CN107708396A - A kind of hierarchical structure wave absorbing agent and preparation method thereof - Google Patents
A kind of hierarchical structure wave absorbing agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of hierarchical structure wave absorbing agent and preparation method thereof, the wave absorbing agent is made up of ternary complex and film forming agent, and the ternary complex is in level clad structure, contains binary metal oxide, RGO and MnO2, the RGO is coated on outside binary metal oxide, the MnO2It is coated on outside RGO.Wherein, binary complex is magnetic loss medium, and RGO is dielectric loss and conduction loss medium.The present invention not only combines magnetic loss and electrical loss together, and by the design of the orderly clad structure of this level, greatly enhances interfacial polarization effect of the compound for electromagnetic wave.Outermost MnO2Not only contribute to the incidence of electromagnetic wave, moreover it is possible to effectively reduce direct reflections of the RGO for electromagnetic wave, further enhancing the absorbing property of compound.
Description
Technical field
The present invention relates to technical field of magnetic materials, more particularly, to a kind of hierarchical structure wave absorbing agent and preparation method thereof.
Background technology
With the fast development of hyundai electronicses information technology, the negative effect of Electromagnetic Radiation on Environment and human health is increasingly
Seriously.Therefore, prepare a kind of material that can effectively shield electromagnetic wave absorption and seem very important.However, due to electromagnetic wave
Complexity, it is desirable to prepare with light weight, thickness of thin, absorb strong, bandwidth efficient wave absorbing agent be still one very
Difficult task.
In general, absorption of the wave absorbing agent to electromagnetic wave depends on two kinds of loss mechanisms, i.e. dielectric loss and magnetic loss
Consumption.Fe3O4, barium ferrite, the ferromagnetic material such as Mn ferrite as most traditional absorbing material, due to its outstanding magnetic loss consumption
Can, it has been widely used in electromagnetic wave shielding field.However, its density is big, the shortcomings of applying thickness and absorption band width, directly
Limit their large-scale applications in high-end science and technology field.In the last few years, it is new for some of representative with graphene (RGO)
Carbon material, because the features such as its density is low, dielectric loss is strong has shown certain application prospect in suction ripple field.Electromagnetic wave was both
With electrical characteristics also with magnetic characteristic, thus only possesses the wave absorbing agent of single loss mechanisms (magnetic loss or electrical loss), not
Actual needs can be met.Based on this, if the strong graphene of the dielectric loss ferrite strong with magnetic loss is compound, perhaps can
Obtain it is a kind of have concurrently electricity, the efficient and light weight absorbing material of magnetic characteristic.
Disclosed in Chinese patent CN102876288B " a kind of preparation method of graphene/barium ferrite composite wave-suction material "
A kind of synthetic method of graphene-supported barium ferrite.Minimal reflection loss of the composite in the range of 2~18GHz
For -22.09dB, effective bandwidth is narrower, only 4.0GHz.
Chinese patent CN105602194A " preparation method of a kind of nanometer particle-modified graphene of Ni and its absorbing material "
A kind of surface by Ni nano-particle deposited graphite alkene is disclosed, it is a kind of with reference to obtained from the good dielectric properties of graphene
Have electricity, the wave absorbing agent of magnetic absorbing ability concurrently.But its wave-sucking performance is poor, minimal reflection loss (- 17.8dB) and effectively absorption are wide
Band (2.5GHz) is all smaller.
But compound may be strengthened just because of the superior electrical property of graphene (RGO), excessively graphene-supported
Direct reflection for electromagnetic wave, causes electromagnetic wave can not be efficiently entering material internal, causes the dielectric constant of compound drastically
Increase, compound are unfavorable for further loss of the compound to electromagnetic wave and absorbed for the reflection enhancement of electromagnetic wave.
