CN105609305A - Preparation method of Fe<3>O<4>/graphene composite membrane - Google Patents
Preparation method of Fe<3>O<4>/graphene composite membrane Download PDFInfo
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- CN105609305A CN105609305A CN201610034514.8A CN201610034514A CN105609305A CN 105609305 A CN105609305 A CN 105609305A CN 201610034514 A CN201610034514 A CN 201610034514A CN 105609305 A CN105609305 A CN 105609305A
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- H—ELECTRICITY
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- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/22—Heat treatment; Thermal decomposition; Chemical vapour deposition
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- H01F10/00—Thin magnetic films, e.g. of one-domain structure
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- H01F10/08—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
- H01F10/10—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
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- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/30—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates for applying nanostructures, e.g. by molecular beam epitaxy [MBE]
- H01F41/301—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates for applying nanostructures, e.g. by molecular beam epitaxy [MBE] for applying ultrathin or granular layers
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Abstract
The invention relates to a preparation method of an Fe<3>O<4>/graphene composite membrane. In summary, according to the method, by the process of mixing graphene oxide with Fe<3>O<4> nano-particles at a certain ratio to obtain a mixture solution, the Fe<3>O<4>/graphene composite membrane is prepared under drying and low-temperature stepped heating reduction conditions. The product prepared by the method is good in complex condition; the Fe<3>O<4> nano-particles are uniform to disperse; and the composite membrane has ferromagnetic property. The method disclosed by the invention is simple and easy to control; industrial production is facilitated; and the prepared self-supported composite membrane has a broad application prospect in the fields of information, electrons, energy, biology, military industry and the like.
Description
Technical field:
The present invention relates to a kind of Fe3O4The preparation method of/graphene composite film, briefly says, the present invention is by graphene oxide glueBody and Fe3O4After nano particle evenly mixes, then process through super-dry and low temperature ladder heat reduction a kind of Fe preparing3O4/ stoneThe method of China ink alkene composite film material.
Background technology:
Along with the continually developing and applying of nanometer technology, nano material receives the concern of increasing scientific research institution and production firm,The range of application of magnetic nano-particle is more extensive, has contained electromagnetic compatibility technology, magnetic data storage, Xeroxing, magneticResonance image-forming, targeted drug transport, biology sensor, magnetic heat therapy, magnetic separation, immune detection etc. All the time, nanometerThe metallic particles of magnitude, for example Fe, FePt, the alloys such as FeCo are widely used in biomedical sector, and they have very highSaturation magnetization, but there is the problem that oxidation very easily occurs in height toxicity and air; By contrast, metal oxideGrain, for example Fe3O4、γ’-Fe2O3Nontoxic, stable chemical nature, biodegradable, carcinogenic rate be low, be easy to synthetic and be difficult forThe advantages such as oxidation occur, and in the time that particle size is less than 20nm, have superparamagnetic characteristic, broad research is made for NMR imagingShadow agent. But this quasi-metal oxides nano particle magnetic a little less than, and also exist simultaneously and be easy to the phenomenon of reuniting.
In addition, follow the development of communication career and military and commercial radar system, electromagnetic interference problem becomes to be affected electronics and establishesThe matter of utmost importance of standby normal operation, can occur that similar devices suddenly out of controlly can not normally use, in military affairs with the electromagnetic wave of informationThere is the problem of information leakage; And research show, electromagnetic signal also can work the mischief to human body, people's long term exposure is at high energyUnder the electromagnetic wave environment of amount, the normal function of health may be affected, and causes various diseases. For this reason, in the urgent need to researchThe effectively absorbing material of electromagnetic wave absorption. In the past few decades, scientific worker has carried out deeply and has ground widelyStudy carefully, developed such as carbon-based material, ferrite and conducting polymer etc. and have the material of wave absorbtion matter. If during according to researchPhase classification, the materials such as ferrite, graphite, conductive fiber belong to traditional microwave absorbing material, nano material, chirality materialMaterial, conduction high polymer etc. can be attributed to novel wave-absorbing material. Ferrite is the more also more ripe absorbing material of research. ItAdvantage is that absorption efficiency is high, coating is thin, service band is wide in range. But it is large that weak point is relative density, tend to extra increaseThe weight of parts, to such an extent as to affect the overall performance of parts is exactly that high frequency is inhaled wave effect and waited to improve more in addition. Along with science and technologyDevelop rapidly, absorbing material is had higher requirement, formed new research direction, comprising development quality light andThe film of thin thickness, does not affect the absorbing material of aircraft mobility; Development has the complicated rings of adaptation such as high temperature resistant, corrosion-resistantBorder ability, and have higher maintainable and compared with the absorbing material of long life.
