CN107010613A - 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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- CN107010613A CN107010613A CN201710096475.9A CN201710096475A CN107010613A CN 107010613 A CN107010613 A CN 107010613A CN 201710096475 A CN201710096475 A CN 201710096475A CN 107010613 A CN107010613 A CN 107010613A
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Classifications
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- H—ELECTRICITY
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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
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
-
- 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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- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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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- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- 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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- 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
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- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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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
- C01P2006/40—Electric properties
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- C—CHEMISTRY; METALLURGY
- 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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- Engineering & Computer Science (AREA)
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- Manufacturing & Machinery (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Nanotechnology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Biomedical Technology (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
A kind of preparation method of conductive magneto-conductive nano-functional material, including：Substrate is pre-processed；Using chemical vapour deposition technique carbon nano-fiber is grown in substrate surface；20cc/min 300cc/min CO is passed through under 400 DEG C 1100 DEG C of temperature conditionss2Gas 10min 180min, or 10cc/min 300cc/min plasma gas 1min 30min are passed through under normal temperature condition, surface-functionalized processing is carried out to carbon nano-fiber；Magnetic nanoparticle dispersion soln is attached to carbon nano-fiber surface.The present invention carries out surface-functionalized processing using gas to carbon nano-fiber, uniformly, comprehensively different oxygen-containing, nitrogen-containing functional groups can be introduced on hydrophobic carbon nano-fiber surface, the surface energy of carbon nano-fiber is improved, increases the binding site of magnetic nanoparticle.Because carbon nano-fiber is grown directly upon substrate surface, Stability Analysis of Structures is difficult for drop-off, carbon nano-fiber ordered arrangement, not only with bigger specific surface area and three-dimensional porous structure, and is more easy to separation and recovery, the shortcoming that nano particle can be overcome easily to reunite.
Description
Technical field
The present invention relates to the preparation side of magnetic conductive nano composite material, more particularly to conductive magneto-conductive nano-functional material
Method.
Background technology
The electric magnetoconductive composite material for turning into study hotspot in recent years is that a kind of double property of structural and functional properties combined are combined
Material, because with magnetic and electric conductivity double grading, sensing technology, nonlinear optical material, electromagnetic shielding, radar absorption,
Had broad application prospects in terms of magnetic recording.
The electric magnetoconductive composite material studied at present mainly includes magnetic particle-conductive polymer composite, carbon system and answered
Conductive magneto-conductive material, metal-oxide iron composite material etc. are closed, preparation method is mainly poly- including blending method, in-situ synthesized, original position
Legal, chemical-electrical plating method etc., the preparation condition of wherein 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 what be can not be ignored；Blending method is simple to operate, still
Nano-particle is easily reunited, it is difficult to be uniformly dispersed, and the structure of combination product has uncertainty.
With the development of society, propose higher and higher requirement to electric magnetoconductive composite material, " thickness of thin, light weight,
Frequency range is wide, intensity is high " be novel conductive composite magnetic material Main Trends of The Development.Magnetic nanoparticle is that a class is intelligent
Nano material, both with property specific to nano material, such as small-size effect, skin effect, quantum size effect, maroscopic quantity
Sub- tunnel-effect etc., has good magnetic conductance tropism, superparamagnetism, quasi-enzyme catalytic characteristic and biocompatibility etc., Ke Yi again
Assemble under stationary magnetic field and positioning, the electromagnetic wave absorption heat production under alternating magnetic field, therefore led magnetic nanoparticle as conduction
Permeability magnetic material in magnetic composite is with a wide range of applications.
Carbon nano-fiber (CNFs) refers to the carbon fiber with nanoscale, can be divided into CNT i.e. according to its architectural characteristic
Hollow Nano carbon fiber and solid carbon nanofiber, are quasi-one-dimensional materials, are led with higher crystalline orientation degree and preferably
Electricity and heat conductivility, as the carrier of magnetic nanoparticle, can obtain light weight, thickness of thin, specific surface area leading greatly
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 nano composite material can be too strong because of the too small adsorptivity of particle, produces easy
Reunite, disperse uneven shortcoming, also, because these shortcomings, it is necessary to add dispersant, adhesive when being applied to product
Deng auxiliary agent, not only cost is high, not environmentally, and obtained coating is also easy to fall off.
