CN107399735A - A kind of preparation method and applications of graphene composite aerogel absorbing material - Google Patents
A kind of preparation method and applications of graphene composite aerogel absorbing material Download PDFInfo
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- CN107399735A CN107399735A CN201710740760.XA CN201710740760A CN107399735A CN 107399735 A CN107399735 A CN 107399735A CN 201710740760 A CN201710740760 A CN 201710740760A CN 107399735 A CN107399735 A CN 107399735A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 67
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 239000004964 aerogel Substances 0.000 title claims abstract description 45
- 239000011358 absorbing material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 229920000642 polymer Polymers 0.000 claims abstract description 41
- 239000002122 magnetic nanoparticle Substances 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
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- 239000000470 constituent Substances 0.000 claims description 6
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- 238000001035 drying Methods 0.000 claims description 5
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
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- 238000000926 separation method Methods 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
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- 229920002125 Sokalan® Polymers 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 3
- 229910000043 hydrogen iodide Inorganic materials 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
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- 150000003233 pyrroles Chemical class 0.000 claims description 3
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- 229920003169 water-soluble polymer Polymers 0.000 claims description 3
- 229910018965 MCl2 Inorganic materials 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 238000005253 cladding Methods 0.000 claims description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 2
- 229930192474 thiophene Natural products 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- 229940126062 Compound A Drugs 0.000 claims 1
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- 239000006096 absorbing agent Substances 0.000 abstract description 2
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 18
- 239000011258 core-shell material Substances 0.000 description 10
- 239000002105 nanoparticle Substances 0.000 description 8
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical class CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 7
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 6
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- 238000004108 freeze drying Methods 0.000 description 4
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- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
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- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 2
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- 230000005670 electromagnetic radiation Effects 0.000 description 2
- 150000002171 ethylene diamines Chemical class 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 125000006160 pyromellitic dianhydride group Chemical group 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical class [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
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- 150000001336 alkenes Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 238000009411 base construction Methods 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 229940113088 dimethylacetamide Drugs 0.000 description 1
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- 125000003916 ethylene diamine group Chemical group 0.000 description 1
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- 239000000835 fiber Substances 0.000 description 1
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- 239000003292 glue Substances 0.000 description 1
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- 239000012535 impurity Substances 0.000 description 1
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- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
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- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
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- 230000035939 shock Effects 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 235000011091 sodium acetates Nutrition 0.000 description 1
- -1 sodium alkyl sulfonate Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0611—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
The invention discloses a kind of preparation method and applications of graphene composite aerogel absorbing material, the material be by reduce graphene oxide, polymer A, coated polymer B the step of magnetic nanoparticle one reduction self-assembling reaction obtain;The absorbing material density is low, and absorption intensity is high, effective Absorber Bandwidth, excellent absorbing property is shown in X-band.In the present invention, graphene content is relatively low, and cost is cheap, and the electromagnetic shielding, Electromgnetic seat protection field in the stealthy of aircraft, radar and communication apparatus have wide application potential and market prospects.
Description
Technical field
The present invention relates to a kind of preparation method and applications of graphene composite aerogel absorbing material, belong to electromagnetic wave suction
Receive field of material preparation.
Technical background
The high speed development of information age 21 century, various electronics, electric equipment emerge in an endless stream, be people's daily life and
Social base construction provides great power-assisted.But current scientific and technological level is limited to, can not with the equipment work of numerous and complicated
Electromagnetic radiation affects people's living environment again with interference problem caused by avoiding.Excessive unordered electromagnetic radiation will be to equipment
Damaged with human body, form Contamination of Electromagnetic Wave.This environmental pollution for being not easy to discover brings a series of social concern, it
Communication is not only influenceed, or even directly threatens the health of the mankind.In electromagnetic protection field, not only civilian sphere is more next for absorbing material
It is more extensive, and also have extremely special critical role in military field.Increasing country falls over each other to put into huge essence
Power conducts a research and has formulated corresponding standard.Therefore, electromagnetic wave shielding or the absorbing material of excellent performance are developed to reduce
The harm of Contamination of Electromagnetic Wave, there is very urgent scientific meaning and application to need.
