CN107010613B - The preparation method of conductive magneto-conductive nano-functional material - Google Patents
The preparation method of conductive magneto-conductive nano-functional material Download PDFInfo
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- CN107010613B CN107010613B CN201710096475.9A CN201710096475A CN107010613B CN 107010613 B CN107010613 B CN 107010613B CN 201710096475 A CN201710096475 A CN 201710096475A CN 107010613 B CN107010613 B CN 107010613B
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- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/49—Oxides or hydroxides of elements of Groups 8, 9,10 or 18 of the Periodic Table; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
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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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C01P2006/00—Physical properties of inorganic compounds
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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- Molecular Biology (AREA)
- Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
A kind of preparation method of conductive magneto-conductive nano-functional material, comprising: substrate is pre-processed；Carbon nano-fiber is grown in substrate surface using chemical vapour deposition technique；The CO of 20cc/min-300cc/min is passed through under the conditions of 400 DEG C -1100 DEG C of temperature2Gas 10min-180min, or it is passed through the plasma gas 1min-30min of 10cc/min-300cc/min under normal temperature conditions, surface-functionalized processing is carried out to carbon nano-fiber；Magnetic nanoparticle dispersion solution is attached to carbon nano-fiber surface.The present invention carries out surface-functionalized processing to carbon nano-fiber using gas, can uniformly, different oxygen-containing, nitrogen-containing functional group are comprehensively introduced on hydrophobic carbon nano-fiber surface, the surface energy for improving carbon nano-fiber, increases the binding site of magnetic nanoparticle.Because carbon nano-fiber is grown directly upon substrate surface, stable structure is not easily to fall off, carbon nano-fiber ordered arrangement, not only has bigger specific surface area and three-dimensional porous structure, but also be easier to separate and recover, and nano particle can be overcome to be easy the shortcomings that reuniting.
Description
Technical field
The present invention relates to magnetic conductive nanocomposites, more particularly to the preparation side of conductive magneto-conductive nano-functional material
Method.
Background technique
In recent years as research hotspot electric magnetoconductive composite material be a kind of structural and functional properties combined double property it is compound
Material, because having magnetic and electric conductivity double grading, sensing technology, nonlinear optical material, electromagnetic shielding, radar absorption,
Magnetic recording etc. has broad application prospects.
The electric magnetoconductive composite material studied at present mainly includes that magnetic particle-conductive polymer composite, carbon system are multiple
Conductive magneto-conductive material, metal-oxide iron composite material etc. are closed, preparation method mainly includes blending method, in-situ synthesized, gathers in situ
Legal, chemical-electrical plating method etc., wherein the preparation condition of in-situ synthesized is harsher, is readily incorporated impurity, reduces product purity；
Chemical-electrical plating method increases the density of material, and the pollution of electroplating effluent is also that cannot be neglected；Blending method is easy to operate, still
Nanoparticle is easy to reunite, it is difficult to be uniformly dispersed, the structure of combination product has uncertainty.
With the development of society, propose increasingly higher demands to electric magnetoconductive composite material, " thickness is thin, light weight,
Frequency range is wide, intensity is high " be novel conductive composite magnetic material Main Trends of The Development.Magnetic nanoparticle is a kind of intelligent
Nano material both has property specific to nano material, such as small-size effect, skin effect, quantum size effect, maroscopic quantity
Sub- tunnel-effect etc., and there is good magnetic conductance tropism, superparamagnetism, quasi-enzyme catalytic characteristic and biocompatibility etc., Ke Yi
Assemble under stationary magnetic field and position, the electromagnetic wave absorption heat production under alternating magnetic field, therefore is led magnetic nanoparticle as conduction
Permeability magnetic material in magnetic composite material is with a wide range of applications.
