CN103012786B - Preparation method of graphene/CoFe2O4/polyaniline composite absorbing material - Google Patents

Preparation method of graphene/CoFe2O4/polyaniline composite absorbing material Download PDF

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CN103012786B
CN103012786B CN201210449807.4A CN201210449807A CN103012786B CN 103012786 B CN103012786 B CN 103012786B CN 201210449807 A CN201210449807 A CN 201210449807A CN 103012786 B CN103012786 B CN 103012786B
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graphene
cofe
preparation
absorbing material
polyaniline compound
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CN103012786A (en
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谢宇
赵杰
凌云
闫思凤
石磊
朱卫多
余远福
刘锦梅
张凯
赖强
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Nanchang Hangkong University
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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

A kind of Graphene/CoFe 2o 4the preparation method of/polyaniline compound wave-absorbing material
Technical background
The invention belongs to electromagnetic wave absorbent material preparation field, particularly a kind of Graphene/CoFe 2o 4the preparation method of/polyaniline compound wave-absorbing material.
Background technology
Ferrite nano powder has excellent magnetics and electric property, and people conduct extensive research its synthesis and characteries in recent years.There is the CoFe of spinel type crystal structure 2o 4be the magneticsubstance of excellent property, there is 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 causes the major reason of the many excellent properties of Graphene.The most outstanding character is that the movement velocity of its electronics reaches 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 the quite similar of theory of relativity neutrino in Graphene.Graphene also has excellent mechanical property, this is because under external force, due to the self-adaptation distortion of atomic plane, C-C key is not easy to disconnect, Graphene crystalline network can keep relative stability, and therefore macroscopically to show as intensity high, not easily produces the phenomenon fractureing, puncture, tear.
Polyaniline is mainly reached by electrical loss electromagnetic absorption, is difficult to obtain satisfied effect, should seek the effective way realizing polyaniline high conductivity or have function solenoid concurrently.Therefore, the present invention from the angle of composite materials by Graphene, CoFe 2o 4, polyaniline organic composite, prepare the Graphene/CoFe having each component advantage concurrently 2o 4/ polyaniline compound wave-absorbing material.
Summary of the invention
The object of this invention is to provide a kind of Graphene/CoFe 2o 4the preparation method of/polyaniline compound wave-absorbing material, Graphene is introduced in matrix material by the method, optimizes CoFe further 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 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 10.0g potassium permanganate is added, stirred at ambient temperature 1h, again at 55 DEG C after supersound process 30min, temperature is adjusted to 70 DEG C and continues supersound process 30min, pours in 1.5L frozen water, add 200mL H after being cooled to room temperature 2o 2, leave standstill after 24h, removing supernatant liquor, throw out is centrifugal, then at 50 DEG C vacuum drying, obtain graphene oxide.Graphene oxide is added a small amount of deionized water, after supersound process 30min, add 300mL ammoniacal liquor, 300mL hydrazine hydrate, under reflux condensation mode condition, after heating in water bath to 95 DEG C reaction 1h, change water distilling apparatus, steam most ammoniacal liquor, residuum centrifugation, 50 DEG C of vacuum-dryings, grinding obtains product Graphene.
(2) CoFe 2o 4preparation: take 4.0g Co (NO respectively 3) 26H 2o, 11.30g Fe (NO 3) 39H 2o is dissolved in deionized water, slowly pours in the solution containing 7.68g citric acid, after magnetic agitation 10min, with ammoniacal liquor regulator solution PH=7, then slowly add the solution being dissolved with 2.0g polyoxyethylene glycol, induction stirring 2h, after aged at room temperature 12h, constantly stir lower 80 DEG C of water-bath 3h, form colloidal sol, continue thermal dehydration and form gel, after self-propagating combustion, grinding, pre-burning 2h at 450 DEG C, at 850 DEG C, calcine 2h again, cooling, grinding obtains CoFe 2o 4.
