CN110255536A - Composite material and preparation method with absorbing property and electromagnetic shielding performance - Google Patents
Composite material and preparation method with absorbing property and electromagnetic shielding performance Download PDFInfo
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- CN110255536A CN110255536A CN201910548639.6A CN201910548639A CN110255536A CN 110255536 A CN110255536 A CN 110255536A CN 201910548639 A CN201910548639 A CN 201910548639A CN 110255536 A CN110255536 A CN 110255536A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The present invention relates to the composite material and preparation methods with absorbing property and electromagnetic shielding performance.In composite material of the invention, Fe3O4With SiO2Form Fe3O4@SiO21-dimention nano ball chain structure, and the Fe3O4@SiO2Nanometer ball chain is evenly embedded into rGO nanoscale twins.Composite material of the invention has light, wideband and high shielding properties, and preparation method is simple, extensive in civilian, military project, field of aerospace application prospect.
Description
Technical field:
The present invention relates to the composite materials with absorbing property and electromagnetic shielding performance, belong to electromagnetic shielding material field.
The invention further relates to the preparation methods of the composite material.
Background technique:
With the progress of modern science and technology and communications industry, either in daily life or in military field,
Electromagnetic wave is generated as information, is propagated, receiving and the important medium of processing has obtained extremely wide application and continuous development.Electricity
Magnetic technology brings while people offer convenience with technology development bring a series of electromagnetic pollution problems with being also difficult to avoid that.One
Aspect, the electromagnetic interference that complicated electromagnetic network is formed cause electronic equipment to can not work normally or reduced performance；On the other hand,
Electromagnetic energy can generate human organ and chemically and physically act on, and irreversible serious wound will be if things go on like this caused to human body
Evil, final damage health.Therefore, electromagnetic pollution becomes one of environmental problem urgently to be resolved in contemporary society's life.
Currently used for protecting effective material of electromagnetic radiation to be divided into two classes according to the difference of its mechanism of action, one kind is to inhale wave
Material, in addition one kind is electromagnetic shielding material.
Absorbing material is to refer to effectively absorb incident electromagnetic wave, and convert its energy to thermal energy or other energy
And a kind of functional material consumed.Since absorbing material can fundamentally weaken or eliminate electromagnetic wave, have become
Effective protection and the maximally efficient approach for weakening electromagnetic radiation, and it is increasingly becoming modern weapons equipment and radar invisible performance
Important technology support.
Electromagnetic shielding material generally uses the good conductor of high conductivity or high magnetic conductivity as matrix, when electromagnetic radiation is by certainly
When by space directive good conductor, inhibit radio-frequency electromagnetic spoke using reflection effect and sink effect of the conductor to electromagnetic radiation to reach
The influence penetrated inhibits its radiation intensity within defined safe range.
Demand of the countries in the world today to electro-magnetic wave absorption and shielding material all increases promptly, and simultaneous is to this
The requirement of class material is also higher and higher, therefore in depth studies electro-magnetic wave absorption and shielding material with very profound significance.
The major defect of traditional absorbing material (ferrite, graphite, ceramic-like materials etc.) is that density is big, absorption band is wide
Deng, thus it is not able to satisfy the requirement of absorbing material " thin, light, wide, strong ".Novel absorbing material mainly has graphene, nanometer material
Material, polycrystalline iron fiber, conduction high polymer etc., wherein graphene nano material and conduction high polymer have become the research in the field
Hot spot.Application study of the graphene in electromagnetic shielding and absorbing material at present can be divided into two major classes: first is that graphene-metal
Composite material；Second is that graphene-polymer composite material.
Composite material of the invention belongs to graphene-metallic composite.In composite material of the invention, Fe3O4With
SiO2Form Fe3O4@SiO21-dimention nano ball chain structure, and the Fe3O4@SiO2Nanometer ball chain is evenly embedded into rGO nanometers
In lamella.Composite material and preparation method thereof of the invention is simple to operation, Fe3O4@SiO21-dimention nano ball chain structure can effectively subtract
Agglomeration between few magnetic nanoparticle, while intergranular directional transmissions function can also be enhanced, and then reinforcing material is most
Whole electromagnetic performance.
