CN107011540A - A kind of carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material, its preparation method and its prepared suction wave plate - Google Patents
A kind of carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material, its preparation method and its prepared suction wave plate Download PDFInfo
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- CN107011540A CN107011540A CN201710164993.XA CN201710164993A CN107011540A CN 107011540 A CN107011540 A CN 107011540A CN 201710164993 A CN201710164993 A CN 201710164993A CN 107011540 A CN107011540 A CN 107011540A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
Abstract
The invention discloses a kind of carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material, its preparation method and its prepared suction wave plate.Carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material, including carbonyl iron dust sandwich layer, the redox graphene layer for being wrapped in carbonyl iron dust sandwich layer periphery and the polyvinylpyrrolidone layer for being wrapped in graphene oxide layer periphery.Carbonyl iron/graphene of the present invention/polyvinylpyrrolidone composite wave-suction material preparation process is simple, electro-magnetic wave absorption ability is strong, it is low to act on bandwidth, cost, has important application value in microwave absorption, solution electromagnetic exposure and electromagnetic shielding etc. field.
Description
Technical field
The present invention relates to a kind of carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material, its preparation method and its
Prepared suction wave plate, belongs to absorbing material field.
Background technology
With the widespread adoption of radio communication device, integrated electronics and military radar, reduction electromagnetic pollution influence,
Eliminate electromagnetic interference, the demand of enhancing military equipment radar invisible ability increasingly urgent.Microwave absorbing material is a kind of with spy
Incident electromagnetic wave, can be converted into other types of energy, what is solved the above problems by the functional material of different electromagnetic performance
During show big advantage.
According to electromagnetic wave and the interaction mechanism of material, the design principle of absorbing material be Reasonable Regulation And Control dielectric constant and
Magnetic conductivity, satisfaction is matched with air impedance, while strengthening electromagnetic wave loss ability.Model split, absorbing material is lost by ripple is inhaled
Dielectric loss type and magnetic loss type can be divided into, microwave absorption is served as using electrically lossy material and magnetic loss consumption material respectively, realized
Absorption to electromagnetic wave.However, the wave absorbing agent of one-component can not simultaneously Effective Regulation electrical parameter and magnetic parameter, meanwhile, be based on
The absorbing material of one-component wave absorbing agent is also increasingly difficult in adapt to requirement more and more harsh in practical application.So, research and development
It is the effective way for improving absorbing material performance to have electricity, the composite wave absorbing agent of magnetic loss performance concurrently.Such as CN101521046A
A kind of binary composite wave-absorbing material is disclosed in " graphene film surface load magnetic alloy particle wave-absorbing material and preparation method thereof "
The preparation method of material, the maximum reflection loss -34.4dB in the range of test frequency range；A kind of CN103554908A " graphene/polyphenyl
A kind of preparation method of tri compound absorbing material is disclosed in amine/cobalt composite wave-suction material and preparation method ", in test frequency range
In the range of maximum reflection loss -30.71dB.But the useful effect frequency range of above-mentioned composite wave-suction material is all narrower, so as to limit
It is used.
The content of the invention
For all narrower etc. defect of the useful effect frequency range for solving composite wave-suction material in the prior art, the present invention provides one
Plant carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material, its preparation method and its prepared suction wave plate.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows：
A kind of carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material, including carbonyl iron dust sandwich layer, be wrapped in
The graphene layer of carbonyl iron dust sandwich layer periphery and the polyvinylpyrrolidone layer for being wrapped in graphene layer periphery, the material of graphene layer
Expect for graphene oxide, reduced graphene or graphene.
The application utilizes the high magnetic loss of carbonyl iron, the two-dimentional conductive structure of graphene and polyvinylpyrrolidone nano particle
Modification to graphene oxide, is prepared for tri compound wave absorbing agent, and the material has that preparation technology is simple, electro-magnetic wave absorption ability
By force, effect bandwidth and the low feature of cost.
In order to further widen the effect bandwidth of composite wave-suction material, carbonyl iron dust sandwich layer, redox graphene layer
Mass ratio with polyvinylpyrrolidone layer is 50:(1-3):(1-4).
