CN108929653A - A kind of three-dimensional grapheme base composite wave-absorbing material and preparation method thereof - Google Patents
A kind of three-dimensional grapheme base composite wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of three-dimensional grapheme base composite wave-absorbing materials and preparation method thereof.The absorbing material is the composite material being made of magnetic Nano Fe-base compound and three-dimensional grapheme, and wherein equably growth in situ is in three-dimensional grapheme lamellar structure for magnetic Nano Fe-base compound, and stable structure is not easily to fall off.The present invention can prepare a series of different magnetic Nano Fe-base compound/three-dimensional grapheme composite wave-suction materials by controlling reaction condition, method is novel, it is with short production cycle, it is at low cost, repeatability is strong and can be prepared on a large scale, and has important reference function to the preparation of graphite alkenyl composite wave-absorbing material；Material of the invention, by the way that the magnetic Nano Fe-base compound of strong dielectric loss and magnetic loss and the graphene of strong resistance loss is compound, wide suction wave frequency section and high suction intensity of wave are realized, and shows excellent absorbing property in low frequency range, meets the needs of actual use.
Description
Technical field
The invention belongs to electromagnetic wave absorbent material fields, and in particular to a kind of three-dimensional grapheme base composite wave-absorbing material and its
Preparation method.
Background technique
With the rapid development of electronic technology, the technologies such as television broadcasting communication, microwave dark room, radar guidance are generalized and answer
With the novel wave-absorbing material of one of effective means of reduction electromagnetic radiation as first choice becomes research hotspot in recent years.Nothing
Demand by military field or civil field to absorbing material is continuously improved, the application study about absorbing material increasingly by
To attention.Graphene is as a kind of new carbon, due to can satisfy novel wave-absorbing material with special structure and performance
The requirement of " thin, wide, light, strong ", makes it have a good application prospect in field of microwave absorption.However the biggish dielectric of graphene
Constant is unfavorable for impedance matching, affects its microwave attenuation performance.In addition, the absorbing property of graphene be also not it is highly desirable and
Higher cost, therefore limit its application.
Graphene absorbing property is poor, is one with other Medium impedence matching performance differences and higher preparation cost and urgently solves
Certainly the problem of.Have in recent years about the study on the modification of grapheme material compared with quantum jump, by answering graphene and other materials
Conjunction constructs composite wave-suction material to adjust its electromagnetic parameter, so as to improve the matching degree of graphene, is expected to obtain lightweight, efficient
Absorbing material can be widely applied to many industries such as absorbing material, electromagnetic shielding, communication apparatus.Therefore, low cost, scale
The three-dimensional grapheme base composite wave-absorbing material haveing excellent performance is controllably prepared, is had extremely for the development of electromagnetic wave absorbent material
Important theoretical and practical significance.Through literature survey, have no that high Temperature Chemical Foaming method prepares three-dimensional graphite alkenyl composite wave-absorbing material
The report of material.
Summary of the invention
The present invention provides a kind of simple, efficient, inexpensive, prepare with scale three-dimensional grapheme base composite wave-absorbing material
Method, material of the invention is by by the magnetic Nano Fe-base compound of strong dielectric loss and magnetic loss and strong resistance loss
Graphene is compound, realizes wide suction wave frequency section and high suction intensity of wave, and excellent absorbing property is shown in low-frequency band,
Meets the needs of actual use.
Composite wave-suction material of the invention is made of magnetic Nano Fe-base compound and three-dimensional grapheme two parts, wherein magnetic
The nanometer iron-based compound homoepitaxial of property is in three-dimensional grapheme lamellar structure, stable structure；Magnetic Nano iron-basedization
Conjunction object is Fe, Fe3C, FexCoy, FexNiy, FexCoyNiz, FexNiyMoz, FexSiy, FexSiyAlz, FexCoyNbzVm,
FexCoyCez, FexCoyYz, FexCoyNz, FexCuyNbzSimBn, Fe3O4, NiFe2O4, BaFe2O4, CoFe2O4, FexCoyNizO,
FexLaySrzZnmO, FexCoyS, FexNiyOne or both of compounds such as S, having a size of between 30nm~500nm and being in
Dispersity, pattern is spherical or close spherical, and uniform load is in graphene sheet layer structure；Above-mentioned magnetic Nano Fe-base compound
Middle chemical formula footmark x, y, z, m, n refer to the chemical formula stoichiometric number of each element in the compound, are controllable numerical value.
