CN103554908B - A kind of graphene/polyaniline/cobalt composite wave-suction material and preparation method - Google Patents
A kind of graphene/polyaniline/cobalt composite wave-suction material and preparation method Download PDFInfo
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Abstract
A kind of graphene/polyaniline/cobalt composite wave-suction material and preparation method thereof, belongs to electromagnetic wave absorbent material preparation field.This absorbing material is made up of film forming material and radio-radar absorber, and wherein, film forming material adopts paraffin, and radio-radar absorber adopts graphene/polyaniline/cobalt ternary complex, and the mass ratio of graphene/polyaniline/cobalt mixture and paraffin is 1:1.This material preparation process is as follows: (1) prepares graphite oxide; (2) graphene oxide/polyaniline binary complex is prepared; (3) graphene/polyaniline/cobalt ternary complex is prepared; (4) take graphene/polyaniline/cobalt ternary complex and paraffin, after mixing, obtain graphene/polyaniline/cobalt absorbing material.This material has that with low cost, preparation technology is simple, electromagnetic wave absorption ability is strong, absorption band is wide and the feature such as density is little, has good electromagnetic performance and stability, has significant application value in microwave absorbing, electromagnetic shielding field.
Description
Technical field:
The invention belongs to electromagnetic wave absorbent material preparation field, particularly a kind of preparation method with the graphene/polyaniline/cobalt advanced composite material of absorbing property.
Background technology:
Along with the development of modern science and technology and the progress of industrial civilization, the application of various electronic equipment is also increasing, it produces increasing electromagnetic radiation, so electromagnetic interference is more and more serious, has become the major obstacle that can much equipment play a role; Electromagnetic pollution has simultaneously penetrated into the every nook and cranny producing and live, has a strong impact on the healthy of people.Therefore, how effectively to prevent and eliminate the important topic that electromagnetic interference has become global scientific and technological circle.
Absorbing material is required to meet that thickness is thin, density is low, frequency range is wide, absorb the features such as strong.According to wave-absorbing mechanism, absorbing material generally can be divided into dielectric loss type, magnetic loss type.The wave-absorbing mechanism of the material that the electroconductibility such as conduction high polymer, graphite is strong is mainly electrical loss, comprises conduction loss and dielectric loss two portions, and loss is mainly derived from electronic polarization, atomic polarization, the sub-oriented polarization of intrinsic electric dipoles and interfacial polarization etc.; The wave-absorbing mechanism of the magneticsubstances such as ferrite, iron carbonyl, nitrided iron is mainly magnetic loss, and magnetic loss can be divided into eddy-current loss, magnetic hysteresis loss and residual loss etc.Large quantity research shows, the wave absorbing agent of single loss-type is difficult to the requirement meeting absorbing material, reason be due to they can only be single adjustment absorbing material in some influence factor, and specific inductivity and magnetic permeability two decisive parameters can not be adjusted simultaneously.Therefore, the matrix material that exploitation has dielectric loss and a magnetic loss is simultaneously only the most effective way solving absorption of electromagnetic wave.
Disclose one reducing atmosphere in Chinese patent CN101521046A " graphite sheet surface load magnetic alloy particle wave-absorbing material and preparation method thereof " and from composite oxides, restore magnetic ion load on graphite flake, by adjustment alloy compositions, the absorbing property of product can be regulated easily.This matrix material reaches-34.4dB at the reflection loss of 2-18GHz range of frequency, but effective bandwidth is narrower.
At present about more as the report of radio-radar absorber using magnetic metallic powder and conductive polymers, but it is less as the report of absorption agent using Graphene, especially Graphene, polyaniline and the compounded multi-element composite material of metal-powder with magnetic loss characteristic not only can be reduced the density of absorption agent, and can absorption band be widened, improve assimilation effect.Therefore, the present invention by Graphene, polyaniline and cobalt organic composite, prepares the graphene/polyaniline/cobalt advanced composite material having each component advantage concurrently from the angle of composite materials.
