CN104448305A - Nano-composite wave-absorbing material and preparation method thereof - Google Patents
Nano-composite wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a nano-composite wave-absorbing material. According to the method, natural graphite powder is taken as a raw material, concentrated sulfuric acid and potassium permanganate are taken as oxidants, and an improved Hummers method is adopted for preparing graphene oxide. Graphene oxide and FeCl3.H2O are placed in ethylene glycol, polyvinylpyrrolidone is taken as a modifier, NH4Ac is taken as a foaming agent, and hollow triiron tetraoxide nanoparticles are successfully loaded onto the surface of a graphene sheet layer through a solvent thermal method. Dodecylbenzenesulfonic acid is taken as a surfactant, a graphene/hollow triiron tetraoxide nano-composite material and an aniline monomer are uniformly mixed, ammonium persulfate is taken as an initiator, and a graphene/hollow triiron tetraoxide/polyaniline nano-composite material is obtained by in-situ polymerization. According to the preparation method disclosed by the invention, a simple hydrothermal method and an in-situ polymerization method are adopted, and the graphene/hollow triiron tetraoxide/polyaniline nano-composite material with excellent wave-absorbing performance can be prepared.
Description
Technical field
The present invention relates to absorbing material field, in particular a kind of preparation method of nano combined absorbing material.
Background technology
Along with science and technology and the development of electronic industry, the application that various electronic equipment is leavened dough in business, industry, health care etc. is increasing, electromagnetic interference has become the fourth-largest environomental pollution source after Industrial " three Waste ", and electromagnetic pollution has become " the stealthy killer " of human society.There are some researches show, excessive electromagenetic wave radiation occurs, except obstacle, even may bring out the serious disease comprising all kinds of cancer except causing neural system, immunity system, reproductive system and blood circulation etc.Be in for a long time in electromagnetic wave environment, damaged by hertzian wave in human body and the damage of the tissue of the self-regeneration that is not able to do in time and organ can become dynamic disease becomes because of long term accumulation, can threat to life time serious.
Graphene, the single layer structure due to its uniqueness makes it have the features such as ultralight density, large specific surface area, specific inductivity that conductivity is excellent and high, becomes a kind of novel wave-absorbing material.In addition, the chemical bond that oxidized graphenic surface exposes in a large number more easily produces the dielectric relaxor of out-shell electron and attenuates electromagnetic waves under the effect of electromagnetic field, for Graphene is inhaling the applications expanding prospect in ripple field.
But Graphene is do not have magnetic and magnetic loss as the shortcoming that absorbing material is maximum, and the single high dielectric loss of Graphene will cause the problem of impedance matching difficulty and affect absorbing property.Therefore, at the hollow ferriferrous oxide nano-particle of graphenic surface carried magnetic, not only can improve magnetism of material energy, the magnetic loss of reinforced composite, be conducive to the impedance matching of matrix material, and ferriferrous oxide particles reduces Graphene again stacking in drying process as spacer medium to be three-dimensional graphite structure, to play considerable effect to stable graphene film Rotating fields.Meanwhile, consider to add conductive polymers in compound system, as coating layer, not only strengthen the interface cohesion of magnetic particle and Graphene, and due to the high dielectric loss of conductive polymers self, reinforced composite material is at the absorbing property of high band.
Technical problem to be solved by this invention is for the deficiencies in the prior art, provides a kind of Graphene/hollow Z 250/polyaniline nano composite wave-suction material and preparation method thereof.
Technical scheme of the present invention is as follows:
A preparation method for Graphene/hollow Z 250/polyaniline nano composite wave-suction material, its step is as follows:
(1) by 2 ~ 4g Graphite Powder 99,2 ~ 3.5g Potassium Persulphate and 2 ~ 3.5g P
2o
5join in 10 ~ 16mL vitriol oil successively, form mixture, mixture ph is 1-2.Stir with 150 ~ 250mL distilled water diluting after 4 ~ 8h at 80 DEG C, the pH value after dilution is 3-4, and filter after placing 10-24h and use distilled water wash until filtrate is to neutrality, products therefrom is at room temperature dried to constant weight, obtains the graphite 2 ~ 3g of preoxidation.
(2) graphite of above-mentioned preoxidation is joined in 100 ~ 150mL vitriol oil stir 30min and make it even, and slowly add 20 ~ 40g KMnO under ice-water bath
4.Treat whole KMnO
4after adding, stir 30 ~ 60min, obtain the graphite of preoxidation.