The content of the invention
The present invention provides a kind of hierarchical structure wave absorbing agent and preparation method thereof, not only melts magnetic loss and electrical loss for one
Body, and the huge specific surface area of graphene is effectively utilized by the design of the orderly clad structure of this level, greatly increase
Contact area between strong component, interfacial polarization effect of the enhancing compound for electromagnetic wave, further increases compound
Electro-magnetic wave absorption performance.
To achieve these goals, the present invention uses following technical scheme：
A kind of hierarchical structure wave absorbing agent, the wave absorbing agent are made up of ternary complex and film forming agent, and the ternary complex is in layer
Level clad structure, contains binary metal oxide, RGO and MnO2, the RGO is coated on outside binary metal oxide, the MnO2
It is coated on outside RGO.Wherein, binary complex is magnetic loss medium, and RGO is dielectric loss and conduction loss medium.
Preferably, the binary metal oxide one of which metallic element is Fe, another kind is Zn, Ba, Ca, Mg,
Any one in Sn, Ti, Sr and Sm.
Preferably, the mass ratio of the ternary complex and film forming agent is 1~5:5~1, wherein the film forming agent is stone
Wax.
Preferably, it the described method comprises the following steps：
(1) hydro-thermal method prepares binary metal oxide：Weigh 1.352~4.056g FeCl3·6H2O and 0.845~2.535g
Another metal salt is dissolved in solvent, then addition 3.6~10.8g NaAc and 1.0~3.0g polyethylene glycol, and ultrasonic agitation 0.5~
1.5h, 10~20h of hydro-thermal reaction is carried out at 180~220 DEG C, naturally cools to room temperature, washing and filtering obtains solid formation.First
Binary metal oxide microballoon is generated by solvent-thermal method, wherein by controlling reaction time, reaction temperature, the concentration of lyonium salt
The size of binary metal oxide microballoon can be controlled；
(2) cladding process prepares binary complex：Solid formation described in step (1) is scattered in deionized water, adds 3- ammonia third
Base-trimethoxy silane stirs, 8~12h of back flow reaction, obtains solid particle, gained solid particle be scattered in again from
In sub- water, mixed liquor A is designated as；Separately weigh 0.5~1.5g graphite (EG) and 3.0~9.0g KMnO4, it is uniformly mixed, Xiang Qi
In be slowly added to 60~200mL concentrated acid solution, heating water bath after stirring 8~12 hours, is cooled to room temperature to 40~60 DEG C,
H is added dropwise2O2Solid product is taken, the solid product is scattered in deionized water in golden yellow, centrifugation to solution, is adjusted
PH is neutrality, is then sonicated to obtain suspension B；Suspension B is mixed with mixed liquor A, regulation pH value is 1~3, back flow reaction 2
~4h, the as binary metal oxide of dry the GO claddings of washing, binary complex.Add into binary metal oxide microballoon
Enter 3- aminopropyls-trimethoxy silane, modified by reflux operation in microsphere surface.Obtained by aoxidizing stripping expanded graphite
To graphene oxide, H is added in course of reaction2O2Remove excessive potassium permanganate；Add NaOH and react away excessive acid, and increase
The ion concentration of big mixed liquor；Solution B is added dropwise in mixed liquor A, it is 2 that the HCl solution for being 1M with concentration, which adjusts its pH,；
When pH is 2, the binary metal oxide microballoon positively charged of 3- aminopropyls-trimethoxy silane has been modified；Graphene oxide because
Substantial amounts of carbonyl, carboxyl functional group are contained in its oxidized gained, surface, therefore negatively charged；Two kinds of materials are because of its surface charge
Thus caused electrostatic interaction makes graphene oxide be coated on binary metal oxide microsphere surface to difference；
(3) thermal reduction prepares ternary complex：By the binary complex described in (2) the step of 0.2~0.8g be dissolved in from
In sub- water, 0.158~0.474g potassium permanganate is added, ultrasonic disperse obtains mixed solution, mixed liquor is entered at 180~220 DEG C
Water-filling 10~24h of thermal response, isolates solid formation, and washing is drying to obtain ternary complex.With oxidation-in-stiu coating and thermal reduction
Method prepares ternary complex.Potassium permanganate thermally decomposes at high temperature, the MnO of generation2Growth in situ in surface of graphene oxide, and
And at high temperature, the oxygenated functional group on graphene oxide (GO) surface can be pyrolyzed reduction, generate redox graphene
(RGO) ternary complex, is ultimately produced；
(4) take ternary complex and film forming agent ground and mixed uniform respectively, obtain wave absorbing agent.