Since the mankind successfully prepare Graphene, its excellent physicochemical characteristics has caused that rapidly scientific circles pay close attention to greatly,Researcher has carried out a large amount of explorations to this new material. The hexagon flat film that Graphene is made up of carbon atom, only onlyThere is a carbon atom thickness, there is carrier mobility, electrical conductivity, thermal conductivity and the intensity of superelevation. The physics of Graphene uniquenessChemical property, mechanical property and biological characteristics have determined that this class material has very wide application, comprise electronic information,The energy, environment, medicine and Aero-Space national defence field etc. And as remaining in one of family member's redox grapheneDefect and group not only can improve its impedance matching property, also can make rapidly it be converted to the state of fermi level, also canThe electric dipole relaxation that polarization relaxation and group occur, these are all conducive to scattering and electromagnetic wave absorption, become and have the micro-of potentialityRipple absorbing material. From 2006 so far, scientific worker is to Fe3O4/ graphene composite material has been carried out a large amount of research. OrderThe front conventional preparation method of this class composite comprises water/solvent-thermal method, coprecipitation, and microwave is assisted synthetic method, sol-gal process,Original position self-assembly method, the hydridization of offing normal method etc. Its performance of composite that uses distinct methods to obtain also respectively has quality, more singleMaterial, the performance of composite is improved and improves.
The invention reside in and proposed a kind of simple to operation preparation method who integrates doping and film forming, large by graphene filmSpecific area effectively improve Fe3O4The decentralization of nano particle, under the prerequisite of the high saturation magnetization of maintenance, improvesThe utilization rate of magnetic-particle. Character based on Graphene uniqueness and efficient performance Fe3O4The magnetic behavior of nano particle, comprehensively withThe application aspect of upper proposition, the Fe that the preparation method who adopts the present invention to propose obtains3O4/ graphene composite film material is expected to gather aroundThere are larger application prospect and practical value.
Summary of the invention:
The present invention proposes a kind of Fe3O4The preparation method of/graphene composite film, the outstanding advantages of the method is to choose low temperature ladderThe method of heat reduction is prepared Fe3O4/ graphene composite film material, film thickness, uniformity are easy to control, and cost is low, operationSimply be easy to realize; The method such as high temperature reduction and electronation of the relative graphene oxide of the method, its reduction temperature is low,Low in energy consumption, impurity is introduced few, the redox graphene composite material film that available can be good.
A kind of Fe3O4The preparation method's of/graphene composite film concrete steps are as follows:
1) utilize improved Hummers method, prepare graphene oxide colloid;
2) utilize citric acid as dispersant by Fe3O4Nano particle is scattered in ultra-pure water, and stirs through ultrasonic dispersion and machineryMix and obtain Fe3O4Nanoparticle suspension;
3) utilize graphene oxide colloid by a certain percentage with Fe3O4Nanoparticle suspension is mixed and is obtained through mechanical agitationTo the mixed solution of composite;
4) utilize composite mixed solution to be transferred to low vacuum drying in glass dish, after dry end under the condition of high vacuumAdopt low temperature ladder heat reduction method to obtain graphene composite material film.
In the present invention, step 1) in the preparation of graphene oxide colloid, after sampling is dry, calculate graphene oxide colloid concentration.
In the present invention, step 2) in citric acid and water ratio be 1:19.
In the present invention, step 2) in ultrasonic dispersion, ultrasonic time is 2 minutes, ultrasonic rear mechanical agitation 10 minutes.
In the present invention, step 3) in the mechanical agitation time be 30 minutes.
In the present invention, step 4) in vacuum drying 24 hours at 60 DEG C, vacuum is 0.06MPa; After being dried, vacuumize,Vacuum is brought up to 0.02MPa, persistently overheating to 120 DEG C, constant temperature 12 hours; Then continue to be warming up to 160 DEG C of constant temperature 12 littleTime. In case, be cooled to room temperature, carefully take off the composite membrane in glassware with tweezers, make Fe3O4/ graphene composite film materialMaterial.