(3) system is warmed up to 35 DEG C, reaction 2h.Subsequently, slowly add 200mL distilled water, then react 2h in system, hierarchy of control temperature is no more than 50 DEG C, again adds 150 ~ 250ml distilled water and 10 ~ 40ml 30%H
2o
2with termination reaction.The hydrochloric acid soln washing of the centrifugal rear 1L of product, finally dialysis obtains 2 ~ 3g product graphite oxide one week.
(4) ultrasonic disperse in 60ml ethylene glycol of the graphite oxide after 0.010 ~ 0.015g frost drying is formed uniform dispersion liquid, then take 0.42 ~ 1.68g Fecl
36H
2o, 0.62 ~ 2.49g polyvinylpyrrolidone (PVP), 1.42 ~ 4.79g NH
4ac is dissolved in the ethylene glycol of 70mL, stirs, makes it to become formation settled solution.
(5) solution of gained is moved in 100mL reactor, after sealing, be heated to 200 ~ 230 DEG C, and be incubated 10 ~ 15h.After having reacted, reactor is taken out, makes it cool to room temperature.By centrifugal for the black powder of gained, adopt dehydrated alcohol and deionized water respectively to wash three times, at 50 ~ 70 DEG C of vacuum-drying 24h, obtain product A.
(6) by product A and 0.8 ~ 1.2g aniline monomer, joining pre-dispersedly has in the solution of 10.65g Witco 1298 Soft Acid, and ultrasonic disperse 30 ~ 60min, forms homogeneous system B.
(7) 1.96 ~ 2.94g ammonium persulphate is dissolved in 50 ~ 100ml distilled water, slowly be added drop-wise in system B, stirring reaction 12h, after reaction terminates, suction filtration, use distilled water, washing with alcohol product colourless to filtrate respectively, 50 ~ 70 DEG C of vacuum-drying 24 ~ 36h, obtain nano combined absorbing material.
(8) X-ray diffractometer is utilized to carry out phase structure analysis to gained sample; Fourier transform infrared spectroscopy and Raman spectrum is utilized to carry out the determination of molecular structure to sample; Field emission scanning electron microscope and the appearance structure of transmission electron microscope to sample is utilized to analyze; The electromagnetic parameter of vector network analysis to sample is utilized to analyze.
Described Potassium Persulphate, P
2o
5, potassium permanganate, ammonium persulphate, Fecl
36H
2o, aniline, Witco 1298 Soft Acid, ethylene glycol and the vitriol oil are analytical pure.
Described preparation method, in step (2), slowly adds KMnO
4time, hierarchy of control temperature, system temperature is no more than 20 DEG C.
Described preparation method, in step (3), the concentration of hydrochloric acid is the hydrochloric acid soln of volume ratio 1:10.
Described preparation method, in step (6), product A accounts for 30 ~ 50% of aniline monomer quality.
Described preparation method obtains Graphene/hollow Z 250/polyaniline nano-composite material.
The preparation method of Graphene of the present invention/hollow Z 250/polyaniline nano composite wave-suction material adopts solvent-thermal method, situ aggregation method, by the growth in situ of Z 250 on graphene sheet layer and the in-situ polymerization of polyaniline on Graphene/ferriferrous oxide composite material surface, thus realize the wave-absorbing effect of material excellence.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum (XRD) of gained sample; In figure, a is graphene oxide, and b is hollow ferriferrous oxide nano sphere, and c is Graphene/hollow ferriferrous oxide nano matrix material, and d is Graphene/hollow Z 250/polyaniline nano-composite material, and e is polyaniline.
Fig. 2 is the infrared spectrogram ((FT-IR) of Graphene/hollow Z 250 and Graphene/hollow Z 250/polyaniline nano-composite material; In figure, a is Graphene/hollow ferriferrous oxide nano matrix material, and b is black alkene/hollow Z 250/polyaniline nano-composite material.
Fig. 3 is field emission scanning electron microscope and the transmission electron microscope picture of hollow ferriferrous oxide nano sphere, Graphene/hollow Z 250 and Graphene/hollow Z 250/polyaniline nano-composite material; Figure a is hollow ferriferrous oxide nano sphere field emission scanning electron microscope figure, figure b is Graphene/hollow ferriferrous oxide nano matrix material field emission scanning electron microscope figure, figure c and figure d is the field emission scanning electron microscope figure of Graphene/hollow Z 250/polyaniline nano-composite material, figure e is respectively Graphene/hollow ferriferrous oxide nano matrix material transmission electron microscope picture, and figure f is Graphene/hollow Z 250/polyaniline nano-composite material transmission electron microscope picture.
