CN105950112A - Nano composite absorbing material and preparation method thereof - Google Patents
Nano composite absorbing material and preparation method thereof Download PDFInfo
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- CN105950112A CN105950112A CN201610361468.2A CN201610361468A CN105950112A CN 105950112 A CN105950112 A CN 105950112A CN 201610361468 A CN201610361468 A CN 201610361468A CN 105950112 A CN105950112 A CN 105950112A
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Abstract
The invention discloses a preparation method of a nano composite absorbing material, belonging to the field of electromagnetic. The preparation method comprises the steps of first preparing alkynyl modified magnetic nano particles, and preparing an azide modified graphene oxide substrate by taking graphite as a raw material, then chelating the alkynyl modified magnetic nano particles on the surface of tazide modified graphene oxide in a covalent manner through a cycloaddition reaction, and finally reducing by using hydrazine hydrate, so as to form the nano composite absorbing material; according to the preparation method disclosed by the invention, magnetic nano particles are chelated on the surface of the graphene in the covalent manner through a click coupling method, and the chelated nano particles are not liable to fall off from the surface of the graphene, thus a graphene-ferrite composite material has good conductivity and magnetic property, and has the advantages of high acid resistance, good stability, high practicability and the like; meanwhile, the impedance matching performance of the absorbing material is improved, the material prepared by the invention has better microwave absorbing property on a C waveband and a Ku waveband, and has important application value in the field of electromagnetic shielding.
Description
Technical field
The present invention relates to electromagnetism field, particularly relate to a kind of nano combined absorbing material and preparation method thereof.
Background technology
Development along with modern science and technology, the electronics such as electric power (power transmission and transformation, household electrical appliance etc.), microwave (microwave oven, microwave signal launching tower etc.), radio wave (handset mobile communications, radio and television launching tower etc.), electrical equipment use the most universal, the complicated electromagnetic environment of formation is the most serious.Produced electromagnetic radiation and electromagnetic interference all produce great harm to human body, electronic equipment, the fourth-largest pollution after atmospheric pollution, noise pollution and water pollute being well recognized as, and become society and the hot issue of scientific circles' concern.As electromagnetic radiation can affect the blood circulation of human body, immunity, reproduction and metabolic function, serious also can induce cancer, and can accelerate the cancer cell multiplication of human body；Electromagnetic Interference broadcast, TV signal and communication signal, the robot control system(RCS) making equipment instrument is malfunctioning, aircraft flight indication signal error etc..Therefore, how to reduce electromagnetic radiation, prevent electromagnetic interference, effectively protect environment, protect health, extremely the most urgent.
Supporting or carry magnetic material with Graphene for substrate and can form mutual supplement with each other's advantages, on the one hand the grapheme material of light weight can reduce the density of material, and on the other hand the compound of bi-material can make material have multi-form electromagnetic consumable.But the absorbing material preparing magnetic nanoparticle at present compound with Graphene typically uses coprecipitation, solvent-thermal method, composite wave-suction material prepared by these methods is all to be deposited on graphenic surface by physical absorption or electrostatic interaction by magnetic nanoparticle, the composite that these methods are formed is unstable, acidproof, oxidation resistance is the strongest, and nano-particle easily reunites, in use easily from shortcomings such as graphenic surface come off.
Therefore, existing absorbing material can not reach stable, acidproof, resistance to oxidation and the requirement of absorption effective to electromagnetic wave.
Summary of the invention
An object of the present invention, in that provide the preparation method of a kind of new nano combined absorbing material, to solve the problems referred to above.
To achieve these goals, the technical solution used in the present invention is such that the preparation method of a kind of nano combined absorbing material, and the graphene oxide matrix that the magnetic nanoparticle modified by alkynyl and Azide are modified is combined；The proportioning of the graphene oxide matrix that the magnetic nanoparticle that alkynyl is modified is modified with Azide is by weight for (5-10): 1 mixs homogeneously, then the magnetic nanoparticle covalency modified by described alkynyl by cycloaddition reaction is sequestered in the surface of graphene oxide that described Azide is modified, finally with hydrazine hydrate reduction, form ferrite-graphene nano composite wave-suction material.
As preferred technical scheme: described magnetic nanoparticle general molecular formula is MFe2O4, wherein M is Co2+, Ni2+, Mg2+, Fe2+One or more in Deng.
