CN106800916A - A kind of graphene-based tri compound absorbing material and preparation method thereof - Google Patents
A kind of graphene-based tri compound absorbing material and preparation method thereof Download PDFInfo
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- CN106800916A CN106800916A CN201710022137.0A CN201710022137A CN106800916A CN 106800916 A CN106800916 A CN 106800916A CN 201710022137 A CN201710022137 A CN 201710022137A CN 106800916 A CN106800916 A CN 106800916A
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- carbonyl iron
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Abstract
The present invention relates to microwave absorption technique field, specifically related to a kind of graphene-based tri compound absorbing material and preparation method thereof, coated with silica carbonyl iron nucleocapsid composite particles are prepared first with sol-gal process, then graphite oxide is prepared using improving Hummers methods, graphite oxide is dispersed in coated with silica carbonyl iron nucleocapsid composite particles dispersion liquid again, graphite oxide is finally reduced into Graphene using ultrasonic reducing process, graphene-based tri compound absorbing material is obtained.Preparation method of the invention is simply efficient, and the composite wave-suction material of preparation is relative to simple carbonyl iron, simple Graphene and carbonyl iron/Graphene binary composite wave-suction material, and its absorbing property is more superior, inhales intensity of wave high, suction wave frequency bandwidth, density smaller；Modulatory character is also equipped with, by adjusting clad SiO2The thickness of thickness, the mass ratio of Graphene and coated core-shell composite particles and trielement composite material can realize the strong suction ripple under different frequency.
Description
Technical field
The present invention relates to microwave absorption technique field, and in particular to a kind of graphene-based tri compound absorbing material and its system
Preparation Method.
Background technology
With radar, the particularly development of microwave communication techniques, wireless communication tool, internet and other communication equipments
Use in gigahertz range, concern of the people to electromagnetic interference and electromagnetic compatibility increasingly rises.Therefore, research has height
The demand of the electromagnetic shielding material that absorbability and broadband absorb is increasingly urgent.At present, absorbing material not only extensive use
In the stealthy field of military radar, and also there are many applications, such as microwave dark room material, microwave attenuation unit device in civil area
Part, electromagnetic compatibility, microwave forming processing technology etc..
Into 21st century, with progress and the innovation of science and technology, and military strategy demand continuous improvement, it is desirable to it is new
The characteristics of absorbing material of type has " thin, light, wide, strong ".And traditional single absorbing material（It is ferrite, carbon-based material, ultra-fine
Magnetic metallic powder, ceramic material etc.）Although wave-sucking performance is strong, density is generally large or absorption band is narrow, it is impossible to
Meet use demand.The Main way of research is, by the Material cladding of different suction wave frequency sections, to prepare binary or polynary new at present
Composite wave-suction material and reach wideband absorption purpose.Therefore study and prepare novel wave-absorbing material electromagnetic wave absorption, for subtracting
Few electromagnetic radiation, improvement human lives' condition and the national military strength of raising, have very important significance.
Carbonyl iron belongs to magnetic metal absorbing material, in microwave frequency band due to magnetic conductivity is higher, magnetic conductivity real part, void
Portion's Dispersion is good, can obtain stronger absorbing property under the conditions of low matching thickness and be widely used.It is relied primarily on
The mechanism such as magnetic hystersis loss, eddy-current loss, domain wall resonance decay and electromagnetic wave absorption.Typically can be by changing magnetic metal configuration
（Sheet, Fiber Aspect Ratio, needle-like whisker）Its magnetic conductivity and dielectric constant are adjusted, high suction is realized to microwave in wide frequency range
Receive, but there is also some shortcomings simultaneously, such as electrical conductivity is high, corrosion resistance is low, density is big.Therefore, using insulating materials（Such as
SiO2、TiO2）Cladding carbonyl ferrimagnet prepares core shell structure composite wave-suction material.By reducing its dielectric constant, improve
Impedance matching property, can further improve absorbing property.
