CN107708396B - 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 agents and preparation method thereof, and the wave absorbing agent is made of ternary complex and film forming agent, and the ternary complex is in level clad structure, contain 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 compound and the interfacial polarization of electromagnetic wave is acted on.Outermost MnO2Not only contribute to the incidence of electromagnetic wave, moreover it is possible to direct reflection of the RGO for electromagnetic wave be effectively reduced, further enhance 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 technique
With the fast development of hyundai electronics information technology, the negative effect of Electromagnetic Radiation on Environment and human health is increasingly
Seriously.Therefore, preparing a kind of material that can effectively shield electromagnetic wave absorption seems very important.However, due to electromagnetic wave
Complexity, it is desirable to prepare with light weight, thickness is thin, absorption is strong, the efficient wave absorbing agent of bandwidth is still a Xiang Shifen
Difficult task.
In general, wave absorbing agent depends on two kinds of loss mechanisms, i.e. dielectric loss and magnetic loss to the absorption of electromagnetic wave
Consumption.Fe3O4, barium ferrite, the ferromagnetic materials 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 disadvantages of applying thickness and absorption band width, directly
Them are limited in the large-scale application in high-end science and technology field.In recent years, being some novel of representative with graphene (RGO)
Carbon material, since the features such as its density is low, dielectric loss is strong shows certain application prospect in suction wave field.Electromagnetic wave was both
Also there is magnetic characteristic with electrical characteristics, thus only have the wave absorbing agent of single loss mechanisms (magnetic loss or electrical loss), not
It is able to satisfy actual needs.Based on this, if the strong graphene of the dielectric loss ferrite strong with magnetic loss is compound, perhaps can
Obtain a kind of efficient and light weight absorbing material for having both electricity, magnetic characteristic.
It is 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 material within the scope of 2~18GHz
For -22.09dB, effective bandwidth is relatively narrow, only 4.0GHz.
Chinese patent CN105602194A " preparation method of a kind of nanometer particle-modified graphene of Ni and its absorbing material "
Disclose a kind of surface that graphene is deposited by Ni nanoparticle, one kind in conjunction with obtained from graphene good dielectric properties
Have both the wave absorbing agent of electricity, magnetic absorbing ability.But its wave-sucking performance is poor, and minimal reflection is lost (- 17.8dB) and effectively absorbs wide
Band (2.5GHz) is all smaller.
But just because of graphene (RGO) superior electrical property, excessively graphene-supported may enhance compound
Direct reflection for electromagnetic wave, causes electromagnetic wave that can not be efficiently entering material internal, causes the dielectric constant of compound sharply
Increase, compound is unfavorable for compound and absorbs to the further loss of electromagnetic wave for the reflection enhancement of electromagnetic wave.
Summary of the invention
The present invention provides a kind of hierarchical structure wave absorbing agent and preparation method thereof, and not only melting magnetic loss and electrical loss is 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, enhancing compound act on the interfacial polarization of electromagnetic wave, further improve compound
Electromagnetic wave absorption performance.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of hierarchical structure wave absorbing agent, the wave absorbing agent are made of ternary complex and film forming agent, the ternary complex
In level clad structure, contain binary metal oxide, RGO and MnO2, the RGO is coated on outside binary metal oxide, institute
State MnO2It 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 be Fe, another kind be 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, the described method comprises the following steps:
(1) hydro-thermal method prepares binary metal oxide: weighing 1.352~4.056g FeCl3·6H2O and 0.845~