The preparation method of above-mentioned carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material, including it is connected in order
Following steps：
1) carbonyl iron dust is milled to particle diameter for 0.5-3 μm；
2) it is that 4 ± 2mg/ml graphene dispersing solution and concentration are 2~8mg/ml polyvinylpyrrolidone to prepare concentration
The aqueous solution, graphene dispersing solution is graphene oxide dispersion, reduced graphene dispersion liquid or graphene dispersing solution；
3) by step 1) obtained by carbonyl iron dust and step 2) obtained by graphene dispersing solution and polyvinylpyrrolidone water
Solution reaction obtains magnetic precipitation, then dries, produces carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material, its
In, the mass ratio of carbonyl iron dust, graphene dispersing solution and aqueous povidone solution is 1:(100±10):(10±2).
In order to be further ensured that grinding effect, and then improve the magnetic particles and effect bandwidth of product, step 1)
To be 1 by mass ratio:(80±10):(10 ± 2) carbonyl iron dust, zirconium oxide bead and absolute ethyl alcohol mixing add ball mill, are turning
Speed filters under conditions of 1000 ± 200rpm, then ball milling 4 ± 1 hours naturally cools to room temperature and removes zirconium oxide bead, then
Dried in the case where temperature is 60 ± 10 DEG C of vacuum conditions to constant weight, obtain the carbonyl iron dust that particle diameter is 0.5-3 μm.
The application preferably carries out mechanical ball mill with planetary ball mill to carbonyl iron dust, and the particle diameter of carbonyl iron dust raw material used is
3-5 microns；The temperature of material is at 40-50 DEG C or so after above-mentioned ball milling；
In order to further improve product magnetic particles and effect bandwidth, step 2) in graphene oxide dispersion
Preparation method be：Graphene oxide dispersion is prepared using Hummer methods are improved.Further preferably, step 2) in graphite oxide
The preparation method of alkene dispersion liquid includes following steps connected in order：
2.1) it is 1 by mass ratio:(0.5±0.2):Graphite powder, the concentrated sulfuric acid and the sodium nitrate low whipping speed of (42.3 ± 5)
To mix 10 ± 2min under conditions of 200 ± 50rpm, then ice-water bath is cooled to less than 5 DEG C；
2.2) potassium permanganate powder of 4 ± 1 times of graphite powder quality is added into step 2.1) obtained by mixture in, stirring is anti-
30 ± 5min is answered, course of reaction temperature control is below 20 DEG C；
2.3) by step 2.2) resulting material is warming up to 35 ± 5 DEG C, reacts 30 ± 5min；
2.4) by step 2.3) deionized water of more than 40 times of graphite powder quality is added in resulting material, it is heated to 90 ± 10
DEG C, then 30 ± 5min of stirring reaction naturally cools to room temperature, the hydrogen peroxide that more than 5 times of addition graphite powder quality；
2.5) by step 2.4) resulting material after centrifuge washing and deionized water dialysis, adds deionized water to required dense
Degree, ultrasonic disperse obtains graphite oxide dispersion.
In order to more effectively ensure the quality of products obtained therefrom, graphite powder is the natural graphite powder that particle diameter is 300 ± 100 mesh；
The concentrated sulfuric acid is the concentrated sulfuric acid that mass concentration is 98%；The mass concentration of hydrogen peroxide is 3%.
In order to more effectively ensure gained composite uniformity and absorbing property, step 3) include it is connected in order as
Lower step：3.1) by carbonyl iron dust, watery hydrochloric acid, absolute ethyl alcohol, graphene oxide dispersion, the L-AA aqueous solution, poly- second
The alkene pyrrolidone aqueous solution is 1 in mass ratio：(100±10)：(10±2)：(100±10)：(10±2)：(10 ± 2) mix,
30 ± 5min of ultrasound, wherein, the mass concentration of watery hydrochloric acid is 0.07 ± 0.02%, the concentration of graphene oxide dispersion for 4 ±
2mg/ml, the concentration of the L-AA aqueous solution is 8 ± 2mg/ml, and the concentration of aqueous povidone solution is 2~8mg/
ml；
3.2) by step 3.1) resulting material hot bath is to 80 ± 10 DEG C, reaction 4 ± 1 hours, then with water and anhydrous second
Magnetic precipitation is collected in alcohol centrifuge washing reaction product, dipping magnetic inclination analysis, and is dried in vacuo 24 ± 3 hours under conditions of 40 ± 5 DEG C, is obtained
To carbonyl iron/graphene/polyvinylpyrrolidone ternary complex.