As preferred technical scheme: the preparation technology of the magnetic nanoparticle that described alkynyl is modified is as follows:
(1) Fe (NO is weighed3)3· 9H2O and M (NO3)2· 6H2O, with water dissolution, and stirs, and regulates the pH of solution > 7, and presoma is poured into and is incubated 4 ~ 24h in reactor at 160 ~ 240 DEG C, the most scrubbed, be dried, and obtains ferrite nano powder body；
(2) the ferrite nano powder body of step (1) gained is scattered in polyacrylic aqueous solution, at 80 ~ 95 DEG C, then stirs 40 ~ 90min, the most acidified, wash, be dried to obtain the magnetic nanoparticle of surface carboxyl groups；
(3) the carboxylated magnetic nanoparticle of step (2) gained is scattered in dimethyl formamide solution, then being sequentially added into carbodiimide hydrochloride, N-hydroxy-succinamide and propargylamine occurs amide to react at normal temperatures, the most scrubbed, be dried to obtain alkynyl modify magnetic nanoparticle.
As preferred technical scheme: the graphene oxide preparation method that described Azide is modified is: is first scattered in dimethylformamide or tetrahydrofuran solution by graphite oxide and obtains graphene oxide dispersion, it is subsequently adding at Hydrazoic acid,sodium salt 30 ~ 60 DEG C stirring 2 ~ 3 days, finally washs, be dried to obtain the graphene oxide (GO-N that Azide is modified3).
As preferred technical scheme: the method for described covalency chelating is: the graphene oxide of magnetic nanoparticle and Azide modification that example weighs alkynyl modification is scattered in dimethyl formamide solution by mass percentage, after by evenly mixing, catalyst is added in mixed solution, there is Dipolar Cycloaddition, through hydrazine hydrate reduction after, obtain described ferrite-graphene nano composite wave-suction material (MFe2O4/ RGO).
As preferred technical scheme: described process for dispersing uses ultrasonic disperse.
Present invention also offers a kind of nano combined absorbing material using above-mentioned preparation method to prepare.
Compared with prior art, it is an advantage of the current invention that: nano-particle can be made preferably to be sequestered on graphenic surface by clicking on coupling, this composite has good electric conductivity, magnetic property, compared to Electrostatic Absorption, the nano-particle of this complex method is difficult to come off from graphenic surface in the application, and has the features such as practical, acid resistance strong, good stability after the coated modification in magnetic nanoparticle surface；Furthermore by magnetic nanoparticle growth in situ at graphenic surface, make Graphene produce electric charge transfer at covalency coupling and form strong dielectric relaxor, improve the impedance matching performance of Graphene and magnetic nanoparticle, there is the absorbing property of excellence, therefore have good using value in absorbing material field.
Accompanying drawing explanation
Fig. 1 is the course of reaction figure of the embodiment of the present invention 1；
Fig. 2 is the mean diameter figure of the cobalt ferrite nanoparticles of the embodiment of the present invention 1；
Fig. 3 is the infrared spectrogram that the embodiment of the present invention 1 clicks on composite；
Fig. 4 is the reflection loss figure of the embodiment of the present invention 1 Conjugate ferrite/reduced graphene composite.
Detailed description of the invention
Below in conjunction with accompanying drawing, the invention will be further described.
Embodiment 1:CoFe2O4
The preparation method of/RGO composite wave-suction material
As it is shown in figure 1, comprise the following steps:
Step (1): the preparation of alkynyl Conjugate ferrite
2:1 weighs Fe (NO in molar ratio3)3· 9H2O and Co (NO3)2· 6H2O dispensing, it is dissolved in the beaker of deionized water, and stir, after it is completely dissolved, adds ammonia and regulate the pH=9 of solution, solution is transferred in inner liner polytetrafluoroethylene reactor, at 180 DEG C, it is incubated 10h, through washing, lyophilization after room temperature cooling, obtains Co ferrite Nano powder, as in figure 2 it is shown, its mean diameter of cobalt ferrite nanoparticles is at 10 ~ 20nm；By Conjugate ferrite than polyacrylic mass ratio 3:1, by cobalt ferrite nanoparticles ultrasonic disperse in polyacrylic aqueous solution, at 95 DEG C, then quickly stir 1h, the most acidified, washing, lyophilization；Weigh a certain amount of carboxylated cobalt ferrite nanoparticles ultrasonic disperse in 30ml dimethyl formamide solution, then it is sequentially added into carbodiimide hydrochloride, N-hydroxy-succinamide and propargylamine and is stirred at room temperature overnight generation amide reaction, the most scrubbed, be dried to obtain the cobalt ferrite nanoparticles of terminal alkynyl.