To achieve the above object, the technical solution adopted by the present invention is as follows:
1) dissolution of nine water ferric nitrates, other one or more metal salts and polyvinylpyrrolidone is matched in deionized water
At mixed solution, 10~20min is stirred by ultrasonic.
2) mixed solution is placed in heat preservation in air dry oven until being completely dried, then pulverized；
3) ground powder is transferred in crucible, then crucible is placed in tube furnace in Ar or N2With 1 in atmosphere
The heating rate of~10 DEG C/min is heated to 900~1500 DEG C, and keeps the temperature 1~2h, after tube furnace is cooled to room temperature, collects black
Color foam-like product, as magnetic Nano ferrous alloy/three-dimensional grapheme or nano-carbide/three-dimensional grapheme composite wave-absorbing material
Material.
4) by magnetic Nano ferrous alloy/three-dimensional grapheme or nano-carbide/three-dimensional grapheme composite wave-absorbing of preparation
Material, which is placed in tube furnace, carries out 3~6h of oxidation processes in air atmosphere, after tube furnace is cooled to room temperature, collects foam-like and produces
Object, as Magnetic nano iron base oxide/three-dimensional grapheme composite wave-suction material.
5) by magnetic Nano ferrous alloy/three-dimensional grapheme or nano-carbide/three-dimensional grapheme composite wave-absorbing of preparation
Material and excessive sublimed sulfur are placed in tube furnace after evenly mixing, in Ar or N2Added in atmosphere with the heating rate of 1~5 DEG C/min
Heat keeps the temperature 2~4h to 300~500 DEG C, after tube furnace is cooled to room temperature, collects foam-like product, as Magnetic nano iron
Base sulfide/three-dimensional grapheme composite wave-suction material.
Further, nine water ferric nitrates, other one or more metal salts and polyvinylpyrrolidone in the step 1)
Mass ratio is (1.5~2.0): (0~2.0): 1, wherein raw material mass mixture ratio (0~2.0) is other one or more metal salts
Quality summation accounting；Other metal salts are to contain Fe, Co, Ni, Ba, Mo, Si, Al, Nb, V, Ce, Y, Cu, B, La, Sr, the gold such as Zn
The nitrate or carbonate or silicate of category element；(K value refers to the viscous of polyvinylpyrrolidone to the K value of polyvinylpyrrolidone
Consistency) range be 13~32.
Further, the drying temperature in the step 2) is 70~80 DEG C.
Further, the oxidation processes in the step 4) are divided into low-temperature oxidation processing or high temperature oxidation process；It is wherein low
Warm oxidation temperature is 150~300 DEG C；High temperature oxidation process temperature is 500~800 DEG C.
Further, the magnetic Nano ferrous alloy/three-dimensional grapheme or nano-carbide/three-dimensional stone in the step 5)
The mass ratio of black alkene composite wave-suction material and sublimed sulfur is 1:(1.0~2.0).
Further, step 2)~5) described in three-dimensional grapheme base composite wave-absorbing material, it is characterised in that institute
State in three-dimensional grapheme base composite wave-absorbing material prepared by step c-e each element in the chemical formula of magnetic Nano Fe-base compound
Stoichiometric number can be regulated and controled by raw material proportioning in step a.
A kind of low cost of three-dimensional grapheme base composite wave-absorbing material proposed by the invention, large-scale preparation method, still
Have no document and other aspects report.Preparation method is simple, at low cost, and method is novel, with short production cycle, can prepare with scale.
Obtained nano-scale magnetic Fe-base compound is dispersed in three-dimensional grapheme lamellar structure, so that the iron-based chemical combination of nano-magnetic
Object/three-dimensional grapheme composite wave-suction material existing graphene resistance loss, and the strong dielectric of nanometer iron-based compound that is magnetic
Loss and mangneto loss, have well solved that independent graphene absorbing property is poor, the problem of impedance matching difference.The three-dimensional stone of preparation
Mertenyl composite wave-suction material is due to that can not only show with special three-dimensional structure and the load of nano-scale magnetic Fe-base compound
It writes and improves its specific surface area, the characteristic that can also inhibit the stacking of graphene, while have quality slim and graceful is expected to lead in absorbing material
Domain is widely used.