Carbon nano-fiber (CNFs) refers to the carbon fiber with nanoscale, can be divided into carbon nanotubes i.e. according to its architectural characteristic
Hollow Nano carbon fiber and solid carbon nanofiber are quasi-one-dimensional materials, crystalline orientation degree with higher and are preferably led
Electricity and heating conduction, as the carrier of magnetic nanoparticle, available light weight, thickness is thin, large specific surface area leads
Electric composite magnetic material.However, current carbon nano-fiber materials are mostly powdered, fibre length is shorter and arranges mixed and disorderly nothing
Chapter, as the carrier of magnetic nanoparticle, obtained nanocomposite can be too strong because of the too small adsorptivity of particle, generates easy
Reunite, the disadvantage that dispersion is uneven, also, because of these disadvantages, when being applied to product, needs to add dispersing agent, adhesive
Equal auxiliary agents, not only at high cost, not environmentally, obtained coating is also easy to fall off.
Summary of the invention
Based on this, the object of the present invention is to provide a kind of preparation methods of conductive magneto-conductive nano-functional material.
A kind of preparation method of conductive magneto-conductive nano-functional material, comprising:
Substrate is pre-processed；
Carbon nano-fiber is grown in the substrate surface using chemical vapour deposition technique；
The CO of 20cc/min-300cc/min is passed through under the conditions of 400 DEG C -1100 DEG C of temperature2Gas 10min-
180min, or it is passed through the plasma gas 1min-30min of 10cc/min-300cc/min under normal temperature conditions, to the carbon
Nanofiber carries out surface-functionalized processing；And
Magnetic nanoparticle dispersion solution is attached to carbon nano-fiber surface.
The magnetic nanoparticle is ferroferric oxide nano granules in one of the embodiments,.
The plasma gas is the plasma gas of nitrogen, oxygen or air in one of the embodiments,.
In one of the embodiments, the substrate be plate, it is netted, tubulose, woven fabric-like or Filamentous.
In one of the embodiments, the substrate be selected from carbon fiber, glass fibre, inorganic oxide fibres, pencil-lead,
One of capillary and wire.
The step that magnetic nanoparticle dispersion solution is attached to carbon nano-fiber surface in one of the embodiments,
Suddenly include by surface growth have the carbon nano-fiber the substrate be immersed in 60 DEG C -80 DEG C magnetic nanoparticle dispersion it is molten
In liquid, or including in the carbon nano-fiber surface, doing magnetic nanoparticle dispersion solution spraying in 60 DEG C of -80 DEG C of vacuum
It is dry.
The process in substrate surface growth carbon nano-fiber further includes catalyst solution in one of the embodiments,
Preparation process, the catalyst solution is the sol-gel solution containing catalyst.
More preferably, the catalyst in the catalyst solution is selected from the alloy of iron, nickel, cobalt metal or any combination thereof, institute
The colloidal sol stated in catalyst solution is selected from silica, titanium dioxide, aluminium oxide, silica/alumina complex or dioxy
SiClx/titanium dioxide complex colloidal sol.
The catalyst solution passes through mixing silica precursor, titanium dioxide forerunner in one of the embodiments,
Body or alumina precursor, metal nitrate, surfactant, distilled water, ethyl alcohol and hydrochloric acid and obtain.More preferably, the gold
Genus nitrobacter is nickel nitrate；The surfactant is polyoxyethylene polyoxypropylene copolymer p 123, F127 or chitosan (molecule
Amount is 5-30 ten thousand)；The silica precursor is one of methyl orthosilicate, ethyl orthosilicate, positive silicic acid propyl ester or more
The mixing of kind；The TiO 2 precursor is sour four fourth vinegar by the emperor himself；The alumina precursor is aluminum sulfate or aluminum nitrate.
The present invention carries out surface-functionalized processing to carbon nano-fiber using gas, can uniformly, comprehensively in hydrophobicity
Carbon nano-fiber surface introduce different oxygen-containing, nitrogen-containing functional group, improve carbon nano-fiber surface can, increase magnetic Nano
The binding site of particle, and can prevent from carrying out falling off for carbon nano-fiber caused by surface-functionalized processing using solution.Cause
The carbon nano-fiber of modified by magnetic nanoparticles is grown directly upon substrate surface, and stable structure is not easily to fall off, and carbon nano-fiber has
Sequence arrangement, not only has bigger specific surface area and three-dimensional porous structure, but also be easier to separate and recover, can overcome nano particle
It is easy the shortcomings that reuniting.