Graphene makes it have and is different from the special of other carbon materials as a kind of new carbon, unique single layer structure
Physicochemical properties, bring new opportunities and challenges to study new carbon-based electromagnetic wave absorbent material.It has light weight, ratio
Surface area is big, good conductivity and the excellent property such as dielectric constant is high, has potential application value in electromagnetic wave absorption field.Change
There are a large amount of defects in graphenic surface prepared by method（Including marginality, topological defect, hole etc.）With the oxygen-containing function of residual
Group, can produce the localization state of fermi level；Chemical bond energy outside is exposed on graphene sheet layer to the open air simultaneously in electromagnetic field effect
The lower dielectric relaxor that outer-shell electron occurs, so as to absorb and electromagnetic wave of decaying.As other carbon materials, Graphene is used as electromagnetism
The maximum shortcoming of ripple absorbing material is that do not have magnetic and magnetic loss, but the huge specific surface area of Graphene carries out function for it
Change compound providing infinitely may.
The content of the invention
In order to overcome the shortcoming and defect of traditional single absorbing material and prior art, it is an object of the invention to provide
A kind of graphene-based tri compound absorbing material, the composite wave-suction material absorbing property is superior, and suction intensity of wave is high, inhale wave frequency band
Wide, density is smaller；Modulatory character is also equipped with, by adjusting clad SiO2Thickness, Graphene and coated core-shell composite particles
The thickness of mass ratio and trielement composite material realizes the strong suction ripple under different frequency.
Another object of the present invention is to provide a kind of preparation method of graphene-based tri compound absorbing material, the preparation
Method preparation process is simple, and less using equipment, the reaction 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 graphite-based tri compound absorbing material, the graphite
Alkenyl tri compound absorbing material is uniformly answered in loading to graphene sheet layer by coated with silica carbonyl iron nucleocapsid composite particles
Conjunction is formed,
Preferably, the inside of the coated with silica carbonyl iron nucleocapsid composite particles is carbonyl iron micron particles, outside cladding
The uniform silica of a layer thickness, thickness is 10-75nm.
Preferably, the coated with silica carbonyl iron nucleocapsid composite particles weight ratio compound with the Graphene is
10-20：1-2.The present invention is controlled by the weight ratio for being combined coated with silica carbonyl iron nucleocapsid composite particles and Graphene
In 10-20：1-2 so that coated with silica carbonyl iron nucleocapsid composite particles are successfully loaded in graphene sheet layer, obtained three
First composite wave-suction material has excellent absorbing property.
Preferably, the carbonyl iron micron particles of stating are for spherical carbonyl iron（A diameter of 0.5-5 μm）And/or sheet carbonyl iron
（Area is at 1-25 μm2, thickness is in 20-30nm）.Typically can be by changing the structure of magnetic metal carbonyl iron（Such as sheet, spherical
Deng）To adjust its magnetic conductivity and dielectric constant, using its magnetic loss high, realize in wide frequency range to the strong absorption of microwave.Piece
Due to its magnetic anisotropy, its magnetic conductivity is substantially better than spherical carbonyl iron to shape carbonyl iron, with magnetic loss higher, absorbing property
Better than spherical carbonyl iron.
Another object of the present invention is achieved through the following technical solutions：A kind of system of graphene-based tri compound absorbing material
Preparation Method, coated with silica carbonyl iron nucleocapsid composite particles are prepared first with sol-gal process, then using improvement
Hummers methods prepare graphite oxide, then graphite oxide is dispersed in into coated with silica carbonyl iron nucleocapsid composite particles
In dispersion liquid, graphite oxide is finally reduced into Graphene using ultrasonic reducing process, graphene-based tri compound is obtained and inhales ripple material
Material.
Preferably, comprise the following steps：
（1）The preparation of coated with silica carbonyl iron nucleocapsid composite particles：
Carbonyl iron micron particles are added in mixed solution of the absolute ethyl alcohol with deionized water, ultrasonic and mechanical agitation 0.5-
1h, obtains carbonyl iron dispersion liquid；Then ammoniacal liquor and tetraethyl orthosilicate, mechanic whirl-nett reaction is added to obtain in carbonyl iron dispersion liquid
To product；Finally by product washing, suction filtration, drying, coated with silica carbonyl iron nucleocapsid composite particles are obtained；
（2）The preparation of graphite oxide：
With natural flake graphite as raw material, graphite oxide is prepared using Hummers methods are improved；Obtained graphite oxide is added
To in deionized water, ultrasonic disperse 0.5-1h obtains graphite oxide dispersion；
（3）The preparation of graphene-based tri compound absorbing material：
First by step（1）The coated with silica carbonyl iron nucleocapsid composite particles of preparation are added in ethylene glycol, ultrasonic disperse
0.5-1h, obtains coated with silica carbonyl iron nucleocapsid composite particles dispersion liquid；Then by step（2）The graphite oxide of preparation point
Dispersion liquid mixes with coated with silica carbonyl iron nucleocapsid composite particles homogeneous dispersion, ultrasonic and mechanical agitation 0.5-1h, obtains
Mixed solution；Concentrated hydrochloric acid is added in mixed solution again, then ultrasound and mechanical agitation 1-3h, finally wash product,
Suction filtration, drying, are obtained graphene-based tri compound absorbing material.
