CN109659111A - A kind of graphene-ferrimagnetism composite membrane and preparation method thereof - Google Patents
A kind of graphene-ferrimagnetism composite membrane and preparation method thereof Download PDFInfo
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- CN109659111A CN109659111A CN201910104426.4A CN201910104426A CN109659111A CN 109659111 A CN109659111 A CN 109659111A CN 201910104426 A CN201910104426 A CN 201910104426A CN 109659111 A CN109659111 A CN 109659111A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F10/00—Thin magnetic films, e.g. of one-domain structure
- H01F10/06—Thin magnetic films, e.g. of one-domain structure characterised by the coupling or physical contact with connecting or interacting conductors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F10/00—Thin magnetic films, e.g. of one-domain structure
- 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
- H01F10/18—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being compounds
- H01F10/20—Ferrites
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- H—ELECTRICITY
- 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
- 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
- H01F41/24—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 from liquids
Abstract
The invention discloses a kind of graphene-ferrimagnetism composite membrane and preparation method thereof, the graphene-ferrimagnetism composite membrane have the characteristics that easily prepare, it is controllable, can scale.The graphene-ferrimagnetism composite membrane magnetic field strength can obtain 0.01 to 0.5 tesla according to different precursor concentrations, therefore have potential application value in fields such as medical treatment, astronomical and military affairs.
Description
Technical field
The present invention relates to a kind of graphene-ferrimagnetism composite membranes and preparation method thereof.
Background technique
Ferrite generally refers to iron group and other one or more metallic elements appropriate composite oxides, belongs to half
Conductor, it is utilized as magnetic medium.Nowadays, ferrite is that a kind of important high frequency light current field is widely used
Nonmetal magnetic material all plays key effect in electroacoustic, telecommunications, ammeter, motor, memory cell and microwave component.So
And ferrite is faced with many technical bottlenecks at present, two of them, which are exactly that conductivity is not high, causes magnetic energy lower and crystal adds
Work molding is more difficult.
Graphene is a kind of two-dimensional layer material being made of carbon atom, special with excellent electricity, mechanics, optics
Property.The graphene oxide presoma most widely used as grapheme material has extraordinary processing performance, can pass through various
Fiber, film and block materials are obtained to high molecular common technique process.It is obtained using the processability of graphene oxide
Graphene-ferrimagnetism composite membrane is considered as a kind of novel method for effectively preparing magnetic material.Have at present
Pertinent literature reports the preparation and application of graphene Yu ferritic composite membrane, and still, efficiently quickly extensive obtain has
Graphene-ferrimagnetism composite membrane of sequence assembling is still that current industry is difficult to realize.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of graphene-ferrimagnetism composite membrane and
Preparation method.
The invention is realized by the following technical scheme: a kind of graphene-ferrimagnetism composite membrane, in the interlayer of graphene
In-situ preparation ferrite crystal, ferrite crystal are uniformly distributed between graphene layer, and graphene forms conductive network, two layers of phase
There is pi-pi bond effect between adjacent graphene layer；The crystallite dimension of ferrite crystal is in 1-200nm, wherein ferrite crystal
Mass content be 3~87%.
A kind of preparation method of graphene-ferrimagnetism composite membrane, comprising the following steps:
(1) with concentration for 10~20mg g-1Graphene oxide dispersion carries out knifing, 0.5~6mm of film thickness.
(2) obtained graphene oxide membrane is transferred in coagulating bath, infiltration 0.5 hour or more.The coagulating bath is chlorine
Change the hydrochloric acid solution of iron, the mass fraction of iron chloride is 0.1wt%~10wt%.
(3) graphene oxide membrane for being crosslinked iron ion is in the water heating kettle equipped with the ammonium hydroxide that concentration is 25~28wt%
Hydro-thermal process is carried out, the temperature of hydro-thermal process is 120 to 200 DEG C, and the time is 0.5~24 hour.
(4) it is transferred in aerobic environment after drying after deionization washing, 300 ° of 0.5~1h of calcining obtain graphene-iron oxygen
Body composite magnetic coating.
Compared with the prior art, the present invention has the following beneficial effects:
(1) present invention provides flexible and electron transport ability, the iron oxide being entrained between graphene layer using graphene
Crystal layer contributes higher magnetism, thus constitutes two-arch tunnel, thus constitutes two-arch tunnel, and the preferable electronics of graphene passes
Movement Capabilities promote the electronics flowing of ferrite crystal, further improve magnetic field performance.
(2) graphene that wet spinning assembles-iron oxide film electrode has good order, so that composite membrane has more
Good electric conductivity and self-supporting ability.
(3) between graphene layer the more traditional iron oxide of the preparation method of in-situ preparation ferric oxide nano particles first prepare after with
The method of graphene mechanical blending is more simple and convenient, and is suitable for large-scale production.
Detailed description of the invention
Fig. 1 is the ferric trichloride hydrochloric acid solution of 0.1% mass fraction as under coagulating bath, finally obtained graphene-iron
The cross-sectional scans electron microscope of oxysome composite magnetic coating and flexible display diagram.