By conductive magneto-conductive nano-functional material obtained by the above method, the electric conductivity and magnetism for having carbon nano-fiber concurrently are received
The orientation in electric field, magnetic field may be implemented in the magnetism of rice grain, and not only density is low, and can come by adjusting each technological parameter
The electromagnetic parameter for adjusting material, makes it have higher saturation magnetization, good physical and chemical stability and corrosion resistance
Can, it is expected to be used widely in terms of sound-absorbing inhales wave.In addition, the electromagnetism separate type performance of the composite material be expected to chemistry,
It is with important application prospects in terms of biology, medicine, environmental area.
Detailed description of the invention
Fig. 1 is the schematic diagram for preparing the conductive magneto-conductive nano-functional material in the present invention on different substrates；
Fig. 2 is the scanning electron microscope (SEM) photograph of the carbon fiber before and after growing carbon nano-fiber；
Fig. 3 is magnetic before and after preparing the conductive magneto-conductive nano-functional material in the present invention on fiberglass woven cloth
Property comparing result.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, right with reference to the accompanying drawings and embodiments
The preparation method of conductive magneto-conductive nano-functional material of the invention is further elaborated.It should be appreciated that described herein
Specific examples are only used to explain the present invention, is not intended to limit the present invention.
Referring to Fig. 1, the embodiment of the present invention provides a kind of preparation method of conductive magneto-conductive nano-functional material, comprising:
Substrate 10 is pre-processed；
Carbon nano-fiber 12 is grown on 10 surface of substrate using chemical vapour deposition technique；
The CO of 20cc/min-300cc/min is passed through under the conditions of 400 DEG C -1100 DEG C of temperature2Gas 10min-
180min, or it is passed through the plasma gas 1min-30min of 10cc/min-300cc/min under normal temperature conditions, to carbon nanometer
Fiber 12 carries out surface-functionalized processing；And
Magnetic nanoparticle dispersion solution is attached to 12 surface of carbon nano-fiber.
The substrate used in the above method can be existing base material, can be selected from carbon fiber, glass fibre (it is hollow or
Solid glass fiber), inorganic oxide fibres (alumina fibre, silicon oxide fibre etc.), wire (stainless steel wire, iron wire, tungsten
Silk, titanium silk etc.), pencil-lead, capillary etc., substrate can be plate, netted, tubulose, woven fabric-like or Filamentous, diameter and size
It can be unfettered.
The magnetic nanoparticle 14 can be the magnetic nano particle of any band, such as iron, cobalt, nickel monomer or oxidation
Object magnetic nanoparticle.
The preprocessing process of above-mentioned substrate may include: ultrasonic treatment, heat treatment, acidification etc., to remove substrate table
The organo-functional group in face improves the hydrophily of substrate surface, increases substrate surface to the contact site of hydrophilic compounds.
The above-mentioned process for growing carbon nano-fiber in substrate surface using chemical vapour deposition technique, comprising: containing catalysis
Substrate is impregnated in the catalyst solution of agent and surfactant, is calcined after dry and is removed surfactant, divides catalyst uniformly
Cloth is in the substrate surface；The substrate that surface is evenly distributed with catalyst layer is heated up under inert gas atmosphere, is passed through hydrogen
Reducing catalyst then passes to carbon-source gas (acetylene, methane, ethylene, ethyl alcohol etc.) and carries out chemical vapour deposition reaction, carbon is made to receive
Rice fiber growth is in substrate surface.
In the embodiment of the present invention, using the catalyst solution containing catalyst and surfactant, especially sol-gel
Solution, as doping iron, nickel, cobalt metal or alloy catalyst meso-porous titanium dioxide silica solution, the purpose is to by using mesoporous two
Silica sol makes catalyst be dispersed in substrate surface as catalyst carrier, and obtained carbon nano-fiber, which has, to intersect
The structure of seam arrangement, large specific surface area, stability is good, large amount of adsorption, and can reduce largely using and subtract for catalyst
Few unnecessary post-processing process.