Summary of the invention:
The object of the present invention is to provide a kind of preparation method of graphene/polyaniline/cobalt advanced composite material, this material has that with low cost, preparation technology is simple, electromagnetic wave absorption ability is strong, absorption band is wide and the feature such as density is little.
A kind of graphene/polyaniline/cobalt composite wave-suction material, it is characterized in that this absorbing material is made up of film forming material and radio-radar absorber, wherein, film forming material adopts paraffin, radio-radar absorber adopts graphene/polyaniline/cobalt ternary complex, and the mass ratio of graphene/polyaniline/cobalt ternary complex and paraffin is 1:1.
The preparation method of graphene/polyaniline/cobalt absorbing material described above, comprises the steps:
(1) preparation of graphene oxide
Adopt improvement Hummers method to be reacted by natural graphite and prepare graphite oxide, raw material adopts 325 order natural flake graphites and SODIUMNITRATE, 98% vitriol oil, KMn0
4, their mass ratioes are 1:0.4 ~ 0.5:70 ~ 92:5; Add in the vitriol oil by aequum graphite and SODIUMNITRATE, ice bath is cooled to 4 DEG C, slowly adds KMn0
4, stirring reaction 90min; Then 30 DEG C of stirring reaction 30min are warming up to; Slowly add deionized water, then after 90 DEG C of stirring reaction 20min, after being cooled to room temperature, add deionized water and hydrogen peroxide, obtain graphite oxide through the drying of centrifuge washing final vacuum;
Graphite oxide is added the ultrasonic 2h of 150ml deionized water, obtain the suspension of graphene oxide.
(2) preparation of graphite oxide/polyaniline binary composite
In the suspension of graphene oxide, add Phenyl Acetic Acid (Powder） solution, graphene oxide and aniline mass ratio 1:8 ~ 20, constant speed stirs 20min, slowly drips containing ammonium persulphate acid solution, aniline: ammonium persulphate mass ratio 1:1.6; Under condition of ice bath, react 12h, within static 12 hours, discard supernatant liquor, decompress filter is with deionized water wash to neutral, and 45 DEG C of vacuum-dryings, obtain graphene oxide/polyaniline binary complex; Wherein, Phenyl Acetic Acid (Powder） solution, ammonium persulphate acid solution all adopt hydrochloric acid or sulphosalicylic acid solution preparation, and the concentration of aniline of Phenyl Acetic Acid (Powder） solution is 6mg/ml-16mg/ml.
(3) preparation of graphene/polyaniline/cobalt trielement composite material
Taking graphene oxide/polyaniline binary complex is scattered in ethanol and deionized water mixed solution, and in ethanol and deionized water mixed solution, the ratio of ethanol and deionized water is 4:1; Accurately taking cobalt chloride adds in ethanol containing binary complex and deionized water mixed solution, binary complex and cobalt salt mass ratio 1:4 ~ 8, ultrasonic 0.5h, adds ammoniacal liquor and regulates PH to 9, then add the hydrazine hydrate of massfraction 80%, hydrazine hydrate and cobalt chloride mass ratio 25:1, ultrasonic 5min, staticly discards supernatant liquor, decompress filter, washing is dry to neutral final vacuum, obtains graphene/polyaniline/cobalt ternary complex;
(4) with graphene/polyaniline/cobalt ternary complex for radio-radar absorber, by radio-radar absorber: the mass ratio 1:1 of paraffin takes graphene/polyaniline/cobalt ternary complex and paraffin, heating mixes, and after naturally cooling, compressing tablet obtains graphene/polyaniline/cobalt absorbing material.
Graphene in the present invention has the features such as dielectric loss performance is strong, density is little.Binary complex is generated at graphenic surface synthesized polyaniline, then form by liquid phase reduction magnetic property and the magnetic loss size that one deck cobalt metal improves ternary complex on the surface of graphene/polyaniline, thus prepare the wide and efficient novel wave-absorbing material of light weight, absorption band.By the control of p-poly-phenyl amine and cobalt relative content, electromagnetic performance and the absorbing property of product effectively can be regulated and controled.