Preferably, solvent described in step (1) is ethylene glycol solution, volume is 40~80mL.
Preferably, in step (2), the addition of 3- aminopropyls-trimethoxy silane is 0.5~1.5mL；The backflow
Reaction temperature is 80~100 DEG C.
Preferably, in step (2), the concentrated acid solution is dense H3PO4With dense H2SO4Mixed liquor, the dense H3PO4With
Dense H2SO4Volume ratio be 1：(5~10).
Preferably, in step (2), graphene oxide (GO) content is 1~3.0mg/mL in gained suspension B.
Preferably, in step (1) and (3), the hydro-thermal reaction is carried out in autoclave.
Preferably, in step (3), the mass ratio of ternary complex and film forming agent is 1~5:5~1, wherein the film forming
Agent is paraffin.
Therefore, the present invention has the advantages that：(1) preparation method is simple, mild condition, easily realizes batch production；
(2) raw material used are simple and easy to get, save cost；(3) prepare compound wave absorbing agent have light weight, thickness of thin,
The features such as absorption band is wide, it is a kind of electromagnetic wave interference preventive material with larger application prospect.
Brief description of the drawings
Fig. 1 is MgFe of the present invention2O4(a),MgFe2O4@GO (b) and MgFe2O4@RGO@MnO2(c) the SEM figures of compound.
Fig. 2 is MgFe of the present invention2O4@GO (b) and MgFe2O4@RGO@MnO2(c) the TEM figures of compound.
Fig. 3 is RGO (a) of the present invention, MgFe2O4@GO (b) and MgFe2O4@RGO@MnO2(c) XRD of compound.
Fig. 4 is MgFe of the present invention2O4@RGO@MO2The absorbing property (wave absorbing agent thickness=2.0mm) of compound.
Embodiment
The present invention will be further described with embodiment below in conjunction with the accompanying drawings.Experiment side in following examples
Method, it is conventional method unless otherwise specified；Used material in example, unless otherwise specified, it is purchased from conventional chemical examination
Agent company.The main component of wave absorbing agent is MgFe2O4@RGO@MnO2Ternary complex, wherein MgFe2O4For magnetic loss medium, RGO
For dielectric loss and conduction loss medium.
Reflection loss calculation formula in following instance is as follows：
ZinRepresent the characteristic impedance of suction ripple medium, Z0Free space impedance is represented, f is microwave frequency, and c represents the light velocity, and d represents to inhale
The thickness of ripple medium, εr(εr=εr’-jεr") and μr(μr=μr’-jμr") it is the relative complex dielectric permittivity for inhaling ripple medium and multiple magnetic
Conductance.