More preferably, the catalyst in the catalyst solution is selected from the alloy of iron, nickel, cobalt metal or any combination thereof, institute
The colloidal sol stated in catalyst solution is selected from silica, titanium dioxide, aluminium oxide, silica/alumina complex or dioxy
SiClx/titanium dioxide complex colloidal sol.
The catalyst solution passes through mixing silica precursor, titanium dioxide forerunner in one of the embodiments,
Body or alumina precursor, metal nitrate, surfactant, distilled water, ethyl alcohol and hydrochloric acid and obtain.More preferably, the gold
Genus nitrobacter is nickel nitrate；The surfactant is polyoxyethylene polyoxypropylene copolymer p 123, F127 or chitosan (molecule
Amount is 5-30 ten thousand)；The silica precursor is one of methyl orthosilicate, ethyl orthosilicate, positive silicic acid propyl ester or more
The mixing of kind；The TiO 2 precursor is sour four fourth vinegar by the emperor himself；The alumina precursor is aluminum sulfate or aluminum nitrate.
Substrate should be immersed in the sufficiently long time in catalyst solution, and catalyst is made to be evenly coated in substrate surface.From catalysis
The substrate is calcined after taking out substrate in agent solution, to completely remove the surfactant as template, keeps catalyst uniform
It is distributed in substrate surface.
It, can be at high temperature using carbon dioxide gas or sharp at normal temperature after to the end of chemical vapour deposition reaction
Surface-functionalized processing is carried out to growth and the carbon nano-fiber of substrate surface with the plasma gas of nitrogen, oxygen, air etc..
In one embodiment, the CO of 20cc/min-300cc/min is passed through under the conditions of 400 DEG C -1100 DEG C of temperature2Gas 10min-
180min introduces oxygen-containing functional group (carboxyl, carbonyl, hydroxyl etc.) on carbon nano-fiber surface.In another embodiment, in room temperature
Under the conditions of be passed through the plasma gas 1min-30min of 10cc/min-300cc/min, carbon nano-fiber is carried out surface-functionalized
Processing, the plasma gas of use can be the plasma gas of nitrogen, oxygen or air, introduce and contain on carbon nano-fiber surface
Oxygen, nitrogenous (amino, pyridine etc.) functional group.When carrying out gas surface treatment, the gas flow being passed through is different, and the processing time is not
Together, it changes in the functional group of carbon nano-fiber Surface Creation.
The present invention carries out surface-functionalized processing to carbon nano-fiber using gas, can uniformly, comprehensively in hydrophobicity
Carbon nano-fiber surface introduce different oxygen-containing, nitrogen-containing functional group, improve carbon nano-fiber surface can, increase magnetic Nano
The binding site of particle, so as to make magnetic nanoparticle be integrated to carbon Nanowire by the modes such as simply impregnating, spraying
Dimension table face, and can prevent from carrying out falling off for carbon nano-fiber caused by surface-functionalized processing using solution, maintain carbon to receive
The primary morphology that rice fiber is grown in substrate surface.
By the modes such as impregnating, spraying, dispersed using the magnetic nanoparticle of different sizes (such as 10nm-500nm) molten
Liquid makes magnetic nanoparticle be integrated to the surface for being grown in the carbon nano-fiber of substrate surface, then preferably at 60 DEG C -80 DEG C
At a temperature of be heat-treated, finally obtain the conductive magneto-conductive nano-functional material in the present invention, heat treatment temperature is unsuitable excessively high, otherwise can
Cause falling off for carbon nano-fiber.In one embodiment, the substrate of carbon nano-fiber can is immersed in magnetic Nano growth
Particle disperses in solution, is heated at 60 DEG C -80 DEG C.In another embodiment, magnetic nanoparticle is divided using spray coating method
It dissipates solution and is coated in carbon nano-fiber surface, and in 60 DEG C of -80 DEG C of vacuum drying.Magnetic nanoparticle is being integrated to carbon nanometer
Should be avoided while fiber surface influences carbon nano-fiber pattern or carbon nano-fiber is made to fall off from substrate surface.
