CN103012786A - Preparation method of graphene/CoFe2O4/polyaniline composite absorbing material - Google Patents
Preparation method of graphene/CoFe2O4/polyaniline composite absorbing material Download PDFInfo
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- CN103012786A CN103012786A CN2012104498074A CN201210449807A CN103012786A CN 103012786 A CN103012786 A CN 103012786A CN 2012104498074 A CN2012104498074 A CN 2012104498074A CN 201210449807 A CN201210449807 A CN 201210449807A CN 103012786 A CN103012786 A CN 103012786A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 38
- 239000011358 absorbing material Substances 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 13
- 229910002518 CoFe2O4 Inorganic materials 0.000 title abstract 5
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000178 monomer Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 12
- 230000005291 magnetic effect Effects 0.000 claims abstract description 6
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 5
- 229910003321 CoFe Inorganic materials 0.000 claims description 57
- 150000001875 compounds Chemical class 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000005303 weighing Methods 0.000 claims description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000002485 combustion reaction Methods 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 239000012065 filter cake Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 3
- -1 polyoxyethylene Polymers 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 229910000608 Fe(NO3)3.9H2O Inorganic materials 0.000 abstract 1
- 238000009767 auto-combustion synthesis reaction Methods 0.000 abstract 1
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 description 14
- QENGPZGAWFQWCZ-UHFFFAOYSA-N 3-Methylthiophene Chemical compound CC=1C=CSC=1 QENGPZGAWFQWCZ-UHFFFAOYSA-N 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000002041 carbon nanotube Substances 0.000 description 5
- 229910021393 carbon nanotube Inorganic materials 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000005415 magnetization Effects 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention provides a preparation method of a graphene/CoFe2O4/polyaniline composite absorbing material. The preparation method comprises the following steps in sequence: preparing the graphene by adopting multi-walled carbon nanotubes with diameter of 30 to 50 nanometers as the raw materials; preparing the CoFe2O4 through a sol-gel auto-combustion method by adopting the Co(NO3)2.6H2O and Fe(NO3)3.9H2O as the raw materials; and then preparing the graphene/CoFe2O4/polyaniline composite absorbing material through an in-situ polymerization method by adopting the prepared graphene, CoFe2O4 and aniline monomer as the raw materials. The composite material is higher in conductivity, magnetic performance and stability, and brings important applications in the microwave absorbing field and the electromagnetic shielding field.
Description
Technical background
The invention belongs to the electromagnetic wave absorbent material preparation field, particularly a kind of Graphene/CoFe
2O
4The preparation method of/polyaniline compound wave-absorbing material.
Background technology
The ferrite nano powder has excellent magnetics and electric property, and people syntheticly conduct extensive research with performance it in recent years.CoFe with spinel type crystal structure
2O
4Be the magneticsubstance of excellent property, have gentle Saturation field, larger coercive force and become extremely competitive magneto-optic recording material of new generation.
The crystalline network of Graphene is very stable, and the stability of this crystalline network is to cause the major reason of the many excellent properties of Graphene.The most outstanding character is that the movement velocity of its electronics has reached 15000cm/Vs, is equivalent to 1/300 of the light velocity, considerably beyond the movement velocity of electronics in general conductor.The character of electronics and theory of relativity neutrino is quite similar in the Graphene.Graphene also has excellent mechanical property, and this is because under external force, because the distortion of the self-adaptation of atomic plane, the C-C key is not easy to disconnect, the Graphene crystalline network can keep relative stability, and therefore shows as intensity in macroscopic view high, the phenomenon that difficult generation fractures, punctures, tears.
Polyaniline mainly reaches by electrical loss electromagnetic absorption, is difficult to obtain satisfied effect, the effective way that should seek to realize the polyaniline high conductivity or have function solenoid concurrently.Therefore, the present invention from the angle of composite materials with Graphene, CoFe
2O
4, the polyaniline organic composite, prepare the Graphene/CoFe that has each component advantage concurrently
2O
4/ polyaniline compound wave-absorbing material.
Summary of the invention
The purpose of this invention is to provide a kind of Graphene/CoFe
2O
4The preparation method of/polyaniline compound wave-absorbing material, the method is introduced Graphene in the matrix material, has further optimized CoFe
2O
4The absorbing property of/polyaniline compound wave-absorbing material, absorption band is wider, and absorption intensity is larger, and density is less.