(3) preparation of Graphene/CoFe2O4/ polyaniline compound wave-absorbing material: by Xg Graphene, YgCoFe2O4, wherein X=0.02 ~ 0.4, Y=0.02 ~ 0.4, add in 20mL1mol/L hydrochloric acid soln, after supersound process 1h, add ZmL aniline monomer, wherein Z=0.50 ~ 0.90, after ice-water bath stirs 10min, continue to stir lower slowly instillation 10mL1mol/L ammonium persulfate solution, continue to stir 3h, suction filtration, filter cake deionized water wash 3 ~ 4 times, vacuum-drying 10h at 60 DEG C, obtains Graphene/CoFe2O4/ polyaniline compound wave-absorbing material.
By Hitachi 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 four point probe conductivity meter to Graphene/CoFe 2o 4the specific conductivity of/polyaniline compound wave-absorbing material measures.With Graphene/CoFe 2o 4/ Polyaniline (X=0.18, Y=0.12, Z=0.70) is example, and mixture specific conductivity is 1.9428S/cm.
Advantage of the present invention: the present invention first with caliber 30 ~ 50nm multi-walled carbon nano-tubes for Graphene prepared by raw material, then 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, finally with Graphene, the CoFe of preparation 2o 4, aniline monomer is raw material, adopts situ aggregation method to prepare Graphene/CoFe 2o 4/ polyaniline composite material.After carbon nanotube is processed into the Graphene that specific conductivity is higher, density is less by the present invention further, then with CoFe 2o 4, aniline monomer in-situ polymerization prepares Graphene/CoFe 2o 4/ polyaniline composite material.This matrix material and CoFe 2o 4/ polyaniline composite material compares the conductivity, the magnetic property that have and more arrive, and wider absorption band has significant application value in the field such as microwave absorbing, electromagnetic shielding.
Embodiment
Below by embodiment, the invention will be further described.
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 temperature 1h, after 55 DEG C of ultrasonic 30min, temperature is adjusted to 70 DEG C and continues ultrasonic 30min, be cooled to room temperature, pour in 1.5L frozen water, add 200mL H 2o 2, leave standstill 24h, removing supernatant liquor, throw out is centrifugal, and 50 DEG C of vacuum dryings, obtain graphene oxide.Graphene oxide is added in a small amount of deionized water, ultrasonic 30min, add 300mL ammoniacal liquor, 300mL hydrazine hydrate, under condensing reflux condition, heating in water bath to 95 DEG C reaction 1h, changes water distilling apparatus, steams most ammoniacal liquor, residuum is centrifugal, 50 DEG C of vacuum-dryings, and grinding obtains product Graphene.
(2) 4.0g Co (NO is taken respectively 3) 26H 2o, 11.30g Fe (NO 3) 39H 2o is dissolved in deionized water, slowly pours in the solution containing 7.68g citric acid, magnetic agitation 10min, with ammoniacal liquor regulator solution PH=7, then slowly add the solution being dissolved with 2.0g polyoxyethylene glycol, induction stirring 2h, aged at room temperature 12h, constantly stirs lower 80 DEG C of water-bath 3h, forms colloidal sol, continue thermal dehydration and form gel, after self-propagating combustion, grinding, pre-burning 2h at 450 DEG C, at 850 DEG C, calcine 2h again, cooling, grinding obtains CoFe 2o 4.
(3) by 0.10g Graphene, 0.40gCoFe 2o 4add in 20mL1mol/L hydrochloric acid soln, supersound process 1h, adds 0.50mL aniline monomer, and ice-water bath stirs 10min, continue to stir lower slowly instillation 10mL1mol/L ammonium persulfate solution, continue to stir 3h, suction filtration, filter cake deionized water wash 3 ~ 4 times, vacuum-drying 10h at 60 DEG C, obtains Graphene/CoFe 2o 4/ polyaniline compound wave-absorbing material (X=0.10, Y=0.40, Z=0.50).Prepared matrix material reaches 16.2GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-39dB.