Because carbon nano-fiber is grown directly upon substrate surface, carbon nano-fiber ordered arrangement not only has bigger ratio
Surface area and three-dimensional porous structure, and be easier to separate and recover, nano particle can be overcome to be easy the shortcomings that reuniting.
The conductive magneto-conductive nano-functional material being grown in substrate prepared by the above method, has carbon nano-fiber concurrently
The orientation in electric field, magnetic field may be implemented in the magnetism of electric conductivity and magnetic nanoparticle, and not only density is low, and can pass through tune
Whole each technological parameter adjusts the electromagnetic parameter of material, and it is steady to make it have higher saturation magnetization, good physical chemistry
Qualitative and corrosion resistance is expected to be used widely in terms of sound-absorbing inhales wave.In addition, the electromagnetism separate type of the composite material
It can be expected to important application prospects in terms of chemistry, biology, medicine, environmental area.
Embodiment 1
In the present embodiment using carbon fiber as base material.
Commercial carbon fiber is ultrasonically treated at room temperature using acetone and ethyl alcohol, and is heat-treated 30 minutes at 500 DEG C,
Remove the epoxy resin pulp layer that carbon fiber surface is smeared.Volume will be used at normal temperatures and pressures except the pure carbon fiber (CFs) after slurry
Than being handled 12 hours for the nitric/sulfuric acid mixed solution acid of 1:3, is washed after filtering, is dry, obtaining acidification carbon fiber.
By acidification impregnated carbon fiber 24 hours in the catalyst solution prepared, catalyst is made to be coated uniformly on carbon fiber
Surface.Above-mentioned catalyst solution passes through mixing ethyl orthosilicate (TEOS), nickel nitrate, surfactant Pluronic P123
(EO20PO70EO20,Mav=5800), distilled water, ethyl alcohol and hydrochloric acid form, and mixed proportion is ethyl orthosilicate: surfactant:
H2O: ethyl alcohol: hydrochloric acid: nickel nitrate=1:0.002:9.36:21.4:0.04:0.023.
Substrate is taken out from catalyst solution, is calcined 30 minutes after dry at 450 DEG C, is obtained to surface and be evenly distributed with catalysis
The carbon fiber of oxidant layer.
Above-mentioned carbon fiber is placed in tube furnace, the inert gas (nitrogen of 150cc/min-300cc/min flow is passed through
Gas, argon gas or helium), 600 DEG C are warming up to the heating rate of 5 DEG C/min, the hydrogen 30 for then passing to 20cc/min flow divides
Clock, reducing catalyst are passed through the carbon-source gas acetylene of 30cc/min flow 30 minutes later, and obtaining surface growth has carbon Nanowire
Tie up the carbon fibre composite (CNFs-CFs) of (CNFs).Fig. 2 is the scanning electron microscope (SEM) photograph and growth carbon nano-fiber of pure carbon fiber
The scanning electron microscope (SEM) photograph of carbon fiber later, it can be seen from the figure that carbon nano-fiber homoepitaxial is in carbon fiber surface.Surface is raw
Carbon fiber with carbon nano-fiber has better electric conductivity compared with pure carbon fiber.
After to the end of chemical vapour deposition reaction, hydrogen and carbon-source gas acetylene are closed, 800 DEG C is warming up to, is passed through
The carbon dioxide gas of 166cc/min 60 minutes carries out surface oxidation treatment, closes carbon dioxide gas later, be cooled to room
Temperature.
By FeCl3·6H2O and FeCl2·4H2O and concentrated hydrochloric acid are dissolved in advance through N2In the deionized water of deoxidation；At 80 DEG C
Under water-bath and mechanical agitation, the above solution is added drop-wise to N dropwise2In the alkaline aqueous solution of protection, continue to lead to after dripping
Enter N2, while insulated and stirred；After reaction, iron oxide nano particle obtained is separated using externally-applied magnetic field；It will
Obtained ferroferric oxide magnetic nanoparticle with twice of washes of absolute alcohol, clean twice by again with toluene.
