CN106753237A - A kind of Graphene/ferroso-ferric oxide composite wave-suction material and preparation method thereof - Google Patents
A kind of Graphene/ferroso-ferric oxide composite wave-suction material and preparation method thereof Download PDFInfo
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Abstract
The present invention is applied to absorbing material field, there is provided a kind of Graphene/ferroso-ferric oxide composite wave-suction material and preparation method thereof.The preparation method is comprised the following steps：Prepare graphene oxide dispersion, FeCl2Solution and FeCl3Solution；Above-mentioned three kinds of liquid is mixed, is stirred 23 hours under 80 120 degree, obtain graphene oxide/Fe3O4Dispersion liquid；By the graphene oxide/Fe3O4Dispersion liquid is vacuum dried, and obtains graphene oxide/Fe3O4Aeroge；By the graphene oxide/Fe3O4Aeroge is heated, and obtains Graphene/Fe3O4Aeroge, by the Graphene/Fe3O4Aeroge carries out Mechanical pressing, obtains Graphene/Fe3O4Composite；Graphene/the Fe3O4Composite is the layer structure of lamella stacking.Graphene/Fe that the present invention is provided3O4The electromagnetic performance matching feature of composite wave-suction material makes it more absorb rather than reflection electromagnetic wave, so as to reduce secondary pollution of the electromagnetic wave to environment.
Description
Technical field
The invention belongs to absorbing material field, more particularly to a kind of Graphene/ferroso-ferric oxide composite wave-suction material and its
Preparation method.
Background technology
Absorbing material refers to that can absorb the electromagnetic wave energy for projecting its surface, and by the dielectric loss of material by electromagnetism
Wave energy is converted to the material of the energy of heat energy or other forms.With modern science and technology technology develop rapidly and people are to strong
The continuous improvement of health quality requirement, the research and development of new and effective absorbing material are by extensive concern.
Graphene is a kind of two-dimensional material of only single carbon atom thickness, and Graphene not only has excellent mechanics, heat
Learn and electric property, but also with good Microwave Absorption Properties.The lamellar structure of Graphene is conducive to improving multiple reflections
Loss, the high conductivity of Graphene advantageously forms good conductive network, reaches the effect of electro-magnetic wave absorption, especially in X ripples
Duan Xiaoguo becomes apparent, and the Graphene of two-dimensional slice structure has advantageous advantage in absorbing material field.Ferrite is inhaled
Wave material is iron-series metal oxide or composite oxides, belongs to ferrimagnetic material.Its absorbing property from ferromagnetism and
Dielectric properties, its relative permeability and relative dielectric constant are in plural form, and dielectric loss can be produced to produce magnetic loss again
Consumption, therefore with good absorbing property.Simultaneously because its resistivity is higher, electromagnetic wave is easily entered and rapid decay, can be made
It remains to keep magnetic conductivity high in high frequency.But because its density is big, the deficiency such as hot properties difference is generally combined and
Obtain good absorbing material.
In Graphene/ferriferrous oxide composite material prepared by traditional method, ferroferric oxide magnetic nanoparticle is difficult
Obtain fully dispersed with graphene oxide substrate；And during reduction, due to the addition of the reducing agents such as hydrazine hydrate, not only
With toxicity, and pollution environment, the recovery time is long, wastes the energy；The Graphene of preparation/ferriferrous oxide composite material conductance
Rate is low, so as to have impact on wave-absorbing effect.In addition, Graphene/ferriferrous oxide composite material prepared by conventional method is usually powder
Last structure, density is big, it is difficult to which film forming, absorption band is narrow, and absorbing property is poor.
Therefore, prior art could be improved.
The content of the invention
In order to solve the above technical problems, the present invention provides a kind of Graphene/ferroso-ferric oxide composite wave-suction material and its system
Preparation Method, it is intended to improve existing Graphene/Fe3O4The performance of composite.