As the suction wave plate prepared by above-mentioned carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material.
The preparation method of above-mentioned suction wave plate, is (1-3) by mass ratio:4 carbonyl iron/graphene/polyvinylpyrrolidone
Tri compound absorbing material and paraffin, heating are well mixed, and tabletting after natural cooling produces radio-radar absorber.
The NM technology of the present invention is with reference to prior art.
Carbonyl iron/graphene of the present invention/polyvinylpyrrolidone composite wave-suction material preparation process is simple, obtained by the application
Composite wave-suction material can be added in coating as additive, be can be applied to equip using coated technique and built surface and formed and inhale ripple
Coating, realizes effective absorption of electromagnetic wave；Composite wave-suction material obtained by the application can also inhale ripple with being mixed with paraffin etc.
Agent is directly used.
Carbonyl ferromagnetism is strong in composite wave-suction material obtained by the application, and magnetic loss is strong；Graphene has nano-lamellar structure,
Electric conductivity is strong, and dielectric loss is high；Polyvinylpyrrolidone is decorated in graphene film layer surface, in ternary in the form of nano particle
Further dielectric regulation and control are realized in composite system, the application prepares the loss of tri compound absorbing material by force, main bag
Containing resistance loss, interlayer polarization loss, eddy-current loss, natural resonance loss, domain wall resonance loss etc.；The application carbonyl iron, stone
The promotion cooperative effect highly significant of black alkene and polyvinylpyrrolidone each other, realizes the Effective Regulation of electromagnetic parameter,
Effective suction wavestrip is expanded wide.
Carbonyl iron/graphene of the present invention/polyvinylpyrrolidone composite wave-suction material preparation process is simple, electro-magnetic wave absorption
Ability is strong, effect bandwidth, cost are low, microwave absorption, solve the field such as electromagnetic exposure and electromagnetic shielding have it is important should
With value.
Brief description of the drawings
Fig. 1 shows for the Scanning Electron of the gained carbonyl iron of embodiment 1/graphene/polyvinylpyrrolidone composite wave-suction material
Micro mirror (SEM) picture；As can be seen from Figure, graphene layer forms good cladding to carbonyl dust core, beneficial to suppression carbonyl iron
Intergranular to reunite, the conduction of the two-dimensional structure of outer layer graphene for charge inducing in the composite provides path, enhances
The impedance matching property of composite.
Fig. 2 shows for the transmitted electron of the gained carbonyl iron of embodiment 1/graphene/polyvinylpyrrolidone composite wave-suction material
Micro mirror (TEM) picture；As can be seen from Figure, a large amount of polyvinylpyrrolidone nano particles are uniformly distributed in surface of graphene oxide,
Abundant electromagnetic consumable interface is formd, beneficial to the wave-absorbing effect of enhancing composite.
Fig. 3 is the electro-magnetic wave absorption of the gained carbonyl iron of embodiment 1/graphene/polyvinylpyrrolidone composite wave-suction material
Design sketch.
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
Composite wave-suction material, including carbonyl iron dust sandwich layer, be wrapped in carbonyl iron dust sandwich layer periphery graphene oxide layer and
It is wrapped in the polyvinylpyrrolidone layer of graphene oxide layer periphery.
Polyvinylpyrrolidone used in embodiment is the K-30 of Chinese medicines group production.
Embodiment 1
The preparation of A composite wave-suction materials
Carbonyl iron dust, zirconium oxide bead, absolute ethyl alcohol are mixed and add planetary ball mill, their mass ratio is 1:80:10,
Drum's speed of rotation maintains 1000rpm, ball milling 4 hours；After natural cooling, filtering of slipping through the net removes zirconium oxide bead, is put into vacuum drying
Stove, 60 DEG C of drying to constant weights obtain the carbonyl iron dust that the particle diameter after ball milling is 0.5-1.5 μm.
