CN103554908A - Graphene/polyaniline/cobalt composite wave-absorbing material and preparation method - Google Patents
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Abstract
The invention relates to a graphene/polyaniline/cobalt composite wave-absorbing material and a preparation method thereof, belonging to the field of preparing an electromagnetic wave absorption material. The wave-absorbing material comprise a film forming material and an electromagnetic wave absorbent, wherein paraffin is adopted as the film forming material, a graphene/polyaniline/cobalt ternary complex is adopted as the electromagnetic wave absorbent, and the mass ratio of the graphene/polyaniline/cobalt ternary complex to the paraffin is 1:1. The preparation method of the material comprises the following steps: (1) preparing graphite oxide; (2) preparing the graphene/polyaniline binary complex; (3) preparing the graphene/polyaniline/cobalt ternary complex; (4) weighing graphene/polyaniline/cobalt ternary complex and paraffin, and evenly mixing to obtain a graphene/polyaniline/cobalt wave-absorbing material. The material has the characteristics of being low in cost, simple in preparation technology, strong in electromagnetic wave absorption capability, wide in absorption frequency band, small in density and the like, achieves good electromagnetic property and stability, and has important application values in the fields of microwave absorption and electromagnetic shielding.
Description
Technical field:
The invention belongs to electromagnetic wave absorbent material preparation field, particularly a kind of preparation method with 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 equipments 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 been penetrated into the every nook and cranny that produces and live, has a strong impact on the healthy of people.Therefore, how effectively prevent and avoid electromagnetic interference has become the important topic of global scientific and technological circle.
Absorbing material is required to meet thin thickness, 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 electrical 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 meet the requirement of absorbing material, reason be due to they can only be single adjusting absorbing material in some influence factor, and can not adjust specific inductivity and two decisive parameters of magnetic permeability simultaneously.Therefore the matrix material that, exploitation has dielectric loss and a magnetic loss is simultaneously only the effective way that solves absorption of electromagnetic wave.
In Chinese patent CN101521046A " graphite sheet surface load magnetic alloy particle wave-absorbing material and preparation method thereof ", disclosing a kind of magnetic ion that restores from composite oxides with reducing atmosphere loads on graphite flake, by adjusting alloy compositions, can regulate easily the absorbing property of product.This matrix material is at reach-34.4dB of the reflection loss of 2-18GHz range of frequency, but effective bandwidth is narrower.
At present more as the report of radio-radar absorber about usining magnetic metallic powder and conductive polymers, but the Graphene of usining is less as the report of absorption agent, especially Graphene, polyaniline and the compounded multi-element composite material of metal-powder with magnetic loss characteristic not only can be reduced to the density of absorption agent, and can widen absorption band, improve assimilation effect.Therefore, the present invention by Graphene, polyaniline and cobalt organic composite, prepares the graphene/polyaniline/cobalt advanced composite material that has 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, the feature such as that this material has is with low cost, preparation technology simple, electromagnetic wave absorption ability is strong, absorption band is wide and density is little.
A kind of graphene/polyaniline/cobalt composite wave-suction material, it is characterized in that this absorbing material is comprised 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, comprises the steps: as mentioned above
(1) preparation of graphene oxide
Adopt to improve Hummers method and prepare graphite oxide by natural graphite reaction, 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; Aequum graphite and SODIUMNITRATE are added in the vitriol oil, and ice bath is cooled to 4 ℃, slowly adds KMn0
4, stirring reaction 90min; Then be warming up to 30 ℃ of stirring reaction 30min; Slowly add deionized water, then after 90 ℃ of stirring reaction 20min, add deionized water and hydrogen peroxide after being cooled to room temperature, through the dry graphite oxide that obtains of centrifuge washing final vacuum;
Graphite oxide is added to the ultrasonic 2h of 150ml deionized water, obtain the suspension of graphene oxide.