Preferably, the step（1）In, the concentration of carbonyl iron dispersion liquid is 10-20mg/mL, absolute ethyl alcohol and deionization
The mass ratio of water is 3.5-4.5：1, ammoniacal liquor is the 2%-5% of mixed liquor volume with the concentration of tetraethyl orthosilicate, and reaction temperature is
Room temperature~60 DEG C, reaction time 3-48h.The present invention is by regulating and controlling concentration, reaction time and the reaction of ammoniacal liquor and tetraethyl orthosilicate
Temperature, the SiO of different-thickness is prepared on carbonyl iron micron particles surface2Shell, adjusts its dielectric constant, improves impedance
Match somebody with somebody.
The step（2）In, the concentration of graphite oxide dispersion is 1-2mg/mL.In golden yellow when dispersion liquid concentration is low,
It is in claret when concentration is high.The present invention is controlled in 1-2mg/mL by by the concentration of graphite oxide dispersion, and its dispersion effect is more
Excellent, obtained tri compound absorbing material has excellent absorbing property.
The step（3）In, the concentration of coated with silica carbonyl iron nucleocapsid composite particles dispersion liquid is 10-20mg/mL,
The addition of concentrated hydrochloric acid is the 0.5 ‰ -2.5 ‰ of mixed liquor volume.Specifically, when the volume of mixed solution is 200mL, it is dense
The addition of hydrochloric acid is 0.1-0.5mL.The present invention is by by the dense of coated with silica carbonyl iron nucleocapsid composite particles dispersion liquid
It is 10-20mg/mL to spend, and its dispersion effect is good, and obtained tri compound absorbing material has excellent absorbing property.The present invention is logical
Cross and control the 0.5 ‰ -2.5 ‰ of mixed liquor volume the addition of concentrated hydrochloric acid, graphite oxide can be fully reduced into stone
Black alkene, and be dispersed in tri compound absorbing material, obtained tri compound absorbing material has excellent wave absorbtion
Energy.
Preferably, the step（1）With the step（3）In, churned mechanically rotating speed is 300-500rpm/min.This hair
Bright to be controlled in 300-500rpm/min by by churned mechanically rotating speed, its dispersion effect is good so that solgel reaction more fills
Point, nucleocapsid composite particles and Graphene are evenly combined.
The step（1）With the step（3）In, washing using deionized water and absolute ethanol washing product to filtrate without
Color, dries and uses 40-80 DEG C of forced air drying 12-24h.The present invention is washed by using deionized water and absolute ethyl alcohol, and
Control drying temperature for 40-80 DEG C, drying time is 12-24h, and product purity is high, dry more completely, obtained composite wave-absorbing material
Material has excellent absorbing property.
The beneficial effects of the present invention are：The present invention prepares coated with silica carbonyl by first with sol-gal process
Iron nucleocapsid composite particles, by reducing carbonyl iron dielectric constant, improve its impedance matching property, further improve absorbing property.
Again by graphite oxide and the coated with silica carbonyl iron abundant ultrasonic agitation of nucleocapsid composite particles it is uniform after, add hydrochloric acid, by oxygen
Graphite is fully reduced into Graphene, and coated with silica carbonyl iron nucleocapsid composite particles are successfully loaded into graphene sheet layer
In, obtained tri compound absorbing material is relative to traditional homogenous material（Carbonyl iron, Graphene）With binary composite, its
Absorbing property is superior, inhales intensity of wave high, suction wave frequency bandwidth, density smaller；Modulatory character is also equipped with, by adjusting clad SiO2
The thickness of thickness, the mass ratio of Graphene and coated core-shell composite particles and trielement composite material is realized strong under different frequency
Inhale ripple.