Using 200 mesh natural graphite powders, 98% concentrated sulfuric acid, sodium nitrate, potassium permanganate, 3% hydrogen peroxide.Graphite powder, dense sulphur
Acid, sodium nitrate in mass ratio 1:0.6:45 magnetic agitation rotating speed 250rpm mixing 8min, ice-water bath is cooled to less than 5 DEG C, then
5 times of potassium permanganate powder of graphite powder quality is slowly added to said mixture, stirring reaction 35min, course of reaction temperature control
System is below 20 DEG C；30 DEG C are then heated to, 35min is reacted in continuing magnetic force stirring (rotating speed 200rpm)；It is slowly added to deionization
Water 45ml, is heated to 100 DEG C, stirring reaction 25min；Naturally cool to after room temperature, add 3% hydrogen peroxide 10ml；Washed through centrifugation
Wash and after deionized water dialysis, add deionized water to graphene oxide concentration 4mg/ml, ultrasonic disperse obtains graphite oxide and disperseed
Liquid.
Carbonyl iron dust, 0.07% watery hydrochloric acid, absolute ethyl alcohol, graphene oxide dispersion (4mg/ml) after mechanical ball mill,
The L-AA aqueous solution (8mg/ml), aqueous povidone solution (2mg/ml) in mass ratio 1：100：10：100：10：
10 uniform mixing, ultrasonic 30min simultaneously；Subsequent 80 DEG C of hot bath, reacts 4 hours；Reacted with water and absolute ethyl alcohol centrifuge washing
Magnetic precipitation is collected in product, dipping magnetic inclination analysis, and 40 DEG C are dried in vacuo 24 hours, obtain carbonyl iron/graphene/polyvinylpyrrolidone three
First compound.
The performance test of B composite wave-suction materials
Using carbonyl iron/graphene/polyvinylpyrrolidone ternary complex as radio-radar absorber, paraffin is film forming matter
Matter, by radio-radar absorber：The mass ratio 1 of film forming matter:1 weighs carbonyl iron/graphene/polyvinylpyrrolidone tri compound
Thing 0.1g and paraffin 0.1g, heating is well mixed, and internal diameter 3.04mm, external diameter 7.0mm coaxial rings is made in tabletting after natural cooling
Sample.Appropriate Network Analyzer tests the relative dielectric constant r and relative permeability r of (Agilent N5242A) test sample,
Reflection loss is derived from using formula (1) and (2)
Zin=Z0(μr/εr)1/2tanh[j2fd(μrεr)1/2/c] (1)
RL=20log [(Zin-Z0)/(Zin+Z0)] (2)
In above formula, RL is reflection loss, and f is incoming electromagnetic wave frequency rate, and d is coating layer thickness (coaxial rings thickness of sample), and c is
The light velocity, Z0 is air characteristics impedance, and Zin is coating input impedance, and j is imaginary unit.
Test result shows, during coating layer thickness 2.5mm, is less than -10dB in 2~18GHz frequency range internal reflections loss value
Frequency bandwidth 12.92Ghz (5.08~18GHz), minimal reflection loss value -29.78dB.
By checking, coating layer thickness does not influence frequency bandwidth.
Embodiment 2
The preparation of A composite wave-suction materials
Carbonyl iron dust, zirconium oxide bead, absolute ethyl alcohol are mixed and add planetary ball mill, their mass ratio is 1:90:12,
Drum's speed of rotation maintains 1100rpm, ball milling 3 hours；After natural cooling, filtering of slipping through the net removes zirconium oxide bead, is put into vacuum drying
Stove, 60 DEG C of drying to constant weights obtain the carbonyl iron dust that the particle diameter after ball milling is 0.5-1.5 μm.
Using 300 mesh natural graphite powders, 98% concentrated sulfuric acid, sodium nitrate, potassium permanganate, 3% hydrogen peroxide.Graphite powder, dense sulphur
Acid, sodium nitrate in mass ratio 1:0.5:42.3 magnetic agitation rotating speed 200rpm mixing 10min, ice-water bath is cooled to less than 5 DEG C, with
The potassium permanganate powder of 4 times of graphite powder quality is slowly added to said mixture, stirring reaction 30min, course of reaction temperature afterwards
Control is below 20 DEG C；35 DEG C are then heated to, 30min is reacted in continuing magnetic force stirring (rotating speed 200rpm)；Be slowly added to from
Sub- water 45ml, is heated to 90 DEG C, stirring reaction 30min；Naturally cool to after room temperature, add 3% hydrogen peroxide 10ml；Washed through centrifugation
Wash and after deionized water dialysis, add deionized water to graphene oxide concentration 4mg/ml, ultrasonic disperse prepares graphite oxide point
Dispersion liquid.