Traditional absorbing material is mostly simple ferrite, barium titanate, metal fine powder, graphite, carborundum, conductive fiber
Deng they generally all have the drawbacks such as narrow, the higher filling proportion of absorption band and complex process, seriously govern it and apply model
Enclose.So proposed to novel wave-absorbing material " layer is thin, light, frequency range, absorb it is strong " requirement, it is desirable to material possess multiband,
The suction baud point that weatherability is strong, shock resistance, structure-function integration etc. is new.Therefore, the absorbing material of novel integrated excellent performance
Gradually show nanosizing and structure composite development trend.
Graphene makees have excellent electrical loss characteristic and ultralow density, but simple two-dimensional graphene material exists
Bad dispersibility in matrix, and the higher electric conductivity of graphene make it that its dielectric loss is too high, cause interface impedance not
Match somebody with somebody, the more difficult material internal that gos deep into of electromagnetic wave is depleted.In addition, single dielectric loss mechanism causes effective frequency of material
Width is difficult to be expanded.Therefore, the graphene of high quality is in most cases inhaled as a kind of electromagnetic shielding material rather than electromagnetism
Wave material is paid close attention to.
The content of the invention
In view of the above-mentioned problems, the present invention provide a kind of new graphene composite aerogel absorbing material preparation method and
It is applied, and the composite light weight, absorbs strong, bandwidth, and excellent absorbing property is shown in X-band.Not only may be used
To be practiced in a manner of powder, can also foam-filled structural material mode directly apply.
The present invention is achieved through the following technical solutions:
A kind of preparation method of graphene composite aerogel absorbing material, its is specific as follows:
By compound constituent element (at least one of polymer solution A or coated polymer B magnetic nano-particle) by stirring
Mix or the mode of ultrasound is dispersed in graphene oxide aqueous dispersions, then add reducing agent, 80-200 DEG C of confined reaction 2-36h
(preferably 90-180 DEG C of confined reaction 6-12h), block composite aquogel is obtained, the compound airsetting of the graphene is obtained after drying
Glue absorbing material, the material have the network structure of three-dimensional UNICOM;
Wherein, the drying refers to be freeze-dried or is dried in vacuo, and preferably -50 DEG C of freeze-drying, 20Pa dries 48h, very
Sky dries preferred normal-temperature vacuum and dries 48h;
Further, graphene oxide used in the present invention is prepared by improved Hummers methods, referring specifically to text
Offer (C Daniela, D V K Marcano, J M Berlin et al.ACS Nano, 2010,4:Disclosed in 4806-4814)
Preparation method, the concentration of prepared graphene oxide aqueous dispersions is 1.0-10mg/mL, preferably 2-4mg/mL;
Reducing agent used in the present invention is one in hydrazine hydrate, ethylenediamine, ascorbic acid, p-phenylenediamine or hydrogen iodide
Kind;
In the present invention, compound constituent element is at least one of polymer A and coated polymer B magnetic nanoparticle;Institute
It is water-soluble polymer to state polymer A, preferably HPMA, polyamic acid salt, polyvinyl alcohol, polyethylene glycol, phenolic resin,
One kind in polyacrylamide, polyacrylic acid or polyvinylpyrrolidone;The polymer A preferred 5%- of concentration of aqueous solution
20wt%;Wherein, polyamic acid salt is preferably polyamic acid triethylamine salt.
In heretofore described coated polymer B magnetic nanoparticle, polymer B is polyacetylene, polythiophene, polypyrrole
Or one kind in polyaniline;Magnetic nanoparticle is MFe2O4Or carbonyl iron, one kind in M Mn, Fe, Co or Ni;Nano particle
A diameter of 30-600nm;Polymer B thickness of the shell is 40-100nm.
In the present invention, the mass ratio of compound constituent element and graphene oxide is 1-26:1, the matter of reducing agent and graphene oxide
It is 0.3-1 to measure ratio:1.