The CNFs-CFs composite material of surface activation process is soaked in ferroferric oxide magnetic nanoparticle dispersion solution
In, magnetic nanoparticle concentration is 50mg/mL, is standing and soaking 12 hours at 60 DEG C, obtains Fe3O4- CNFs-CFs composite material.
Embodiment 2
In the present embodiment, using fiberglass woven cloth as base material.
Acidification fiberglass woven cloth (SFs) in the same manner as in the example 1, and it is uniform on the acidification surface SFs
Catalyst layer grows carbon nano-fiber on fiberglass woven cloth surface using chemical vapour deposition technique.
After to the end of chemical vapour deposition reaction, hydrogen and carbon-source gas are closed, 800 DEG C is warming up to, is passed through 166cc/
The carbon dioxide gas of min 30 minutes carries out surface oxidation treatment, closes carbon dioxide gas later, be cooled to room temperature.
The CNFs-SFs composite material of surface active is soaked in various sizes of magnetic nanoparticle dispersion solution, is stirred
It mixes uniformly, is placed in reaction kettle and seals, reacted, finally obtain Fe3O4- CNFs-SFs composite material.Magnetic nanoparticle
Size Control is in 20-100nm.
Or magnetic nanoparticle dispersion solution is coated uniformly on by CNFs-SFs composite material surface using spray coating method,
80 DEG C are dried in vacuo 24 hours, finally obtain Fe3O4- CNFs-SFs composite material.Attached drawing 3 compared CNFs-SFs composite material
And Fe3O4The magnetism of-CNFs-SFs composite material, it can be seen that the Fe of modifying magnetic nano particle3O4- CNFs-SFs composite wood
Material has apparent magnetic.
Embodiment 3
In the present embodiment, base material is used as using pencil-lead (2H, 0.5mm).
Pencil-lead is handled 10 minutes with the nitric/sulfuric acid mixed solution acid that volume ratio is 1:3 at normal temperatures and pressures, filtering
It washs afterwards, is dry, obtaining acidification pencil-lead.
Pencil-lead is impregnated in the catalyst solution prepared 24 hours, drying is taken out, calcines 30 minutes and goes at 450 DEG C
Except the surfactant as template, catalyst is made to be coated uniformly on acidification pencil wicking surface.Catalyst in the present embodiment
Solution is identical as catalyst solution used in Example 1.Carbon is grown in above-mentioned pencil wicking surface using chemical vapour deposition technique
Nanofiber.
Surface activation process is carried out to carbon nano-fiber in method same as Example 2, and magnetic nanoparticle is divided
Scattered solution is attached to carbon nano-fiber surface.
Embodiment 4
In the present embodiment, base material is used as using capillary (0.5mm).
Capillary is used 10% hydrofluoric acid solution acid handle at normal temperatures and pressures 60 minutes, is washed after taking-up, is dry.
Using syringe, catalyst solution is passed through inside capillary, it is dry, and 30 minutes are calcined at 450 DEG C with removal
As the surfactant of template, catalyst is made to be evenly distributed on the inner surface of capillary.Above-mentioned catalyst solution and implementation
Catalyst solution in example 1 is identical.
Carbon nano-fiber is grown in above-mentioned capillary inner surface using chemical vapour deposition technique.With same as Example 2
Method carries out surface activation process to carbon nano-fiber.
The magnetic nanoparticle of preconfigured 30mg/mL is dispersed into solution, using pipette inside capillary, is made
Magnetic nanoparticle is evenly applied to the inner surface of capillary, is dried in vacuo 24 hours at 80 DEG C, finally obtains hollow Fe3O4-
CNFs- capillary composite material.
Embodiment 5
In the present embodiment, base material is used as using iron wire (0.3mm, 10cm).
Iron wire is calcined 30 minutes at 300 DEG C.Iron wire is impregnated in the catalyst solution prepared 24 hours, is taken out dry
It is dry, surfactant of the removal in 30 minutes as template is calcined at 450 DEG C, and catalyst is made to be coated uniformly on iron wire surface.This
Catalyst solution in embodiment is identical as catalyst solution used in Example 1.