Embodiment 1
A kind of preparation method of hierarchical structure wave absorbing agent：
(1) 1.352g FeCl are weighed respectively3·6H2O and 0.845MgSO4·7H2O is dissolved in 40mL ethylene glycol solutions, is then added
Enter 3.6g NaAc and 1.0g polyethylene glycol, be stirred by ultrasonic 0.5 hour.Gained mixed liquor is transferred in stainless steel cauldron,
180 DEG C are reacted 12 hours, naturally cool to room temperature, are filtered.With deionized water and ethanol, respectively washing three times, will be solid respectively for solid formation
Phase thing ultrasonic disperse adds 0.5mL 3- aminopropyls-trimethoxy silane and stirred in 20mL deionized waters, and 100 DEG C are returned
Stream reaction 8h, gained solid particle are scattered in 20mL deionized waters again, are designated as mixed liquor A；The another 0.5g that weighs may expand stone
Black (EG) and 3.0g KMnO4It is placed in 500mL three-neck flasks, is uniformly mixed, is slowly added to 60mL volume ratio thereto
For 1:9 dense H3PO4With dense H2SO4Mixed liquor, heating water bath to 50 DEG C, stir 8 hours；Reactant is cooled to room temperature, it is small
The heart is poured into the beaker for filling frozen water, and H is added dropwise2O2To mixed solution in golden yellow；Centrifuge, supernatant liquor is discarded, by its point
Dissipate in 500mL deionized waters, the NaOH for being 1M with concentration regulation pH value of solution is neutral.Then by it ultrasonic 8 in ice-water bath
Hour, obtain suspension B (GO contents are about 1mg/mL)；Solution B is added dropwise in mixed liquor A, the HCl for being 1M with concentration is molten
It is back flow reaction 2 hours at 1,80 DEG C that liquid, which adjusts its pH,.Solid product is separated to obtain with magnet, it is each with ethanol with deionized water respectively
Washing three times, is dried under vacuum to constant weight and produces MgFe2O4@GO binary complexs；
(2) MgFe is prepared with oxidation-in-stiu coating and thermal reduction2O4@RGO@MnO2Compound.By 0.2g MgFe2O4@GO
Compound is dissolved in 30mL deionized waters, is added 0.158g potassium permanganate, ultrasonic disperse, it is stainless that mixed liquor is transferred into 100mL
180 DEG C are reacted 16 hours in steel reactor.Solid formation is isolated with magnet, is respectively washed twice with ethanol with deionized water respectively,
Solid formation is dried under vacuum to constant weight in 50~80 DEG C, produces MgFe2O4@RGO@MnO2Compound (sample 1)；
(3) it is radio-radar absorber with sample 1, using paraffin as film forming agent, by absorbent：The mass ratio of film forming agent is 1:2 weigh
Each material, ground and mixed are uniform；Obtain wave absorbing agent；
(4) above-mentioned wave absorbing agent is pressed into the circular ring plate that internal diameter is 3.0mm, external diameter 7.0mm, thickness are 2mm, uses vector network
Analysis-e/or determining sample 2~18GHz scopes complex dielectric permittivity and complex permeability, according to correlation formula calculate sample reflection
Loss.
Embodiment 2：
A kind of preparation method of hierarchical structure wave absorbing agent：
(1) 2.702g FeCl are weighed respectively3·6H2O and 1.690MgSO4·7H2O is dissolved in 60mL ethylene glycol solutions, is then added
Enter 7.2g NaAc and 2.0g polyethylene glycol, be stirred by ultrasonic 1.0 hours.Gained mixed liquor is transferred in stainless steel cauldron,
200 DEG C are reacted 12 hours, naturally cool to room temperature, are filtered.Mixed liquor A (1.0mL is prepared by the method for (1) the step of embodiment 1
3- aminopropyls-trimethoxy silane)；Separately weigh 1.0g expansible graphites (EG) and 6.0g KMnO4It is placed in 500mL three-neck flasks
In, it is uniformly mixed, the volume ratio for being slowly added to 140mL thereto is 1:9 dense H3PO4With dense H2SO4Mixed liquor, press
The method of the step of embodiment 1 (1) prepares suspending liquid A (RGO contents are about 2mg/mL)；Solution B is added dropwise to mixed liquor A
In, it is back flow reaction 3 hours at 1,80 DEG C that the HCl solution for being 1M with concentration, which adjusts its pH,.Solid product is separated to obtain with magnet, point
Not Yong deionized water and ethanol respectively washing three times, is dried under vacuum to constant weight and produces MgFe2O4@GO binary complexs；
(2) MgFe is prepared with oxidation-in-stiu coating and thermal reduction2O4@RGO@MnO2Compound.By 0.4g MgFe2O4@GO
Compound is dissolved in 30mL deionized waters, and MgFe is prepared by the method for the step of embodiment 1 (1)2O4@RGO@MnO2Compound (sample
2)；
(3) it is radio-radar absorber with sample 2, using scale paraffin as film forming agent, by absorbent：The mass ratio of film forming agent is 1:2
Each material is weighed, ground and mixed is uniform to obtain wave absorbing agent；
(4) method is the same as the step of embodiment 1 (4).