Further, heretofore described coated polymer B magnetic nanoparticle is obtained by:
Magnetic nanoparticle is prepared using water/solvent thermal process or coprecipitation method, the magnetic nanoparticle is MFe2O4
(M Mn, Fe, Co, Ni) or carbonyl iron:
Concretely comprise the following steps:
(1) by MFe2O4Precursor compound ultrasonic disperse forms uniform solution in a solvent, and water/solvent heat can be selected
Or coprecipitation method prepares magnetic nanoparticle, then product is washed and dried (60 DEG C of vacuum drying);The solvent is distillation
One kind in water, ethanol, methanol or acetone, preferred alcohol and acetone;
Wherein, MFe2O4Precursor compound refers to trichlorine high ferro, ferric acetyl acetonade, MCl2In (M Mn, Co, Ni, Fe)
One or two, water/solvent heat or coprecipitation reaction temperature are 60-220 DEG C, reaction time 6-12h;
Water/the solvent heat or coprecipitation reaction can be according to (Marc Port, Sophie Laurent, Caroline
Robic, et al.Chem.Rev.2008,108,2064-2110) method progress disclosed in document.
(2) magnetic nanoparticle is dispersed in distilled water, adds Fe3+Source (such as FeCl3·6H2O、FeCl3Deng), in magnetic
Property particle surface fully adsorb trigger polymerization Fe3+, after abundant reaction, add surfactant and polymer B monomer, stirring
6-12h is reacted, then by hydromagnetic separation product, is washed successively with distilled water and ethanol, dries, obtains coated polymer B's
Magnetic nanoparticle (i.e. core-shell structure magnetic particle);
Above-mentioned polymer B cladding nano-particle method can also according to (Aihua, Haiqiao Wang, Bin Zhao,
Xiaoyu Li.Synthetic Metals.2003,139,411-415) method progress disclosed in document.
Wherein, polymer B monomer is one kind in pyrroles, thiophene, aniline, acetylene;Polymer B monomer and magnetic Nano
The mass ratio of grain is 0.2-0.8:1, prepare the lauryl sodium sulfate that surfactant used in polymer B is 2.0-6.0wt%
Or the aqueous solution of dodecyl sodium sulfate, control surface activating agent are 1 with graphene oxide mass ratio:0.05-1.5.
The present invention not only make it that conductivity stabilization is suitable horizontal at one using the high porosity of graphene aerogel,
Relatively low electrical conductivity makes dielectric constant be located at a more suitable section, easily reaches when electromagnetic wave incident is to material surface
Impedance matching;The density of material has been greatly reduced it so that material meets the requirement of absorbing material " lightweight ".
Compared with prior art, the present invention has the advantages that:
1. the invention provides a kind of graphene oxide comprising reduction, polymer A and coated polymer B magnetic Nano
The preparation method of the graphene composite aerogel of the three-dimensional net structure of one or more of compositions in particle, this method is simple
A step reduction self-assembling method, experiment condition is gentle, energy-conserving and environment-protective;Foaming structure and function can be achieved by the regulation and control of composition
Integration.
2. coated polymer B magnetic nanoparticle is a kind of magnetic using magnetic particle as core, conducting polymer for shell
Nano-particle, the structure make full use of functional group and the phase interaction of oxygen-containing functional group in graphene oxide layer on polymer chain
With improving magnetic particle because quality is big and be difficult to the problem disperseed in graphene oxide water solution.
It is a kind of ultralight height 3. composite aerogel absorbing material light weight prepared by the present invention, wave absorbing efficiency are high, bandwidth
Strong composite wave-suction material.
4. in graphene composite aerogel prepared by the present invention, the effect of polymer mainly improves stone within the specific limits
The dielectric loss ability of black alkene aeroge and the mechanical strength for improving aeroge, the effect of magnetic particle is effectively to adjust electromagnetism
The position of ripple absworption peak so that composite aerogel shows outstanding absorbing property in X-band.
Brief description of the drawings
Fig. 1 is Fe prepared by embodiment 13O4、Fe3O4/ polypyrrole (Ppy) and graphene composite aerogel (GFP1:3)XRD
Figure.