Carbonyl iron dust, 0.07% watery hydrochloric acid, absolute ethyl alcohol, graphene oxide dispersion (4mg/ml) after mechanical ball mill,
The L-AA aqueous solution (8mg/ml), aqueous povidone solution (4mg/ml) in mass ratio 1：110：11：110：11：
11 uniform mixing, ultrasonic 35min simultaneously；Subsequent 90 DEG C of hot bath, reacts 5 hours；Reacted with water and absolute ethyl alcohol centrifuge washing
Magnetic precipitation is collected in product, dipping magnetic inclination analysis, and 45 DEG C are dried in vacuo 25 hours, obtain carbonyl iron/graphene/polyvinylpyrrolidone three
First compound.
The performance test of B composite wave-suction materials
Using carbonyl iron/graphene/polyvinylpyrrolidone ternary complex as radio-radar absorber, paraffin is film forming matter
Matter, by radio-radar absorber：The mass ratio 1 of film forming matter:1 weighs carbonyl iron/graphene/polyvinylpyrrolidone tri compound
Thing 0.1g and paraffin 0.1g, heating is well mixed, and internal diameter 3.04mm, external diameter 7.0mm coaxial rings is made in tabletting after natural cooling
Sample.
Test result shows, during coating layer thickness 2.5mm, is less than -10dB in 2~18GHz frequency range internal reflections loss value
Frequency bandwidth 14.80Ghz (4.2~18GHz), minimal reflection loss value -27.5dB.
Embodiment 3
The preparation of A composite wave-suction materials
Carbonyl iron dust, zirconium oxide bead, absolute ethyl alcohol are mixed and add planetary ball mill, their mass ratio is 1:70:8,
Drum's speed of rotation maintains 900rpm, ball milling 5 hours；After natural cooling, filtering of slipping through the net removes zirconium oxide bead, is put into vacuum drying
Stove, 60 DEG C of drying to constant weights obtain the carbonyl iron dust that the particle diameter after ball milling is 0.8-2.3 μm.
Using 400 mesh natural graphite powders, 98% concentrated sulfuric acid, sodium nitrate, potassium permanganate, 3% hydrogen peroxide.Graphite powder, dense sulphur
Acid, sodium nitrate in mass ratio 1:0.4:38 magnetic agitation rotating speed 150rpm mixing 12min, ice-water bath is cooled to less than 5 DEG C, then
3 times of potassium permanganate powder of graphite powder quality is slowly added to said mixture, stirring reaction 25min, course of reaction temperature control
System is below 20 DEG C；40 DEG C are then heated to, 25min is reacted in continuing magnetic force stirring (rotating speed 200rpm)；It is slowly added to deionization
Water 45ml, is heated to 85 DEG C, stirring reaction 25min；Naturally cool to after room temperature, add 3% hydrogen peroxide 10ml；Through centrifuge washing
After deionized water dialysis, deionized water is added to graphene oxide concentration 4mg/ml, ultrasonic disperse is prepared graphite oxide and disperseed
Liquid.
Carbonyl iron dust, 0.07% watery hydrochloric acid, absolute ethyl alcohol, graphene oxide dispersion (4mg/ml) after mechanical ball mill,
The L-AA aqueous solution (8mg/ml), aqueous povidone solution 8mg/ml) in mass ratio 1：90：9：90：9：10 is same
When uniformly mix, ultrasonic 28min；Subsequent 75 DEG C of hot bath, reacts 3 hours；With water and absolute ethyl alcohol centrifuge washing reaction product,
Magnetic precipitation is collected in dipping magnetic inclination analysis, and 35 DEG C are dried in vacuo 23 hours, is obtained carbonyl iron/graphene/polyvinylpyrrolidone ternary and is answered
Compound.
The performance test of B composite wave-suction materials
Using carbonyl iron/graphene/polyvinylpyrrolidone ternary complex as radio-radar absorber, paraffin is film forming matter
Matter, takes carbonyl iron/graphene/polyvinylpyrrolidone ternary complex 0.3g and paraffin 0.4g, and heating is well mixed, naturally cold
But internal diameter 3.04mm, external diameter 7.0mm coaxial rings sample is made in tabletting after.