It is simple to operation when graphene/polyaniline/cobalt absorbing material prepared by the present invention uses, with this material for additive adds in coating, the graphene/polyaniline/cobalt absorbing material adopting coated technique the present invention to be prepared forms uniform suction ripple layer at buildings or component surface, and then microwave absorbing coating can be had at suction ripple layer surface daub on a wall common building coating can be ornamental.Polyaniline in absorption agent and Graphene are dielectric loss type media, have higher electrical loss tangent value, carry out attenuation and absorption incident electromagnetic wave by the electronic polarization of media interior or interfacial polarization; Cobalt in absorption agent belongs to magnetic loss type medium, and have higher magnetic loss tangent value, it carrys out attenuation and absorption incident electromagnetic wave by magnetic hysteresis loss, and therefore this absorbing material has electromagnetic consumable dual-use function simultaneously.
Lower cost for material provided by the invention, preparation technology are simple, density is little, have good electromagnetic performance and stability, thus have larger application prospect in electromagnetic wave shielding, the field such as ripple and stealth material of inhaling.
Accompanying drawing explanation
Fig. 1 is transmission electron microscope (TEM) picture of graphene/polyaniline binary complex
Fig. 2 is transmission electron microscope (TEM) picture of graphene/polyaniline/cobalt ternary complex
Fig. 3 is the electromagnetic wave absorption design sketch of graphene/polyaniline/cobalt ternary complex
Embodiment
Below by embodiment, preparation method of the present invention is described further, but the present invention is not limited to these embodiments.Experimental technique in following example, is ordinary method if no special instructions; Material used in example, if no special instructions, all purchased from conventional chemical Reagent Company.
Embodiment 1
The preparation of A absorbing material
(1) 1g natural flake graphite and 0.5g SODIUMNITRATE are added the 40ml vitriol oil, ice bath is cooled to 4 DEG C, slowly adds 5gKMn0
4, stirring reaction 90min; Then 30 DEG C of reaction 30min are warming up to; Slowly add 50ml deionized water, then after 90 DEG C of stirring reaction 20min, after being cooled to room temperature, add 100ml deionized water and 10ml hydrogen peroxide, obtain graphite oxide through the drying of centrifuge washing final vacuum.
Take 0.11g graphite oxide, add the ultrasonic 2h of 150ml deionized water, obtain the suspension of graphene oxide.The acid solution of 130ml containing 1.12g aniline is added in the suspension of above-mentioned graphene oxide, constant speed stirs 20min, slow dropping 20ml is containing 1.82g ammonium persulphate acid solution, 12h is reacted under condition of ice bath, within static 12 hours, discard supernatant liquor, decompress filter, with deionized water wash to neutral, 45 DEG C of vacuum-dryings, obtain graphene oxide/polyaniline binary complex.
(3) take graphene oxide/polyaniline binary complex prepared by 0.05g aforesaid method to be scattered in 40ml ethanol and 10ml deionized water mixed solution, accurately take 0.2g cobalt chloride (CoCl
26H
2o) add in above-mentioned solution, ultrasonic 0.5h, add ammoniacal liquor and regulate PH to 9, then add 5g hydrazine hydrate, ultrasonic 5min, staticly discard supernatant liquor, decompress filter, washing is dry to neutral final vacuum, obtains graphene/polyaniline/cobalt ternary complex.
The performance test of B absorbing material
With graphene/polyaniline/cobalt ternary complex for radio-radar absorber, by radio-radar absorber: the mass ratio 1:1 of paraffin takes graphene/polyaniline/cobalt ternary complex 0.08g and paraffin 0.08g, heating mixes, after naturally cooling, compressing tablet is prepared into race diameter 7.0mm, inner ring diameter 3.0mm loop sample.Prepared matrix material reaches 3.31GHz at 2 ~ 18GHz internal reflection loss value lower than the frequency span of-10dB, and minimal reflection loss value can reach-30.71dB.