Fig. 2 is Fe prepared by embodiment 13O4、Fe3O4/ Ppy and graphene composite aerogel (GFP1:3) FTIR figures.
Fig. 3 is core shell structure Fe prepared by embodiment 13O4/ Ppy TEM figures.
Fig. 4 is the SEM figures of graphene composite aerogel absorbing material prepared by embodiment 1.
Fig. 5 is the absorbing property figure of graphene composite aerogel absorbing material prepared by embodiment 1.
Fig. 6 is the SEM figures of graphene composite aerogel absorbing material prepared by example 2.
Fig. 7 is the absorbing property of graphene composite aerogel absorbing material prepared by example 2.
Fig. 8 is the SEM figures of graphene composite aerogel absorbing material prepared by example 3.
Fig. 9 is the absorbing property of graphene composite aerogel absorbing material prepared by example 3.
Embodiment
Inventive concept is described further below in conjunction with specific embodiment, accompanying drawing:
In following examples graphene oxide using Hummers methods prepare, preparation method referring to document (C Daniela,
D V K Marcano,J M Berlin et al.ACS Nano,2010,4:4806-4814), graphene oxide aqueous dispersions
Concentration is controlled in the range of 1.0-10mg/mL.
Embodiment 1
In the present embodiment, Fe is controlled3O4It is 1 with pyrrole monomer mass ratio:0.5802, core shell structure Fe3O4/ Ppy (poly- pyrroles
Cough up) with graphene oxide mass ratio be 3:1, the mass ratio of ethylenediamine and graphene oxide is0.3-1:1;
The specific preparation process of graphene composite aerogel is as follows:
1st, 2.7g FeCl are weighed first3·6H2O is dissolved in 80mL ethylene glycol, while stirring add 7.2g sodium acetates and
2.0g polyethylene glycol 400s, continue stirring until forming uniform clear yellow viscous thing, clear yellow viscous thing is attached to hydrothermal reaction kettle
In, preheating is put into 200 DEG C of baking oven, to maintain this temperature 8h.After question response terminates, natural cooling, hydromagnetic separation, and with steaming
Distilled water and ethanol wash three times successively, and 60 DEG C of vacuum drying obtain product Fe3O4Particle.
2 and then weigh 0.5g Fe3O4Particle is dispersed in the presence of mechanical agitation in 100mL distilled water, is obtained
Fe3O4Moisture suspension;Weigh 9.0g FeCl simultaneously3·6H2O is dissolved in 50mL distilled water, treats FeCl3·6H2O is completely molten
This solution is added to Fe after solution3O4In aqueous dispersions, and 3 hours maintenance reaction time.
3rd, next by the lauryl sodium sulfate of 0.3mL pyrrole monomers (quality is about 0.2901g) and 20mL6.0wt%
The aqueous solution is slowly dropped in the reaction solution of step 2 acquisition, continues to react 12h.After question response terminates, hydromagnetic separation, and with steaming
Three times, by obtained black powder in -50 DEG C, 20Pa is freeze-dried 12 hours washed product, that is, is obtained successively for distilled water and ethanol
Fe3O4- Ppy powder (i.e. core shell structure Fe3O4/ Ppy), it is standby;
Magnetic nanoparticle in the present embodiment is second particle aggregation, and a diameter of 400-600nm (had been embodied
The purpose of invention can be achieved in the range of 30-600nm in Cheng Zhong, the particle diameter of magnetic nanoparticle), Ppy thickness of the shells are 40-
60nm。
4th, 120mg Fe is weighed3O4- Ppy powder is added in 10mL graphene oxides (GO, 4mg/mL) aqueous dispersions, is surpassed
Sound (80MHz) is scattered 1 hour, then injects 25 μ L ethylenediamines (about 0.0225g), and fast sealing is in 60 × 30mm measuring cup
In, and obtain black columnar water gel within 6 hours in 95 DEG C of reactions.Next hydrogel is removed with distilled water immersion soluble miscellaneous
It is aging for one week while matter, be then freeze-dried (- 50 DEG C, 20Pa) 48 hours (in specific implementation process, can also be in normal temperature
Vacuum drying 48h) obtain composite aerogel.