Carbon nano-fiber is grown on above-mentioned iron wire surface using chemical vapour deposition technique.In method same as Example 2
Surface activation process is carried out to carbon nano-fiber.
The CNFs- iron wire composite material of surface activation process is soaked in various sizes of magnetic nanoparticle dispersion solution
In, magnetic nanoparticle concentration is 30mg/mL, and the size Control of magnetic nanoparticle impregnates 12 at 60 DEG C in 20nm-100nm
Hour, obtain Fe3O4- CNFs- iron wire composite material.
Or by above-mentioned magnetic nanoparticle dispersion solution spraying in above-mentioned CNFs- iron wire composite material surface, at 80 DEG C
Vacuum drying 24 hours, finally obtains Fe3O4- CNFs- iron wire composite material.
In the present invention, make carbon nano-fiber homoepitaxial in substrate surface using chemical vapour deposition technique, can be applied to
Different substrates does not limit material, the shapes and sizes of substrate.By controlling the controlled distribution technology of catalyst, effectively control
Growth morphology, length, the thickness of carbon nano-fiber processed, improve the spatial ordering of molecular arrangement, obtain large specific surface area, tool
There are three-dimensional porous road structure, ordering growth in the carbon nano-fiber layer of substrate surface, assigns base conductive ability, it is negative to improve substrate
Carry the effective area of magnetic nanoparticle.
By using meso-porous titanium dioxide silica solution isosol as catalyst carrier, catalyst can be made to be dispersed in base
Bottom surface, and the carbon nano-fiber of herringbone arrangement is obtained, the specific surface area of substrate is further increased, stability is obtained
Good, large amount of adsorption coating layer.
The present invention carries out surface-functionalized processing to carbon nano-fiber using gas, can uniformly, comprehensively in hydrophobicity
Carbon nano-fiber surface introduce different oxygen-containing, nitrogen-containing functional group, improve carbon nano-fiber surface can, increase magnetic Nano
The binding site of particle, and can prevent from carrying out falling off for carbon nano-fiber caused by surface-functionalized processing using solution.Cause
The carbon nano-fiber of modified by magnetic nanoparticles is grown directly upon substrate surface, and stable structure is not easily to fall off, and carbon nano-fiber has
Sequence arrangement, not only has bigger specific surface area and three-dimensional porous structure, but also be easier to separate and recover, can overcome nano particle
It is easy the shortcomings that reuniting.
By conductive magneto-conductive nano-functional material obtained by the above method, the electric conductivity and magnetism for having carbon nano-fiber concurrently are received
The orientation in electric field, magnetic field may be implemented in the magnetism of rice grain, and not only density is low, and can come by adjusting each technological parameter
The electromagnetic parameter for adjusting material, makes it have higher saturation magnetization, good physical and chemical stability and corrosion resistance
Can, it is expected to be used widely in terms of sound-absorbing inhales wave.In addition, the electromagnetism separate type performance of the composite material be expected to chemistry,
It is with important application prospects in terms of biology, medicine, environmental area.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification and accompanying drawing content is applied directly or indirectly in other relevant skills
Art field, is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of conductive magneto-conductive nano-functional material, comprising:
Substrate is pre-processed；
Carbon nano-fiber is grown in the substrate surface using chemical vapour deposition technique；
The CO of 20cc/min-300cc/min is passed through under the conditions of 400 DEG C -1100 DEG C of temperature2Gas 10min-180min, or
It is passed through the plasma gas 1min-30min of 10cc/min-300cc/min under normal temperature conditions, the carbon nano-fiber is carried out
Surface-functionalized processing；And
Magnetic nanoparticle dispersion solution is attached to the carbon nano-fiber surface, including surface growth is had into the carbon nanometer
The substrate of fiber is immersed in magnetic nanoparticle dispersion solution and is heated, or by the magnetic nanoparticle
Dispersion solution spraying is dried in vacuo in the carbon nano-fiber surface,
Wherein, the magnetic nanoparticle partial size is 10nm-500nm.