The content of the invention
Based on this, it is an object of the invention to provide a kind of preparation method of conductive magneto-conductive nano-functional material.
A kind of preparation method of conductive magneto-conductive nano-functional material, including：
Substrate is pre-processed；
Using chemical vapour deposition technique carbon nano-fiber is grown in the substrate surface；
20cc/min-300cc/min CO is passed through under 400 DEG C -1100 DEG C of temperature conditionss2Gas 10min-
180min, or 10cc/min-300cc/min plasma gas 1min-30min is passed through under normal temperature condition, to the carbon
Nanofiber carries out surface-functionalized processing；And
Magnetic nanoparticle dispersion soln is attached to carbon nano-fiber surface.
In one of the embodiments, 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, the substrate be tabular, it is netted, tubulose, woven fabric-like or thread.
In one of the embodiments, the substrate be selected from carbon fiber, glass fibre, inorganic oxide fibres, pencil-lead,
One kind in capillary and wire.
In one of the embodiments, the step that magnetic nanoparticle dispersion soln is attached to carbon nano-fiber surface
The rapid magnetic nanoparticle for including the substrate that superficial growth has the carbon nano-fiber being immersed in 60 DEG C -80 DEG C disperses molten
It is dry in 60 DEG C of -80 DEG C of vacuum in liquid, or including magnetic nanoparticle dispersion soln is sprayed at into the carbon nano-fiber surface
It is dry.
In one of the embodiments, the process for growing carbon nano-fiber in substrate surface also includes catalyst solution
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 its any combination, institute
The colloidal sol stated in catalyst solution is selected from silica, titanium dioxide, aluminum oxide, silica/alumina complex or dioxy
SiClx/titanium dioxide complex colloidal sol.
In one of the embodiments, the catalyst solution is by mixing silica precursor, titanium dioxide forerunner
Body or alumina precursor, metal nitrate, surfactant, distilled water, ethanol 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
Measure as 5-30 ten thousand)；The silica precursor is one kind or many in methyl silicate, tetraethyl orthosilicate, positive silicic acid propyl ester
The mixing planted；The TiO 2 precursor is sour four fourths vinegar by the emperor himself；The alumina precursor is aluminum sulfate or aluminum nitrate.
The present invention using gas to the surface-functionalized processing of carbon nano-fiber progress, can uniformly, comprehensively in hydrophobicity
Carbon nano-fiber surface introduce different oxygen-containing, nitrogen-containing functional groups, improve carbon nano-fiber surface can, increase magnetic Nano
The binding site of particle, and can prevent from carrying out coming 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 Stability Analysis of Structures is difficult for drop-off, and carbon nano-fiber has
Sequence is arranged, not only with bigger specific surface area and three-dimensional porous structure, and is more easy to separation and recovery, can overcome nano particle
The shortcoming easily reunited.
The conductive magneto-conductive nano-functional material obtained by the above method, the electric conductivity and magnetic for having carbon nano-fiber concurrently is received
The magnetic of rice grain, it is possible to achieve the orientation in electric field, magnetic field, not only density is low, and can by adjust each technological parameter come
The electromagnetic parameter of material is adjusted, higher saturation magnetization, good physical and chemical stability and corrosion resistance is made it have
Can, it is expected to be used widely in terms of sound-absorbing inhales ripple.In addition, the electromagnetism separate type performance of the composite be expected to chemistry,
There is important application prospect in terms of biological, medicine, environmental area.
Brief description of the drawings
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 the magnetic before and after the conductive magneto-conductive nano-functional material in the present invention is prepared on fiberglass woven cloth
Property comparing result.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with drawings and Examples pair
The preparation method of the conductive magneto-conductive nano-functional material of the present invention is further elaborated.It should be appreciated that described herein
Specific embodiment only to explain the present invention, be 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, including：
Substrate 10 is pre-processed；
Using chemical vapour deposition technique in the superficial growth carbon nano-fiber 12 of substrate 10；
20cc/min-300cc/min CO is passed through under 400 DEG C -1100 DEG C of temperature conditionss2Gas 10min-
180min, or 10cc/min-300cc/min plasma gas 1min-30min is passed through under normal temperature condition, to carbon nanometer
Fiber 12 carries out surface-functionalized processing；And
Magnetic nanoparticle dispersion soln is attached to the surface of carbon nano-fiber 12.