A kind of Fe3O4The preparation method of/graphene composite film, is characterized in that, in conjunction with X-ray diffraction, the sub-energy of X-ray photoelectricSpectrum, FFIR test discovery, composite film material is Fe3O4Nano particle and redox graphene are compoundThing; By sem observation, Fe3O4Nano particle is combined with graphene sheet layer well, and particle size is that 20nm arrives50nm, redox graphene film presents typical pleated structure, and film thickness is less than 1 μ m; Adopt superconducting quantum interference device (SQUID)Carry out magnetic behavior sign, find to add Fe3O4The composite material film magnetic of nano particle is good, and saturation magnetization is high.
Brief description of the drawings:
Fig. 1 is graphene oxide in embodiment, redox graphene, Fe3O4The x-ray diffraction pattern of/graphene composite film material.
Fig. 2 is Fe in embodiment3O4The scanning electron microscope diagram of/graphene composite film material surface pattern, multiplication factor is 300Doubly.
Fig. 3 is Fe in embodiment3O4The scanning electron microscope diagram of/graphene composite film material surface pattern, multiplication factor is 5000Doubly.
Fig. 4 is Fe in embodiment3O4The scanning electron microscope diagram of/graphene composite film material surface pattern, multiplication factor is 30000Doubly.
Fig. 5 is Fe in embodiment3O4The scanning electron microscope diagram of/graphene composite film material surface pattern, multiplication factor is 50000Doubly.
Fig. 6 is the x-ray photoelectron spectroscopy figure of redox graphene C1s core level in embodiment.
Fig. 7 is Fe in embodiment3O4The x-ray photoelectron spectroscopy figure of/graphene composite film material C 1s core level.
Fig. 8 is Fe in embodiment3O4The x-ray photoelectron spectroscopy figure of the Fe2p of/graphene composite film material.
Fig. 9 is Fe in embodiment3O4The x-ray photoelectron spectroscopy figure of the O1s core level of/graphene composite film material.
Figure 10 is graphene oxide in embodiment, redox graphene, Fe3O4The Fourier transformation of/graphene composite film material is redExternal spectrum figure.
Figure 11 is pure Fe in embodiment3O4The hysteresis curve figure of nano particle.
Figure 12 is different quality Fe in embodiment3O4The hysteresis curve figure of/graphene composite film material.
Detailed description of the invention is as follows:
Embodiment:
A kind of Fe3O4The preparation method's of/graphene composite film experiment condition and parameter are as follows:
1) in conical flask by 1.5gNaNO3Be dissolved in the 69ml concentrated sulfuric acid and add 2g graphite, stir; Put into ice-water bathIn add KMnO49g, ice-water bath 12 hours; Be warming up to 35 DEG C of constant temperature 1 hour; Then be warming up to 60 DEG C, perseveranceTemperature 18 hours; Be cooled to room temperature, add the dilution of 200ml frozen water evenly; Dropwise add hydrogen peroxide to solution without bubbleGeneration and color become glassy yellow; Leave standstill after 24 hours with 10% salt acid elution centrifugal for 4 times, then wash with water fromThe heart 3 times, obtains graphene oxide colloid; Get the dry graphene oxide that obtains of a certain amount of colloid, calculate graphene oxideColloid concentration, concentration is 19.24mg/ml;
2) 5ml citric acid is joined in 95ml deionized water, stir; Get 800mgFe3O4Nano particle is scattered inIn above-mentioned citric acid solution, by mechanical agitation after ultrasonic solution 2 minutes 10 minutes, obtaining concentration was 8mg/mlFe3O4The suspension of nano particle;
3) press graphene oxide: Fe3O4Nano particle=200mg:160mg, gets graphene oxide colloid 10.4ml, Fe3O4ReceiveRice corpuscles suspension 20ml mixes, and obtains Fe3O4/ graphene oxide mixed solution; Mixed solution is added water rareRelease to volume be 50ml; Mechanical agitation 30 minutes, makes to mix;
4) mixed solution is transferred in glass dish, under the condition that is 0.06MPa in vacuum, is dried 24 hours, obtain Fe3O4/Graphene oxide composite material film; Vacuumize vacuum is increased to 0.02MPa, be then warming up to 120 DEG C, perseveranceTemperature 12 hours; Then continue to be warming up to 160 DEG C of constant temperature 12 hours again, in drying box, be cooled to room temperature and obtain Fe3O4/Graphene composite film material.