Fig. 4 is the Raman spectrogram of sample; In figure, a is graphene oxide, and b is Graphene/hollow ferriferrous oxide nano matrix material, and c is Graphene/hollow Z 250/polyaniline nano-composite material.
Fig. 5 is the relation curve of Graphene/hollow Z 250/polyaniline nano-composite material magnetic loss angle tangent and tangent of the dielectric loss angle and frequency; Wherein, figure a is the relation curve of magnetic loss angle tangent and frequency, and figure b is the relation curve of dielectric loss tangent and frequency.
Fig. 6 is the suction curve line of Graphene/hollow Z 250/polyaniline nano-composite material; In figure, a is thickness 1.0mm, b be thickness 1.5mm, c is thickness 2.0mm.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
(1) (1) is by 2 ~ 4g Graphite Powder 99,2 ~ 3.5g Potassium Persulphate and 2 ~ 3.5g P
2o
5join in 10 ~ 16mL vitriol oil successively, form mixture, mixture ph is 1-2.Stir with 150 ~ 250mL distilled water diluting after 4 ~ 8h at 80 DEG C, the pH value after dilution is 3-4, and filter after placing 10-24h and use distilled water wash until filtrate is to neutrality, products therefrom is at room temperature dried to constant weight, obtains the graphite 2 ~ 3g of preoxidation.
(2) graphite of above-mentioned preoxidation is joined in 100 ~ 150mL vitriol oil stir 30min and make it even, and slowly add 20 ~ 40g KMnO under ice-water bath
4.Treat whole KMnO
4after adding, stir 30 ~ 60min, obtain the graphite of preoxidation.
(3) system is warmed up to 35 DEG C, reaction 2h.Subsequently, slowly add 200mL distilled water, then react 2h in system, hierarchy of control temperature is no more than 50 DEG C, again adds 150 ~ 250ml distilled water and 10 ~ 40ml 30%H
2o
2with termination reaction.The hydrochloric acid soln washing of the centrifugal rear 1L of product, finally dialysis obtains 2 ~ 3g product graphite oxide one week.
(4) ultrasonic disperse in 60ml ethylene glycol of the graphite oxide after 0.010 ~ 0.015g frost drying is formed uniform dispersion liquid, then take 0.42 ~ 1.68g Fecl
36H
2o, 0.62 ~ 2.49g polyvinylpyrrolidone (PVP), 1.42 ~ 4.79g NH
4ac is dissolved in the ethylene glycol of 70mL, stirs, makes it to become formation settled solution.
(5) solution of gained is moved in 100mL reactor, after sealing, be heated to 200 ~ 230 DEG C, and be incubated 10 ~ 15h.After having reacted, reactor is taken out, makes it cool to room temperature.By centrifugal for the black powder of gained, adopt dehydrated alcohol and deionized water respectively to wash three times, at 50 ~ 70 DEG C of vacuum-drying 24h, obtain product A.
(6) by product A and 0.8 ~ 1.2g aniline monomer, joining pre-dispersedly has in the solution of 10.65g Witco 1298 Soft Acid, and ultrasonic disperse 30 ~ 60min, forms homogeneous system B.
(7) 1.96 ~ 2.94g ammonium persulphate is dissolved in 50 ~ 100ml distilled water, slowly be added drop-wise in system B, stirring reaction 12h, after reaction terminates, suction filtration, use distilled water, washing with alcohol product colourless to filtrate respectively, 50 ~ 70 DEG C of vacuum-drying 24 ~ 36h, obtain nano combined absorbing material.
X-ray diffractometer is utilized to carry out phase structure analysis to gained sample; Fourier transform infrared spectroscopy and Raman spectrum is utilized to carry out the determination of molecular structure to sample; Field emission scanning electron microscope and the appearance structure of transmission electron microscope to sample is utilized to analyze; The electromagnetic parameter of vector network analysis to sample is utilized to analyze.Test result is shown in shown in Fig. 1 ~ 6.