The substrate used in the above method can be existing base material, may 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 tabular, netted, tubulose, woven fabric-like or thread, its diameter and size
Can be with unfettered.
The magnetic nanoparticle 14 can be the magnetic nano particle of any band, such as iron, cobalt, nickel monomer or oxidation
Thing magnetic nanoparticle.
The preprocessing process of above-mentioned substrate can include：Ultrasonically treated, heat treatment, acidification etc., to remove substrate table
The organo-functional group in face, improves the hydrophily of substrate surface, contact site of the increase substrate surface to hydrophilic compounds.
Above-mentioned utilization chemical vapour deposition technique grows the process of carbon nano-fiber in substrate surface, including：Containing catalysis
Substrate is impregnated in the catalyst solution of agent and surfactant, calcining removes surfactant after drying, and catalyst is uniformly divided
Cloth is in the substrate surface；The substrate that surface is evenly distributed with into catalyst layer heats up under inert gas atmosphere, is passed through hydrogen
Reducing catalyst, then passes to carbon-source gas (acetylene, methane, ethene, ethanol etc.) and carries out chemical vapour deposition reaction, carbon is received
Rice fiber growth is in substrate surface.
In the embodiment of the present invention, using the catalyst solution containing catalyst and surfactant, particularly sol-gel
Solution, such as doping iron, nickel, the meso-porous titanium dioxide Ludox of cobalt metal or alloy catalyst, 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, specific surface area is big, stability is good, adsorbance is big, 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 its any combination, institute
The colloidal sol stated in catalyst solution is selected from silica, titanium dioxide, aluminum oxide, silica/alumina complex or dioxy
SiClx/titanium dioxide complex colloidal sol.
In one of the embodiments, the catalyst solution is by mixing silica precursor, titanium dioxide forerunner
Body or alumina precursor, metal nitrate, surfactant, distilled water, ethanol 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
Measure as 5-30 ten thousand)；The silica precursor is one kind or many in methyl silicate, tetraethyl orthosilicate, positive silicic acid propyl ester
The mixing planted；The TiO 2 precursor is sour four fourths 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, catalyst is evenly coated in substrate surface.From catalysis
The substrate is calcined after taking out substrate in agent solution, to remove the surfactant as template completely, makes catalyst uniform
It is distributed in substrate surface.
, can be at high temperature using carbon dioxide or sharp at normal temperatures after treating that chemical vapour deposition reaction terminates
Surface-functionalized processing is carried out to the carbon nano-fiber grown with substrate surface with the plasma gas of nitrogen, oxygen, air etc..
In one embodiment, 20cc/min-300cc/min CO is passed through under 400 DEG C -1100 DEG C of temperature conditionss2Gas 10min-
180min, oxygen-containing functional group (carboxyl, carbonyl, hydroxyl etc.) is introduced on carbon nano-fiber surface.In another embodiment, in normal temperature
Under the conditions of be passed through 10cc/min-300cc/min plasma gas 1min-30min, 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 processing time is not
Together, changed in the functional group of carbon nano-fiber Surface Creation.
The present invention using gas to the surface-functionalized processing of carbon nano-fiber progress, can uniformly, comprehensively in hydrophobicity
Carbon nano-fiber surface introduce different oxygen-containing, nitrogen-containing functional groups, improve carbon nano-fiber surface can, increase magnetic Nano
The binding site of particle, so as to by the mode such as simply impregnating, spraying, make magnetic nanoparticle be attached to carbon Nanowire
Dimension table face, and can prevent from carrying out coming off for carbon nano-fiber caused by surface-functionalized processing using solution, maintain carbon to receive
The primary morphology that rice fiber grows in substrate surface.
By modes such as dipping, sprayings, the magnetic nanoparticle using different sizes (such as 10nm-500nm) disperses molten
Liquid, makes magnetic nanoparticle be attached to the surface for the carbon nano-fiber for being grown in substrate surface, then preferably at 60 DEG C -80 DEG C
At a temperature of be heat-treated, finally give the conductive magneto-conductive nano-functional material in the present invention, heat treatment temperature is unsuitable too high, otherwise can
Cause coming off for carbon nano-fiber.In one embodiment, the substrate that growth has carbon nano-fiber can be immersed in magnetic Nano
In particle dispersion soln, heated at 60 DEG C -80 DEG C.In another embodiment, magnetic nanoparticle is divided using spraying process
Scattered solution is coated in carbon nano-fiber surface, and in 60 DEG C of -80 DEG C of vacuum drying.Magnetic nanoparticle is being attached to carbon nanometer
Influence carbon nano-fiber pattern should be avoided while fiber surface or carbon nano-fiber is come off from substrate surface.