Fig. 1 and Fig. 2 is the XRD and FTIR collection of illustrative plates (GFP1 for the plural gel that the present embodiment step 4 obtains:3 be compound gas
Gel).From the visible Fe of Fig. 1 and Fig. 23O4With Ppy presence, other impurities phases are had no.
Fig. 3 is core shell structure Fe prepared by the present embodiment step 33O4/ Ppy TEM schemes, as can be seen from Figure 3 magnetic particle
It is with Fe3O4For the core shell structure that core, Ppy are shell.
Fig. 4 is the SEM figures that the present embodiment step 4 obtains composite aerogel absorbing material, as seen from Figure 4 the graphene
Composite aerogel has three-dimensional net structure, and magnetic nano-particle is uniformly supported on net wall.
Composite aerogel powder prepared by the present embodiment step 4 and paraffin wax in mass ratio 1:1 mixing, it is pressed into interior
Footpath 3mm, external diameter 7mm annulus, annulus thickness 2-4mm, its suction is tested by vector network analyzer (Agilent, N5244A)
Ripple performance, test frequency 2-18GHz;Fig. 5 is the absorbing property curve of the material, it can be seen that the composite aerogel it is minimum
Reflection loss value is -39.15dB, and at 9.0GHz, absorption frequency range is 4.04GHz (7.28-11.32GHz), corresponding thickness
For 3.5mm.And it is -23.86dB that it corresponds to the minimum reflection loss of 2.5mm thickness wave-absorbers at 13.44GHz, and its is effective
Absorb frequency range and reach 5.12GHz (11.12-16.24GHz).
Reducing agent used in the present embodiment is ethylenediamine, and in a particular application, reducing agent can select hydrazine hydrate, second two
Any one in amine, ascorbic acid, p-phenylenediamine or hydrogen iodide.
In the present embodiment, magnetic nanoparticle Fe3O4, in a particular application, can select with formula
MFe2O4(M Mn, Fe, Co, Ni) or carbonyl iron any nano particle;The polymer B of coated magnetic nano particle
One kind in polyacetylene, polythiophene, polypyrrole or polyaniline can be selected;The quality of polymer B monomer and magnetic nanoparticle
Than for 0.2-0.8:1, prepare the lauryl sodium sulfate or 12 that surfactant used in polymer B is 2.0-6.0wt%
The aqueous solution of sodium alkyl sulfonate, control surface activating agent are 1 with graphene oxide mass ratio:0.05-1.5;Invention can be achieved
Purpose.
Embodiment 2
The present embodiment graphene composite aerogel preparation process is as follows:
1st, 4.31g 4,4 '-diaminodiphenyl ether (ODA) are dissolved in 51g DMAc (dimethyl acetamide), treat that its is complete
4.69g pyromellitic dianhydrides (PMDA) are added after dissolving, 0 DEG C of reaction 5h is kept, above-mentioned solution is then added to distillation at 0 DEG C
Precipitated in water, wash drying.Then sediment is dispersed in water, triethylamine is added dropwise until forming the uniform aqueous solution, configuration
Into solid content be 15% uniform water-soluble polyamic acid triethylamine salt solution (in practical application, polymer solution A concentration range
In 5%-20wt%, the purpose of invention can be achieved).
2nd, compound concentration is that (in concrete application, GO aqueous dispersions concentration can be selected 2mg/mL in the range of 1.0-10mg/mL
Select) graphene oxide aqueous dispersions 20mL, the polyamic acid triethylamine salt solution that 6g steps 1 obtain is added, after stirring 0.5h
Pour into water heating kettle and add ethylenediamine solution (about 25 μ L), 180 DEG C of reaction 12h obtain black columnar water gel, washing leaching
It is one week to steep the time, then obtains graphene composite aerogel by freeze-drying.
