CN107974236A - A kind of graphene/ferroso-ferric oxide absorbing meta-material and preparation method thereof - Google Patents
A kind of graphene/ferroso-ferric oxide absorbing meta-material and preparation method thereof Download PDFInfo
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- CN107974236A CN107974236A CN201610938419.0A CN201610938419A CN107974236A CN 107974236 A CN107974236 A CN 107974236A CN 201610938419 A CN201610938419 A CN 201610938419A CN 107974236 A CN107974236 A CN 107974236A
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Abstract
The present invention provides a kind of graphene/ferroso-ferric oxide (Fe3O4) absorbing meta-material and preparation method thereof, this method includes：Prepare graphene oxide；A certain amount of graphene oxide is taken afterwards, is sufficiently stirred and is dissolved in ethylene glycol, and ultrasound, adds FeCl3Solution in, fully reaction is dry by product filtering and washing, obtains graphene oxide/Fe2O3Composite material；And by the graphene oxide/Fe2O3Composite material is placed under nitrogen atmosphere, and calcining, obtains graphene/Fe3O4Absorbing meta-material.This method is simple and practicable, and is related to less chemical reagent, and environment will not be polluted.
Description
Technical field
The present invention relates to absorbing material field, more particularly, to a kind of graphene/Fe3O4Absorbing meta-material and its preparation
Method.
Background technology
With the rapid development of modern Detection Techniques and precision guided weapon, the requirement to absorbing meta-material is higher and higher,
Single absorbing meta-material is difficult to meet integration requirement, and therefore, composite wave-absorbing Meta Materials are increasingly becoming the hot spot of research.
Fe3O4It is double damage media with good absorbing property, the loss to electromagnetic wave includes magnetic loss, ion and electronics
Resonant loss, polarization loss etc., therefore electromagnetic wave absorbent material can be used as, but Fe3O4Itself easily reunites.Graphene is unique
Single layer structure make it have big specific surface area, the features such as electric conductivity is excellent, itself has electrical loss to electromagnetic wave, is a kind of
Preferable carrier.
In the patent Shen of disclosed Application No. 201510016209.1,201510016214.2 and 201510016271.0
Please in, although ferroso-ferric oxide is successfully loaded to graphene surface, method (for example, solvent-thermal method) step used is numerous
It is trivial, and to be related to organic reagent more for reaction process, the problems such as be easy to causeing environmental pollution.
The content of the invention
The present invention is by using hydro-thermal method synthesizing graphite alkene and Fe3O4Composite material, preparation method is simple and practicable, inhales ripple effect
Fruit is good, and the organic reagent involved in reaction is few, is conducive to environmental protection, will not cause environmental pollution etc..
The present invention provides one kind to prepare graphene/Fe3O4The method of absorbing meta-material, including：Graphene is put into appearance
In device, the concentrated sulfuric acid is added, is transferred to after stirring in ice-water bath, add KMnO4, adding procedure is maintained at the first temperature, stirring the
It is transferred to after one time in oil bath, is heated to second temperature in oil bath and reacted for the second time, reactant is down to room temperature,
Pour into the beaker for filling ice, be stirred continuously, hydrogen peroxide is added dropwise in most backward reactant, and the first obtained product is carried out centrifugation and is washed
Wash, washed respectively with water, absolute ethyl alcohol afterwards, dry 3rd time, obtains graphene oxide at a temperature of the 3rd；Stone will be aoxidized
Black alkene is dissolved in ethylene glycol, and ultrasound, then adds FeCl3Solution in, at a temperature of the 4th react the 4th time, by second
Product filtering and washing, dry 5th time, obtains graphene oxide/Fe at a temperature of the 5th2O3Composite material；And by described in
Graphene oxide/Fe2O3Composite material is placed under nitrogen atmosphere, in the 6th time of the 6th temperature lower calcination, obtain graphene/
Fe3O4Absorbing meta-material.
In the above-mentioned methods, wherein, the graphene, the concentrated sulfuric acid, the KMnO4With the mass ratio of the hydrogen peroxide
For 1:110:6:2.
In the above-mentioned methods, wherein, first temperature≤4 DEG C, the first time >=20min.
In the above-mentioned methods, wherein, the second temperature is 50 DEG C, and the second time was 6h.
In the above-mentioned methods, wherein, the 3rd temperature is 60 DEG C, and the 3rd time was 24h.
In the above-mentioned methods, wherein, the graphene oxide, the ethylene glycol and the FeCl3Mass ratio be 30:
55:10-500。
In the above-mentioned methods, wherein, the 4th temperature is 100-160 DEG C, and the 4th time is 1-2h.
In the above-mentioned methods, wherein, the 5th temperature is 60 DEG C, and the 5th time is 24h.
In the above-mentioned methods, wherein, the 6th temperature is 450 DEG C, and the 6th time is 3h.