Because carbon nano-fiber is grown directly upon substrate surface, carbon nano-fiber ordered arrangement, not only with bigger ratio
Surface area and three-dimensional porous structure, and it is more easy to separation and recovery, the shortcoming that nano particle can be overcome easily to reunite.
The conductive magneto-conductive nano-functional material being grown in substrate prepared by the above method, has carbon nano-fiber concurrently
The magnetic of electric conductivity and magnetic nanoparticle, it is possible to achieve the orientation in electric field, magnetic field, not only density is low, and can be by adjusting
Whole each technological parameter adjusts the electromagnetic parameter of material, makes it have higher saturation magnetization, good physical chemistry steady
Qualitative and decay resistance, is expected to be used widely in terms of sound-absorbing inhales ripple.In addition, the electromagnetism separate type of the composite
It can be expected to that there is important application prospect in terms of chemistry, biological, medicine, environmental area.
Embodiment 1
Base material is used as using carbon fiber in the present embodiment.
It is ultrasonically treated to the progress of commercial carbon fiber at room temperature using acetone and ethanol, and be 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 for 1:3 nitric/sulfuric acid mixed solution acid treatment 12 hours, washs after filtering, dries, and obtains being acidified carbon fiber.
By acidifying impregnated carbon fiber 24 hours in the catalyst solution prepared, catalyst is set to be coated uniformly on carbon fiber
Surface.Above-mentioned catalyst solution is by mixing tetraethyl orthosilicate (TEOS), nickel nitrate, surfactant Pluronic P123
(EO20PO70EO20,Mav=5800), distilled water, ethanol and hydrochloric acid form, mixed proportion is tetraethyl orthosilicate:Surfactant:
H2O:Ethanol: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 at 450 DEG C after drying, is obtained to surface and be evenly distributed with catalysis
The carbon fiber of oxidant layer.
Above-mentioned carbon fiber is positioned in tube furnace, the inert gas (nitrogen of 150cc/min-300cc/min flows is passed through
Gas, argon gas or helium), 600 DEG C are warming up to 5 DEG C/min heating rate, 30 points of the hydrogen of 20cc/min flows is then passed to
Clock, reducing catalyst is passed through the carbon-source gas acetylene of 30cc/min flows 30 minutes afterwards, and obtaining superficial 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 afterwards, it can be seen that carbon nano-fiber homoepitaxial is in carbon fiber surface.Give birth on surface
Carbon fiber with carbon nano-fiber is compared with pure carbon fiber, with more preferable electric conductivity.
After treating that chemical vapour deposition reaction terminates, hydrogen and carbon-source gas acetylene are closed, 800 DEG C is warming up to, is passed through
166cc/min carbon dioxide 60 minutes, carries out surface oxidation treatment, carbon dioxide is closed afterwards, room is cooled to
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, above solution is added drop-wise to N dropwise2Continue logical in the alkaline aqueous solution of protection, after dripping
Enter N2, while insulated and stirred；After reaction terminates, obtained iron oxide nano particle is separated using externally-applied magnetic field；Will
Twice of washes of absolute alcohol of obtained ferroferric oxide magnetic nanoparticle, again with toluene is cleaned twice.
The CNFs-CFs composites of surface activation process are soaked in ferroferric oxide magnetic nanoparticle dispersion soln
In, magnetic nanoparticle concentration is 50mg/mL, is standing and soak at 60 DEG C 12 hours, obtains Fe3O4- CNFs-CFs composites.
Embodiment 2
In the present embodiment, base material is used as using fiberglass woven cloth.
Acidification fiberglass woven cloth (SFs), and in the same manner as in the example 1 uniform on acidifying SFs surfaces
Catalyst layer, using chemical vapour deposition technique in fiberglass woven cloth superficial growth carbon nano-fiber.
After treating that chemical vapour deposition reaction terminates, hydrogen and carbon-source gas are closed, 800 DEG C is warming up to, is passed through 166cc/
Min carbon dioxide 30 minutes, carries out surface oxidation treatment, carbon dioxide is closed afterwards, room temperature is cooled to.