The present invention is by the uniform load insulating materials SiO in graphene sheet layer2Cladding carbonyl iron nucleocapsid composite particles, no
The magnetic property of composite can be only improved, strengthens magnetic loss, also improve the impedance matching of composite.Additionally, SiO2Bag
Cover Graphene during carbonyl iron nucleocapsid composite particles advantageously reduce drying process as spacer medium and be stacked into three-dimensional graphite again
Structure.Novel graphite alkenyl tri compound absorbing material of the invention has the advantages that " thin, light, wide, strong " that optimization tradition is single
The absorbing property of material, high-selenium corn is realized in wide frequency range to microwave, for reducing electromagnetic radiation, improving human lives' condition
With the national military strength of raising, have very important significance.
Preparation method of the invention prepares silica shell using sol-gal process, and reaction temperature is low, can be by reaction
Time and reactant concentration regulation and control clad SiO2Thickness.
Graphite oxide is reduced into Graphene by preparation method of the invention using ultrasonic reducing process, strong with other without high temperature
Reducing agent, the reaction time is shorter, simple and fast.
Preparation method of the invention is by using sol-gal process and the ultrasonic reducing process graphene-based compound suction of synthesis of ternary
Wave material, preparation process is simple, pollution-free, environmental protection, it is possible to achieve large-scale production less using equipment.
Brief description of the drawings
Fig. 1 be spherical carbonyl iron before cladding in embodiment 1 SEM figures, cladding after core-shell particle SEM and TEM figure, aoxidize
The SEM figures of graphite and graphene-based tri compound absorbing material（SCI@SiO2/RGO）SEM figure；Wherein,（a）It is embodiment
The SEM figures of spherical carbonyl iron before being coated in 1；（b）It is spherical carbonyl iron@SiO after being coated in embodiment 12The SEM of core-shell particle
Figure；（c）It is spherical carbonyl iron@SiO after being coated in embodiment 12The TEM figures of core-shell particle；（d）To be improved in embodiment 1
The SEM figures of graphite oxide prepared by Hummers methods；（e）It is graphene-based tri compound absorbing material in embodiment 1（SCI@
SiO2/RGO）SEM figure.
Fig. 2 be sheet carbonyl iron before cladding in embodiment 2 SEM figures, cladding after core-shell particle SEM figures and Graphene
Base tri compound absorbing material（FCI@SiO2/RGO）SEM figure；Wherein,（a）It is sheet carbonyl iron before being coated in embodiment 2
SEM schemes；（b）It is sheet carbonyl iron SiO after being coated in embodiment 12The SEM figures of core-shell particle；（c）It is Graphene in embodiment 1
Base tri compound absorbing material（FCI@SiO2/RGO）SEM figure.
Fig. 3 is spherical carbonyl iron@silica/Graphene tri compound absorbing material in embodiment 1（SCI
@SiO2/RGO）Absorbing property figure.
Fig. 4 is sheet carbonyl iron@silica/Graphene tri compound absorbing material in embodiment 2（FCI@SiO2/
RGO）Absorbing property figure.
Specific embodiment
For the ease of the understanding of those skilled in the art, further is made to the present invention with reference to embodiment and accompanying drawing 1-4
Explanation, the content that implementation method is referred to not limitation of the invention.
Embodiment 1
A kind of preparation method of graphene-based tri compound absorbing material, comprises the following steps：
（1）The preparation of coated with silica carbonyl iron nucleocapsid composite particles
The spherical carbonyl irons of 2g are added in mixed solution of the 160mL absolute ethyl alcohols with 40mL deionized waters, ultrasonic and machinery is stirred
1h is mixed, 4mL ammoniacal liquor and 4mL tetraethyl orthosilicates are then added in mixed solution, mechanical agitation is anti-under 40 DEG C of reaction temperature
After answering 21h, reaction to terminate, suction filtration is simultaneously colourless to filtrate using deionized water and absolute ethanol washing product respectively, using 40 DEG C
Forced air drying 24h, is obtained the spherical carbonyl iron nucleocapsid composite particles of coated with silica（SCI@SiO2）.