Embodiment 3：
A kind of preparation method of hierarchical structure wave absorbing agent：
(1) 4.056g FeCl are weighed respectively3·6H2O and 2.535MgSO4·7H2O is dissolved in 80mL ethylene glycol solutions, is then added
Enter 10.8g NaAc and 3.0g polyethylene glycol, be stirred by ultrasonic 1.5 hours.Gained mixed liquor is transferred in stainless steel cauldron,
220 DEG C are reacted 12 hours, naturally cool to room temperature, are filtered.Mixed liquor A (1.5mL is prepared by the method for (1) the step of embodiment 1
3- aminopropyls-trimethoxy silane)；Separately weigh 1.5g expansible graphites (EG) and 9.0g KMnO4It is placed in 500mL three-neck flasks
In, it is uniformly mixed, the volume ratio for being slowly added to 200mL thereto is 1:9 dense H3PO4With dense H2SO4Mixed liquor, press
The method of the step of embodiment 1 (1) prepares suspending liquid A (RGO contents are about 3mg/mL)；Solution B is added dropwise to mixed liquor A
In, it is back flow reaction 3 hours at 1,80 DEG C that the HCl solution for being 1M with concentration, which adjusts its pH,.Solid product is separated to obtain with magnet, point
Not Yong deionized water and ethanol respectively washing three times, is dried under vacuum to constant weight and produces MgFe2O4@GO binary complexs；
(2) MgFe is prepared with oxidation-in-stiu coating and thermal reduction2O4@RGO@MnO2Compound.By 0.6g MgFe2O4@GO
Compound is dissolved in 30mL deionized waters, and MgFe is prepared by the method for the step of embodiment 1 (1)2O4@RGO@MnO2Compound (sample
3)；
(3) it is radio-radar absorber with sample 3, using scale paraffin as film forming agent, by absorbent：The mass ratio of film forming agent is 1:2
Each material is weighed, ground and mixed is uniform, obtains wave absorbing agent；
(4) method is the same as the step of embodiment 1 (4).
Absorbing property test, test result such as table are carried out to the sample 1 obtained by the various embodiments described above, sample 2 and sample 3
Shown in 1：
The absorbing property of 1 each example of table
Embodiment described above is a kind of preferable scheme of the present invention, not makees any formal limit to the present invention
System, there are other variants and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (10)
1. a kind of hierarchical structure wave absorbing agent, it is characterized in that, the wave absorbing agent is made up of ternary complex and film forming agent, the ternary
Compound is in level clad structure, contains binary metal oxide, RGO and MnO2, the RGO is coated on binary metal oxide
Outside, the MnO2It is coated on outside RGO.
2. a kind of hierarchical structure wave absorbing agent according to claim 1, it is characterized in that, the binary metal oxide wherein one
Kind metallic element is Fe, and another kind is any one in Zn, Ba, Ca, Mg, Sn, Ti, Sr and Sm.
3. a kind of hierarchical structure wave absorbing agent according to claim 1, it is characterized in that, the ternary complex and film forming agent
Mass ratio is 1 ~ 5:5 ~ 1, wherein the film forming agent is paraffin.