2. the preparation method of conductive magneto-conductive nano-functional material according to claim 1, which is characterized in that the magnetism is received
Rice grain is ferroferric oxide nano granules.
3. the preparation method of conductive magneto-conductive nano-functional material according to claim 1, which is characterized in that the plasma
Gas is the plasma gas of nitrogen, oxygen or air.
4. the preparation method of conductive magneto-conductive nano-functional material according to claim 1, which is characterized in that the substrate is
It is plate, netted, tubulose, woven fabric-like or Filamentous.
5. the preparation method of conductive magneto-conductive nano-functional material according to claim 1, which is characterized in that the substrate choosing
From one of carbon fiber, glass fibre, inorganic oxide fibres, pencil-lead, capillary and wire.
6. the preparation method of conductive magneto-conductive nano-functional material according to claim 1, which is characterized in that it is described will be magnetic
The step of nano particle dispersion solution is attached to carbon nano-fiber surface includes the institute that surface growth is had the carbon nano-fiber
It states substrate to be immersed in 60 DEG C -80 DEG C of magnetic nanoparticle dispersion solution, or including magnetic nanoparticle is dispersed solution
It is sprayed at the carbon nano-fiber surface, in 60 DEG C of -80 DEG C of vacuum drying.
7. the preparation method of conductive magneto-conductive nano-functional material according to claim 1, which is characterized in that described in substrate
The process of surface growth carbon nano-fiber further includes being handled in advance in the substrate surface using catalyst solution, is urged to be formed
The preparation process of agent layer, the catalyst solution are the sol-gel solutions containing catalyst.
8. the preparation method of conductive magneto-conductive nano-functional material according to claim 7, which is characterized in that the catalyst
Catalyst in solution is selected from the alloy of iron, nickel, cobalt metal or any combination thereof, and the colloidal sol in the catalyst solution is selected from two
Silica, titanium dioxide, aluminium oxide, silica/alumina complex or earth silicon/titanic oxide composite sol.
9. the preparation method of conductive magneto-conductive nano-functional material according to claim 7, which is characterized in that the catalyst
Solution passes through mixing silica precursor, TiO 2 precursor or alumina precursor, metal nitrate, surface-active
Agent, distilled water, ethyl alcohol and hydrochloric acid and obtain.
10. the preparation method of conductive magneto-conductive nano-functional material according to claim 9, which is characterized in that the metal
Nitrate is nickel nitrate；The surfactant is polyoxyethylene polyoxypropylene copolymer p 123, F127 or chitosan；Described two
Siliconoxide precursor is one of methyl orthosilicate, ethyl orthosilicate, positive silicic acid propyl ester or a variety of mixing；The titanium dioxide
Titanium precursors are sour four fourth vinegar by the emperor himself；The alumina precursor is aluminum sulfate or aluminum nitrate.
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| CN110438589A (en) * | 2019-08-15 | 2019-11-12 | 南京林业大学 | A kind of high heat conducting nano carbon fiber production method |
| CN110776658B (en) * | 2019-11-25 | 2022-06-21 | 西安工程大学 | Cotton fiber-based flexible carbon composite film and preparation method thereof |
| CN113550141B (en) * | 2021-07-22 | 2023-02-28 | 山东科技大学 | Method for loading carbon fiber with iron oxide, composite material of porous carbon fiber loaded with iron oxide and application |
| CN113548658A (en) * | 2021-07-22 | 2021-10-26 | 山东科技大学 | Preparation method of carbon nanotube loaded iron oxide, product and application thereof |
| CN115445593B (en) * | 2022-09-08 | 2023-12-01 | 洛阳理工学院 | Photoelectrocatalysis material, electrochemical preparation method and application thereof |
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Inventor after: Meng Longyue Inventor after: Li Donghao Inventor after: Wang Chendi Inventor after: Zou Yilin Inventor before: Meng Longyue Inventor before: Li Donghao Inventor before: Wang Chendi Inventor before: Zou Yilin |