Summary of the invention:
It is an object of that present invention to provide it is a kind of novel while with excellent absorbing property and electromagnetic shielding performance
rGO/Fe3O4@SiO2Composite material.
In rGO/Fe of the invention3O4@SiO2In composite material, Fe3O4With SiO2Form Fe3O4@SiO21-dimention nano ball chain
Structure, and Fe3O4@SiO2Nanometer ball chain is evenly embedded into redox graphene (rGO) nanoscale twins.Of the invention
rGO/Fe3O4@SiO2In composite material, rGO and Fe3O4@SiO2Mass ratio be 1:1,2:1 or 4:1.As rGO and Fe3O4@
SiO2Mass ratio when being 4:1, shield effectiveness is best, and average electromagnet shield effect is 30dB, is to reach at 18GHz in frequency
Peak 37dB；As rGO and Fe3O4@SiO2Mass ratio be 2:1 when, composite material exhibits go out excellent absorption intensity, most
Good absorption peak is -48.34dB, and effective Absorber Bandwidth is 4.02GHz；As rGO and Fe3O4@SiO2Mass ratio be 1:1 when,
Effective absorption band of composite material electromagnetic wave absorption is wide to reach 5.5GHz, far more than the Absorber Bandwidth of most of wave absorbing agents.
RGO/Fe of the present invention is prepared the present invention also provides a kind of3O4@SiO2The method of composite material.
In the method for the invention, the uniform Fe of pattern is prepared using hydro-thermal method first3O4Magnetic nanoparticle utilizes
Its magnetic responsiveness can and combine the hydrolytic process of tetraethyl orthosilicate, synthesize the Fe with One-Dimensional Spherical chain structure3O4@SiO2
Nanometer ball chain；Then by Fe obtained3O4@SiO2The rGO of nanometer ball chain and different proportion progress is compound, prepares and has excellent suction
The rGO/Fe of wave performance and electromagnetic shielding performance3O4@SiO2Composite material.
Detailed preparation step is as follows,
The first step, using solvent structure Fe3O4Magnetic nanoparticle:
(1) it prepares solution: weighing 2.028g ferric chloride hexahydrate (FeCl respectively3.6H2O), 3.69g sodium acetate (NaAc),
0.0224g disodium EDTA (EDTA-2Na) and 60ml ethylene glycol (EG) are added in the reaction kettle liner of 100ml,
(2) it pre-processes: magnetic agitation being carried out to the mixed solution that back obtains and is aided with ultrasonic treatment, be allowed to be formed steady
The uniform turbid of fixed khaki, this process last about greatly 2h,
(3) pyroreaction: reaction system is encapsulated, and handles 10h in 200 DEG C of baking oven high temperatures,
(4) sample collection: after reaction to system natural cooling, collecting brownish black precipitated product, with dehydrated alcohol and
Deionized water alternately ultrasonic cleaning four times, and place it in 50 DEG C of baking ovens and be dried for standby；
Second step, Fe3O4@SiO2The preparation of nano chain:
(1) it prepares solution: weighing the Fe that 0.0258g is prepared by the above method3O4Sample and by it with 6mL deionized water,
40mL dehydrated alcohol and 1mL concentrated ammonia liquor are added in three-necked flask jointly,
(2) it pre-processes: mixed solution being placed in ultrasonic machine and is ultrasonically treated 0.5h,
(3) it coats process: 170 μ L tetraethyl orthosilicates (TEOS) being added dropwise into ultrasonic agitation system,
(4) induce chaining: TEOS continues ultrasound 20min after being added, and then draws 20mL mixed solution from system and is put into
In small beaker, and the beaker is placed in away from about 3 seconds at the 2cm of circular magnet center immediately；Then beaker is removed and is placed in no magnet ring
In border, 25min is stood,
(5) it sample collection: after standing, is precipitated with the solid in washes of absolute alcohol three times beaker, obtained product
It is dried for standby in 50 DEG C of baking ovens；
Third step, rGO/Fe3O4@SiO2The preparation of composite material:
(1) graphene oxide of 40mg (rGO) is added in 250ml round-bottomed flask, 60ml deionized water, ultrasound is added
2h makes it at uniform solution,
(2) above-mentioned solution is put into 90 DEG C of oil baths, slowly instills 70ul hydrazine hydrate, magnetic stirs 2h, turns off oil bath, cooling
To room temperature, magneton is taken out,
(3) by above-mentioned solution ultrasonic disperse, according to rGO and Fe3O4@SiO2Mass ratio be respectively 1:1,2:1,4:1 be added
The Fe being prepared in second step3O4@SiO2Nanometer ball chain, ultrasonic 2h,
(4) above-mentioned solution is centrifuged, is replaced 3 times using ethyl alcohol and deionized water, places into freeze dryer and be freeze-dried,
Obtain rGO/Fe3O4@SiO2Composite material.