The graphene composite aerogel absorbing material SEM pictures that the present embodiment obtains are as shown in Figure 6.
The absorbing property of the material is tested in the same manner as in Example 1, as a result as shown in Figure 7.As seen from Figure 7, with
Thickness increase, minimum reflection loss moves to low frequency direction, and the minimum reflection loss value of composite aerogel is -26.92dB, occurs
In 15.3GHz or so, thickness 2mm, while effective frequency range is 5.47 under the thickness;Reflection loss is less than -10dB frequency range
14.10GHz(3.90-18.0GHz)。
In the present embodiment, polymer A is polyamic acid triethylamine salt, in a particular application, can select HPMA,
The water-soluble polymers such as polyvinyl alcohol, polyethylene glycol, phenolic resin, polyacrylamide, polyacrylic acid or polyvinylpyrrolidone
In one or more.
Embodiment 3
The present embodiment graphene composite aerogel preparation process is as follows:
1、Fe3O4The preparation of nano-particle is the same as the step 1 of embodiment 1.
2nd, 0.5g Fe are weighed3O4Particle is dispersed in distilled water, then weighs 9g FeCl3Continue to dissolve, react 3h.Add
Enter the surfactant sodium dodecyl base sulfonic acid sodium water solution 20mL that mass fraction is 5.8%, 0.4mL aniline monomers are added dropwise dropwise
(its quality about 0.4080g), react 12h.Hydromagnetic separates, and washs drying, obtains Fe3O4(its shell is thick for-PANI core shell structures particle
Spend for 80-100nm).
3rd, 3mg/mL GO aqueous solution 20mL are prepared, and add 20mg ascorbic acid and the above-mentioned core shell structure particles of 120mg,
90 DEG C of reaction 6h obtain graphene composite aquogel, and finally freeze-drying obtains graphene composite aerogel.It is freeze-dried parameter
For -50 DEG C, 20Pa, 48h.
The graphene composite aerogel absorbing material SEM pictures that the present embodiment obtains are as shown in Figure 8.
The phenetic analysis of absorbing property is minimum as thickness increases as a result as shown in figure 9, as seen from Figure 9 with embodiment 1
Reflection loss moves to low frequency direction, and the minimum reflection loss value of composite aerogel is -48.63dB, appears in 11.5GHz or so,
Thickness is 3mm, while effective frequency range is 5.19 under the thickness;Frequency range of the reflection loss less than -10dB is 13.48GHz (4.52-
18.0GHz)。
Embodiment 4
The present embodiment graphene composite aerogel preparation process is as follows:
1st, Fe is prepared using coprecipitation first3O4Nano-particle, by FeCl2·4H2O and FeCl3·6H2O is by material
Amount is than being 1:2 ratio mixed dissolution adds distilled water 200mL, temperature is room temperature in flask.It is added dropwise while strong agitation
0.4mol/L ammonia spirit, until pH=9, then moves into solution in three-necked flask, the timing of high temperature constant temperature water-bath crystallization one
Between.Precipitation particle is centrifuged out, is washed to neutrality, is dried in vacuo, that is, obtains Fe3O4Nano particle, its particle diameter are 30-
50nm, it is standby.
2nd, Fe is weighed3O4Nano particle 0.5g, it is dissolved in 200mL and contains 9g FeCl3·6H2Ultrasound point in the O aqueous solution
Dissipate, and mechanical agitation 3h, then addition 5.8% surfactant sodium dodecyl base sulfonic acid sodium water solution 20mL, it is added dropwise dropwise
0.4mL pyrrole monomers (its quality is about 0.3868g), continue stirring reaction 12h.Hydromagnetic separates, successively with absolute ethyl alcohol and steaming
Distilled water is washed, and vacuum drying, obtains Fe3O4- Ppy core shell structures particle (its thickness of the shell is 60-80nm) is stand-by.