The present invention is achieved like this, and its preparation method is:
1, a kind of Graphene/CoFe
2O
4The preparation method of/polyaniline compound wave-absorbing material is characterized in that the preparation method is as follows:
(1) preparation of Graphene: 6.0g caliber 30～50nm multi-walled carbon nano-tubes is added in the 400mL vitriol oil, leave standstill 24h, then add 10.0g potassium permanganate, stir 1h under the room temperature, again behind 55 ℃ of lower supersound process 30min, temperature transfers to 70 ℃ and continues supersound process 30min, pours in the 1.5L frozen water after being cooled to room temperature, adds 200mL H
2O
2, leave standstill 24h after, remove supernatant liquor, throw out is centrifugal, at 50 ℃ of lower vacuum dryings, gets graphene oxide again.Graphene oxide is added a small amount of deionized water, behind the supersound process 30min, add 300mL ammoniacal liquor, 300mL hydrazine hydrate, under the reflux condensation mode condition, behind heating in water bath to the 95 ℃ reaction 1h, change water distilling apparatus, steam most ammoniacal liquor, the residuum centrifugation, 50 ℃ of vacuum-dryings are ground and are obtained the product Graphene.
(2) CoFe
2O
4Preparation: take by weighing respectively 4.0g Co (NO
3)
26H
2O, 11.30g Fe (NO
3)
39H
2O is dissolved in the deionized water, slowly pours in the solution that contains the 7.68g citric acid, behind the magnetic agitation 10min, with ammoniacal liquor regulator solution PH=7, then slowly add the solution that is dissolved with the 2.0g polyoxyethylene glycol, induction stirring 2h, behind the aging 12h, constantly stir lower 80 ℃ of water-bath 3h under the room temperature, form colloidal sol, continue thermal dehydration and form gel, behind the self-propagating combustion, grind, at 450 ℃ of lower pre-burning 2h, at 850 ℃ of lower calcining 2h, cooling is ground and is obtained CoFe again
2O
4
(3) Graphene/CoFe
2O
4The preparation of/polyaniline compound wave-absorbing material: with Xg(X=0.02～0.4) Graphene, Yg(Y=0.02～0.4) CoFe
2O
4Add in the 20mL 1mol/L hydrochloric acid soln, behind the supersound process 1h, add ZmL(Z=0.50～0.90) aniline monomer, after ice-water bath stirs 10min, continue to stir the lower 10mL 1mol/L ammonium persulfate solution that slowly splashes into, continue to stir 3h, suction filtration, filter cake deionized water wash 3～4 times, 60 ℃ of lower vacuum-drying 10h obtain Graphene/CoFe
2O
4/ polyaniline compound wave-absorbing material.
With Hitachi's HITACHI/SU1510 scanning electronic microscope to Graphene/CoFe
2O
4Particle form and the size of/polyaniline compound wave-absorbing material are observed.With Graphene/CoFe
2O
4/ Polyaniline (X=0.04, Y=0.06, Z=0.90) is example, and mixture is stacked in multi-layers in the form of sheets, and lamella length is about 700nm, and width is about 400nm.
With the four point probe conductivity meter to Graphene/CoFe
2O
4The specific conductivity of/polyaniline compound wave-absorbing material is measured.With Graphene/CoFe
2O
4/ Polyaniline (X=0.18, Y=0.12, Z=0.70) is example, and the mixture specific conductivity is 1.9428S/cm.
With vibrating sample magnetometer (VSM) barium ferrite/carbon nano-tube/poly 3 methyl thiophene composite wave-suction material is carried out magnetism testing.Be example with barium ferrite/carbon nano-tube/poly 3 methyl thiophene mixture (X=0.18, Y=0.12, Z=0.70), test result is: coercive force is 3456.82Oe, and saturation magnetization is 72.95emug
-1, residual magnetization is 69.09emug
-1
Adopt Agilent 8722ES vector network analyzer test barium ferrite/carbon nano-tube/poly 3 methyl thiophene composite wave-suction material at the reflectivity of 2 ~ 18GHz.Be example with barium ferrite/carbon nano-tube/poly 3 methyl thiophene mixture (X=0.18, Y=0.12, Z=0.70), test result is: maximum absorption band appears in the 7.2GHz place, and peak value is-46dB, and reflectivity loss value is lower than-the wide 9.4GHz of reaching of absorption band of 10dB.