Test result shows, during coating layer thickness 2.5mm, is less than -10dB in 2~18GHz frequency range internal reflections loss value
Frequency bandwidth 13.24Ghz (4.76~18GHz), minimal reflection loss value -20.31dB.
Claims (10)
1. a kind of carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material, it is characterised in that：Including carbonyl dust core
Layer, the graphene layer for being wrapped in carbonyl iron dust sandwich layer periphery and the polyvinylpyrrolidone layer for being wrapped in graphene layer periphery, stone
The material of black alkene layer is graphene oxide, reduced graphene or graphene.
2. carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material as claimed in claim 1, it is characterised in that：Carbonyl
The mass ratio of base iron powder sandwich layer, graphene layer and polyvinylpyrrolidone layer is 50:(1-3):(1-4).
3. the preparation method of carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material described in claim 1 or 2, its
It is characterised by：Including following steps connected in order：
1) carbonyl iron dust is milled to particle diameter for 0.5-3 μm；
2) polyvinylpyrrolidone that the graphene dispersing solution and concentration that preparation concentration is 4 ± 2mg/ml are 2~8mg/ml is water-soluble
Liquid, graphene dispersing solution is graphene oxide dispersion, reduced graphene dispersion liquid or graphene dispersing solution；
3) by step 1) obtained by carbonyl iron dust and step 2) obtained by graphene dispersing solution and aqueous povidone solution
Reaction obtains magnetic precipitation, then dries, produces carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material, wherein,
The mass ratio of carbonyl iron dust, graphene dispersing solution and aqueous povidone solution is 1:(100±10):(10±2).
4. preparation method as claimed in claim 3, it is characterised in that：Step 1) be by mass ratio be 1:(80±10):(10±
2) carbonyl iron dust, zirconium oxide bead and absolute ethyl alcohol mixing add ball mill, under conditions of rotating speed is 1000 ± 200rpm, ball milling
4 ± 1 hours, room temperature is then naturally cooled to, filtering removes zirconium oxide bead, then is dried in the case where temperature is 60 ± 10 DEG C of vacuum conditions
To constant weight, the carbonyl iron dust that particle diameter is 0.5-3 μm is obtained.
5. preparation method as claimed in claim 3, it is characterised in that：Step 2) in graphene oxide dispersion preparation method
For：Graphene oxide dispersion is prepared using Hummer methods are improved.
6. preparation method as claimed in claim 5, it is characterised in that：Step 2) in graphene oxide dispersion preparation method
Including following steps connected in order：
2.1) it is 1 by mass ratio:(0.5±0.2):Graphite powder, the concentrated sulfuric acid and the sodium nitrate low whipping speed of (42.3 ± 5) be
10 ± 2min is mixed under conditions of 200 ± 50rpm, then ice-water bath is cooled to less than 5 DEG C；
2.2) potassium permanganate powder of 4 ± 1 times of graphite powder quality is added into step 2.1) obtained by mixture in, stirring reaction 30
± 5min, course of reaction temperature control is below 20 DEG C；
2.3) by step 2.2) resulting material is warming up to 35 ± 5 DEG C, reacts 30 ± 5min；
2.4) by step 2.3) deionized water of more than 40 times of graphite powder quality is added in resulting material, 90 ± 10 DEG C are heated to,
30 ± 5min of stirring reaction, then naturally cools to room temperature, the hydrogen peroxide that more than 5 times of addition graphite powder quality；
2.5) by step 2.4) resulting material through centrifuge washing and deionized water dialysis after, add deionized water to required concentration,
Ultrasonic disperse obtains graphite oxide dispersion.
7. preparation method as claimed in claim 6, it is characterised in that：Graphite powder is the native graphite that particle diameter is 300 ± 100 mesh
Powder；The concentrated sulfuric acid is the concentrated sulfuric acid that mass concentration is 98%；The mass concentration of hydrogen peroxide is 3%.