The method of lifting according to foregoing invention, can prepare Fe3O4/ graphene composite film material, its feature is as follows:
1) prepared sample is carried out to X-line diffraction analysis, in conjunction with contrast standard diffraction maximum PDF card, can see oxidationGraphene (GO), redox graphene (rGO) and Fe3O4The obvious feature diffraction of/graphene composite film materialPeak position. Tentatively judge that graphene oxide, after 160 DEG C of heating, reduction reaction has occurred, same, graphene oxide and Fe3O4Nano particle mixed solution is through heat treated, and deoxidation process has occurred graphene oxide, has obtained by oxygen reduction fossilChina ink alkene and Fe3O4The molecular composite film material of nanoparticle.
2), in order to obtain the surface appearance feature of composite film material, we have carried out SEM to prepared sample and have dividedAnalyse. Result shows, redox graphene film presents typical pleated structure, Fe3O4Nano particle is regular ballShape, size evenly, particle size be 20nm to 50nm, due to the existence of Graphene, Fe in compound3O4NanoparticleSon is evenly distributed, and demonstrates excellent dispersiveness.
3) adopt x-ray photoelectron spectroscopy to analyze composition and the chemical binding state of sample. Graphene oxide is also carried out to heatAfter the x-ray photoelectron spectroscopy figure deconvolution processing of the C1s of the former sample obtaining, result shows, 284.5eV, 285.8eV,286.9eV, 288.3eV and 289.2eV can be attributed to respectively sp2C＝C、sp3C-C, C-OH, C=O and O=C-OHGroup, 287.8eV is corresponding to C-O-C functional group, and 290.3eV is corresponding to π-π * oscillating satellite peak. The combination of Fe elementEnergy and Fe3O4The combination of 2P3/2 can (708.1eV) consistent, be positioned at the defending for 2P3/2 of peak position of 718.6eVStar peak. Due to Fe in sample3O4The content few (being 1.6mg after compound with redox graphene) of nano particle, thereforeX-ray photoelectron spectroscopy characteristic peak intensity a little less than. Oxygen element in laminated film sample has been carried out to the sub-energy of X-ray photoelectricAnalysis of spectrum, wherein the combination of 532.0eV can be corresponding to C-O-C, and the combination of 533.0eV can be corresponding to H2O，533.8eVCombination can be corresponding to OH-O, and the combination of 531.0eV can be corresponding to O=C.
4) with FTIS, sample is analyzed. Result shows, GO curve is at 3421cm-1Place's correspondenceThe stretching vibration peak of should be-OH of absworption peak, 1739cm-1Place belongs to the stretching vibration peak of C=O key, 1626cm-1Place belongs toThe flexural vibrations absworption peak of C-OH, 1171cm-1With 1044cm-1Place should be the vibration absorption peak of C-O-C. Curve rGOAnd Fe3O4/ rGO, at 1738cm-1With 1734cm-1What place was corresponding is the stretching vibration peak of the two keys of C=O, 1233cm-1With 1245cm-1Place is the stretching vibration peak of C-O. For Fe3O4/ rGO curve, the absworption peak of Fe-O key should be at 580cm-1Near occur, but there is not this absworption peak in sample in test, may with Fe in sample3O4Content is less relevant.
5) use superconducting quantum interference device (SQUID) to carry out magnetometric analysis to sample, respectively to pure Fe3O4Nanoparticle powder and non-homogeneityThe composite film material sample of amount is tested. Result shows, pure Fe3O4The saturation magnetization of nano particle is about96.2emu/g, coercivity size is about 126.3Oe; The saturation magnetization of composite film material becomes 63.7emu/g(1.6mg), 37.0emu/g (1.0mg), 16.2emu/g (0.5mg). Can find out, along with Fe3O4Nano particle containsThe increase of amount, the saturation magnetization of composite membrane presents the trend of increase, but coercivity size does not change substantially, explanationWith the compound Fe that do not change of graphene film3O4The anisotropy field of nano particle, soft magnetic property does not change. ByIn composite film material nano particle be coated by graphene sheet layer and content lower, the inevitable purer Fe of saturation magnetization3O4Nano particle decreases.