Another metal salt of 2.535g is dissolved in solvent, and 3.6~10.8g NaAc and 1.0~3.0g polyethylene glycol is then added, and ultrasound is stirred
0.5~1.5h is mixed, 10~20h of hydro-thermal reaction, cooled to room temperature are carried out at 180~220 DEG C, solid phase is filtered to obtain in washing
Object.Binary metal oxide microballoon is generated by solvent-thermal method first, wherein passing through the control reaction time, reaction temperature, solvent
The concentration of salt can control the size of binary metal oxide microballoon；
(2) cladding process prepares binary complex: dispersing solid formation described in step (1) in deionized water, 3- is added
Aminopropyl-trimethoxy silane stirs evenly, 8~12h of back flow reaction, obtains solid particle, and obtained solid particle is scattered in again
In deionized water, it is denoted as mixed liquor A；Separately weigh 0.5~1.5g graphite (EG) and 3.0~9.0g KMnO4, it is uniformly mixed,
It is slowly added to the concentrated acid solution of 60~200mL thereto, heating water bath after stirring 8~12 hours, is cooled to room to 40~60 DEG C
H is added dropwise in temperature2O2To solution in golden yellow, centrifuge separation takes solid product, disperses the solid product in deionized water, adjusts
Saving PH is neutrality, is then sonicated to obtain suspension B；Suspension B is mixed with mixed liquor A, adjusting pH value is 1~3, back flow reaction
2~4h washs the binary metal oxide of dry GO cladding, as binary complex.Into binary metal oxide microballoon
3- aminopropyl-trimethoxy silane is added, is modified by reflux operation in microsphere surface.Expanded graphite is removed by oxidation
Graphene oxide is obtained, H is added in reaction process2O2Remove excessive potassium permanganate；NaOH is added and reacts away excessive acid, and
Increase the ion concentration of mixed liquor；Solution B is added dropwise in mixed liquor A, adjusting its pH with the HCl solution that concentration is 1M is
2；When pH is 2, it is positively charged 3- aminopropyl-trimethoxy silane binary metal oxide microballoon has been modified；Graphene oxide
Because it is through oxidation gained, a large amount of carbonyl, carboxyl functional group are contained in surface, therefore negatively charged；Two kinds of substances are because of its surface charge
Difference thus caused by electrostatic interaction so that graphene oxide has been coated on binary metal oxide microsphere surface；
(3) thermal reduction prepares ternary complex: binary complex described in (2) the step of 0.2~0.8g is dissolved in
In deionized water, 0.158~0.474g potassium permanganate is added, ultrasonic disperse obtains mixed solution, by mixed liquor in 180~220 DEG C
Lower progress hydro-thermal reaction 10~for 24 hours, solid formation is isolated, washing is drying to obtain ternary complex.With oxidation-in-stiu coating and heat
Reduction method prepares ternary complex.Potassium permanganate thermally decomposes at high temperature, the MnO of generation2Growth in situ is in graphene oxide table
Face, and at high temperature, the oxygenated functional group on the surface graphene oxide (GO) can be pyrolyzed reduction, generate redox graphene
(RGO), ternary complex is ultimately produced；
(4) it takes ternary complex and film forming agent ground and mixed uniform respectively, obtains wave absorbing agent.
Preferably, solvent described in step (1) is ethylene glycol solution, volume is 40~80mL.
Preferably, 3- aminopropyl-trimethoxy silane additive amount is 0.5~1.5mL in step (2)；The reflux
Reaction temperature is 80~100 DEG C.
Preferably, the concentrated acid solution is dense H in step (2)3PO4With dense H2SO4Mixed liquor, the dense H3PO4With
Dense H2SO4Volume ratio be 1:(5~10).
Preferably, graphene oxide (GO) content is 1~3.0mg/mL in gained suspension B in step (2).
Preferably, the hydro-thermal reaction carries out in a high pressure reaction kettle in step (1) and (3).
Preferably, the mass ratio of ternary complex and film forming agent is 1~5:5~1, wherein the film forming in step (3)
Agent is paraffin.
Therefore, simple, mild condition that the invention has the following beneficial effects: (1) preparation methods, easily realizes batch production；
(2) raw material used are simple and easy to get, save cost；(3) the compound wave absorbing agent prepared has light weight, thickness
Thin, the features such as absorption band is wide, be a kind of electromagnetic wave interference preventive material with larger application prospect.