The present invention is achieved in that a kind of preparation method of Graphene/ferroso-ferric oxide composite wave-suction material, including with
Lower step：
Prepare graphene oxide dispersion, FeCl2Solution and FeCl3Solution；
Above-mentioned three kinds of liquid is mixed, is stirred in 80-120 degree and mixed, obtain graphene oxide/Fe3O4Dispersion liquid；
By the graphene oxide/Fe3O4Dispersion liquid is vacuum dried, and obtains graphene oxide/Fe3O4Aeroge；
By the graphene oxide/Fe3O4Aeroge is heated, and obtains Graphene/Fe3O4Aeroge, by the Graphene/
Fe3O4Aeroge carries out Mechanical pressing, obtains Graphene/Fe3O4Composite；Graphene/the Fe3O4Composite is lamella
The layer structure of stacking.
Further, the preparation process of the graphene oxide dispersion includes：Graphene oxide is soluble in water, ultrasound
Treatment 30-40min；The concentration of the graphene oxide dispersion is 0.1-10mg/ml, FeCl2The concentration of solution is 10-
20mg/ml, FeCl3The concentration of solution is 20-30mg/ml.
Further, the graphene oxide dispersion, FeCl2Solution and FeCl3The volume ratio of solution is 5-10:1-3:
2-4。
Further, the graphene oxide/Fe3O4Fe in dispersion liquid3O4Content is 10-50%, the Fe3O4Grain
Footpath is 20-60nm.
Further, the vacuum drying temperature is 60-80 degree, and the time is 18-24h.
Further, the heating-up temperature is 200-400 DEG C, and the time is 2-4 hours.
Further, the Graphene/Fe3O4The density of aeroge is 0.1-1g/cm3。
Further, the Graphene/Fe3O4The thickness of composite is 0.01-5nm.
Further, the Graphene/Fe3O4The thickness of composite is 1-2 μm, and it is 25-62dB to inhale ripple efficiency.
Present invention also offers a kind of Graphene/ferroso-ferric oxide composite wave-suction material, using above-mentioned preparation method system
Into.
Compared with prior art, beneficial effect is the present invention：Graphene/ferroso-ferric oxide provided in an embodiment of the present invention
The preparation method of composite wave-suction material, makes full use of in graphene oxide rich in-OH, the functional group such as-COOH, can be as nucleation
Site, with iron ion and ferrous ion reaction generation Fe3O4.The preparation method first uses graphene oxide dispersion, FeCl2
Solution and FeCl3Solution prepares graphene oxide/Fe3O4Aeroge, Fe3O4Uniform load is in the surface of Graphene carrier and piece
Layer；Again by graphene oxide/Fe3O4Graphene oxide reduction in aeroge, is derived from the stone of the layer structure of lamella stacking
Black alkene/Fe3O4Composite wave-suction material.
In the Graphene/Fe3O4In composite wave-suction material, magnetic nanoparticle --- Fe3O4Uniform load is in Graphene
The surface of carrier and lamella, not only density is light, intensity is high for the composite wave-suction material of formation, and has magnetic loss and electrical loss concurrently,
And dielectric constant is adjustable.Graphene/the Fe3O4The electromagnetic performance matching feature of composite wave-suction material makes its more absorption
Rather than reflection electromagnetic wave, so as to reduce secondary pollution of the electromagnetic wave to environment.