Compared with existing material, this material has following advantage:
(1) in composite material of the present invention, Fe3O4@SiO2The one-dimentional structure of nanometer ball chain can effectively reduce magnetic Nano
The agglomeration of intergranular, while intergranular directional transmissions function can also be enhanced, and then the electromagnetic performance that reinforcing material is final.
(2) composite material of the invention has excellent absorbing property and electromagnetic shielding performance simultaneously.
(3) preparation method of composite material of the present invention can play fixed Fe using tetraethyl orthosilicate hydrolysate3O4?
The effect of grain, while dexterously applying a uniform magnetic field during hydrolysis, and then successfully induce Fe3O4@SiO2It is fixed into
Straight chain structure.
(4) the preparation method majority of material of the present invention is physical method, easy to operate, and time-consuming is few, and energy consumption is few, and without making
It is environmentally protective to accomplish with other chemical reagent.
Detailed description of the invention:
Fig. 1 a:Fe3O4The SEM photograph of the microscopic appearance of nano particle；
Fig. 1 b:Fe3O4Surface layer has coated the SEM photograph of the microscopic appearance of the nano particle of silica；
Fig. 1 c and Fig. 1 d: the Fe of one-dimensional catenary structure3O4@SiO2The SEM photograph of the microscopic appearance of nanometer ball chain；
Fig. 2 a:rGO and Fe3O4@SiO2Mass ratio be 1:1 when rGO/Fe3O4@SiO2The reflection loss of composite material is bent
Line；
Fig. 2 b:rGO and Fe3O4@SiO2Mass ratio be 2:1 when rGO/Fe3O4@SiO2The reflection loss of composite material is bent
Line；
Fig. 2 c:rGO and Fe3O4@SiO2Mass ratio be 4:1 when rGO/Fe3O4@SiO2The reflection loss of composite material is bent
Line.