Step (2): Azide graphene oxide (GO-N3) preparation
Graphite oxide is prepared first with Hummers method, take 0.2g graphite oxide ultrasonic disperse and obtain graphene oxide dispersion in 200ml dimethyl formamide solution, being subsequently adding 0.2g Hydrazoic acid,sodium salt insulated and stirred 2 days at 40 DEG C, the most scrubbed, centrifugal, lyophilization obtains the graphene oxide (RO-N that azido is modified3)；
Step (3): Conjugate ferrite/Graphene clicks on compound preparation
The cobalt ferrite nanoparticles of alkynyl step 1 obtained and Azide graphene oxide (mass ratio 10:1) ultrasonic disperse are in 30ml dimethyl formamide solution, ferrite is made to mix homogeneously with graphene oxide after ultrasonic, then in solution, sodium ascorbate and copper sulfate are added as catalyst, make ethynylation magnetic nanoparticle and Azide graphene oxide generation Dipolar Cycloaddition, even if magnetic nanoparticle covalency is sequestered in surface of graphene oxide, infared spectrum such as Fig. 3 after chelating, the peak value appearance that azido disappears new；Product Magneto separate, after distilled water wash, add hydrazine hydrate (m graphene oxide: m hydrazine hydrate=10:7) reduction, scrubbed, after drying obtain click on preparation CoFe2O4
/ RGO composite wave-suction material A.
After tested, the composite wave-suction material A prepared by discovery in 2 ~ 18GHz, minimum-40 dB of reflection loss (6.8GHz)；At Ku wave band 15.2GHz, reflection loss can reach-25dB, and the effective Absorber Bandwidth less than-10dB is 5.2GHz.Can be seen that composite wave-suction material prepared by the present invention all has excellent microwave absorbing property at C-band (i.e. 4-8 GHz) and Ku wave band (i.e. 12-18 GHz) in conjunction with example, see Fig. 4.
Embodiment 2:
NiFe2O4, Graphene preparation method respectively with embodiment 1 step (1), step (2), 5:1 in mass ratio weighs alkynyl NiFe2O4With Azide Graphene, preparation method, with embodiment 1 step (3), obtains NiFe2O4/ RGO composite wave-suction material B.The bandwidth that prepared composite B is less than-10dB in 2 ~ 18GHz internal reflection rate penalty values reaches 4.8GHz, and minimum reflectance penalty values is up to-44dB (5.6GHz).
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, should be included within the scope of the present invention.
Claims (7)
1. the preparation method of a nano combined absorbing material, it is characterised in that: the graphene oxide matrix that the magnetic nanoparticle modified by alkynyl and Azide are modified is combined；The proportioning of the graphene oxide matrix that the magnetic nanoparticle that alkynyl is modified is modified with Azide is by weight for (5-10): 1 mixs homogeneously, then the magnetic nanoparticle covalency modified by described alkynyl by cycloaddition reaction is sequestered in the surface of graphene oxide that described Azide is modified, finally with hydrazine hydrate reduction, form ferrite-graphene nano composite wave-suction material.
Preparation method the most according to claim 1, it is characterised in that described in the magnetic nanoparticle general molecular formula that is sequestered on graphenic surface be MFe2O4, wherein M is divalent transition metal ion Co2+、Ni2+、Mg2+And Zn2+In one or more.
Preparation method the most according to claim 2, it is characterised in that the preparation technology of the magnetic nanoparticle that described alkynyl is modified is as follows:
(1) Fe (NO is weighed3)3· 9H2O and M (NO3)2· 6H2O, with water dissolution, and stirs, and regulates the pH of solution > 7, is then incubated 4 ~ 24h at 16 ~ 240 DEG C, the most scrubbed, be dried, and obtains ferrite nano powder body；
(2) the ferrite nano powder body of step (1) gained is scattered in polyacrylic aqueous solution, at 80 ~ 95 DEG C, then stirs 40 ~ 90min, the most acidified, wash, be dried to obtain the magnetic nanoparticle of surface carboxyl groups；
(3) the carboxylated magnetic nanoparticle of step (2) gained is scattered in dimethylformamide or tetrahydrofuran solution, then being sequentially added into carbodiimide hydrochloride, N-hydroxy-succinamide and propargylamine occurs amide to react at normal temperatures, the most scrubbed, be dried to obtain alkynyl modify magnetic nanoparticle.