（2）The preparation of graphite oxide
With natural flake graphite as raw material, graphite oxide is prepared using Hummers methods are improved；Obtained graphite oxide is added
To in deionized water, ultrasonic disperse 1h obtains the graphite oxide dispersion of concentration 1mg/mL；
（3）Graphene-based tri compound absorbing material（SCI@SiO2/RGO）Preparation
First by step（1）The spherical carbonyl iron nucleocapsid composite particles of coated with silica of preparation are added in ethylene glycol, ultrasound point
1h is dissipated, the dispersion liquid of concentration 6.67mg/mL is obtained；It is subsequently adding step（2）The graphite oxide dispersion volume ratio 1 of preparation:1 is equal
Even mixing, ultrasound and mechanical agitation 1h, control rotating speed for 500rpm/min, obtain mixed solution；200mL mixed solutions are taken, plus
Enter the concentrated hydrochloric acid of 0.2mL, then ultrasound and mechanical agitation 1h, it is 500rpm/min to control rotating speed；The black powder for obtaining is
Wide band spherical carbonyl iron@silica/Graphene tri compound absorbing material is absorbed by force（SCI@SiO2/RGO）.
In embodiment 1：The SEM figures of the spherical carbonyl iron of raw material are shown in Fig. 1 before cladding（a）；Spherical carbonyl iron@SiO after cladding2Core
Capsomeric SEM and TEM figures are shown in Fig. 1 respectively（b）With Fig. 1（c）, visible spherical carbonyl iron coated with uniform one is schemed by TEM
The silica of layer about 45nm；The SEM figures for improving graphite oxide prepared by Hummers methods are shown in Fig. 1（d）；Spherical carbonyl iron@dioxies
SiClx/Graphene tri compound absorbing material（SCI@SiO2/RGO）SEM figures see Fig. 1（e）, it is seen that coated with silica sheet
Carbonyl iron nucleocapsid composite particles are successfully loaded in graphene sheet layer.
By the spherical carbonyl iron@silica in embodiment 1/Graphene tri compound inhale ripple powder and solid paraffin according to
Mass ratio 60%：40% uniform mixing, be pressed into particular manufacturing craft external diameter 7.00mm, internal diameter 3.04mm, thickness about 3mm it is coaxial
Annulus sample, its absorbing property is tested with model KeysightN5242A vector network analyzers, and test frequency is 2-18GHz.
The absorbing property of spherical carbonyl iron@silica/Graphene tri compound absorbing material is as shown in figure 3, when the composite sample
Matching thickness is 1.5mm, and at 16.70GHz, absorbing property preferably reaches -26.89dB, wherein the effective suction less than -10dB
The a width of 5.06GHz of take-up（12.94-18.0GHz）, the Absorber Bandwidth less than -20dB is 2.16GHz（15.50-17.66GHz）.
Embodiment 2
A kind of preparation method of graphene-based tri compound absorbing material, comprises the following steps：
（1）The preparation of coated with silica carbonyl iron nucleocapsid composite particles
2g sheet carbonyl irons are added in mixed solution of the 160mL absolute ethyl alcohols with 40mL deionized waters, ultrasonic and machinery is stirred
1h is mixed, 4mL ammoniacal liquor and 4mL tetraethyl orthosilicates are then added in mixed solution, mechanical agitation is anti-under 40 DEG C of reaction temperature
After answering 21h, reaction to terminate, suction filtration is simultaneously colourless to filtrate using deionized water and absolute ethanol washing product respectively, using 40 DEG C
Forced air drying 24h, is obtained coated with silica sheet carbonyl iron nucleocapsid composite particles（FCI@SiO2）.
（2）The preparation of graphite oxide
With natural flake graphite as raw material, graphite oxide is prepared using Hummers methods are improved；Obtained graphite oxide is added
To in deionized water, ultrasonic disperse 1h obtains the graphite oxide dispersion of concentration 1mg/mL；
（3）Graphene-based tri compound absorbing material（FCI@SiO2/RGO）Preparation
First by step（1）The coated with silica sheet carbonyl iron nucleocapsid composite particles of preparation are added in ethylene glycol, ultrasound point
1h is dissipated, the dispersion liquid of concentration 20mg/mL is obtained；It is subsequently adding step（2）The graphite oxide dispersion volume ratio 1 of preparation:1 is uniform
Mixing, ultrasound and mechanical agitation 1h, control rotating speed for 500rpm/min, obtain mixed solution；200mL mixed solutions are taken, is added
The concentrated hydrochloric acid of 0.2mL, then ultrasound and mechanical agitation 1h, control rotating speed for 500rpm/min；The black powder for obtaining is by force
Absorb wide band sheet carbonyl iron@silica/Graphene tri compound absorbing material（FCI@SiO2/RGO）.