Detailed description of the invention
Fig. 1 is MgFe of the present invention2O4(a),MgFe2O4@GO (b) and MgFe2O4@RGO@MnO2(c) the SEM figure of compound.
Fig. 2 is MgFe of the present invention2O4@GO (b) and MgFe2O4@RGO@MnO2(c) the TEM figure of compound.
Fig. 3 is RGO (a) of the present invention, MgFe2O4@GO (b) and MgFe2O4@RGO@MnO2(c) XRD diagram of compound.
Fig. 4 is MgFe of the present invention2O4@RGO@MO2The absorbing property (wave absorbing agent thickness=2.0mm) of compound.
Specific embodiment
The present invention will be further described with specific embodiment with reference to the accompanying drawing.Experiment side in following examples
Method is conventional method unless otherwise specified；Used material in example is purchased from conventional chemical examination unless otherwise specified
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:
ZinIndicate the characteristic impedance of suction wave medium, Z0Indicate free space impedance, f is microwave frequency, and c indicates the light velocity, d table
Show the thickness for inhaling wave medium, εr(εr=εr’-jεr") and μr(μr=μr’-jμr") be inhale wave medium opposite complex dielectric permittivity with
Complex permeability.
Embodiment 1
A kind of preparation method of hierarchical structure wave absorbing agent:
(1) 1.352g FeCl is weighed respectively3·6H2O and 0.845MgSO4·7H2O is dissolved in 40mL ethylene glycol solution, with
3.6g NaAc and 1.0g polyethylene glycol is added afterwards, is stirred by ultrasonic 0.5 hour.Gained mixed liquor is transferred to stainless steel cauldron
In, 180 DEG C are reacted 12 hours, cooled to room temperature, filtering.Solid formation is respectively washed three times with deionized water and ethyl alcohol respectively,
By solid formation ultrasonic disperse in 20mL deionized water, 0.5mL 3- aminopropyl-trimethoxy silane is added and stirs evenly, 100
DEG C back flow reaction 8h, obtained solid particle are scattered in again in 20mL deionized water, are denoted as mixed liquor A；Separately weighing 0.5g can be swollen
Swollen graphite (EG) and 3.0g KMnO4It is placed in 500mL three-neck flask, is uniformly mixed, be slowly added to the body of 60mL thereto
Product is than the dense H for 1:93PO4With dense H2SO4Mixed liquor, heating water bath to 50 DEG C, stir 8 hours；Reactant is cooled to room
Temperature is carefully poured into the beaker for filling ice water, and H is added dropwise2O2To mixed solution in golden yellow；Centrifuge separation, discards supernatant liquor,
It is scattered in 500mL deionized water, it is neutral that the NaOH for being 1M with concentration, which adjusts pH value of solution,.Then by it in ice-water bath
Ultrasound 8 hours, obtains suspension B (GO content is about 1mg/mL)；Solution B is added dropwise in mixed liquor A, is 1M's with concentration
It is back flow reaction 2 hours at 1,80 DEG C that HCl solution, which adjusts its pH,.Separate to obtain solid product with magnet, respectively with deionized water with
Ethyl alcohol respectively washs three times, is dried under vacuum to constant weight up to MgFe2O4@GO binary complex；
(2) MgFe is prepared with oxidation-in-stiu coating and thermal reduction2O4@RGO@MnO2Compound.By the MgFe of 0.2g2O4@
GO compound is dissolved in 30mL deionized water, and 0.158g potassium permanganate is added, and mixed liquor is transferred to 100mL not by ultrasonic disperse
It is reacted 16 hours for 180 DEG C in rust steel reaction kettle.Solid formation is isolated with magnet, respectively washs two with deionized water and ethyl alcohol respectively
Secondary, solid formation is dried under vacuum to constant weight in 50~80 DEG C to get MgFe2O4@RGO@MnO2Compound (sample 1)；
It (3) 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
Each substance is weighed, ground and mixed is uniform；Obtain wave absorbing agent；
(4) by above-mentioned wave absorbing agent be pressed into internal diameter be 3.0mm, outer diameter 7.0mm, with a thickness of the circular ring plate of 2mm, use vector
Network Analyzer measures sample in the complex dielectric permittivity and complex permeability of 2~18GHz range, calculates sample according to correlation formula
Reflection loss.