Embodiment 2
Graphene, CoFe 2o 4preparation method respectively with embodiment 1 step (1), step (2), take 0.20g Graphene, 0.30gCoFe 2o 4, measure 0.50mL aniline monomer, preparation method, with embodiment 1 step (3), obtains Graphene/CoFe 2o 4/ polyaniline compound wave-absorbing material (X=0.20, Y=0.30, Z=0.50).Prepared matrix material reaches 14.5GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-41dB.
Embodiment 3
Graphene, CoFe 2o 4preparation method respectively with embodiment 1 step (1), step (2), take 0.30g Graphene, 0.20gCoFe 2o 4, measure 0.50mL aniline monomer, preparation method, with embodiment 1 step (3), obtains Graphene/CoFe 2o 4/ polyaniline compound wave-absorbing material (X=0.30, Y=0.20, Z=0.50).Prepared matrix material reaches 12.4GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-43dB.
Embodiment 4
Graphene, CoFe 2o 4preparation method respectively with embodiment 1 step (1), step (2), take 0.40g Graphene, 0.10gCoFe 2o 4, measure 0.50mL aniline monomer, preparation method, with embodiment 1 step (3), obtains Graphene/CoFe 2o 4/ polyaniline compound wave-absorbing material (X=0.40, Y=0.10, Z=0.50).Prepared matrix material reaches 10.3GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-45dB.
Embodiment 5
Graphene, CoFe 2o 4preparation method respectively with embodiment 1 step (1), step (2), take 0.06g Graphene, 0.24gCoFe 2o 4, measure 0.70mL aniline monomer, preparation method, with embodiment 1 step (3), obtains Graphene/CoFe 2o 4/ polyaniline compound wave-absorbing material (X=0.06, Y=0.24, Z=0.70).Prepared matrix material reaches 11.5GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-44dB.
Embodiment 6
Graphene, CoFe 2o 4preparation method respectively with embodiment 1 step (1), step (2), take 0.12g Graphene, 0.18gCoFe 2o 4, measure 0.70mL aniline monomer, preparation method, with embodiment 1 step (3), obtains Graphene/CoFe 2o 4/ polyaniline compound wave-absorbing material (X=0.12, Y=0.18, Z=0.70).Prepared matrix material reaches 10.4GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-45dB.
Embodiment 7
Graphene, CoFe 2o 4preparation method respectively with embodiment 1 step (1), step (2), take 0.18g Graphene, 0.12gCoFe 2o 4, measure 0.70mL aniline monomer, preparation method, with embodiment 1 step (3), obtains Graphene/CoFe 2o 4/ polyaniline compound wave-absorbing material (X=0.18, Y=0.12, Z=0.70).Prepared matrix material reaches 9.4GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-46dB.
Embodiment 8
Graphene, CoFe 2o 4preparation method respectively with embodiment 1 step (1), step (2), take 0.24g Graphene, 0.06gCoFe 2o 4, measure 0.70mL aniline monomer, preparation method, with embodiment 1 step (3), obtains Graphene/CoFe 2o 4/ polyaniline compound wave-absorbing material (X=0.24, Y=0.06, Z=0.70).Prepared matrix material reaches 8.3GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-47dB.
Embodiment 9
Graphene, CoFe 2o 4preparation method respectively with embodiment 1 step (1), step (2), take 0.02g Graphene, 0.08gCoFe 2o 4, measure 0.90mL aniline monomer, preparation method, with embodiment 1 step (3), obtains Graphene/CoFe 2o 4/ polyaniline compound wave-absorbing material (X=0.02, Y=0.08, Z=0.90).Prepared matrix material reaches 15.6GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-42dB.