Embodiment 2
The preparation of A absorbing material
(1) 1g natural flake graphite and 0.5g SODIUMNITRATE are added the 40ml vitriol oil, ice bath is cooled to 4 DEG C, slowly adds 5gKMn0
4, stirring reaction 90min; Then 30 DEG C of reaction 30min are warming up to; Slowly add 50ml deionized water, then after 90 DEG C of stirring reaction 20min, after being cooled to room temperature, add 100ml deionized water and 10ml hydrogen peroxide, obtain graphite oxide through the drying of centrifuge washing final vacuum.
Take 0.11g graphite oxide, add the ultrasonic 2h of 150ml deionized water, obtain the suspension of graphene oxide.The acid solution of 130ml containing 1.67g aniline is added in the suspension of above-mentioned graphene oxide, constant speed stirs 20min, slow dropping 20ml is containing 2.71g ammonium persulphate acid solution, 12h is reacted under condition of ice bath, within static 12 hours, discard supernatant liquor, decompress filter, with deionized water wash to neutral, 45 DEG C of vacuum-dryings, obtain graphene oxide/polyaniline binary complex.
(3) take 0.05g graphene oxide/polyaniline binary complex to be scattered in 40ml ethanol and 10ml deionized water mixed solution, accurately take 0.2g cobalt chloride (CoCl
26H
2o) add in above-mentioned solution, ultrasonic 0.5h, add ammoniacal liquor and regulate PH to 9, then add 5g hydrazine hydrate, ultrasonic 5min, staticly discard supernatant liquor, decompress filter, washing is dry to neutral final vacuum, obtains graphene/polyaniline/cobalt ternary complex.
The performance test of B absorbing material
With graphene/polyaniline/cobalt ternary complex for radio-radar absorber, by radio-radar absorber: the mass ratio 1:1 of paraffin takes graphene/polyaniline/cobalt ternary complex 0.08g and paraffin 0.08g, heating mixes, after naturally cooling, compressing tablet is prepared into race diameter 7.0mm, inner ring diameter 3.0mm loop sample.Prepared matrix material reaches 2.38GHz at 2 ~ 18GHz internal reflection loss value lower than the frequency span of-10dB, and minimal reflection loss value can reach-24.5dB.
Example 3
The preparation of A absorbing material
(1) 1g natural flake graphite and 0.5g SODIUMNITRATE are added the 40ml vitriol oil, ice bath is cooled to 4 DEG C, slowly adds 5gKMn0
4, stirring reaction 90min; Then 30 DEG C of reaction 30min are warming up to; Slowly add 50ml deionized water, then after 90 DEG C of stirring reaction 20min, after being cooled to room temperature, add 100ml deionized water and 10ml hydrogen peroxide, obtain graphite oxide through the drying of centrifuge washing final vacuum.
Take 0.11g graphite oxide, add the ultrasonic 2h of 150ml deionized water, obtain the suspension of graphene oxide.The acid solution of 130ml containing 1.12g aniline is added in the suspension of above-mentioned graphene oxide, constant speed stirs 20min, slow dropping 20ml is containing 1.82g ammonium persulphate acid solution, 12h is reacted under condition of ice bath, within static 12 hours, discard supernatant liquor, decompress filter, with deionized water wash to neutral, 45 DEG C of vacuum-dryings, obtain graphene oxide/polyaniline binary complex.
(3) take 0.05g graphene oxide/polyaniline binary complex to be scattered in 40ml ethanol and 10ml deionized water mixed solution, accurately take 0.1g cobalt chloride (CoCl
26H
2o) add in above-mentioned solution, ultrasonic 0.5h, add ammoniacal liquor and regulate PH to 9, then add 2.5g hydrazine hydrate, ultrasonic 5min, staticly discard supernatant liquor, decompress filter, washing is dry to neutral final vacuum, obtains graphene/polyaniline/cobalt ternary complex.