Embodiment 2:
A kind of preparation method of hierarchical structure wave absorbing agent:
(1) 2.702g FeCl is weighed respectively3·6H2O and 1.690MgSO4·7H2O is dissolved in 60mL ethylene glycol solution, with
7.2g NaAc and 2.0g polyethylene glycol is added afterwards, is stirred by ultrasonic 1.0 hours.Gained mixed liquor is transferred to stainless steel cauldron
In, 200 DEG C are reacted 12 hours, cooled to room temperature, filtering.Mixed liquor A is prepared by the method for (1) the step of embodiment 1
(1.0mL 3- aminopropyl-trimethoxy silane)；Separately weigh 1.0g expansible graphite (EG) and 6.0g KMnO4It is placed in 500mL tri-
It in neck flask, is uniformly mixed, the volume ratio for being slowly added to 140mL thereto is the dense H of 1:93PO4With dense H2SO4Mixing
Liquid prepares suspending liquid A by the method for 1 step of embodiment (1) (RGO content is about 2mg/mL)；Solution B is added dropwise to mixing
In liquid A, adjusting its pH with the HCl solution that concentration is 1M is back flow reaction 3 hours at 1,80 DEG C.Solid phase production is separated to obtain with magnet
Object is respectively washed three times with deionized water and ethyl alcohol respectively, is dried under vacuum to constant weight up to MgFe2O4@GO binary complex；
(2) MgFe is prepared with oxidation-in-stiu coating and thermal reduction2O4@RGO@MnO2Compound.By the MgFe of 0.4g2O4@
GO compound is dissolved in 30mL deionized water, prepares MgFe by the method for 1 step of embodiment (1)2O4@RGO@MnO2Compound (sample
Product 2)；
It (3) 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 weighs each substance, and ground and mixed is uniform to obtain wave absorbing agent；
(4) method is the same as 1 step of embodiment (4).
Embodiment 3:
A kind of preparation method of hierarchical structure wave absorbing agent:
(1) 4.056g FeCl is weighed respectively3·6H2O and 2.535MgSO4·7H2O is dissolved in 80mL ethylene glycol solution, with
10.8g NaAc and 3.0g polyethylene glycol is added afterwards, is stirred by ultrasonic 1.5 hours.Gained mixed liquor is transferred to stainless steel cauldron
In, 220 DEG C are reacted 12 hours, cooled to room temperature, filtering.Mixed liquor A is prepared by the method for (1) the step of embodiment 1
(1.5mL 3- aminopropyl-trimethoxy silane)；Separately weigh 1.5g expansible graphite (EG) and 9.0g KMnO4It is placed in 500mL tri-
It in neck flask, is uniformly mixed, the volume ratio for being slowly added to 200mL thereto is the dense H of 1:93PO4With dense H2SO4Mixing
Liquid prepares suspending liquid A by the method for 1 step of embodiment (1) (RGO content is about 3mg/mL)；Solution B is added dropwise to mixing
In liquid A, adjusting its pH with the HCl solution that concentration is 1M is back flow reaction 3 hours at 1,80 DEG C.Solid phase production is separated to obtain with magnet
Object is respectively washed three times with deionized water and ethyl alcohol respectively, is dried under vacuum to constant weight up to MgFe2O4@GO binary complex；
(2) MgFe is prepared with oxidation-in-stiu coating and thermal reduction2O4@RGO@MnO2Compound.By the MgFe of 0.6g2O4@
GO compound is dissolved in 30mL deionized water, prepares MgFe by the method for 1 step of embodiment (1)2O4@RGO@MnO2Compound (sample
Product 3)；
It (3) 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 weighs each substance, and ground and mixed is uniform, obtains wave absorbing agent；
(4) method is the same as 1 step of embodiment (4).