Brief description of the drawings
Fig. 1 is Graphene/Fe provided in an embodiment of the present invention3O4The photo of composite wave-suction material；
Fig. 2 is Graphene/Fe provided in an embodiment of the present invention3O4The SEM figures of composite wave-suction material, wherein Fig. 2 a are surface
Shape appearance figure, Fig. 2 b are construction profile；
Fig. 3 a be it is provided in an embodiment of the present invention be Graphene/Fe3O4The XRD of composite wave-suction material, Fig. 3 b are graphite
Alkene/Fe3O4The Raman spectrogram of composite wave-suction material；
Fig. 4 is the Graphene/Fe of different-thickness provided in an embodiment of the present invention3O4The suction ripple effect test knot of composite
Fruit is schemed.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The embodiment of the invention provides a kind of preparation method of Graphene/ferroso-ferric oxide composite wave-suction material, including with
Lower step：
Prepare graphene oxide dispersion, FeCl2Solution and FeCl3Solution；
Above-mentioned three kinds of liquid is mixed, mixing 2-3 hours is stirred under 80-120 degree (preferably 100 degree), obtain oxidation stone
Black alkene/Fe3O4Dispersion liquid；
By the graphene oxide/Fe3O4Dispersion liquid is vacuum dried, and obtains graphene oxide/Fe3O4Aeroge；
By the graphene oxide/Fe3O4Aeroge is heated, and obtains Graphene/Fe3O4Aeroge, by the Graphene/
Fe3O4Aeroge carries out Mechanical pressing, obtains Graphene/Fe3O4Composite；Graphene/the Fe3O4Composite is lamella
The layer structure of stacking.
The preparation method of Graphene provided in an embodiment of the present invention/ferroso-ferric oxide composite wave-suction material, makes full use of oxygen
The functional groups such as-OH ,-COOH are rich in graphite alkene, can be as nucleation site, with iron ion and ferrous ion reaction generation
Fe3O4.The preparation method first uses graphene oxide dispersion, FeCl2Solution and FeCl3Solution prepare graphene oxide/
Fe3O4Aeroge, Fe3O4Uniform load is in the surface of Graphene carrier and lamella；Again by graphene oxide/Fe3O4In aeroge
Graphene oxide reduction, be derived from lamella stacking layer structure Graphene/Fe3O4Composite wave-suction material.
In the Graphene/Fe3O4In composite wave-suction material, magnetic nanoparticle --- Fe3O4Uniform load is in Graphene
The surface of carrier and lamella, not only density is light, intensity is high for the composite wave-suction material of formation, and has magnetic loss and electrical loss concurrently,
And dielectric constant is adjustable.Graphene/the Fe3O4The electromagnetic performance matching feature of composite wave-suction material makes its more absorption
Rather than reflection electromagnetic wave, so as to reduce secondary pollution of the electromagnetic wave to environment.
Specifically, the preparation process of the graphene oxide dispersion includes：Graphene oxide is soluble in water, at ultrasound
Reason 30-40min；The concentration of the graphene oxide dispersion is 0.1-10mg/ml, FeCl2The concentration of solution is 10-20mg/
Ml, FeCl3The concentration of solution is 20-30mg/ml.The graphene oxide dispersion, FeCl2Solution and FeCl3The volume of solution
Than being 5-10:1-3:2-4, preferably 6:1:2.
Graphene oxide/the Fe3O4Fe in dispersion liquid3O4Content is 10-50%.Fe3O4Content is too low, magnetic Nano
The wave-absorbing effect of particle is not obvious；Too high levels not only waste consumptive material, and increase the weight of composite.The Fe3O4Grain
Footpath is 20-60nm, and the particle diameter is controlled by the concentration and reaction time of iron ion and ferrous ion.The particle size can
To ensure Fe3O4Equably it is supported on surface and the lamella of Graphene carrier.
The vacuum drying temperature is 60-80 degree, and the time is 18-24h, 60 degree of preferable temperature, time 24h.It is described to add
Hot temperature is 200-400 DEG C, and the time is 2-4 hours.It is adjusted by the temperature and time to the heating, control is obtained
Graphene/Fe3O4The density of aeroge.Graphene/the Fe3O4The density of aeroge is 0.1-1g/cm3。
Specifically, the Graphene/Fe3O4The thickness of composite is 0.01-5 μm.
Graphene/the Fe3O4The thickness of composite is 1-2 μm, and it is 25-62dB to inhale ripple efficiency.