(2) preparation of graphite oxide/polyaniline binary matrix material
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 ℃ 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
Take graphene oxide/polyaniline binary complex and be scattered in ethanol and deionized water mixed solution, in ethanol and deionized water mixed solution, the ratio of ethanol and deionized water is 4:1; Accurately taking cobalt chloride adds in the ethanol and deionized water mixed solution that contains binary complex, binary complex and cobalt salt mass ratio 1:4～8, ultrasonic 0.5h, adds ammoniacal liquor to regulate PH to 9, then adds the hydrazine hydrate of massfraction 80%, hydrazine hydrate and cobalt chloride mass ratio 25:1, ultrasonic 5min, the static supernatant liquor that discards, decompress filter, washing is dry to neutral final vacuum, obtains graphene/polyaniline/cobalt ternary complex;
(4) take graphene/polyaniline/cobalt ternary complex is 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.On Graphene surface, synthesized polyaniline generates binary complex, then on the surface of graphene/polyaniline, by liquid phase reduction, form magnetic property and the magnetic loss size that one deck cobalt metal improves ternary complex, thereby prepare light weight, absorption band is wide and efficient novel wave-absorbing material.By the control of p-poly-phenyl amine and cobalt relative content, can effectively regulate and control electromagnetic performance and the absorbing property of product.
It is simple to operation when graphene/polyaniline/cobalt absorbing material prepared by the present invention is used, take this material adds in coating as additive, graphene/polyaniline/cobalt the absorbing material that adopts coated technique prepared by the present invention forms uniform suction ripple layer at buildings or component surface, and then can microwave absorbing coating 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, and electronic polarization or interfacial polarization by medium inside carry out attenuation and absorption incident electromagnetic wave; Cobalt in absorption agent belongs to magnetic loss type medium, has higher magnetic loss tangent value, and it carrys out attenuation and absorption incident electromagnetic wave by magnetic hysteresis loss, so this absorbing material has electromagnetic consumable dual-use function simultaneously.
Lower cost for material provided by the invention, preparation technology is simple, density is little, have good electromagnetic performance and stability, thereby has larger application prospect in electromagnetic wave shielding, the fields 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 embodiment.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 to the 40ml vitriol oil, ice bath is cooled to 4 ℃, slowly adds 5gKMn0
4, stirring reaction 90min; Then be warming up to 30 ℃ of reaction 30min; Slowly add 50ml deionized water, then after 90 ℃ of stirring reaction 20min, add 100ml deionized water and 10ml hydrogen peroxide after being cooled to room temperature, through the dry graphite oxide that obtains of centrifuge washing final vacuum.
Take 0.11g graphite oxide, add the ultrasonic 2h of 150ml deionized water, obtain the suspension of graphene oxide.In the suspension of above-mentioned graphene oxide, add 130ml to contain the acid solution of 1.12g aniline, constant speed stirs 20min, slowly drip 20ml containing 1.82g ammonium persulphate acid solution, under condition of ice bath, react 12h, within static 12 hours, discard supernatant liquor, decompress filter, extremely neutral with deionized water wash, 45 ℃ of vacuum-dryings, obtain graphene oxide/polyaniline binary complex.
(3) take graphene oxide/polyaniline binary complex prepared by 0.05g aforesaid method and 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, adds ammoniacal liquor to regulate PH to 9, then adds 5g hydrazine hydrate, ultrasonic 5min, and the static supernatant liquor that discards, decompress filter, washing is dry to neutral final vacuum, obtains graphene/polyaniline/cobalt ternary complex.
The performance test of B absorbing material
Graphene/polyaniline/cobalt ternary complex of take is 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 annular sample.Prepared matrix material reaches 3.31GHz, can reach-30.71dB of minimal reflection loss value at 2～18GHz internal reflection loss value lower than the frequency span of-10dB.
The preparation of A absorbing material
(1) 1g natural flake graphite and 0.5g SODIUMNITRATE are added to the 40ml vitriol oil, ice bath is cooled to 4 ℃, slowly adds 5gKMn0
4, stirring reaction 90min; Then be warming up to 30 ℃ of reaction 30min; Slowly add 50ml deionized water, then after 90 ℃ of stirring reaction 20min, add 100ml deionized water and 10ml hydrogen peroxide after being cooled to room temperature, through the dry graphite oxide that obtains of centrifuge washing final vacuum.
Take 0.11g graphite oxide, add the ultrasonic 2h of 150ml deionized water, obtain the suspension of graphene oxide.In the suspension of above-mentioned graphene oxide, add 130ml to contain the acid solution of 1.67g aniline, constant speed stirs 20min, slowly drip 20ml containing 2.71g ammonium persulphate acid solution, under condition of ice bath, react 12h, within static 12 hours, discard supernatant liquor, decompress filter, extremely neutral with deionized water wash, 45 ℃ of vacuum-dryings, obtain graphene oxide/polyaniline binary complex.