8. preparation method as claimed in claim 6, it is characterised in that：Step 3) include following steps connected in order：
3.1) by carbonyl iron dust, watery hydrochloric acid, absolute ethyl alcohol, graphene oxide dispersion, the L-AA aqueous solution, polyethylene pyrrole
The pyrrolidone aqueous solution is 1 in mass ratio：(100±10)：(10±2)：(100±10)：(10±2)：(10 ± 2) mix, ultrasound
30 ± 5min, wherein, the mass concentration of watery hydrochloric acid is 0.07 ± 0.02%, and the concentration of graphene oxide dispersion is 4 ± 2mg/
Ml, the concentration of the L-AA aqueous solution is 8 ± 2mg/ml, and the concentration of aqueous povidone solution is 2~8mg/ml；
3.2) by step 3.1) resulting material hot bath, to 80 ± 10 DEG C, reacts 4 ± 1 hours, then with water and absolute ethyl alcohol from
Magnetic precipitation is collected in heart washing reaction product, dipping magnetic inclination analysis, and is dried in vacuo 24 ± 3 hours under conditions of 40 ± 5 DEG C, obtains carbonyl
Base iron/graphene/polyvinylpyrrolidone ternary complex.
9. as the suction prepared by carbonyl iron/graphene/polyvinylpyrrolidone composite wave-suction material described in claim 1 or 2
Wave plate.
10. the preparation method of the suction wave plate described in claim 9, it is characterised in that：It is (1-3) by mass ratio:4 carbonyl iron/
Graphene/polyvinylpyrrolidone tri compound absorbing material and paraffin, heating are well mixed, and tabletting after natural cooling is produced
Inhale wave plate.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN107936575A (en) * | 2017-12-04 | 2018-04-20 | 中国航发北京航空材料研究院 | A kind of graphene composite wave-absorbing fluorine silicone encapsulant and preparation method thereof |
| CN108190876A (en) * | 2018-02-26 | 2018-06-22 | 北京环境特性研究所 | A kind of graphene composite absorber and preparation method thereof |
| CN109451715A (en) * | 2018-10-31 | 2019-03-08 | 中北大学 | A kind of graphene-carbonyl iron dust@ferroso-ferric oxide electro-magnetic wave absorption composite material |
| CN109942026A (en) * | 2019-03-11 | 2019-06-28 | 常州讯宛德电子有限公司 | A kind of preparation method of monodisperse porous nano structure Ferrite Material |
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| CN112812563A (en) * | 2020-12-30 | 2021-05-18 | 上海聚威新材料股份有限公司 | Conductive wave-absorbing PPS composite material and preparation method thereof |
| CN115093518A (en) * | 2022-07-19 | 2022-09-23 | 四川大学 | Wave absorber with core-shell structure and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107399735A (en) * | 2017-08-25 | 2017-11-28 | 南京航空航天大学 | A kind of preparation method and applications of graphene composite aerogel absorbing material |
| CN107399735B (en) * | 2017-08-25 | 2020-11-06 | 南京航空航天大学 | Preparation method and application of graphene composite aerogel wave-absorbing material |
| CN107936575A (en) * | 2017-12-04 | 2018-04-20 | 中国航发北京航空材料研究院 | A kind of graphene composite wave-absorbing fluorine silicone encapsulant and preparation method thereof |
| CN108190876A (en) * | 2018-02-26 | 2018-06-22 | 北京环境特性研究所 | A kind of graphene composite absorber and preparation method thereof |
| CN109451715A (en) * | 2018-10-31 | 2019-03-08 | 中北大学 | A kind of graphene-carbonyl iron dust@ferroso-ferric oxide electro-magnetic wave absorption composite material |
| CN111320165A (en) * | 2018-12-13 | 2020-06-23 | 山东欧铂新材料有限公司 | Graphene oxide/carbonyl iron composite material, preparation method thereof and graphene-based wave-absorbing material |
| CN109942026A (en) * | 2019-03-11 | 2019-06-28 | 常州讯宛德电子有限公司 | A kind of preparation method of monodisperse porous nano structure Ferrite Material |
| CN112812563A (en) * | 2020-12-30 | 2021-05-18 | 上海聚威新材料股份有限公司 | Conductive wave-absorbing PPS composite material and preparation method thereof |
| CN115093518A (en) * | 2022-07-19 | 2022-09-23 | 四川大学 | Wave absorber with core-shell structure and preparation method thereof |
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