Fig. 1 is the X ray diffracting spectrum (XRD) of gained sample.As can be seen from Fig. 1 a, natural graphite pruinescence is successfully oxidized and peels off into graphene oxide.As can be seen from Fig. 1 b, prepared ferriferrous oxide particles and standard P DF card coincide (PDF No.8801315), and without dephasign.From Fig. 1 c and Fig. 1 d, in Graphene/hollow Z 250 binary and Graphene/hollow Z 250/polyaniline ternary nano compound, Z 250 can be observed by clear mutually, and this shows Z 250 by successful load at graphenic surface.Meanwhile, in Fig. 1 c and Fig. 1 d, the diffraction peak of graphene oxide disappears, and this shows that graphene oxide is in solvent thermal reaction, under the effect of ethylene glycol, be successfully reduced into Graphene.Comparison diagram 1 (d) and Fig. 1 (e), stronger Z 250 diffraction peak and the diffraction peak of more weak polyaniline is there is in ternary nano compound, diffraction peak position slightly offsets, illustrate that polyaniline and Z 250 are all present in ternary complex, and have existence to interact.Fig. 2 is the infrared spectrogram of Graphene/hollow Z 250 and Graphene/hollow Z 250/polyaniline nano-composite material.Comparison diagram 2a and Fig. 2 b is known, in Graphene/hollow Z 250 binary nano complex, Fe-O charateristic avsorption band does not occur in ternary nano composite material, and the charateristic avsorption band of obvious polyaniline in ternary nano composite material, can be observed, this means that polyaniline success is coated on Graphene/hollow ferriferrous oxide nano compound surface completely, form charge-transfer complex.But, the charateristic avsorption band of carbonyl functional group does not all occur in binary, ternary complex, also further demonstrate that graphene oxide is successfully reduced to Graphene, and the Graphene be reduced and Z 250, there is Charger transfer between polyaniline, be conducive to forming binary, trielement composite material.Fig. 3 is field emission scanning electron microscope figure and the transmission electron microscope picture of hollow ferriferrous oxide nano sphere, Graphene/hollow Z 250 and Graphene/hollow Z 250/polyaniline nano-composite material.Can see that from Fig. 3 a Z 250 is hollow structure, particle diameter is between 250 ~ 400nm.Can observe from Fig. 3 b, hollow ferroferric oxide nano granules is adsorbed on Graphene transparent sheet.Fig. 3 c and Fig. 3 d shows, polyaniline is successfully coated on Graphene and Z 250 surface.Fig. 3 e and Fig. 3 f presents the microtexture of matrix material more clearly, and its result is analyzed consistent with field emission scanning electron microscope, XRD and FT-IR.Fig. 4 is the Raman spectrogram of sample.As can be seen from Figure 4, all there are two Characteristic Raman absorption peaks of Graphene in binary, ternary complex, and compared with simple graphite oxide, nano composite material I
d/ I
gvalue increases all to some extent.This is because in recombination process, the Z 250 of growth in situ reduces the regularity of Graphene crystalline network, and Fe
3+existence more easily cause the textural defect such as physics, chemistry on graphene sheet layer border; After polyaniline compound, the π-π * interaction of electrons between Graphene and polyaniline makes the defect of Graphene own and disordered lattice vibration increase.This also absolutely proves: Graphene, there is strong interaction between hollow Z 250 and polyaniline three.Fig. 5 is the relation curve of Graphene/hollow Z 250/polyaniline nano-composite material magnetic loss angle tangent and tangent of the dielectric loss angle and frequency.As can be seen from Figure 5, Graphene/hollow Z 250/polyaniline nano-composite material has stronger magnetic loss and dielectric loss concurrently, more be worth mentioning and be, magnetic loss and dielectric loss have good matching properties, for the absorbing property realizing nano composite material excellence has laid solid foundation.Fig. 6 is the suction curve line of Different matching thickness Graphene/hollow Z 250/polyaniline nano-composite material.As can be seen from Figure 6, the maximum absorption band being 1.0mm when sample match thickness is positioned at 14.5GHz, and its reflectance value is-29.5dB, and the bandwidth value that reflectivity is less than-10dB reaches 4.3GHz; Thickness of sample is that the maximum absorption band of 1.5mm is positioned at 10.8GHz, and its reflectance value is-24.8GHz, and the bandwidth value that reflectivity is less than-10dB reaches 4.5GHz; Thickness of sample is that the maximum absorption band of 2.0mm is positioned at 8.9GHz, and its reflectance value is-17.5GHz, and the bandwidth value that reflectivity is less than-10dB reaches 4.4GHz.