Preparation method the most according to claim 1, it is characterized in that, the graphene oxide preparation method that described Azide is modified is: prepare graphite oxide (GO) with graphite for raw material first with Hummers method, gained graphite oxide is scattered in dimethylformamide or tetrahydrofuran solution and obtains graphene oxide dispersion, it is subsequently adding Hydrazoic acid,sodium salt to stir 2 ~ 7 days at 30 ~ 80 DEG C, finally washs, be dried to obtain the graphene oxide GO-N that Azide is modified3。
Preparation method the most according to claim 1, it is characterized in that, the method of described covalency chelating is: the graphene oxide of the magnetic nanoparticle and Azide modification that weigh alkynyl modification by mass percentage is scattered in dimethylformamide or tetrahydrofuran solution, after by evenly mixing, catalyst is added in mixed solution, there is Dipolar Cycloaddition, after through hydrazine hydrate reduction, obtain described ferrite-graphene nano composite wave-suction material MFe2O4/RGO。
6. according to the preparation method described in claim 3-5 any one, it is characterised in that: described process for dispersing uses ultrasonic disperse.
7. use the nano combined absorbing material that the preparation method described in claim 1-5 any one prepares.
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Cited By (7)
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| CN107936525A (en) * | 2017-11-21 | 2018-04-20 | 南京理工大学 | Polymeric material of graphene oxide composite material filling being covalently attached layer by layer and preparation method thereof |
| CN108675283A (en) * | 2018-04-04 | 2018-10-19 | 高猛 | A kind of composite Nano electromagnetic wave absorbent material and preparation method thereof prepared using graphene |
| CN109174039A (en) * | 2018-10-09 | 2019-01-11 | 李忠 | A kind of composite nano materials and preparation method thereof for air cleaning |
| CN110054869A (en) * | 2019-05-13 | 2019-07-26 | 青岛碳智新材料科技有限公司 | A kind of graphene oxide/nano silica/epoxy resin composite material preparation method |
| CN110272243A (en) * | 2019-06-21 | 2019-09-24 | 中国人民解放***箭军工程大学 | A kind of double-layer cement base wave-absorbing material and preparation method thereof |
| CN110724492A (en) * | 2019-09-29 | 2020-01-24 | 安徽理工大学 | Ferroferric oxide/nano oxide hybrid wave-absorbing material and preparation method thereof |
| CN110724493A (en) * | 2019-09-29 | 2020-01-24 | 安徽理工大学 | Multi-walled carbon nanotube/ferroferric oxide/nano oxide hybrid wave-absorbing material and preparation method thereof |
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| CN107936525A (en) * | 2017-11-21 | 2018-04-20 | 南京理工大学 | Polymeric material of graphene oxide composite material filling being covalently attached layer by layer and preparation method thereof |
| CN108675283A (en) * | 2018-04-04 | 2018-10-19 | 高猛 | A kind of composite Nano electromagnetic wave absorbent material and preparation method thereof prepared using graphene |
| CN110104635A (en) * | 2018-04-04 | 2019-08-09 | 朱晶晶 | Utilize the preparation method of the composite Nano electromagnetic wave absorbent material of graphene preparation |
| CN109174039A (en) * | 2018-10-09 | 2019-01-11 | 李忠 | A kind of composite nano materials and preparation method thereof for air cleaning |
| CN110054869A (en) * | 2019-05-13 | 2019-07-26 | 青岛碳智新材料科技有限公司 | A kind of graphene oxide/nano silica/epoxy resin composite material preparation method |
| CN110272243A (en) * | 2019-06-21 | 2019-09-24 | 中国人民解放***箭军工程大学 | A kind of double-layer cement base wave-absorbing material and preparation method thereof |
| CN110272243B (en) * | 2019-06-21 | 2021-11-05 | 中国人民解放***箭军工程大学 | Double-layer cement-based wave-absorbing material and preparation method thereof |
| CN110724492A (en) * | 2019-09-29 | 2020-01-24 | 安徽理工大学 | Ferroferric oxide/nano oxide hybrid wave-absorbing material and preparation method thereof |
| CN110724493A (en) * | 2019-09-29 | 2020-01-24 | 安徽理工大学 | Multi-walled carbon nanotube/ferroferric oxide/nano oxide hybrid wave-absorbing material and preparation method thereof |
| CN110724493B (en) * | 2019-09-29 | 2022-11-18 | 安徽理工大学 | Multi-walled carbon nanotube/ferroferric oxide/nano oxide hybrid wave-absorbing material and preparation method thereof |
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