Embodiment 10
Graphene, CoFe 2o 4preparation method respectively with embodiment 1 step (1), step (2), take 0.04g Graphene, 0.06gCoFe 2o 4, measure 0.90mL aniline monomer, preparation method, with embodiment 1 step (3), obtains Graphene/CoFe 2o 4/ polyaniline compound wave-absorbing material (X=0.04, Y=0.06, Z=0.90).Prepared matrix material reaches 14.2GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-44dB.
Embodiment 11
Graphene, CoFe 2o 4preparation method respectively with embodiment 1 step (1), step (2), take 0.06g Graphene, 0.04gCoFe 2o 4, measure 0.90mL aniline monomer, preparation method, with embodiment 1 step (3), obtains Graphene/CoFe 2o 4/ polyaniline compound wave-absorbing material (X=0.06, Y=0.04, Z=0.90).Prepared matrix material reaches 12.3GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-46dB.
Embodiment 12
Graphene, CoFe 2o 4preparation method respectively with embodiment 1 step (1), step (2), take 0.08g Graphene, 0.02gCoFe 2o 4, measure 0.90mL aniline monomer, preparation method, with embodiment 1 step (3), obtains Graphene/CoFe 2o 4/ polyaniline compound wave-absorbing material (X=0.08, Y=0.02, Z=0.90).Prepared matrix material reaches 11.4GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-48dB.

Claims (3)

1. Graphene/CoFe 2o 4the preparation method of/polyaniline compound wave-absorbing material, is characterized in that 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 10.0g potassium permanganate is added, stirred at ambient temperature 1h, again at 55 DEG C after supersound process 30min, temperature is adjusted to 70 DEG C and continues supersound process 30min, pours in 1.5L frozen water, add 200mL H after being cooled to room temperature 2o 2, leave standstill after 24h, removing supernatant liquor, throw out is centrifugal, then at 50 DEG C vacuum drying, obtain graphene oxide; Graphene oxide is added a small amount of deionized water, after supersound process 30min, add 300mL ammoniacal liquor, 300mL hydrazine hydrate, under reflux condensation mode condition, after heating in water bath to 95 DEG C reaction 1h, change water distilling apparatus, steam most ammoniacal liquor, residuum centrifugation, 50 DEG C of vacuum-dryings, grinding obtains product Graphene;
(2) CoFe 2o 4preparation: take 4.0g Co (NO respectively 3) 26H 2o, 11.30g Fe (NO 3) 39H 2o is dissolved in deionized water, slowly pours in the solution containing 7.68g citric acid, after magnetic agitation 10min, with ammoniacal liquor regulator solution PH=7, then slowly add the solution being dissolved with 2.0g polyoxyethylene glycol, induction stirring 2h, after aged at room temperature 12h, constantly stir lower 80 DEG C of water-bath 3h, form colloidal sol, continue thermal dehydration and form gel, after self-propagating combustion, grinding, pre-burning 2h at 450 DEG C, at 850 DEG C, calcine 2h again, cooling, grinding obtains CoFe 2o 4;
(3) Graphene/CoFe 2o 4the preparation of/polyaniline compound wave-absorbing material: by Xg Graphene, YgCoFe 2o 4, wherein X=0.02 ~ 0.4, Y=0.02 ~ 0.4, adds in 20mL 1mol/L hydrochloric acid soln, after supersound process 1h, add ZmL aniline monomer, wherein Z=0.50 ~ 0.90, after ice-water bath stirs 10min, continue to stir lower slowly instillation 10mL1mol/L ammonium persulfate solution, continue to stir 3h, suction filtration, filter cake deionized water wash 3 ~ 4 times, vacuum-drying 10h at 60 DEG C, obtains Graphene/CoFe2O4/ 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: in this composite wave-suction material, aniline proportion is 50% ~ 90%, Graphene and CoFe 2o 4summation proportion 10% ~ 50%, and Graphene and CoFe 2o 4be that 1:4,2:3,3:2,4:1 distribute respectively with mass ratio.
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 reaches 8.3 ~ 16.2GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-39 ~-48dB.
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