Fig. 2 is the ferric trichloride hydrochloric acid solution of 1% mass fraction as under coagulating bath, finally obtained graphene-iron oxygen
The cross-sectional scans electron microscope of body composite magnetic coating and flexible display diagram.
Fig. 3 is the ferric trichloride hydrochloric acid solution of 10% mass fraction as under coagulating bath, finally obtained graphene-iron oxygen
The cross-sectional scans electron microscope of body composite magnetic coating.
Fig. 4 is graphene-ferrimagnetism composite membrane magnetic force display diagram.
Specific embodiment
The present invention uses ferric ion as crosslinking agent and source of iron.Graphene oxide dispersion is scraped with debita spissitudo
Film is transferred to containing a large amount of ion (Fe3+, Cl-Deng) coagulating bath, graphene oxide sheet crosslinking, formed aquagel membrane.By the water-setting
Glue film is dried after hydro-thermal process in the water-bath of ammonium hydroxide, is reduced to the black film of electric conductivity, is collected by rewinding machine.
Above-mentioned graphene-ferrimagnetism composite membrane have the characteristics that it is height-oriented, replace layer by layer, crystalline size it is controllable,
Magnetic material application be can be used as in each related fields, significantly reduce material resistance while guaranteeing high magnetic field intensity.Base
In features above, graphene of the invention-ferrimagnetism composite membrane as magnetic material significantly improve script ferrite compared with
Low magnetic energy density, while certain flexibility is had both, the electricity being hopeful under lightweight electronic component and specific condition
It is applied on machine.
The XRD of product the result shows that, which has 002 peak, shows wherein to contain a large amount of pi-pi bond
Effect, this is the building of conductive network, the promotion of electron transport ability is laid a good foundation.The preferable electron transport ability of graphene
The electronics flowing for promoting ferrite crystal, further improves magnetic field performance.
Fig. 1 illustrates the good magnetism that above-mentioned material has as self-supported membrane.By graphene-ferrite magnetic of 5mg
Property composite membrane be placed in the position from iron prop about 3.5cm and can occur strong magnetic fields, be detached from ground.
The present invention is specifically described below by embodiment, the present embodiment is served only for doing further the present invention
It is bright, it should not be understood as limiting the scope of the invention, those skilled in the art makes one according to the content of foregoing invention
A little nonessential changes and adjustment, all belong to the scope of protection of the present invention.
Embodiment 1:
It (1) is 10mgg with concentration-1Graphene oxide dispersion carry out knifing, film thickness 0.5mm.
(2) obtained graphene oxide membrane is impregnated into 0.5h in coagulating bath, coagulating bath is the trichlorine of mass fraction 0.1%
Change molysite acid solution, concentration of hydrochloric acid 0.1mol L-1。
(3) the full cross-linked graphene oxide membrane of iron ion is immersed in the water heating kettle of the ammonium hydroxide equipped with 28wt% concentration
Hydro-thermal process is carried out, the temperature of hydro-thermal process is 120 DEG C, and the time is 0.5 hour.
(4) it is transferred in aerobic environment after drying after deionization washing, 300 ° of 0.5~1h of calcining obtain graphene-iron oxygen
Body composite magnetic coating.
As shown in Fig. 2, obtained graphene-ferrimagnetism composite membrane has apparent stratiform knot by above step
Structure, ferrite content only have mass fraction 3.3%, and crystalline size is about 1-2nm or so.Graphene-iron under this embodiment
Oxysome composite magnetic coating only has the magnetic field strength of about 0.01 tesla, but it can significantly bend with good flexibility
Without rupturing, conductivity has also reached 1500S m-1。
Embodiment 2:
It (1) is 12mgg with concentration-1Graphene oxide dispersion carry out knifing, film thickness 1mm.
(2) obtained graphene oxide membrane is impregnated into 1h in coagulating bath, coagulating bath is the tri-chlorination of mass fraction 0.5%
Molysite acid solution, concentration of hydrochloric acid 0.5mol L-1。
(3) the full cross-linked graphene oxide membrane of iron ion is immersed in the water heating kettle of the ammonium hydroxide equipped with 28wt% concentration
Hydro-thermal process is carried out, the temperature of hydro-thermal process is 150 DEG C, and the time is 1 hour.
(4) graphene-ferrimagnetism composite membrane is dried to obtain after deionization washing.
By above step, obtained graphene-ferrimagnetism composite membrane has apparent layer structure, and ferrite contains
Amount only has mass fraction 16.4%, and crystalline size is about 2-5nm or so.Graphene-ferrimagnetism under this embodiment is multiple
The magnetic field strength that film only has about 0.03 tesla is closed, but it is with good flexibility, can significantly bent without rupturing, electricity
Conductance has also reached 1300S m-1。
Embodiment 3:
(1) with concentration for 15mg g-1Graphene oxide dispersion carry out knifing, film thickness 2mm.