The performance test of B absorbing material
With graphene/polyaniline/cobalt ternary complex for radio-radar absorber, by radio-radar absorber: the mass ratio 1:1 of paraffin takes graphene/polyaniline/cobalt ternary complex 0.08g and paraffin 0.08g, heating mixes, after naturally cooling, compressing tablet is prepared into race diameter 7.0mm, inner ring diameter 3.0mm loop sample.Prepared matrix material reaches 1.19GHz at 2 ~ 18GHz internal reflection loss value lower than the frequency span of-10dB, and minimal reflection loss value can reach-13.83dB.
Claims (1)
1. the preparation method of a graphene/polyaniline/cobalt composite wave-suction material, it is characterized in that this absorbing material is made up of film forming material and radio-radar absorber, wherein, film forming material adopts paraffin, radio-radar absorber adopts graphene/polyaniline/cobalt ternary complex, and the mass ratio of graphene/polyaniline/cobalt ternary complex and paraffin is 1:1;
Concrete preparation process is as follows:
(1) preparation of graphene oxide:
Adopt improvement Hummers method to be reacted by natural graphite and prepare graphite oxide, raw material adopts 325 order natural flake graphites and SODIUMNITRATE, 98% vitriol oil, KMnO
4, their mass ratioes are 1:0.4 ~ 0.5:70 ~ 92:5; Add in the vitriol oil by aequum graphite and SODIUMNITRATE, ice bath is cooled to 4 DEG C, slowly adds KMnO
4, stirring reaction 90min; Then 30 DEG C of stirring reaction 30min are warming up to; Slowly add deionized water, then after 90 DEG C of stirring reaction 20min, after being cooled to room temperature, add deionized water and hydrogen peroxide, obtain graphite oxide through the drying of centrifuge washing final vacuum;
Graphite oxide is added the ultrasonic 2h of 150ml deionized water, obtain the suspension of graphene oxide;
(2) preparation of graphite oxide/polyaniline binary composite:
In the suspension of graphene oxide, add Phenyl Acetic Acid (Powder） solution, graphene oxide and aniline mass ratio 1:8 ~ 20, constant speed stirs 20min, slowly drips containing ammonium persulphate acid solution, aniline: ammonium persulphate mass ratio 1:1.6; Under condition of ice bath, react 12h, within static 12 hours, discard supernatant liquor, decompress filter is with deionized water wash to neutral, and 45 DEG C of vacuum-dryings, obtain graphene oxide/polyaniline binary complex;
(3) preparation of graphene/polyaniline/cobalt trielement composite material:
Taking graphene oxide/polyaniline binary complex is scattered in ethanol and deionized water mixed solution, and in ethanol and deionized water mixed solution, the ratio of ethanol and deionized water is 4:1; Accurately taking cobalt chloride adds in ethanol containing binary complex and deionized water mixed solution, binary complex and cobalt salt mass ratio 1:4 ~ 8, ultrasonic 0.5h, adds ammoniacal liquor and regulates PH to 9, then add the hydrazine hydrate of massfraction 80%, hydrazine hydrate and cobalt chloride mass ratio 25:1, ultrasonic 5min, staticly discards supernatant liquor, decompress filter, washing is dry to neutral final vacuum, obtains graphene/polyaniline/cobalt ternary complex;
(4) with graphene/polyaniline/cobalt ternary complex for radio-radar absorber, by radio-radar absorber: the mass ratio 1:1 of paraffin takes graphene/polyaniline/cobalt ternary complex and paraffin, heating mixes, and after naturally cooling, compressing tablet obtains graphene/polyaniline/cobalt absorbing material;
Wherein in step (2), Phenyl Acetic Acid (Powder） solution, ammonium persulphate acid solution all adopt hydrochloric acid or sulphosalicylic acid solution preparation, and the concentration of aniline of Phenyl Acetic Acid (Powder） solution is 6mg/ml-16mg/ml.
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