In embodiment 2：The SEM figures of raw material sheet carbonyl iron are shown in Fig. 2 before cladding（a）；Spherical carbonyl iron@SiO after cladding2Core
Capsomeric SEM figures are shown in Fig. 2（b）, it is seen that sheet carbonyl iron coated with uniform layer of silicon dioxide；Sheet carbonyl iron@bis-
Silica/Graphene tri compound absorbing material（FCI@SiO2/RGO）SEM figures see Fig. 2（c）, it is seen that coated with silica piece
Shape carbonyl iron nucleocapsid composite particles are successfully loaded in graphene sheet layer.
By the spherical carbonyl iron@silica in embodiment 2/Graphene tri compound inhale ripple powder and solid paraffin according to
Mass ratio 60%：40% uniform mixing, be pressed into particular manufacturing craft external diameter 7.00mm, internal diameter 3.04mm, thickness about 3mm it is coaxial
Annulus sample, its absorbing property is tested with model KeysightN5242A vector network analyzers, and test frequency is 2-18GHz.
The absorbing property of sheet carbonyl iron/Graphene composite sample as shown in figure 4, when the thickness of the composite sample is 2.0mm,
At 10.40GHz, absorbing property can reach -28.87dB, wherein the effective Absorber Bandwidth less than -10dB is 5.92GHz（7.60-
13.55GHz）, the Absorber Bandwidth less than -20dB is 1.73GHz（9.54-11.27GHz）.When the matching thickness of the composite sample
It is 1.5mm, at 13.76GHz, absorbing property can reach -39.68dB, wherein the effective Absorber Bandwidth less than -10dB is
8.00GHz（10.00-18.00GHz）, the Absorber Bandwidth less than -20dB is 2.09GHz（12.57-14.66GHz）.
Above-described embodiment is the present invention preferably implementation, and in addition, the present invention can be realized with other manner,
Any obvious replacement is within protection scope of the present invention on the premise of not departing from present inventive concept.
Claims (10)
1. a kind of graphene-based tri compound absorbing material, it is characterised in that：The graphene-based tri compound absorbing material by
Coated with silica carbonyl iron nucleocapsid composite particles are uniformly composited in loading to graphene sheet layer.
2. a kind of graphene-based tri compound absorbing material according to claim 1, it is characterised in that：The silica
The inside for coating carbonyl iron nucleocapsid composite particles is carbonyl iron micron particles, the outside cladding uniform silica of a layer thickness,
Thickness is 10-75nm.
3. a kind of graphene-based tri compound absorbing material according to claim 1, it is characterised in that：The silica
Cladding carbonyl iron nucleocapsid composite particles are 10-20 with the weight ratio that the Graphene is combined：1-2.
4. a kind of graphene-based tri compound absorbing material according to claim 3, it is characterised in that：The carbonyl iron is micro-
Rice grain is spherical carbonyl iron and/or sheet carbonyl iron.
5. a kind of graphene-based tri compound absorbing material according to claim 4, it is characterised in that：The carbonyl iron is micro-
Rice grain is spherical carbonyl iron, a diameter of 0.5-5 μm of spherical carbonyl iron.
6. a kind of graphene-based tri compound absorbing material according to claim 4, it is characterised in that：The carbonyl iron is micro-
Rice grain is sheet carbonyl iron, and sheet carbonyl iron is area at 1-25 μm2, thickness 20-30nm irregular shape thin slice.
7. the preparation method of a kind of graphene-based tri compound absorbing material as described in claim any one of 1-6, its feature
It is：Coated with silica carbonyl iron nucleocapsid composite particles are prepared first with sol-gal process, then using improving Hummers
Method prepares graphite oxide, then graphite oxide is dispersed in into coated with silica carbonyl iron nucleocapsid composite particles dispersion liquid
In, graphite oxide is finally reduced into Graphene using ultrasonic reducing process, graphene-based tri compound absorbing material is obtained.