In the above-mentioned methods, wherein, the container includes there-necked flask, and the hydrogen peroxide is the dioxygen that mass fraction is 30%
Water.
In the above-mentioned methods, wherein, the first obtained product is carried out centrifuge washing includes with mass fraction being 10%
Obtained first product is carried out centrifuge washing by dilute hydrochloric acid.
Present invention also offers a kind of graphene/Fe prepared according to above method3O4Absorbing meta-material.
Graphene/Fe is prepared by kind provided by the invention3O4The method of absorbing meta-material, enormously simplify to form graphite
Alkene/Fe3O4The step of absorbing meta-material, and the organic reagent that reaction process is related to is less, and environment will not be polluted.
The present invention has synthesized the good graphene/Fe of absorbing property using hydro-thermal method3O4Absorbing meta-material, by determining to close
Graphene oxide and FeCl during3Mass ratio, reaction temperature and reaction time, synthesized comprehensive graphene and Fe3O4's
The absorbing meta-material of performance, had not only met the performance requirement to composite material, but also enormously simplify preparation process, had saved reaction
Time.In graphene oxide/Fe2O3The preparation of composite material and graphene/Fe3O4During the preparation of absorbing meta-material, only use
Ethylene glycol solvent, other steps are simple and practicable and without reference to organic solvent, and therefore, environment will not be polluted.
Brief description of the drawings
Fig. 1 is graphene/Fe3O4Absorbing meta-material synthesis process flow diagram.
Embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit in any way
The present invention.
Graphene powder is put into three-necked flask, adds the concentrated sulfuric acid, is transferred to after stirring 1-2h in ice-water bath, slowly
Add KMnO4, adding procedure keeps temperature≤4 DEG C, is transferred in oil bath after stirring >=20min, is heated to 50 DEG C in oil bath
And 6h is reacted, after question response, reactant is down to room temperature, is poured slowly into the beaker for filling 400-600mg ice, constantly
The hydrogen peroxide that mass fraction is 30% is added dropwise in stirring, most backward reactant, by obtained product mass fraction be 10% it is dilute
Hydrochloric acid carries out centrifuge washing, is washed respectively with water, absolute ethyl alcohol afterwards, dry 24h at 60 DEG C, up to graphene oxide.Graphite
Alkene powder, the concentrated sulfuric acid, KMnO4Mass ratio with hydrogen peroxide can be 1:110:6:2.
A certain amount of graphene oxide is taken, is sufficiently stirred and is dissolved in ethylene glycol, ultrasonic 1-2h, adds FeCl3Solution
In, fully reaction 1-24h at 100-160 DEG C, by product filtering and washing, dry 24h at 60 DEG C, up to graphene oxide/Fe2O3
Composite material.Graphene oxide, ethylene glycol and FeCl3Mass ratio can be 30:55:10-500.
By the graphene oxide/Fe2O3Composite material is placed under nitrogen atmosphere, and 3h is calcined at 450 DEG C, up to graphene/
Fe3O4Absorbing meta-material.
Embodiment one
6g graphene powders are put into three-necked flask, add the 360mL concentrated sulfuric acids, ice-water bath is transferred to after stirring 1h
In, it is slowly added to 36g KMnO4, 4 DEG C of adding procedure holding, is transferred in oil bath after stirring 20min, is heated to 50 in oil bath
DEG C and react 6h, after question response, reactant is down to room temperature, is poured slowly into the beaker for filling 500mg ice, constantly stirs
To mix, the hydrogen peroxide of 10mL 30% is added dropwise in most backward reactant, and obtained product is carried out centrifuge washing with 10% dilute hydrochloric acid,
Washed respectively with water, absolute ethyl alcohol afterwards, dry 24h at 60 DEG C, up to graphene oxide.
30mg graphene oxides are taken, is sufficiently stirred and is dissolved in 50mL ethylene glycol, ultrasonic 1h, adds 10mg FeCl3It is molten
In liquid, fully reaction 1h at 100 DEG C, by product filtering and washing, dry 24h at 60 DEG C, up to graphene oxide/Fe2O3Composite wood
Material.
By the graphene oxide/Fe2O3Composite material is placed under nitrogen atmosphere, and 3h is calcined at 450 DEG C, up to graphene/
Fe3O4Absorbing meta-material.
Embodiment two
6g graphene powders are put into three-necked flask, add the 360mL concentrated sulfuric acids, ice-water bath is transferred to after stirring 2h
In, it is slowly added to 36g KMnO4, 3 DEG C of adding procedure holding, is transferred in oil bath after stirring 25min, is heated to 50 in oil bath
DEG C and react 6h, after question response, reactant is down to room temperature, is poured slowly into the beaker for filling 600mg ice, constantly stirs
To mix, the hydrogen peroxide of 10mL 30% is added dropwise in most backward reactant, and obtained product is carried out centrifuge washing with 10% dilute hydrochloric acid,
Washed respectively with water, absolute ethyl alcohol afterwards, dry 24h at 60 DEG C, up to graphene oxide.