Specific embodiment
Embodiment 1
The first step, using solvent structure Fe3O4Magnetic nanoparticle:
(1) it prepares solution: weighing 2.028g ferric chloride hexahydrate (FeCl respectively3.6H2O), 3.69g sodium acetate (NaAc),
0.0224g disodium EDTA (EDTA-2Na) and 60ml ethylene glycol (EG) are added in the reaction kettle liner of 100ml,
(2) it pre-processes: magnetic agitation being carried out to the mixed solution that back obtains and is aided with ultrasonic treatment, be allowed to be formed steady
The uniform turbid of fixed khaki, this process last about greatly 2h,
(3) pyroreaction: reaction system is encapsulated, and handles 10h in 200 DEG C of baking oven high temperatures,
(4) sample collection: after reaction to system natural cooling, collecting brownish black precipitated product, with dehydrated alcohol and
Deionized water alternately ultrasonic cleaning four times, and place it in 50 DEG C of baking ovens and be dried for standby；
Second step, Fe3O4@SiO2The preparation of nanometer ball chain:
(1) it prepares solution: weighing the Fe that 0.0258g is prepared by the above method3O4Sample and by it with 6mL deionized water,
40mL dehydrated alcohol and 1mL concentrated ammonia liquor are added in three-necked flask jointly,
(2) it pre-processes: mixed solution being placed in ultrasonic machine and is ultrasonically treated 0.5h,
(3) it coats process: 170 μ L tetraethyl orthosilicates (TEOS) being added dropwise into ultrasonic agitation system,
(4) induce chaining: TEOS continues ultrasound 20min after being added, and then draws 20mL mixed solution from system and is put into
In small beaker, and the beaker is placed in away from about 3 seconds at the 2cm of circular magnet center immediately；Then beaker is removed and is placed in no magnet ring
In border, 25min is stood,
(5) it sample collection: after standing, is precipitated with the solid in washes of absolute alcohol three times beaker, obtained product
It is dried for standby in 50 DEG C of baking ovens；
Third step, rGO/Fe3O4@SiO2The preparation of composite material:
(1) graphene oxide of 40mg (rGO) is added in 250ml round-bottomed flask, 60ml deionized water, ultrasound is added
2h makes it at uniform solution,
(2) above-mentioned solution is put into 90 DEG C of oil baths, slowly instills 70ul hydrazine hydrate, magnetic stirs 2h, turns off oil bath, cooling
To room temperature, magneton is taken out,
(3) by above-mentioned solution ultrasonic disperse, according to rGO and Fe3O4@SiO2Mass ratio be 1:1 be added second step in prepare
Obtained Fe3O4@SiO2, ultrasonic 2h,
(4) above-mentioned solution is centrifuged, ethyl alcohol and deionized water replace 3 times, place into freeze dryer and are freeze-dried, are obtained
rGO/Fe3O4@SiO2Composite material.
Embodiment 2
It is identical as the step in embodiment 1, in addition in third step rGO/Fe3O4@SiO2In the preparation of composite material, adjustment
(4) step rGO and Fe3O4@SiO2Mass ratio be 2:1 so that obtained rGO/Fe3O4@SiO2RGO and Fe in composite material3O4
Mass ratio be 2:1.
Embodiment 3
It is identical as the step in embodiment 1, in addition in third step rGO/Fe3O4@SiO2In the preparation of composite material, adjustment
(4) step rGO and Fe3O4@SiO2Mass ratio be 4:1 so that obtained rGO/Fe3O4@SiO2RGO and Fe in composite material3O4
Mass ratio be 4:1.
In conjunction with the embodiments, with reference to attached drawing 2, rGO/Fe of the present invention is analyzed3O4@SiO2The performance of composite material.
Figure it is seen that rGO/Fe3O4@SiO2In composite material, as rGO and Fe3O4@SiO2Mass ratio be 1:1
When, effective absorption band of composite material electromagnetic wave absorption is wide to reach 5.5GHz, far more than the Absorber Bandwidth of most of wave absorbing agents.When
RGO and Fe3O4@SiO2Mass ratio when being 2:1, composite material exhibits go out excellent absorbing property, optimal absorption peak value is-
48.34dB, effective Absorber Bandwidth are 4.02GHz.As rGO and Fe3O4@SiO2Mass ratio be 4:1 when, shield effectiveness is best, put down
Equal electromagnet shield effect is 30dB, is the peak for reaching 37dB at 18GHz in frequency.
Claims (6)
1. the composite material with absorbing property and electromagnetic shielding performance, which is characterized in that in the composite material, Fe3O4With SiO2
Form Fe3O4@SiO21-dimention nano ball chain structure, and the Fe3O4@SiO2Nanometer ball chain is evenly embedded into rGO nanoscale twins
In.
2. composite material according to claim 1, wherein rGO and Fe3O4@SiO2Mass ratio be 1:1,2:1 or 4:
1。
3. composite material according to claim 2, wherein as rGO and Fe3O4@SiO2Mass ratio be 1:1 when, it is compound
Effective absorption band of material electromagnetic wave absorption is wide to reach 5.5GHz.