The CNFs-SFs composites of surface active are soaked in various sizes of magnetic nanoparticle dispersion soln, stirred
Mix uniform, be placed in reactor and seal, reacted, finally give Fe3O4- CNFs-SFs composites.Magnetic nanoparticle
Size Control is in 20-100nm.
Or magnetic nanoparticle dispersion soln is coated uniformly on by CNFs-SFs composite material surfaces using spraying process,
80 DEG C are dried in vacuo 24 hours, finally give Fe3O4- CNFs-SFs composites.Accompanying drawing 3 compared for CNFs-SFs composites
And Fe3O4The magnetic of-CNFs-SFs composites, it can be seen that the Fe of modifying magnetic nano particle3O4- CNFs-SFs composite woods
Material has obvious magnetic.
Embodiment 3
In the present embodiment, base material is used as using pencil-lead (2H, 0.5mm).
It is at normal temperatures and pressures 1 with volume ratio by pencil-lead:3 nitric/sulfuric acid mixed solution acid treatment 10 minutes, filtering
Wash, dry afterwards, obtain being acidified pencil-lead.
Pencil-lead is impregnated in the catalyst solution prepared 24 hours, takes out drying, gone within 30 minutes in 450 DEG C of calcinings
Except the surfactant as template, catalyst is set to be coated uniformly on acidifying pencil wicking surface.Catalyst in the present embodiment
Solution is identical with the catalyst solution used in embodiment 1.Using chemical vapour deposition technique in above-mentioned pencil-lead superficial growth carbon
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).
By capillary at normal temperatures and pressures with 10% hydrofluoric acid solution acid treatment 60 minutes, wash, dry after taking-up.
Using syringe, catalyst solution is passed through inside capillary, dried, and 30 minutes are calcined with removal at 450 DEG C
As the surfactant of template, catalyst is set to be evenly distributed on the inner surface of capillary.Above-mentioned catalyst solution is with implementing
Catalyst solution in example 1 is identical.
Using chemical vapour deposition technique carbon nano-fiber is grown in above-mentioned capillary inner surface.With same as Example 2
Method carries out surface activation process to carbon nano-fiber.
By the magnetic nanoparticle dispersion soln for the 30mg/mL being pre-configured with, using pipette inside capillary, make
Magnetic nanoparticle is evenly applied to the inner surface of capillary, is dried in vacuo 24 hours at 80 DEG C, finally gives hollow Fe3O4-
CNFs- capillary composites.
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, takes out dry
Surfactant that is dry, being removed in 450 DEG C of calcinings as template for 30 minutes, makes catalyst be coated uniformly on iron wire surface.This
Catalyst solution in embodiment is identical with the catalyst solution used in embodiment 1.
Using chemical vapour deposition technique in above-mentioned iron wire superficial growth carbon nano-fiber.In method same as Example 2
Surface activation process is carried out to carbon nano-fiber.
The CNFs- iron wire composites of surface activation process are soaked in various sizes of magnetic nanoparticle dispersion soln
In, magnetic nanoparticle concentration is 30mg/mL, and the size Control of magnetic nanoparticle soaks 12 in 20nm-100nm at 60 DEG C
Hour, obtain Fe3O4- CNFs- iron wire composites.
Or above-mentioned magnetic nanoparticle dispersion soln is sprayed at above-mentioned CNFs- iron wires composite material surface, at 80 DEG C
Vacuum drying 24 hours, finally gives Fe3O4- CNFs- iron wire composites.
In the present invention, make carbon nano-fiber homoepitaxial in substrate surface using chemical vapour deposition technique, can be applied to
Different substrates, material, the shapes and sizes of substrate are not limited.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 that specific surface area is big, tool
There is the carbon nano-fiber layer of three-dimensional porous road structure, ordering growth in substrate surface, assign base conductive ability, improve substrate and bear
Carry the effective area of magnetic nanoparticle.
By using meso-porous titanium dioxide Ludox isosol as catalyst carrier, catalyst can be made to be dispersed in base
Basal surface, and the carbon nano-fiber of herringbone arrangement is obtained, the specific surface area of substrate is further improved, stability is obtained
The big coating layer of good, adsorbance.