Absorbing property test, test result such as table are carried out to sample 1, sample 2 obtained by the various embodiments described above and sample 3
Shown in 1:
The absorbing property of each example of table 1
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form
Limitation, there are also other variations and modifications on the premise of not exceeding the technical scheme recorded in the claims.
Claims (7)
1. a kind of hierarchical structure wave absorbing agent, characterized in that the wave absorbing agent is made 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；The binary metal oxide one of which metallic element be Fe, another kind be Zn, Ba,
Any one in Ca, Mg, Sn, Ti, Sr and Sm；
The preparation method of the hierarchical structure wave absorbing agent, comprising the following steps:
(1) hydro-thermal method prepares binary metal oxide: weighing 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, carries out 10 ~ 20 h of hydro-thermal reaction, cooled to room temperature at 180 ~ 220 DEG C, and solid formation is filtered to obtain in washing；
(2) cladding process prepares binary complex: dispersing solid formation described in step (1) in deionized water, is added 0.5 ~ 1.5
3- aminopropyl-trimethoxy silane of mL stirs evenly, and flows 8 ~ 12 h of reaction next time in 80 ~ 100 DEG C of temperature conditions, obtains solid
Particle, obtained solid particle are scattered in deionized water again, are denoted as mixed liquor A；Separately weigh 0.5 ~ 1.5 g graphite and 3.0 ~
9.0 g KMnO4, be uniformly mixed, be slowly added to the concentrated acid solution of 60 ~ 200 mL thereto, heating water bath to 40 ~ 60 DEG C,
It after stirring 8 ~ 12 hours, is cooled to room temperature, H is added dropwise2O2To solution in golden yellow, centrifuge separation takes solid product, will be described solid
Phase product is scattered in deionized water, and adjusting PH is neutrality, is then sonicated to obtain suspension B；Suspension B is mixed with mixed liquor A
It closes, adjusting pH value is 1 ~ 3,2 ~ 4h of back flow reaction, washs the binary metal oxide of dry GO cladding, and as binary is compound
Object；
(3) thermal reduction prepares ternary complex: binary complex described in (2) the step of 0.2 ~ 0.8g is dissolved in deionization
In water, 0.158 ~ 0.474g potassium permanganate is added, ultrasonic disperse obtains mixed solution, mixed liquor is carried out water at 180 ~ 220 DEG C
Thermal response 10 ~ for 24 hours, solid formation is isolated, washing is drying to obtain ternary complex；
(4) it takes ternary complex and film forming agent ground and mixed uniform respectively, obtains wave absorbing agent.
2. a kind of hierarchical structure wave absorbing agent according to claim 1, characterized in that the ternary complex and film forming agent
Mass ratio is 1 ~ 5: 5 ~ 1, wherein the film forming agent is paraffin.
3. a kind of preparation method of hierarchical structure wave absorbing agent according to claim 1, characterized in that described in step (1)
Solvent is ethylene glycol solution, and volume is 40 ~ 80 mL.
4. a kind of preparation method of hierarchical structure wave absorbing agent according to claim 1, characterized in that described in step (2)
Concentrated acid solution is dense H3PO4With dense H2SO4Mixed liquor, the dense H3PO4With dense H2SO4Volume ratio be 1:(5 ~ 10).
5. a kind of preparation method of hierarchical structure wave absorbing agent according to claim 1, characterized in that in step (2), gained
Graphene oxide content is 1 ~ 3.0 mg/mL in suspension B.
6. a kind of preparation method of hierarchical structure wave absorbing agent according to claim 1, characterized in that step (1) and (3)
In, the hydro-thermal reaction carries out in a high pressure reaction kettle.
7. a kind of preparation method of hierarchical structure wave absorbing agent according to claim 1, characterized in that in step (3), ternary
The mass ratio of compound and film forming agent is 1 ~ 5: 5 ~ 1, wherein the film forming agent is paraffin.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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