4. composite material according to claim 2, wherein as rGO and Fe3O4@SiO2Mass ratio be 2:1 when, it is compound
Material optimal absorption peak value is -48.34dB, and effective Absorber Bandwidth is 4.02GHz.
5. composite material according to claim 2, wherein as rGO and Fe3O4@SiO2Mass ratio when being 4:1, it is average
Electromagnet shield effect is 30dB, is to reach peak 37dB at 18GHz in frequency.
6. the method for preparing composite material described in any one of the claims 1-5 comprising following steps,
The first step, using solvent structure Fe3O4Magnetic nanoparticle:
(1) it prepares solution: weighing 2.028g ferric chloride hexahydrate (FeCl respectively3.6H2O), 3.69g sodium acetate (NaAc),
0.0224g disodium EDTA (EDTA-2Na) and 60ml ethylene glycol (EG) are added in the reaction kettle liner of 100ml,
(2) it pre-processes: magnetic agitation being carried out to the mixed solution that back obtains and is aided with ultrasonic treatment, is allowed to be formed stable
The uniform turbid of khaki, this process last about greatly 2h,
(3) pyroreaction: reaction system is encapsulated, and handles 10h in 200 DEG C of baking oven high temperatures,
(4) sample collection: after reaction to system natural cooling, collecting brownish black precipitated product, with dehydrated alcohol and go from
Alternately ultrasonic cleaning four times of sub- water, and place it in 50 DEG C of baking ovens and be dried for standby；
Second step, Fe3O4@SiO2The preparation of nanometer ball chain:
(1) it prepares solution: weighing the Fe that 0.0258g is prepared by the above method3O4Sample and by it with 6mL deionized water, 40mL without
Water-ethanol and 1mL concentrated ammonia liquor are added in three-necked flask jointly,
(2) it pre-processes: mixed solution being placed in ultrasonic machine and is ultrasonically treated 0.5h,
(3) it coats process: 170 μ L tetraethyl orthosilicates (TEOS) being added dropwise into ultrasonic agitation system,
(4) induce chaining: TEOS continues ultrasound 20min after being added, and then draws 20mL mixed solution from system and is put into small burning
In cup, and the beaker is placed in away from about 3 seconds at the 2cm of circular magnet center immediately；Then beaker is removed and is placed in non-magnetic environment,
25min is stood,
(5) it sample collection: after standing, is precipitated with the solid in washes of absolute alcohol three times beaker, obtained product is in 50
It is dried for standby in DEG C baking oven；
Third step, rGO/Fe3O4@SiO2The preparation of composite material:
(1) graphene oxide of 40mg (rGO) is added in 250ml round-bottomed flask, 60ml deionized water is added, ultrasonic 2h makes
Its at uniform solution,
(2) above-mentioned solution is put into 90 DEG C of oil baths, slowly instills 70ul hydrazine hydrate, magnetic stirs 2h, turns off oil bath, be cooled to room
Temperature takes out magneton,
(3) by above-mentioned solution ultrasonic disperse, according to rGO and Fe3O4@SiO2Mass ratio be respectively 1:1,2:1,4:1 be added second
The Fe being prepared in step3O4@SiO2Nanometer ball chain, ultrasonic 2h,
(4) above-mentioned solution is centrifuged, is replaced 3 times using ethyl alcohol and deionized water, places into freeze dryer and be freeze-dried, obtained
rGO/Fe3O4@SiO2Composite material.
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| CN112897531A (en) * | 2021-04-02 | 2021-06-04 | 安徽工业大学 | Method for preparing silicon dioxide with wave absorbing function by using blast furnace slag |
| CN114715952A (en) * | 2022-03-23 | 2022-07-08 | 三峡大学 | Graphene Fe3O4@SiO2Method for preparing composite particles |
| CN115466596A (en) * | 2022-07-20 | 2022-12-13 | 哈尔滨工业大学 | Fe-Fe 3 O 4 @mSiO 2 @ RGO composite material and magnetic property controllable preparation method and application thereof |
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Application publication date: 20190920 |