30mg graphene oxides are taken, is sufficiently stirred and is dissolved in 50mL ethylene glycol, ultrasonic 1.5h, adds 200mg FeCl3
Solution in, fully reaction 12h at 130 DEG C, by product filtering and washing, dry 24h at 60 DEG C, up to graphene oxide/Fe2O3
Composite material.
By the graphene oxide/Fe2O3Composite material is placed under nitrogen atmosphere, and 3h is calcined at 450 DEG C, up to graphene/
Fe3O4Absorbing meta-material.
Embodiment three
6g graphene powders are put into three-necked flask, add the 360mL concentrated sulfuric acids, ice-water bath is transferred to after stirring 1.5h
In, it is slowly added to 36g KMnO4, 4 DEG C of adding procedure holding, is transferred in oil bath after stirring 25min, is heated to 50 in oil bath
DEG C and react 6h, after question response, reactant is down to room temperature, is poured slowly into the beaker for filling 400mg ice, constantly stirs
To mix, the hydrogen peroxide of 10mL 30% is added dropwise in most backward reactant, and obtained product is carried out centrifuge washing with 10% dilute hydrochloric acid,
Washed respectively with water, absolute ethyl alcohol afterwards, dry 24h at 60 DEG C, up to graphene oxide.
30mg graphene oxides are taken, is sufficiently stirred and is dissolved in 50mL ethylene glycol, ultrasonic 2h, adds 500mg FeCl3's
In solution, fully reaction 24h at 160 DEG C, by product filtering and washing, dry 24h at 60 DEG C, up to graphene oxide/Fe2O3It is multiple
Condensation material.
By the graphene oxide/Fe2O3Composite material is placed under nitrogen atmosphere, and 3h is calcined at 450 DEG C, up to graphene/
Fe3O4Absorbing meta-material.
Example IV
6g graphene powders are put into three-necked flask, add the 360mL concentrated sulfuric acids, ice-water bath is transferred to after stirring 1h
In, it is slowly added to 36g KMnO4, 2 DEG C of adding procedure holding, is transferred in oil bath after stirring 25min, is heated to 50 in oil bath
DEG C and react 6h, after question response, reactant is down to room temperature, is poured slowly into the beaker for filling 500mg ice, constantly stirs
To mix, the hydrogen peroxide of 10mL 30% is added dropwise in most backward reactant, and obtained product is carried out centrifuge washing with 10% dilute hydrochloric acid,
Washed respectively with water, absolute ethyl alcohol afterwards, dry 24h at 60 DEG C, up to graphene oxide.
30mg graphene oxides are taken, is sufficiently stirred and is dissolved in 50mL ethylene glycol, ultrasonic 2h, adds 300mg FeCl3's
In solution, fully reaction 24h at 150 DEG C, by product filtering and washing, dry 24h at 60 DEG C, up to graphene oxide/Fe2O3It is multiple
Condensation material.
By the graphene oxide/Fe2O3Composite material is placed under nitrogen atmosphere, and 3h is calcined at 450 DEG C, up to graphene/
Fe3O4Absorbing meta-material.
Embodiment five
3g graphene powders are put into three-necked flask, add the 180mL concentrated sulfuric acids, ice-water bath is transferred to after stirring 1h
In, it is slowly added to 18g KMnO4, 4 DEG C of adding procedure holding, is transferred in oil bath after stirring 20min, is heated to 50 in oil bath
DEG C and react 6h, after question response, reactant is down to room temperature, is poured slowly into the beaker for filling 400mg ice, constantly stirs
To mix, the hydrogen peroxide of 5mL 30% is added dropwise in most backward reactant, and obtained product is carried out centrifuge washing with 10% dilute hydrochloric acid, it
Washed respectively with water, absolute ethyl alcohol afterwards, dry 24h at 60 DEG C, up to graphene oxide.
15mg graphene oxides are taken, is sufficiently stirred and is dissolved in 25mL ethylene glycol, ultrasonic 1h, adds 5mg FeCl3It is molten
In liquid, fully reaction 1h at 160 DEG C, by product filtering and washing, dry 24h at 60 DEG C, up to graphene oxide/Fe2O3Composite wood
Material.
By the graphene oxide/Fe2O3Composite material is placed under nitrogen atmosphere, and 3h is calcined at 450 DEG C, up to graphene/
Fe3O4Absorbing meta-material.