The Mechanical pressing is by the Graphene/Fe3O4Aeroge is placed in 10-20MPa, is preferably carried out under 15MPa pressure
Mechanical pressing, obtained Graphene/Fe can be controlled by the size for adjusting mechanical pressure3O4The thickness of composite.
The embodiment of the present invention additionally provides a kind of Graphene/ferroso-ferric oxide composite wave-suction material, using above-mentioned preparation
Method is made.
Fig. 1 is the Graphene/Fe prepared according to technical scheme3O4The photo of composite wave-suction material, it is described compound
Absorbing material can according to demand be made the different size of films of 1cm × 1cm to 10cm × 10cm, and thickness can for 0.01-5nm
Adjust.
Fig. 2 is Graphene/Fe3O4The SEM figures (electron scanning imaging figure) of composite wave-suction material, wherein Fig. 2 a are surface shape
Looks figure, Fig. 2 b are construction profile.From figure 2 it can be seen that Graphene/the Fe3O4It is the layer structure of lamella stacking, stone
Black alkene shows the pleated structure of gel, and ferroferric oxide nano granules are evenly distributed in the surface of graphene sheet layer.
Fig. 3 a are Graphene/Fe3O4The XRD (X-ray diffractogram) of composite wave-suction material, it can be seen that typical
Ferroso-ferric oxide characteristic peak can be observed out, and the characteristic peak without graphene oxide illustrates graphene oxide
Thoroughly it has been reduced into Graphene.Fig. 3 b are Graphene/Fe3O4The Raman spectrogram of composite wave-suction material, can observe from figure
To the raman characteristic peak of Graphene.
Graphene paper/the Fe of the different-thickness that will be prepared according to technical scheme3O4Composite carries out inhaling ripple effect
Can test, as a result as shown in Figure 4.It can be seen that the composite wave-suction material is under thin thickness (2mm), ripple effect is inhaled
Can reach 62dB.This is unapproachable in lightweight composite before, and composite has absorption band (2- wide
18GHz), the characteristics of suction ripple efficiency is good.
Graphene/Fe prepared by the embodiment of the present invention3O4Composite wave-suction material have light weight, thickness of thin, intensity it is high, inhale
Bandwidth is received, the characteristics of absorbing property is good, is had in radome, Medical Devices, electronic equipment or even military field and widely should
Use prospect.
Technical scheme is described in detail below in conjunction with specific embodiment.
Embodiment 1
The preparation of graphene oxide：Graphene oxide is prepared using Hummer methods, ultrasound prepares graphene oxide after peeling off
Dispersion liquid, concentration is 0.8mg/ml；
Graphene paper/Fe3O4The preparation of composite wave-suction material：
0.4g graphene oxide powders are dissolved in 100ml water, ultrasonic 35min, supersonic frequency is dense for 200-300Hz is formed
Spend the graphene oxide dispersion for 4mg/ml；
Weigh 0.4g FeCl2·4H2O is simultaneously dissolved in 20ml water, weighs 1g FeCl3·6H2O is simultaneously dissolved in 40ml water；
The above-mentioned solution for preparing is added in the graphene oxide solution, is stirred 2.5 hours under 100 degree, formed
Graphene oxide/Fe3O4Uniform dispersion liquid (wherein Fe3O4Content be 25%, Fe3O4Particle diameter be 30nm)；
By graphene oxide/Fe3O4Dispersion liquid freeze-drying 24h under vacuo, forms graphene oxide/Fe3O4Airsetting
Glue；
By graphene oxide/Fe3O4Aeroge is heated 3 hours in the electric furnace at 300 DEG C, forms Graphene/Fe3O4Airsetting
(density of aeroge is 0.5g/cm to glue3)；
By Graphene/Fe3O4Aeroge forms graphene paper/Fe in 15MPa mechanical pressure lower sheetings3O4Composite wave-absorbing material
Material.
