperse 1h, the graphite oxide obtaining concentration 1mg/mL divides
Dispersion liquid；
（3）Fibrous carbonyl iron is added in ethylene glycol, ultrasonic disperse 1h, obtains the fibrous carbonyl iron of concentration 20mg/mL
Dispersion liquid；
（4）Graphite oxide dispersion is mixed with fibrous carbonyl iron homogeneous dispersion, ultrasonic and mechanical agitation 1h, control rotating speed
For 500rpm/min, obtain mixed solution；
（5）Take 200mL mixed solution, add the concentrated hydrochloric acid of 0.2mL, then ultrasonic and mechanical agitation 1h, control rotating speed is
500rpm/min；
（6）After reaction terminates, sucking filtration, colourless to filtrate using deionized water and absolute ethanol washing product respectively, using 40 DEG C
Forced air drying 24h, the black powder obtaining is strong absorption wide band threadiness carbonyl iron/Graphene composite wave-suction material.
In embodiment 3, the SEM figure of material piece shape carbonyl iron is shown in Fig. 1（c）.Product threadiness carbonyl iron/graphite in embodiment 3
The SEM figure of alkene is shown in Fig. 2（c）It is seen that lamellar carbonyl iron is mixed with graphene uniform.
By the black powder product in embodiment 3 with hard paraffin according to mass ratio 60%：40% uniformly mixes, in die for special purpose
It is pressed into the coaxial annulus sample of external diameter 7.00mm, internal diameter 3.04mm, thickness about 3mm, with model Keysight N5242A in tool
Vector network analyzer tests its absorbing property, and test frequency is 2-18GHz.Fibrous carbonyl iron/Graphene composite sample
Absorbing property as shown in fig. 6, when the thickness of this composite sample is 2.0mm, at 10.38GHz, absorbing property can reach-
38.69dB, the effective Absorber Bandwidth being wherein less than -10dB is 6.05GHz（7.51-13.56GHz）, less than the absorption band of -20dB
A width of 1.72GHz（9.55-11.27GHz）.When the matching thickness of this composite sample is 1.5mm, at 15.37GHz, wave absorbtion
Can reach -29.23dB, the effective Absorber Bandwidth being wherein less than -10dB is 6.5GHz（11.50-18GHz）, less than -20dB's
Absorber Bandwidth is 2.1GHz（14.60-16.70GHz）.
Above-described embodiment is the present invention preferably implementation, and in addition, the present invention can be realized with alternate manner,
Without departing from obvious replacement any on the premise of present inventive concept all within protection scope of the present invention.
Claims (10)
1. a kind of Graphene composite wave-suction material it is characterised in that：Described Graphene composite wave-suction material is by carbonyl iron and graphite
Alkene is uniformly composited.
2. a kind of Graphene composite wave-suction material according to claim 1 it is characterised in that：Described carbonyl iron and described stone
The weight that black alkene is combined ratio is for 10-20：1-2.
3. a kind of Graphene composite wave-suction material according to claim 1 it is characterised in that：Described carbonyl iron is spherical carbonyl
At least one in base ferrum, lamellar carbonyl iron and fibrous carbonyl iron.
4. a kind of Graphene composite wave-suction material according to claim 3 it is characterised in that：Described carbonyl iron is spherical carbonyl
Base ferrum, a diameter of 0.5-5 μm of spherical carbonyl iron.
5. a kind of Graphene composite wave-suction material according to claim 3 it is characterised in that：Described carbonyl iron is lamellar carbonyl
Base ferrum, lamellar carbonyl iron is area at 1-25 μm2, thickness 20-30nm irregularly shaped thin slice.
6. a kind of Graphene composite wave-suction material according to claim 3 it is characterised in that：Described carbonyl iron is threadiness
Carbonyl iron, a diameter of 0.01nm-1 μm of fibrous carbonyl iron, length is 20-100 μm.
7. a kind of Graphene composite wave-suction material as described in any one of claim 1-6 preparation method it is characterised in that：First
Prepare graphite oxide using improving Hummers method, then graphite oxide is dispersed in carbonyl iron dispersion liquid；Then sharp again
With ultrasonic reducing process, graphite oxide is reduced into Graphene, prepared Graphene composite wave-suction material.
8. a kind of Graphene composite wave-suction material according to claim 7 preparation method it is characterised in that：Including as follows
Step：
（1）With natural flake graphite as raw material, prepare graphite oxide using improving Hummers method；
（2）The graphite oxide being obtained is added in deionized water, ultrasonic disperse 0.5-1h, obtains graphite oxide dispersion；
（3）Carbonyl iron is added in ethylene glycol, ultrasonic disperse 0.5-1h, obtains carbonyl iron dispersion liquid；
（4）Graphite oxide dispersion is mixed with carbonyl iron homogeneous dispersion, ultrasonic and mechanical agitation 0.5-1h, obtain mixing molten
Liquid；
（5）Add concentrated hydrochloric acid, then ultrasonic and mechanical agitation 1-3h in mixed solution, obtain reactant liquor；
（6）By reactant liquor sucking filtration, wash, be dried, prepared Graphene composite wave-suction material.
9. a kind of Graphene composite wave-suction material according to claim 7 preparation method it is characterised in that：Described step
（2）In, the concentration of graphite oxide dispersion is 1-2mg/mL；Described step（3）In, the concentration of carbonyl iron dispersion liquid is 10-
20mg/mL；Described step（5）In, the addition of concentrated hydrochloric acid is the 0.5 ‰ -2.5 ‰ of mixed liquor volume.
10. a kind of Graphene composite wave-suction material according to claim 7 preparation method it is characterised in that：Described step
Suddenly（4）With described step（5）In, churned mechanically rotating speed is 300-500rpm/min；Described step（6）In, washing is using going
Ionized water and absolute ethanol washing product are colourless to filtrate, are dried and adopt 40-80 DEG C of forced air drying 12-24h.
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