The present invention using gas to the surface-functionalized processing of carbon nano-fiber progress, can uniformly, comprehensively in hydrophobicity
Carbon nano-fiber surface introduce different oxygen-containing, nitrogen-containing functional groups, improve carbon nano-fiber surface can, increase magnetic Nano
The binding site of particle, and can prevent from carrying out coming 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 Stability Analysis of Structures is difficult for drop-off, and carbon nano-fiber has
Sequence is arranged, not only with bigger specific surface area and three-dimensional porous structure, and is more easy to separation and recovery, can overcome nano particle
The shortcoming easily reunited.
The conductive magneto-conductive nano-functional material obtained by the above method, the electric conductivity and magnetic for having carbon nano-fiber concurrently is received
The magnetic of rice grain, it is possible to achieve the orientation in electric field, magnetic field, not only density is low, and can by adjust each technological parameter come
The electromagnetic parameter of material is adjusted, higher saturation magnetization, good physical and chemical stability and corrosion resistance is made it have
Can, it is expected to be used widely in terms of sound-absorbing inhales ripple.In addition, the electromagnetism separate type performance of the composite be expected to chemistry,
There is important application prospect in terms of biological, medicine, environmental area.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
Equivalent structure or equivalent flow conversion that bright specification and accompanying drawing content are made, or directly or indirectly it is used in other related 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, including：
Substrate is pre-processed；
Using chemical vapour deposition technique carbon nano-fiber is grown in the substrate surface；
20cc/min-300cc/min CO is passed through under 400 DEG C -1100 DEG C of temperature conditionss2Gas 10min-180min, or
10cc/min-300cc/min plasma gas 1min-30min is passed through under normal temperature condition, the carbon nano-fiber is carried out
Surface-functionalized processing；And
Magnetic nanoparticle dispersion soln is attached to the carbon nano-fiber surface.
2. the preparation method of conductive magneto-conductive nano-functional material according to claim 1, it is characterised in that the magnetic is received
Rice grain is ferroferric oxide nano granules.
3. the preparation method of conductive magneto-conductive nano-functional material according to claim 1, it is characterised 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, it is characterised in that the substrate is
It is tabular, netted, tubulose, woven fabric-like or thread.
5. the preparation method of conductive magneto-conductive nano-functional material according to claim 1, it is characterised in that the substrate choosing
One kind from 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, it is characterised in that described by magnetic
The step of nano particle dispersion soln is attached to carbon nano-fiber surface is including superficial growth to be had to the institute of the carbon nano-fiber
Substrate is stated to be immersed in 60 DEG C -80 DEG C of magnetic nanoparticle dispersion soln, or including by magnetic nanoparticle dispersion soln
The carbon nano-fiber surface is sprayed at, 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, it is characterised in that described in substrate
The process of superficial growth carbon nano-fiber also includes handling using catalyst solution in the substrate surface in advance, is urged so as to be formed
The preparation process of agent layer, the catalyst solution is the sol-gel solution containing catalyst.
8. the preparation method of conductive magneto-conductive nano-functional material according to claim 7, it is characterised in that the catalyst
The colloidal sol that catalyst in solution is selected from the alloy of iron, nickel, cobalt metal or its any combination, the catalyst solution is selected from two
Silica, titanium dioxide, aluminum 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, it is characterised in that the catalyst
Solution is by mixing silica precursor, TiO 2 precursor or alumina precursor, metal nitrate, surface-active
Agent, distilled water, ethanol and hydrochloric acid and obtain.
10. the preparation method of conductive magneto-conductive nano-functional material according to claim 9, it is characterised 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 or more mixing in methyl silicate, tetraethyl orthosilicate, positive silicic acid propyl ester；The titanium dioxide
Titanium precursors are sour four fourths vinegar by the emperor himself；The alumina precursor is aluminum sulfate or aluminum nitrate.
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| 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 |
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| CN115445593A (en) * | 2022-09-08 | 2022-12-09 | 洛阳理工学院 | Photoelectrocatalysis material, electrochemical preparation method and application thereof |
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| 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 |
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| 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 |
| CN115445593A (en) * | 2022-09-08 | 2022-12-09 | 洛阳理工学院 | Photoelectrocatalysis material, electrochemical preparation method 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 |
| CN116031023A (en) * | 2023-03-21 | 2023-04-28 | 中化学科学技术研究有限公司 | Metal nanowire, extraction method thereof and transparent conductive film |
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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 |