Advantage of the present invention: the present invention prepares Graphene take caliber 30～50nm multi-walled carbon nano-tubes as raw material first, again with Co (NO
3)
26H
2O, Fe (NO
3)
39H
2O is that raw material adopts sol-gel auto-combustion to prepare CoFe
2O
4, last Graphene, CoFe with preparation
2O
4, aniline monomer is raw material, adopts situ aggregation method to prepare Graphene/CoFe
2O
4/ polyaniline composite material.After the present invention further is processed into the Graphene that specific conductivity is higher, density is less with carbon nanotube, again with CoFe
2O
4, the aniline monomer in-situ polymerization prepares Graphene/CoFe
2O
4/ polyaniline composite material.This matrix material and CoFe
2O
4/ polyaniline composite material is compared has conductivity, the magnetic property that more arrives, and wider absorption band has significant application value in fields such as microwave absorbing, electromagnetic shieldings.
Embodiment
The invention will be further described below by embodiment.
Embodiment 1
(1) 6.0g caliber 30～50nm multi-walled carbon nano-tubes is added in the 400mL vitriol oil, leave standstill 24h, then add 10.0g potassium permanganate, stirring at room 1h, behind 55 ℃ of ultrasonic 30min, temperature transfers to 70 ℃ and continues ultrasonic 30min, be cooled to room temperature, pour in the 1.5L frozen water, add 200mL H
2O
2, leave standstill 24h, remove supernatant liquor, throw out is centrifugal, and 50 ℃ of vacuum dryings get graphene oxide.Graphene oxide is added in a small amount of deionized water, and ultrasonic 30min adds 300mL ammoniacal liquor, 300mL hydrazine hydrate, under the condensing reflux condition, heating in water bath to 95 ℃ reaction 1h changes water distilling apparatus, steams most ammoniacal liquor, residuum is centrifugal, and 50 ℃ of vacuum-dryings are ground and obtained the product Graphene.
(2) take by weighing respectively 4.0g Co (NO
3)
26H
2O, 11.30g Fe (NO
3)
39H
2O is dissolved in the deionized water, slowly pours in the solution that contains the 7.68g citric acid magnetic agitation 10min into, with ammoniacal liquor regulator solution PH=7, then slowly add the solution that is dissolved with the 2.0g polyoxyethylene glycol, induction stirring 2h, aging 12h constantly stirs lower 80 ℃ of water-bath 3h under the room temperature, forms colloidal sol, continue thermal dehydration and form gel, behind the self-propagating combustion, grind, 450 ℃ of lower pre-burning 2h, at 850 ℃ of lower calcining 2h, cooling is ground and is obtained CoFe again
2O
4
(3) with 0.10g Graphene, 0.40gCoFe
2O
4Add in the 20mL 1mol/L hydrochloric acid soln, supersound process 1h adds the 0.50mL aniline monomer, and ice-water bath stirs 10min, continue to stir the lower 10mL 1mol/L ammonium persulfate solution that slowly splashes into, continue to stir 3h, suction filtration, filter cake deionized water wash 3～4 times, 60 ℃ of lower vacuum-drying 10h obtain Graphene/CoFe
2O
4/ polyaniline compound wave-absorbing material (X=0.10, Y=0.40, Z=0.50).Prepared matrix material is lower than in 2～18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 16.2GHz, and minimum reflectance loss value can reach-39dB.
Embodiment 2
Graphene, CoFe
2O
4The preparation method respectively with embodiment 1 step (1), step (2), take by weighing 0.20g Graphene, 0.30gCoFe
2O
4, measuring the 0.50mL aniline monomer, the preparation method obtains Graphene/CoFe with embodiment 1 step (3)
2O
4/ polyaniline compound wave-absorbing material (X=0.20, Y=0.30, Z=0.50).Prepared matrix material is lower than in 2 ~ 18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 14.5GHz, and minimum reflectance loss value can reach-41dB.
Embodiment 3
Graphene, CoFe
2O
4The preparation method respectively with embodiment 1 step (1), step (2), take by weighing 0.30g Graphene, 0.20gCoFe
2O
4, measuring the 0.50mL aniline monomer, the preparation method obtains Graphene/CoFe with embodiment 1 step (3)
2O
4/ polyaniline compound wave-absorbing material (X=0.30, Y=0.20, Z=0.50).Prepared matrix material is lower than in 2 ~ 18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 12.4GHz, and minimum reflectance loss value can reach-43dB.