Compared with prior art, this method has the advantage that
1) method is simple to operation, at low cost, can prepare with scale, it is reproducible；Magnetism in composite wave-suction material is received
Rice Fe-base compound growth in situ is in graphene sheet layer structure, and not easily to fall off, stability is good；The three-dimensional grapheme prepared
Base composite wave-absorbing material light specific gravity, suction wave frequency section is low, electromagnetic parameter is adjustable, it is high to inhale intensity of wave；And material of the invention is general
The low-frequency band range table that material is extremely difficult to reveals excellent absorbing property.
2) different knots can be prepared by the regulation of content to other metal salts, type and heat treatment heating rate
Structure and the magnetic Nano of type Fe-base compound/three-dimensional grapheme composite wave-suction material, to other relevant three-dimensional graphite alkenyls
The synthesis regulation of composite wave-suction material has directive significance.
Detailed description of the invention
Fig. 1 is that magnetic Nano prepared by embodiment three vulcanizes ferro-cobalt/three-dimensional grapheme composite wave-suction material XRD diagram
Spectrum.
Fig. 2 is that magnetic Nano prepared by embodiment three vulcanizes ferro-cobalt/three-dimensional grapheme composite wave-suction material Raman figure
Spectrum.It can be seen that typical graphene characteristic peak: the peak D and the peak G occurs in material table of the present invention from map, and related to the number of plies
The peak 2D.
Fig. 3 is that magnetic Nano prepared by embodiment three vulcanizes ferro-cobalt/three-dimensional grapheme composite wave-suction material SEM photograph
Piece.By can be seen that material of the present invention is three-dimensional porous structures in figure, wherein graphene film is connected by three-dimensional graphite skeletal support
Constitute three-dimensional grapheme frame structure.
Fig. 4 is that magnetic Nano prepared by embodiment three vulcanizes ferro-cobalt/three-dimensional grapheme composite wave-suction material TEM photograph
Piece.It can be seen that magnetic Nano cobalt sulfide iron particle uniform load is on graphene film.
Fig. 5 is that magnetic Nano prepared by embodiment three vulcanizes ferro-cobalt/three-dimensional grapheme composite wave-suction material AFM photograph
Piece.The obtained graphene thickness of the present invention is about 1.35nm, about 4 layers of graphene.
Fig. 6 is that magnetic Nano prepared by embodiment three vulcanizes ferro-cobalt/three-dimensional grapheme composite wave-suction material wave absorbtion
It can curve.By figure it can be seen that material of the invention not only to absorb frequency range wide, absorption intensity is high, and also shows in low frequency range excellent
Different absorbing property.When absorbing material coating layer thickness is 1.5mm, absorbing frequency range wide can reach 10GHz, and absorption intensity exists
- 85dB is up to when 11.6GHz.
Fig. 7 is Magnetic nano iron cobalt-nickel alloy/three-dimensional grapheme composite wave-suction material suction wave prepared by embodiment two
Performance curve.There is figure it is found that the composite material shows excellent absorbing property in low frequency range: when matching thickness is 2.5mm, frequency
When rate is 4.8GHz, minimal reflection loss is -14dB；When matching thickness is 4.0mm.When frequency is 2.5GHz, minimal reflection damage
Consumption is -12dB.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further elaborated, and non-present invention further limits；With
Used raw material is this field general chemical in lower embodiment.
Embodiment one
1.5:0.8:1 in mass ratio weighs nine water ferric nitrates, cobalt nitrate hexahydrate and polyvinylpyrrolidonepowder powder, then molten
10min is stirred by ultrasonic in deionized water and obtains mixed solution for solution, then mixed solution is placed in 80 DEG C of heat preservations in air dry oven
Until being completely dried, the product after drying is then ground into powder and powder is transferred in crucible, crucible is placed in tube furnace
In be heated to 1000 DEG C in Ar atmosphere with the heating rate of 5 DEG C/min, keep the temperature 2h, collect black foam after tube furnace is cooling
Shape product obtains Magnetic nano iron cobalt alloy/three-dimensional grapheme composite wave-suction material.