Should be understood that, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (7)
1. a preparation method for nano combined absorbing material, is characterized in that, its step is as follows:
(1) by 2 ~ 4g Graphite Powder 99,2 ~ 3.5g Potassium Persulphate and 2 ~ 3.5g P
2o
5join in 10 ~ 16mL vitriol oil successively, form mixture, mixture ph is 1-2, this mixture is stirred at 80 DEG C after 4 ~ 8h with 150 ~ 250mL distilled water diluting, after dilution, the pH value of mixture is 3-4, filter after placing 10-24h and use distilled water wash until filtrate is to neutrality, products therefrom is at room temperature dried to constant weight, the graphite 2 ~ 3g of obtained preoxidation;
(2) graphite of above-mentioned preoxidation is joined stir 30min in about 100 ~ 150mL vitriol oil and make it even, and slowly add 20 ~ 40g KMnO under ice-water bath
4, treat whole KMnO
4after adding, stir 30 ~ 60min, obtain the graphite of preoxidation;
(3) above-mentioned system is warmed up to 35 DEG C, reaction 2h, subsequently, slowly add 200mL distilled water, then react 2h in system, hierarchy of control temperature is no more than 50 DEG C, again adds 150 ~ 250ml distilled water and 10 ~ 40ml 30%H
2o
2with termination reaction, product centrifugation 10min, rotating speed 8000 ~ 10000r/min, the hydrochloric acid soln washing of centrifugation after product 1L, finally dialysis obtains 2 ~ 3g product graphite oxide one week; .
(4) ultrasonic disperse in 60ml ethylene glycol of the graphite oxide after 0.10 ~ 0.15g frost drying is formed uniform dispersion liquid, then take 0.42 ~ 1.68g Fecl
36H
2o, 0.62 ~ 2.49g polyvinylpyrrolidone (PVP), 1.42 ~ 4.79g NH
4ac is dissolved in the ethylene glycol of 70mL, stirs, makes it to become formation settled solution;
(5) solution of gained is moved in 100mL reactor, after sealing, be heated to 200 ~ 230 DEG C, and be incubated 10 ~ 15h.After having reacted, reactor is taken out, makes it cool to room temperature, by the black powder centrifugation 10min of gained, rotating speed 8000 ~ 10000r/min, dehydrated alcohol and deionized water is adopted respectively to wash three times, at 50 ~ 70 DEG C of vacuum-drying 24h, obtain product A 0.2 ~ 0.55g;
(6) by product A 0.8 ~ 1.2g and 0.8 ~ 1.2g aniline monomer, joining pre-dispersedly has in the solution of 10.65g Witco 1298 Soft Acid, and ultrasonic disperse 30 ~ 60min, forms homogeneous system B.
(7) 1.96 ~ 2.94g ammonium persulphate is dissolved in 50 ~ 100ml distilled water, slowly be added drop-wise in system B, stirring reaction 12h, after reaction terminates, suction filtration, use distilled water, washing with alcohol product colourless to filtrate respectively, 50 ~ 70 DEG C of vacuum-drying 24 ~ 36h, obtain laminar nano composite wave-suction material.
2. preparation method according to claim 1, is characterized in that, described Potassium Persulphate, P
2o
5, potassium permanganate, ammonium persulphate, Fecl
36H
2o, aniline, Witco 1298 Soft Acid, ethylene glycol and the vitriol oil are analytical pure.
3. preparation method according to claim 1, is characterized in that, in step (2), slowly adds KMnO
4time, hierarchy of control temperature, system temperature is no more than 20 DEG C.
4. preparation method according to claim 1, is characterized in that, in step (3), the concentration of described hydrochloric acid is the hydrochloric acid soln of volume ratio 1:10.
5. preparation method according to claim 1, is characterized in that, in step (6), product A accounts for 30 ~ 50% of aniline monomer quality.
6. preparation method according to claims 1 to 4 obtains a kind of nano combined absorbing material.
7. nano combined absorbing material according to claim 6, it is characterized in that, this nano combined absorbing material is laminar nano composite wave-suction material, on graphene sheet layer, load particle diameter is hollow four oxidation three particles of 200-400nm, and polyaniline-coated has the graphene sheet layer surface of hollow nano ferriferrous oxide in load.
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