Embodiment 4
Graphene, CoFe
2O
4The preparation method respectively with embodiment 1 step (1), step (2), take by weighing 0.40g Graphene, 0.10gCoFe
2O
4, measuring the 0.50mL aniline monomer, the preparation method obtains Graphene/CoFe with embodiment 1 step (3)
2O
4/ polyaniline compound wave-absorbing material (X=0.40, Y=0.10, Z=0.50).Prepared matrix material is lower than in 2～18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 10.3GHz, and minimum reflectance loss value can reach-45dB.
Embodiment 5
Graphene, CoFe
2O
4The preparation method respectively with embodiment 1 step (1), step (2), take by weighing 0.06g Graphene, 0.24gCoFe
2O
4, measuring the 0.70mL aniline monomer, the preparation method obtains Graphene/CoFe with embodiment 1 step (3)
2O
4/ polyaniline compound wave-absorbing material (X=0.06, Y=0.24, Z=0.70).Prepared matrix material is lower than in 2～18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 11.5GHz, and minimum reflectance loss value can reach-44dB.
Embodiment 6
Graphene, CoFe
2O
4The preparation method respectively with embodiment 1 step (1), step (2), take by weighing 0.12g Graphene, 0.18gCoFe
2O
4, measuring the 0.70mL aniline monomer, the preparation method obtains Graphene/CoFe with embodiment 1 step (3)
2O
4/ polyaniline compound wave-absorbing material (X=0.12, Y=0.18, Z=0.70).Prepared matrix material is lower than in 2～18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 10.4GHz, and minimum reflectance loss value can reach-45dB.
Embodiment 7
Graphene, CoFe
2O
4The preparation method respectively with embodiment 1 step (1), step (2), take by weighing 0.18g Graphene, 0.12gCoFe
2O
4, measuring the 0.70mL aniline monomer, the preparation method obtains Graphene/CoFe with embodiment 1 step (3)
2O
4/ polyaniline compound wave-absorbing material (X=0.18, Y=0.12, Z=0.70).Prepared matrix material is lower than in 2～18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 9.4GHz, and minimum reflectance loss value can reach-46dB.
Embodiment 8
Graphene, CoFe
2O
4The preparation method respectively with embodiment 1 step (1), step (2), take by weighing 0.24g Graphene, 0.06gCoFe
2O
4, measuring the 0.70mL aniline monomer, the preparation method obtains Graphene/CoFe with embodiment 1 step (3)
2O
4/ polyaniline compound wave-absorbing material (X=0.24, Y=0.06, Z=0.70).Prepared matrix material is lower than in 2～18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 8.3GHz, and minimum reflectance loss value can reach-47dB.
Embodiment 9
Graphene, CoFe
2O
4The preparation method respectively with embodiment 1 step (1), step (2), take by weighing 0.02g Graphene, 0.08gCoFe
2O
4, measuring the 0.90mL aniline monomer, the preparation method obtains Graphene/CoFe with embodiment 1 step (3)
2O
4/ polyaniline compound wave-absorbing material (X=0.02, Y=0.08, Z=0.90).Prepared matrix material is lower than in 2 ~ 18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 15.6GHz, and minimum reflectance loss value can reach-42dB.
Embodiment 10
Graphene, CoFe
2O
4The preparation method respectively with embodiment 1 step (1), step (2), take by weighing 0.04g Graphene, 0.06gCoFe
2O
4, measuring the 0.90mL aniline monomer, the preparation method obtains Graphene/CoFe with embodiment 1 step (3)
2O
4/ polyaniline compound wave-absorbing material (X=0.04, Y=0.06, Z=0.90).Prepared matrix material is lower than in 2 ~ 18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 14.2GHz, and minimum reflectance loss value can reach-44dB.
Embodiment 11
Graphene, CoFe
2O
4The preparation method respectively with embodiment 1 step (1), step (2), take by weighing 0.06g Graphene, 0.04gCoFe
2O
4, measuring the 0.90mL aniline monomer, the preparation method obtains Graphene/CoFe with embodiment 1 step (3)
2O
4/ polyaniline compound wave-absorbing material (X=0.06, Y=0.04, Z=0.90).Prepared matrix material is lower than in 2～18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 12.3GHz, and minimum reflectance loss value can reach-46dB.