Embodiment two
1.5:1.0:1 in mass ratio weighs nine water ferric nitrates, (cobalt nitrate hexahydrate and six water nickel nitrates) and polyvinyl pyrrole
Alkanone powder, wherein raw material proportioning 0.8 is the quality summation accounting of cobalt nitrate hexahydrate and six water ferric nitrates；Be then dissolved in from
15min is stirred by ultrasonic in sub- water and obtains mixed solution, then mixed solution is placed in air dry oven and is kept the temperature until completely for 80 DEG C
It is dry, the product after drying is then ground into powder and powder is transferred in crucible, crucible is placed in tube furnace in Ar atmosphere
1000 DEG C are heated to the heating rate of 5 DEG C/min in enclosing, keeps the temperature 2h, collects black foam shape product after tube furnace is cooling,
Obtain Magnetic nano iron cobalt-nickel alloy/three-dimensional grapheme composite wave-suction material.
Embodiment three
The cobalt alloy of Magnetic nano iron prepared by embodiment one/three-dimensional grapheme composite wave-suction material and sublimed sulfur are pressed into matter
Amount is placed in tube furnace after evenly mixing than 1:1, is heated to 300 DEG C in Ar atmosphere with the heating rate of 2 DEG C/min, and keep the temperature
3h collects foam-like product after tube furnace is cooled to room temperature, and as magnetic Nano vulcanizes the compound suction of ferro-cobalt/three-dimensional grapheme
Wave material.
Example IV
1.5:0:1 in mass ratio weighs nine water ferric nitrates, other one or more metal salts and polyvinylpyrrolidone powder
End is then dissolved in ultrasonic agitation 10min in deionized water and obtains mixed solution, then mixed solution is placed in air dry oven
Product after drying is then ground into powder and powder is transferred in crucible, crucible is set by 80 DEG C of heat preservations up to being completely dried
1200 DEG C are heated to the heating rate of 5 DEG C/min in Ar atmosphere in tube furnace, keeps the temperature 2h, is collected after tube furnace is cooling
Black foam shape product obtains Magnetic nano iron/three-dimensional grapheme composite wave-suction material.
Claims (7)
1. a kind of three-dimensional grapheme base composite wave-absorbing material, which is characterized in that the composite wave-suction material is by Magnetic nano iron
Based compound and three-dimensional grapheme two parts are constituted, and wherein magnetic Nano Fe-base compound homoepitaxial is in three-dimensional grapheme lamella
In structure, stable structure；The magnetic Nano Fe-base compound is Fe, Fe3C, FexCoy, FexNiy, FexCoyNiz,
FexNiyMoz, FexSiy, FexSiyAlz, FexCoyNbzVm, FexCoyCez, FexCoyYz, FexCoyNz, FexCuyNbzSimBn,
Fe3O4, NiFe2O4, BaFe2O4, CoFe2O4, FexCoyNizO, FexLaySrzZnmO, FexCoyS, FexNiyOne in S compound
Kind or two kinds, having a size of between 30nm~500nm and be in dispersity, pattern be it is spherical or close spherical, uniform load is in stone
In black alkene lamellar structure；Chemical formula footmark x in above-mentioned magnetic Nano Fe-base compound, y, z, m, n refer to each member in the compound
The chemical formula stoichiometric number of element, is controllable numerical value.
2. the preparation method of three-dimensional grapheme base composite wave-absorbing material according to claim 1, it is characterised in that preparation step
It is rapid as follows:
A. the dissolution of nine water ferric nitrates, other one or more metal salts and polyvinylpyrrolidone is made into deionized water mixed
Solution is closed, 10~20min is stirred by ultrasonic；
B. mixed solution is placed in heat preservation in air dry oven until being completely dried, then pulverized；
C. ground powder is transferred in crucible, then crucible is placed in tube furnace in Ar or N2With 1~10 in atmosphere
DEG C/heating rate of min is heated to 900~1500 DEG C, and keeps the temperature 1~2h, after tube furnace is cooled to room temperature, collect black bubble
Foam shape product, as magnetic Nano ferrous alloy/three-dimensional grapheme or nano-carbide/three-dimensional grapheme composite wave-suction material；
D. by magnetic Nano ferrous alloy/three-dimensional grapheme or nano-carbide/three-dimensional grapheme composite wave-suction material of preparation
It is placed in tube furnace progress 3~6h of oxidation processes in air atmosphere, after tube furnace is cooled to room temperature, foam-like is collected and produces
Object, as Magnetic nano iron base oxide/three-dimensional grapheme composite wave-suction material；
E. by magnetic Nano ferrous alloy/three-dimensional grapheme or nano-carbide/three-dimensional grapheme composite wave-suction material of preparation
It is placed in tube furnace after evenly mixing with excessive sublimed sulfur, in Ar or N2It is heated in atmosphere with the heating rate of 1~5 DEG C/min
300~500 DEG C, and 2~4h is kept the temperature, after tube furnace is cooled to room temperature, collect foam-like product, the as iron-based sulphur of magnetic Nano
Compound/three-dimensional grapheme composite wave-suction material.