3rd, 4mg/mL GO aqueous solution 20mL, the core shell structure particle that addition 80mg steps 2 obtain, 35 μ L ethylenediamines are prepared
(its quality is 0.0315g) and 2g polyvinyl alcohol, 95 DEG C of confined reaction 6h obtain graphene composite aquogel, and freeze-drying obtains
Graphene composite aerogel macroscopic view block.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, some improvement can also be made under the premise without departing from the principles of the invention, and these improvement also should be regarded as the present invention's
Protection domain.
Claims (9)
1. a kind of preparation method of graphene composite aerogel absorbing material, it is characterised in that comprise the following steps that:
Compound constituent element, reducing agent and graphene oxide aqueous dispersions are mixed after 90-180 DEG C of confined reaction 6-12h, dried,
Obtain graphene composite aerogel absorbing material;Wherein, the reducing agent be hydrazine hydrate, ethylenediamine, ascorbic acid, to benzene two
One kind in amine or hydrogen iodide;
The compound constituent element is at least one of polymer solution A or coated polymer B magnetic nanoparticle;
The polymer A is water-soluble polymer;
Polymer B is one kind in polyacetylene, polythiophene, polypyrrole or polyaniline;
Magnetic nanoparticle is MFe2O4Or carbonyl iron, one kind in M Mn, Fe, Co or Ni.
2. the preparation method of graphene composite aerogel absorbing material according to claim 1, it is characterised in that described poly-
Compound A includes HPMA, polyamic acid salt, polyvinyl alcohol, polyethylene glycol, phenolic resin, polyacrylamide, polyacrylic acid
Or at least one of polyvinylpyrrolidone.
3. the preparation method of graphene composite aerogel absorbing material according to claim 2, it is characterised in that
The mass ratio of the compound constituent element and graphene oxide is 1-26:1, the mass ratio of reducing agent and graphene oxide is 0.3-
1:1。
4. the preparation method of graphene composite aerogel absorbing material according to claim 3, it is characterised in that the bag
Cover what the magnetic nanoparticle of polymer B was obtained by:
(1)By MFe2O4Precursor compound ultrasonic disperse forms uniform solution in a solvent, utilizes water/solvent heat or coprecipitated
Shallow lake method, in 60-220 DEG C, 6-12h is reacted, prepare magnetic nanoparticle, product obtains magnetic Nano after washing and drying
Grain;
The solvent is one kind in distilled water, ethanol, methanol or acetone;
The MFe2O4Precursor compound refers to trichlorine high ferro, ferric acetyl acetonade or MCl2At least one of, M Mn, Co,
One kind in Ni or Fe;
Magnetic nanoparticle is dispersed in distilled water, adds Fe3+Source, surfactant and polymer B monomer, stirring reaction 6-
12h, then by hydromagnetic separation product, washed, dried successively with distilled water and ethanol, that is, obtain coated polymer B magnetic
Nano particle;Wherein, polymer B monomer is one kind in pyrroles, thiophene, aniline or acetylene;Surfactant is 2.0-
6.0wt% lauryl sodium sulfate or the aqueous solution of dodecyl sodium sulfate, surfactant and graphene oxide mass ratio
For 1:0.05-1.5.
5. the preparation method of graphene composite aerogel absorbing material according to claim 4, it is characterised in that the bag
In the magnetic nanoparticle for covering polymer B, the mass ratio of polymer B monomer and magnetic nanoparticle is 0.2-0.8:1.
6. the preparation method of the graphene composite aerogel absorbing material according to one of claim 1-5, it is characterised in that
The concentration of the graphene oxide aqueous dispersions is 1.0-10 mg/mL.
7. the preparation method of the graphene composite aerogel absorbing material according to one of claim 1-5, it is characterised in that
The concentration of the polymer A aqueous solution is 5-20wt%.
8. the preparation method of the graphene composite aerogel absorbing material according to one of claim 1-5, it is characterised in that
In the magnetic nanoparticle of the coated polymer B, magnetic nanoparticle particle diameter is 30-600nm, and polymer B cladding thickness is
40-100nm。
9. if the graphene composite aerogel absorbing material of one of claim 1-5 methods described preparation is in Stealth, electricity
Application in magnetic screen, Electromgnetic seat protection and microwave dark room field.
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