4. a kind of preparation method of hierarchical structure wave absorbing agent according to claim 1 or 2, it is characterized in that, methods described bag
Include following steps：
（1）Hydro-thermal method prepares binary metal oxide：Weigh 1.352 ~ 4.056g FeCl3·6H2O and 0.845 ~ 2.535 g are another
One metal salt is dissolved in solvent, then 3.6 ~ 10.8 g NaAc of addition and 1.0 ~ 3.0 g polyethylene glycol, and ultrasonic agitation 0.5 ~
1.5h, the h of hydro-thermal reaction 10 ~ 20 is carried out at 180 ~ 220 DEG C, naturally cools to room temperature, washing and filtering obtains solid formation；
（2）Cladding process prepares binary complex：By step（1）Described in solid formation be scattered in deionized water, add 3- ammonia third
Base-trimethoxy silane stirs, the h of back flow reaction 8 ~ 12, obtains solid particle, gained solid particle be scattered in again from
In sub- water, mixed liquor A is designated as；Separately weigh 0.5 ~ 1.5 g graphite（EG）With 3.0 ~ 9.0 g KMnO4, it is uniformly mixed, to
60 ~ 200 mL concentrated acid solution is wherein slowly added to, heating water bath after stirring 8 ~ 12 hours, is cooled to room temperature to 40 ~ 60 DEG C,
H is added dropwise2O2Solid product is taken, the solid product is scattered in deionized water in golden yellow, centrifugation to solution, is adjusted
PH is neutrality, is then sonicated to obtain suspension B；Suspension B is mixed with mixed liquor A, regulation pH value is 1 ~ 3, back flow reaction 2 ~
4h, the as binary metal oxide of dry the GO claddings of washing, binary complex；
（3）Thermal reduction prepares ternary complex：The step of by 0.2 ~ 0.8g（2）Described in binary complex be dissolved in deionization
In water, 0.158 ~ 0.474g potassium permanganate is added, ultrasonic disperse obtains mixed solution, mixed liquor is entered into water-filling at 180 ~ 220 DEG C
10 ~ 24h of thermal response, isolates solid formation, and washing is drying to obtain ternary complex；
（4）Take ternary complex and film forming agent ground and mixed uniform respectively, obtain wave absorbing agent.
5. a kind of preparation method of hierarchical structure wave absorbing agent according to claim 4, it is characterized in that, step（1）Described in
Solvent is ethylene glycol solution, and volume is 40 ~ 80 mL.
6. a kind of preparation method of hierarchical structure wave absorbing agent according to claim 4, it is characterized in that, step（2）In, 3- ammonia
The addition of propyl-trimethoxysilane is 0.5 ~ 1.5 mL；The back flow reaction temperature is 80 ~ 100 DEG C.
7. a kind of preparation method of hierarchical structure wave absorbing agent according to claim 4, it is characterized in that, step（2）In, it is described
Concentrated acid solution is dense H3PO4With dense H2SO4Mixed liquor, the dense H3PO4With dense H2SO4Volume ratio be 1：（5~10）.
8. according to a kind of preparation method of any described hierarchical structure wave absorbing agent in claim 4 to 7, it is characterized in that, step
（2）In, graphene oxide in gained suspension B（GO）Content is 1 ~ 3.0 mg/mL.
9. a kind of preparation method of hierarchical structure wave absorbing agent according to claim 8, it is characterized in that, step（1）With（3）
In, the hydro-thermal reaction is carried out in autoclave.
10. a kind of preparation method of hierarchical structure wave absorbing agent according to claim 9, it is characterized in that, step（3）In, three
The mass ratio of first compound and film forming agent is 1 ~ 5:5 ~ 1, wherein the film forming agent is paraffin.
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| CN105384159A (en) * | 2015-11-05 | 2016-03-09 | 云南大学 | Usage of manganese dioxide coated carbon particle dielectric materials as electromagnetic wave absorption materials |
| CN106867263A (en) * | 2017-03-24 | 2017-06-20 | 浙江师范大学 | ZnFe2O4@SiO2@RGO wave absorbing agents and its preparation technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105384159A (en) * | 2015-11-05 | 2016-03-09 | 云南大学 | Usage of manganese dioxide coated carbon particle dielectric materials as electromagnetic wave absorption materials |
| CN106867263A (en) * | 2017-03-24 | 2017-06-20 | 浙江师范大学 | ZnFe2O4@SiO2@RGO wave absorbing agents and its preparation technology |
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