Claims (9)
1. a Fe3O4The preparation method of/graphene composite film, is characterized in that, product is by X-ray diffraction, X-rayPhotoelectron spectroscopy, Fourier turn infrared, thin-film material is Fe3O4The compound of/Graphene; Scanning electron microscopySem observation, Fe3O4It is spherical that nano particle is, and be evenly distributed, and size scope is that 20nm is to 50nm; Adopt superconduction amountSub-interferometer carries out magnetism testing to sample, and result shows that composite film material has ferromagnetic property.
2. a Fe3O4The preparation method of/graphene composite film, is characterized in that, this invention comprises the steps:
1) adopt improved Hummers method, prepare graphene oxide colloid;
2) adopt citric acid as dispersant, after ultrasonic dispersion and mechanical agitation, obtain Fe3O4Nanoparticle suspension;
3) by a certain proportion of graphene oxide colloid and Fe3O4Nanoparticle suspension is mixed, and obtains through mechanical agitationThe mixed solution of composite;
4) composite mixed solution be transferred in glassware and carry out vacuum drying treatment, after dry end, adopting low temperatureLadder heat reduction method obtains graphene-based composite film material.
3. a kind of Fe as claimed in claim 23O4The preparation method of/graphene composite film, is characterized in that step 1)Prepare the graphene oxide colloid of certain mass concentration.
4. a kind of Fe as claimed in claim 23O4The preparation method of/graphene composite film, is characterized in that step 2)Select citric acid as Fe3O4The dispersant of nano particle, citric acid: water=1:19.
5. a kind of Fe as claimed in claim 23O4The preparation method of/graphene composite film, is characterized in that step 2)In ultrasonic time in 5 minutes, preferably 2 minutes; The mechanical agitation time is 5 to 15 minutes, preferably 10 minutes.
6. a kind of Fe as claimed in claim 23O4The preparation method of/graphene composite film, is characterized in that step 3)In the mass ratio of material be graphene oxide: Fe3O4Nano particle=200mg:160mg/200mg:80mg/200mg:40mg,Preferably 200mg:160mg.
7. a kind of Fe as claimed in claim 23O4The preparation method of/graphene composite film, is characterized in that step 3)In the mixing time 10 to 60 minutes of mixed solution, preferably 30 minutes.
8. a kind of Fe as claimed in claim 23O4The preparation method of/graphene composite film, is characterized in that step 4)Vacuum drying in vacuum be 0.05MPa to 0.08MPa, preferably 0.06MPa; Baking temperature is 60 DEG C, and the time 24 is littleTime.
9. a kind of Fe as claimed in claim 23O4The preparation method of/graphene composite film, is characterized in that step 4)Dry final vacuum degree is increased to 0.02MPa, is warming up to 120 DEG C of constant temperature 12 hours, is then warming up to 160 DEG C of constant temperature 12 hours,In drying box, be cooled to room temperature.
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Cited By (3)
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| CN106252091A (en) * | 2016-08-30 | 2016-12-21 | 郑州轻工业学院 | A kind of Fe3o4/ graphene composite material and preparation method thereof |
| CN107840324A (en) * | 2017-11-23 | 2018-03-27 | 吉林大学 | A kind of lightweight, Flexible graphene Quito member composite wave-absorbing film and preparation method thereof |
| CN109346848A (en) * | 2018-10-31 | 2019-02-15 | 哈尔滨工业大学 | A kind of SiC- ferrite/carbonaceous material high temperature Wave suction composite material and preparation method thereof |
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| CN103594220A (en) * | 2013-11-21 | 2014-02-19 | 中国科学院长春应用化学研究所 | Functionalized grapheme/superparamagnetic ferroferric oxide nano particle composite material and preparation method thereof |
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| CN104689798A (en) * | 2015-01-12 | 2015-06-10 | 冯云 | Method for preparing composite mesoporous material |
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| CN106252091A (en) * | 2016-08-30 | 2016-12-21 | 郑州轻工业学院 | A kind of Fe3o4/ graphene composite material and preparation method thereof |
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| CN109346848A (en) * | 2018-10-31 | 2019-02-15 | 哈尔滨工业大学 | A kind of SiC- ferrite/carbonaceous material high temperature Wave suction composite material and preparation method thereof |
| CN109346848B (en) * | 2018-10-31 | 2021-03-12 | 哈尔滨工业大学 | SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material and preparation method thereof |
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