Embodiment 2
The preparation of graphene oxide：Graphene oxide is prepared using Hummer methods, ultrasound prepares graphene oxide after peeling off
Dispersion liquid, concentration is 7.5mg/ml；
Graphene paper/Fe3O4The preparation of composite wave-suction material：
0.4g graphene oxide powders are dissolved in 100ml water, ultrasonic 40min, supersonic frequency is 200-300Hz, are formed
Concentration is the graphene oxide dispersion of 4mg/ml；
Weigh 0.4g FeCl2·4H2O is simultaneously dissolved in 20ml water, weighs 1g FeCl3·6H2O is simultaneously dissolved in 40ml water；
The above-mentioned solution for preparing is added in the graphene oxide solution, is stirred 3 hours under 100 degree, form oxygen
Graphite alkene/Fe3O4Uniform dispersion liquid (wherein Fe3O4Content be 45%, Fe3O4Particle diameter be 45nm)；
By graphene oxide/Fe3O4Dispersion liquid freeze-drying 24h under vacuo, forms graphene oxide/Fe3O4Airsetting
Glue；
By graphene oxide/Fe3O4Aeroge is heated 2.6 hours in the electric furnace at 220 DEG C, forms Graphene/Fe3O4Gas
(density of aeroge is 0.3g/cm to gel3)；
By Graphene/Fe3O4Aeroge forms graphene paper/Fe in 15MPa mechanical pressure lower sheetings3O4Composite wave-absorbing material
Material.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (10)
1. the preparation method of a kind of Graphene/ferroso-ferric oxide composite wave-suction material, it is characterised in that comprise the following steps：
Prepare graphene oxide dispersion, FeCl2Solution and FeCl3Solution；
Above-mentioned three kinds of liquid is mixed, is stirred in 80-120 degree and mixed, obtain graphene oxide/Fe3O4Dispersion liquid；
By the graphene oxide/Fe3O4Dispersion liquid is vacuum dried, and obtains graphene oxide/Fe3O4Aeroge；
By the graphene oxide/Fe3O4Aeroge is heated, and obtains Graphene/Fe3O4Aeroge, by the Graphene/Fe3O4
Aeroge carries out Mechanical pressing, obtains Graphene/Fe3O4Composite；Graphene/the Fe3O4Composite is stacked for lamella
Layer structure.
2. preparation method as claimed in claim 1, it is characterised in that the preparation process bag of the graphene oxide dispersion
Include：Graphene oxide is soluble in water, ultrasonically treated 30-40min；The concentration of the graphene oxide dispersion is 0.1-
10mg/ml, the FeCl2The concentration of solution is 10-20mg/ml, the FeCl3The concentration of solution is 20-30mg/ml.
3. preparation method as claimed in claim 2, it is characterised in that the graphene oxide dispersion, FeCl2Solution and
FeCl3The volume ratio of solution is 5-10:1-3:2-4.
4. preparation method as claimed in claim 1, it is characterised in that the graphene oxide/Fe3O4Fe in dispersion liquid3O4
Content is 10-50%, the Fe3O4Particle diameter be 20-60nm.
5. preparation method as claimed in claim 1, it is characterised in that the vacuum drying temperature is 60-80 degree, the time is
18-24h。
6. preparation method as claimed in claim 1, it is characterised in that the heating-up temperature is 200-400 DEG C, and the time is 2-4
Hour.
7. preparation method as claimed in claim 1, it is characterised in that the Graphene/Fe3O4The density of aeroge is 0.1-
1g/cm3。
8. preparation method as claimed in claim 1, it is characterised in that the Graphene/Fe3O4The thickness of composite is
0.01-5nm。
9. preparation method as claimed in claim 1, it is characterised in that the Graphene/Fe3O4The thickness of composite is 1-2
μm, it is 25-62dB to inhale ripple efficiency.
10. a kind of Graphene/ferroso-ferric oxide composite wave-suction material, it is characterised in that use claim 1 to 9 any one
Described preparation method is made.
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