3. the preparation method of three-dimensional grapheme base composite wave-absorbing material according to claim 2, it is characterised in that the step
Nine water ferric nitrates, other one or more metal salts and polyvinylpyrrolidone mass ratio are (1.5~2.0) in rapid a: (0~
2.0): 1, wherein (0~2.0) is other one or more metal salt quality summation accountings in raw material mass mixture ratio；Other metals
Salt is to contain Fe, Co, Ni, Ba, Mo, Si, Al, Nb, V, Ce, Y, Cu, B, La, Sr, the nitrate or carbonate of Zn metallic element
Or silicate；The K value range of polyvinylpyrrolidone is 13~32.
4. the preparation method of three-dimensional grapheme base composite wave-absorbing material according to claim 2, it is characterised in that the step
Drying temperature in rapid b is 70~80 DEG C.
5. the preparation method of three-dimensional grapheme base composite wave-absorbing material according to claim 2, it is characterised in that the step
Oxidation processes in rapid d are low-temperature oxidation processing or high temperature oxidation process；Wherein low-temperature oxidation treatment temperature is 150~300 DEG C；
High temperature oxidation process temperature is 500~800 DEG C.
6. the preparation method of three-dimensional grapheme base composite wave-absorbing material according to claim 2, it is characterised in that the step
Magnetic Nano ferrous alloy/three-dimensional grapheme or nano-carbide/three-dimensional grapheme composite wave-suction material and sublimed sulfur in rapid e
Mass ratio be 1:(1.0~2.0).
7. three-dimensional grapheme base composite wave-absorbing material according to claim 2, it is characterised in that the step c~e is made
In standby three-dimensional grapheme base composite wave-absorbing material in the chemical formula of magnetic Nano Fe-base compound each element stoichiometric number
It can be regulated and controled by raw material proportioning in step a.
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| CN109936974A (en) * | 2019-04-03 | 2019-06-25 | 厦门大学 | A kind of synthetic method of sandwich structure CoFe@C/ graphene electromagnetic wave absorbent material |
| CN110092420A (en) * | 2019-05-14 | 2019-08-06 | 北京科技大学 | A kind of Fe3O4The preparation method of/porous graphene composite material |
| CN110129108A (en) * | 2019-05-20 | 2019-08-16 | 青岛鑫乐驰润滑油有限公司 | A kind of graphene/CoFe2O4Composite Nano magnetic retention method for preparing lubricant |
| CN110951455A (en) * | 2019-11-27 | 2020-04-03 | 中国电子科技集团公司第三十三研究所 | Preparation method of light heat-insulating wave-absorbing material based on graphene |
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| CN113186481A (en) * | 2021-04-13 | 2021-07-30 | 天津大学 | Preparation method of wave-absorbing stealth composite coating |
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| CN110092420A (en) * | 2019-05-14 | 2019-08-06 | 北京科技大学 | A kind of Fe3O4The preparation method of/porous graphene composite material |
| CN110129108A (en) * | 2019-05-20 | 2019-08-16 | 青岛鑫乐驰润滑油有限公司 | A kind of graphene/CoFe2O4Composite Nano magnetic retention method for preparing lubricant |
| CN110951455B (en) * | 2019-11-27 | 2022-07-12 | 中国电子科技集团公司第三十三研究所 | Preparation method of light heat-insulating wave-absorbing material based on graphene |
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