Embodiment 12
Graphene, CoFe
2O
4The preparation method respectively with embodiment 1 step (1), step (2), take by weighing 0.08g Graphene, 0.02gCoFe
2O
4, measuring the 0.90mL aniline monomer, the preparation method obtains Graphene/CoFe with embodiment 1 step (3)
2O
4/ polyaniline compound wave-absorbing material (X=0.08, Y=0.02, Z=0.90).Prepared matrix material is lower than in 2～18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 11.4GHz, and minimum reflectance loss value can reach-48dB.
Claims (3)
1. Graphene/CoFe
2O
4The preparation method of/polyaniline compound wave-absorbing material is characterized in that the preparation method is as follows:
(1) preparation of Graphene: 6.0g caliber 30～50nm multi-walled carbon nano-tubes is added in the 400mL vitriol oil, leave standstill 24h, then add 10.0g potassium permanganate, stir 1h under the room temperature, again behind 55 ℃ of lower supersound process 30min, temperature transfers to 70 ℃ and continues supersound process 30min, pours in the 1.5L frozen water after being cooled to room temperature, adds 200mL H
2O
2, leave standstill 24h after, remove supernatant liquor, throw out is centrifugal, at 50 ℃ of lower vacuum dryings, gets graphene oxide again;
Graphene oxide is added a small amount of deionized water, behind the supersound process 30min, add 300mL ammoniacal liquor, 300mL hydrazine hydrate, under the reflux condensation mode condition, behind heating in water bath to the 95 ℃ reaction 1h, change water distilling apparatus, steam most ammoniacal liquor, the residuum centrifugation, 50 ℃ of vacuum-dryings are ground and are obtained the product Graphene;
(2) CoFe
2O
4Preparation: take by weighing respectively 4.0g Co (NO
3)
26H
2O, 11.30g Fe (NO
3)
39H
2O is dissolved in the deionized water, slowly pours in the solution that contains the 7.68g citric acid, behind the magnetic agitation 10min, with ammoniacal liquor regulator solution PH=7, then slowly add the solution that is dissolved with the 2.0g polyoxyethylene glycol, induction stirring 2h, behind the aging 12h, constantly stir lower 80 ℃ of water-bath 3h under the room temperature, form colloidal sol, continue thermal dehydration and form gel, behind the self-propagating combustion, grind, at 450 ℃ of lower pre-burning 2h, at 850 ℃ of lower calcining 2h, cooling is ground and is obtained CoFe again
2O
4
(3) Graphene/CoFe
2O
4The preparation of/polyaniline compound wave-absorbing material: with Xg(X=0.02～0.4) Graphene, Yg(Y=0.02～0.4) CoFe
2O
4Add in the 20mL 1mol/L hydrochloric acid soln, behind the supersound process 1h, add ZmL(Z=0.50～0.90) aniline monomer, after ice-water bath stirs 10min, continue to stir the lower 10mL 1mol/L ammonium persulfate solution that slowly splashes into, continue to stir 3h, suction filtration, filter cake deionized water wash 3～4 times, 60 ℃ of lower vacuum-drying 10h obtain Graphene/CoFe
2O
4/ polyaniline compound wave-absorbing material.
2. a kind of Graphene/CoFe according to claim 1
2O
4The preparation method of/polyaniline compound wave-absorbing material is characterized in that: the aniline proportion is 50%～90% in this composite wave-suction material, Graphene and CoFe
2O
4Summation proportion 10%～50%, and Graphene and CoFe
2O
4Respectively take mass ratio as 1:4,2:3,3:2,4:1 distribute.
3. a kind of Graphene/CoFe according to claim 1
2O
4The preparation method of/polyaniline compound wave-absorbing material is characterized in that: this composite wave-suction material is lower than in 2～18GHz internal reflection rate loss value-frequency span of 10dB reaches 8.3～16.2GHz, and minimum reflectance loss value can reach-39～-48dB.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210449807.4A CN103012786B (en) | 2012-11-12 | 2012-11-12 | Preparation method of graphene/CoFe2O4/polyaniline composite absorbing material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210449807.4A CN103012786B (en) | 2012-11-12 | 2012-11-12 | Preparation method of graphene/CoFe2O4/polyaniline composite absorbing material |
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