8. the preparation method of a kind of graphene-based tri compound absorbing material according to claim 7, it is characterised in that：Bag
Include following steps：
（1）The preparation of coated with silica carbonyl iron nucleocapsid composite particles：
Carbonyl iron micron particles are added in mixed solution of the absolute ethyl alcohol with deionized water, ultrasonic and mechanical agitation 0.5-
1h, obtains carbonyl iron dispersion liquid；Then ammoniacal liquor and tetraethyl orthosilicate, mechanic whirl-nett reaction is added to obtain in carbonyl iron dispersion liquid
To product；Finally by product washing, suction filtration, drying, coated with silica carbonyl iron nucleocapsid composite particles are obtained；
（2）The preparation of graphite oxide：
With natural flake graphite as raw material, graphite oxide is prepared using Hummers methods are improved；Obtained graphite oxide is added
To in deionized water, ultrasonic disperse 0.5-1h obtains graphite oxide dispersion；
（3）The preparation of graphene-based tri compound absorbing material：
First by step（1）The coated with silica carbonyl iron nucleocapsid composite particles of preparation are added in ethylene glycol, ultrasonic disperse
0.5-1h, obtains coated with silica carbonyl iron nucleocapsid composite particles dispersion liquid；Then by step（2）The graphite oxide of preparation point
Dispersion liquid mixes with coated with silica carbonyl iron nucleocapsid composite particles homogeneous dispersion, ultrasonic and mechanical agitation 0.5-1h, obtains
Mixed solution；Concentrated hydrochloric acid is added in mixed solution again, then ultrasound and mechanical agitation 1-3h, finally wash product,
Suction filtration, drying, are obtained graphene-based tri compound absorbing material.
9. the preparation method of a kind of graphene-based tri compound absorbing material according to claim 7, it is characterised in that：Institute
State step（1）In, the concentration of carbonyl iron dispersion liquid is 10-20mg/mL, and absolute ethyl alcohol is 3.5- with the mass ratio of deionized water
4.5：1, ammoniacal liquor is the 2%-5% of mixed liquor volume with the concentration of tetraethyl orthosilicate, and reaction temperature is room temperature~60 DEG C, during reaction
Between 3-48h；The step（2）In, the concentration of graphite oxide dispersion is 1-2mg/mL；The step（3）In, silica bag
The concentration of carbonyl iron nucleocapsid composite particles dispersion liquid is covered for 10-20mg/mL, and the addition of concentrated hydrochloric acid is mixed liquor volume
0.5‰-2.5‰。
10. the preparation method of a kind of graphene-based tri compound absorbing material according to claim 7, it is characterised in that：
The step（1）With the step（3）In, churned mechanically rotating speed is 300-500rpm/min；The step（1）With the step
Suddenly（3）In, washing is colourless to filtrate using deionized water and absolute ethanol washing product, dries and uses 40-80 DEG C of forced air drying
12-24h。
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| CN112689452A (en) * | 2020-12-02 | 2021-04-20 | 中国人民解放***箭军工程大学 | Co/C/carbonyl iron fiber composite wave-absorbing material derived from metal organic framework and preparation method thereof |
| CN112533466A (en) * | 2020-12-02 | 2021-03-19 | 中国人民解放***箭军工程大学 | MOFs derived porous carbon coated sheet carbonyl iron composite wave-absorbing material and preparation method thereof |
| CN113423256A (en) * | 2021-07-15 | 2021-09-21 | 华东理工大学 | Composite wave-absorbing material and preparation method and application thereof |
| CN113423256B (en) * | 2021-07-15 | 2022-04-19 | 华东理工大学 | Composite wave-absorbing material and preparation method and application thereof |
| CN114149786A (en) * | 2021-12-08 | 2022-03-08 | 陕西铁路工程职业技术学院 | Interface polarization enhanced TiO2Preparation method of/RGO wave-absorbing material |
| CN114149786B (en) * | 2021-12-08 | 2023-08-04 | 陕西铁路工程职业技术学院 | Interface polarization enhanced TiO 2 Preparation method of RGO wave-absorbing material |
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| CN116063082A (en) * | 2022-11-16 | 2023-05-05 | 哈尔滨工业大学（威海） | Silicon oxide coated graphene composite wave-absorbing material and preparation method thereof |
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