Embodiment six
3g graphene powders are put into three-necked flask, add the 180mL concentrated sulfuric acids, ice-water bath is transferred to after stirring 1.5h
In, it is slowly added to 18g KMnO4, 3 DEG C of adding procedure holding, is transferred in oil bath after stirring 20min, is heated to 50 in oil bath
DEG C and react 6h, after question response, reactant is down to room temperature, is poured slowly into the beaker for filling 400mg ice, constantly stirs
To mix, the hydrogen peroxide of 5mL 30% is added dropwise in most backward reactant, and obtained product is carried out centrifuge washing with 10% dilute hydrochloric acid, it
Washed respectively with water, absolute ethyl alcohol afterwards, dry 24h at 60 DEG C, up to graphene oxide.
15mg graphene oxides are taken, is sufficiently stirred and is dissolved in 25mL ethylene glycol, ultrasonic 1.5h, adds 250mg FeCl3
Solution in, fully reaction 24h at 160 DEG C, by product filtering and washing, dry 24h at 60 DEG C, up to graphene oxide/Fe2O3
Composite material.
By the graphene oxide/Fe2O3Composite material is placed under nitrogen atmosphere, and 3h is calcined at 450 DEG C, up to graphene/
Fe3O4Absorbing meta-material.
The present invention has synthesized graphene and Fe using hydro-thermal method3O4Composite material, the composite material overcome single suction ripple and surpass
The deficiency of material, and using the big advantage of graphene specific surface area, make Fe3O4Its surface is preferably loaded to, is overcome
Fe3O4The shortcomings that easily reuniting, Fe is given full play to3O4Good absorbing property, be prepared for it is of good performance suction ripple surpass material
Material, while preparation method is simple and practicable, the organic reagent involved in reaction is few, is conducive to environmental protection, and environment will not be caused dirty
Dye etc..
It will be understood by those skilled in the art that above example is only exemplary embodiment, in the spirit without departing substantially from the present invention
In the case of scope, a variety of changes can be carried out, replaces and changes.
Claims (12)
1. one kind prepares graphene/Fe3O4The method of absorbing meta-material, it is characterised in that including：
Graphene is put into container, the concentrated sulfuric acid is added, is transferred to after stirring in ice-water bath, adds KMnO4, adding procedure guarantor
Hold in the first temperature, be transferred to after stirring first time in oil bath, when being heated to second temperature in oil bath and reacting second
Between, reactant is down to room temperature, is poured into the beaker for filling ice, is stirred continuously, hydrogen peroxide is added dropwise in most backward reactant, will obtain
The first product carry out centrifuge washing, washed respectively with water, absolute ethyl alcohol afterwards, at a temperature of the 3rd dry the 3rd time, obtain
To graphene oxide；
Graphene oxide is dissolved in ethylene glycol, ultrasound, then adds FeCl3Solution in, at a temperature of the 4th react the 4th
Time, by the second product filtering and washing, dry 5th time, obtains graphene oxide/Fe at a temperature of the 5th2O3Composite material；
And
By the graphene oxide/Fe2O3Composite material is placed under nitrogen atmosphere, in the 6th time of the 6th temperature lower calcination, is obtained
Graphene/Fe3O4Absorbing meta-material.
2. according to the method described in claim 1, it is characterized in that, the graphene, the concentrated sulfuric acid, the KMnO4With it is described
The mass ratio of hydrogen peroxide is 1:110:6:2.
3. according to the method described in claim 1, it is characterized in that, first temperature≤4 DEG C, the first time >=
20min。
4. according to the method described in claim 1, it is characterized in that, the second temperature is 50 DEG C, the second time was 6h.
5. according to the method described in claim 1, it is characterized in that, the 3rd temperature is 60 DEG C, the 3rd time was 24h.
6. according to the method described in claim 1, it is characterized in that, the graphene oxide, the ethylene glycol and the FeCl3
Mass ratio be 30:55:10-500.
7. according to the method described in claim 1, it is characterized in that, the 4th temperature be 100-160 DEG C, the 4th time
For 1-2h.
8. according to the method described in claim 1, it is characterized in that, the 5th temperature is 60 DEG C, the 5th time is
24h。
9. according to the method described in claim 1, it is characterized in that, the 6th temperature is 450 DEG C, the 6th time is
3h。
10. according to the method described in claim 1, it is characterized in that, the container includes there-necked flask, the hydrogen peroxide is quality
Fraction is 30% hydrogen peroxide.
11. according to the method described in claim 1, it is characterized in that, the first obtained product is carried out centrifuge washing includes using
Obtained first product is carried out centrifuge washing by the dilute hydrochloric acid that mass fraction is 10%.
A kind of 12. graphene/Fe prepared by method according to any one of claim 1-113O4Absorbing meta-material.
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Cited By (1)
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| CN115000361A (en) * | 2022-04-25 | 2022-09-02 | 齐鲁工业大学 | Fe 3 Se 4 Graphene sodium battery negative electrode material and preparation method thereof |
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Application publication date: 20180501 |