(2) obtained graphene oxide membrane is impregnated into 2h in coagulating bath, coagulating bath is the ferric trichloride of mass fraction 1%
Hydrochloric acid solution, concentration of hydrochloric acid 1mol L-1。
(3) the full cross-linked graphene oxide membrane of iron ion is immersed in the water heating kettle of the ammonium hydroxide equipped with 28wt% concentration
Hydro-thermal process is carried out, the temperature of hydro-thermal process is 180 DEG C, and the time is 2 hours.
(4) it is transferred in aerobic environment after drying after deionization washing, 300 ° of 0.5~1h of calcining obtain graphene-iron oxygen
Body composite magnetic coating.
As shown in figure 3, obtained graphene-ferrimagnetism composite membrane has apparent stratiform knot by above step
Structure, ferrite content reach mass fraction 29.7%, and crystalline size is about 5-10nm or so.Graphene-under this embodiment
There is ferrimagnetism composite membrane the magnetic field strength of about 0.11 tesla can bend by a small margin with certain flexibility
Without rupturing, conductivity has also reached 1000S m-1。
Embodiment 4:
It (1) is 20mgg with concentration-1Graphene oxide dispersion carry out knifing, film thickness 6mm.
(2) obtained graphene oxide membrane is impregnated into 5h in coagulating bath, coagulating bath is the ferric trichloride of mass fraction 5%
Hydrochloric acid solution, concentration of hydrochloric acid 5mol L-1。
(3) the full cross-linked graphene oxide membrane of iron ion is immersed in the water heating kettle of the ammonium hydroxide equipped with 28wt% concentration
Hydro-thermal process is carried out, the temperature of hydro-thermal process is 200 DEG C, and the time is 18 hours.
(4) it is transferred in aerobic environment after drying after deionization washing, 300 ° of 0.5~1h of calcining obtain graphene-iron oxygen
Body composite magnetic coating.
By above step, obtained graphene-ferrimagnetism composite membrane has apparent layer structure, and ferrite contains
Amount reaches mass fraction 64.3%, and crystalline size is about 10-50nm or so.Graphene-ferrimagnetism under this embodiment
Composite membrane reaches the magnetic field strength of 0.31 tesla of Liao Yue, but its flexibility is bad, can only carry out miniature deformation without rupturing electricity
Conductance is only 600S m-1。
Embodiment 5:
It (1) is 15mgg with concentration-1Graphene oxide dispersion carry out knifing, film thickness 2mm.
(2) obtained graphene oxide membrane is impregnated into 4h in coagulating bath, coagulating bath is the tri-chlorination of mass fraction 10%
Molysite acid solution, concentration of hydrochloric acid 1mol L-1。
(3) the full cross-linked graphene oxide membrane of iron ion is immersed in the water heating kettle of the ammonium hydroxide equipped with 25wt% concentration
Hydro-thermal process is carried out, the temperature of hydro-thermal process is 180 DEG C, and the time is 2 hours.
(4) it is transferred in aerobic environment after drying after deionization washing, 300 ° of 0.5~1h of calcining obtain graphene-iron oxygen
Body composite magnetic coating.
As shown in figure 4, due in coagulating bath ferric trichloride concentration of hydrochloric acid it is higher so that obtained graphene-ferrite magnetic
Property composite membrane there is apparent layer structure, ferrite content reached mass fraction 86.5%, and crystalline size is about 100-
200nm or so.The magnetic field strength of graphene-ferrimagnetism composite membrane about 0.5 tesla under this embodiment, but its is several
There is no flexibility, can not bend strongly, conductivity is only 200S m-1。
Claims (5)
1. a kind of graphene-ferrimagnetism composite membrane preparation method, which comprises the following steps:
(1) with concentration for 10~20mgg-1Graphene oxide dispersion carries out knifing, 0.5~6mm of film thickness.
(2) obtained graphene oxide membrane is transferred in coagulating bath, infiltration 0.5 hour or more.The coagulating bath is iron chloride
Hydrochloric acid solution, the mass fraction of iron chloride is 0.1wt%~10wt%.
(3) graphene oxide membrane for being crosslinked iron ion carries out in the water heating kettle equipped with the ammonium hydroxide that concentration is 25~28wt%
Hydro-thermal process, the temperature of hydro-thermal process are 120 to 200 DEG C, and the time is 0.5~24 hour.
(4) it is transferred in aerobic environment after drying after deionization washing, 300 ° of 0.5~1h of calcining obtain graphene-ferrite magnetic
Property composite membrane.
2. the method according to claim 1, wherein the concentration of hydrochloric acid is less than in the coagulating bath of the step 2
5mol L-1。
3. the method according to claim 1, wherein in the coagulating bath of the step 2, the mass fraction of iron chloride
For 0.5wt% or less.
4. a kind of graphene that method as described in claim 1 is prepared-ferrimagnetism composite membrane.
5. composite membrane according to claim 2, which is characterized in that ferrite crystal is uniformly distributed between graphene layer,
Graphene forms conductive network, has pi-pi bond effect between two layers of adjacent graphene layer；The crystallite dimension of ferrite crystal is
In 1-200nm, wherein the mass content of ferrite crystal is 3~87%.
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