(3) take 0.05g graphene oxide/polyaniline binary complex and 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, adds ammoniacal liquor to regulate PH to 9, then adds 5g hydrazine hydrate, ultrasonic 5min, and the static supernatant liquor that discards, decompress filter, washing is dry to neutral final vacuum, obtains graphene/polyaniline/cobalt ternary complex.
The performance test of B absorbing material
Graphene/polyaniline/cobalt ternary complex of take is 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 annular sample.Prepared matrix material reaches 2.38GHz, can reach-24.5dB of minimal reflection loss value at 2～18GHz internal reflection loss value lower than the frequency span of-10dB.
Example 3
The preparation of A absorbing material
(1) 1g natural flake graphite and 0.5g SODIUMNITRATE are added to the 40ml vitriol oil, ice bath is cooled to 4 ℃, slowly adds 5gKMn0
4, stirring reaction 90min; Then be warming up to 30 ℃ of reaction 30min; Slowly add 50ml deionized water, then after 90 ℃ of stirring reaction 20min, add 100ml deionized water and 10ml hydrogen peroxide after being cooled to room temperature, through the dry graphite oxide that obtains of centrifuge washing final vacuum.
Take 0.11g graphite oxide, add the ultrasonic 2h of 150ml deionized water, obtain the suspension of graphene oxide.In the suspension of above-mentioned graphene oxide, add 130ml to contain the acid solution of 1.12g aniline, constant speed stirs 20min, slowly drip 20ml containing 1.82g ammonium persulphate acid solution, under condition of ice bath, react 12h, within static 12 hours, discard supernatant liquor, decompress filter, extremely neutral with deionized water wash, 45 ℃ of vacuum-dryings, obtain graphene oxide/polyaniline binary complex.
(3) take 0.05g graphene oxide/polyaniline binary complex and 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, adds ammoniacal liquor to regulate PH to 9, then adds 2.5g hydrazine hydrate, ultrasonic 5min, and the static supernatant liquor that discards, decompress filter, washing is dry to neutral final vacuum, obtains graphene/polyaniline/cobalt ternary complex.
The performance test of B absorbing material
Graphene/polyaniline/cobalt ternary complex of take is 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 annular sample.Prepared matrix material reaches 1.19GHz, can reach-13.83dB of minimal reflection loss value at 2～18GHz internal reflection loss value lower than the frequency span of-10dB.
Claims (3)
1. graphene/polyaniline/cobalt composite wave-suction material, it is characterized in that this absorbing material is comprised 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.
2. the preparation method of a kind of graphene/polyaniline/cobalt composite wave-suction material according to claim 1, is characterized in that comprising being prepared as follows step:
(1) preparation of graphene oxide
Adopt to improve Hummers method and prepare graphite oxide by natural graphite reaction, 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; Aequum graphite and SODIUMNITRATE are added in the vitriol oil, and ice bath is cooled to 4 ℃, slowly adds KMn0
4, stirring reaction 90min; Then be warming up to 30 ℃ of stirring reaction 30min; Slowly add deionized water, then after 90 ℃ of stirring reaction 20min, add deionized water and hydrogen peroxide after being cooled to room temperature, through the dry graphite oxide that obtains of centrifuge washing final vacuum;
Graphite oxide is added to the ultrasonic 2h of 150ml deionized water, obtain the suspension of graphene oxide.
(2) preparation of graphite oxide/polyaniline binary matrix material
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 ℃ of vacuum-dryings, obtain graphene oxide/polyaniline binary complex;
(3) preparation of graphene/polyaniline/cobalt trielement composite material
Take graphene oxide/polyaniline binary complex and be scattered in ethanol and deionized water mixed solution, in ethanol and deionized water mixed solution, the ratio of ethanol and deionized water is 4:1; Accurately taking cobalt chloride adds in the ethanol and deionized water mixed solution that contains binary complex, binary complex and cobalt salt mass ratio 1:4～8, ultrasonic 0.5h, add ammoniacal liquor to regulate PH to 9, then add the hydrazine hydrate (hydrazine hydrate and cobalt chloride mass ratio 25:1) of massfraction 80%, ultrasonic 5min, the static supernatant liquor that discards, decompress filter, washing is dry to neutral final vacuum, obtains graphene/polyaniline/cobalt ternary complex;
(4) take graphene/polyaniline/cobalt ternary complex is 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.
3. the preparation method of graphene/polyaniline/cobalt composite wave-suction material according to claim 2, it is characterized in that 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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