CN109659111B - Graphene-ferrite magnetic composite film and preparation method thereof - Google Patents

Graphene-ferrite magnetic composite film and preparation method thereof Download PDF

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CN109659111B
CN109659111B CN201910104426.4A CN201910104426A CN109659111B CN 109659111 B CN109659111 B CN 109659111B CN 201910104426 A CN201910104426 A CN 201910104426A CN 109659111 B CN109659111 B CN 109659111B
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graphene
magnetic composite
ferrite
composite film
ferrite magnetic
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CN109659111A (en
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高超
黄铁骑
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Zhejiang University ZJU
Hangzhou Gaoxi Technology Co Ltd
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Zhejiang University ZJU
Hangzhou Gaoxi Technology Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F10/00Thin magnetic films, e.g. of one-domain structure
    • H01F10/06Thin magnetic films, e.g. of one-domain structure characterised by the coupling or physical contact with connecting or interacting conductors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/0018Mixed oxides or hydroxides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F10/00Thin magnetic films, e.g. of one-domain structure
    • H01F10/08Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
    • H01F10/10Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
    • H01F10/18Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being compounds
    • H01F10/20Ferrites
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/14Apparatus 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
    • H01F41/24Apparatus 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

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  • Chemical & Material Sciences (AREA)
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  • Nanotechnology (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Organic Chemistry (AREA)
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  • Inorganic Chemistry (AREA)
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  • Compounds Of Iron (AREA)

Abstract

The invention discloses a graphene-ferrite magnetic composite film and a preparation method thereof. The magnetic field intensity of the graphene-ferrite magnetic composite film can be 0.01 to 0.5 Tesla according to different precursor concentrations, so that the graphene-ferrite magnetic composite film has potential application value in the fields of medical treatment, astronomy, military and the like.

Description

Graphene-ferrite magnetic composite film and preparation method thereof
Technical Field
The invention relates to a graphene-ferrite magnetic composite film and a preparation method thereof.
Background
Ferrite generally refers to a compound oxide of iron group and other one or more suitable metal elements, and belongs to a semiconductor, and is used as a magnetic medium. Nowadays, ferrite is an important nonmetal magnetic material with wide application in the fields of high frequency and weak current, and plays a key role in electroacoustic, telecommunication, ammeter, motor, memory element and microwave element. However, ferrite currently faces many technical bottlenecks, two of which are low magnetic energy due to low electrical conductivity and difficult crystal processing.
Graphene is a two-dimensional layered material composed of carbon atoms, and has excellent electrical, mechanical, and optical properties. Graphene oxide, as the most widely used precursor of graphene materials, has very good processability and can be used to obtain fiber, film and bulk materials through various common technical procedures on macromolecules. Obtaining a graphene-ferrite magnetic composite film using the processability of graphene oxide is considered to be a novel and effective method for preparing a magnetic material. At present, relevant documents report the preparation and application of the graphene and ferrite composite film, but the efficient and rapid large-scale acquisition of the orderly-assembled graphene-ferrite magnetic composite film is still difficult to realize in the industry at present.
Disclosure of Invention
The invention aims to provide a graphene-ferrite magnetic composite film and a preparation method thereof, aiming at the defects of the prior art.
The invention is realized by the following technical scheme: a graphene-ferrite magnetic composite film is characterized in that ferrite crystals are generated in situ between graphene layers, the ferrite crystals are uniformly distributed between the graphene layers, the graphene forms a conductive network, and a pi-pi bond effect is formed between two adjacent graphene layers; the ferrite crystal has a grain size of 1-200nm, wherein the ferrite crystal has a mass content of 3-87%.
A preparation method of a graphene-ferrite magnetic composite film comprises the following steps:
(1) the concentration is 10-20 mg g-1And scraping the film of the graphene oxide dispersion liquid to a thickness of 0.5-6 mm.
(2) The obtained graphene oxide film was transferred to a coagulation bath and immersed for 0.5 hour or more. The coagulating bath is hydrochloric acid solution of ferric chloride, and the mass fraction of the ferric chloride is 0.1-10 wt%.
(3) Carrying out hydrothermal treatment on the graphene oxide membrane subjected to iron ion crosslinking in a hydrothermal kettle filled with ammonia water with the concentration of 25-28 wt%, wherein the temperature of the hydrothermal treatment is 120-200 ℃, and the time is 0.5-24 hours.
(4) And (3) washing with deionized water, drying, transferring to an aerobic environment, and calcining at 300 ℃ for 0.5-1 h to obtain the graphene-ferrite magnetic composite membrane.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, the graphene is utilized to provide flexibility and electron transmission capability, and the iron oxide crystal layer sandwiched between the graphene layers contributes to higher magnetism, so that a bicontinuous phase is formed, and the bicontinuous phase is formed.
(2) The graphene-iron oxide membrane electrode obtained by wet spinning assembly has good orderliness, so that the composite membrane has better conductivity and self-supporting capability.
(3) Compared with the traditional method of preparing the iron oxide and then mechanically blending the iron oxide with the graphene, the preparation method of generating the iron oxide nano particles in situ between the graphene layers is simpler and more convenient, and is suitable for large-scale production.
Drawings
Fig. 1 is a cross-sectional scanning electron microscope image and a flexibility display image of a finally obtained graphene-ferrite magnetic composite film with 0.1% mass fraction ferric trichloride hydrochloric acid solution as a coagulating bath.
Fig. 2 is a cross-sectional scanning electron microscope image and a flexibility display image of the finally obtained graphene-ferrite magnetic composite film with a 1% mass fraction ferric trichloride hydrochloric acid solution as a coagulating bath.
FIG. 3 is a scanning electron microscope image of the cross section of the finally obtained graphene-ferrite magnetic composite film with 10% by mass of ferric trichloride hydrochloric acid solution as a coagulating bath.
Fig. 4 is a magnetic force display diagram of the graphene-ferrite magnetic composite film.
Detailed Description
The present invention uses ferric ions as a cross-linking agent and an iron source. The graphene oxide dispersion liquid is scraped at a proper concentration and is transferred to a solution containing a large amount of ions (Fe)3+,Cl-Etc.) the graphene oxide sheets are crosslinked to form a hydrogel film. The hydrogel film is subjected to hydrothermal treatment in a water bath of ammonia water and then dried, and is reduced into a conductive black film, and the conductive black film is collected by a rewinderAnd (4) collecting.
The graphene-ferrite magnetic composite film has the characteristics of high orientation, layer-by-layer alternation and controllable crystal size, can be used as a magnetic material to be applied to various related fields, and obviously reduces the resistance of the material while ensuring high magnetic field intensity. Based on the characteristics, the graphene-ferrite magnetic composite film provided by the invention is used as a magnetic material, so that the original ferrite lower magnetic energy density is obviously improved, and meanwhile, the graphene-ferrite magnetic composite film has certain flexibility, and is hopeful to be applied to light electronic components and motors under special conditions.
The XRD result of the product shows that the graphene-iron oxide film has a 002 peak, which shows that the graphene-iron oxide film contains a large amount of pi-pi bond effect, and the basis is laid for the construction of a conductive network and the improvement of electron transmission capability. The better electron transport ability of the graphene promotes the electron flow of the ferrite crystal, and further improves the magnetic field performance.
Fig. 1 shows the good magnetic properties of the above materials as self-supporting films. The 5mg graphene-ferrite magnetic composite film is placed at a position about 3.5cm away from an iron column to generate a strong magnetic field effect, and is separated from the ground.
The present invention is described in detail by the following embodiments, which are only used for further illustration of the present invention and should not be construed as limiting the scope of the present invention, and the non-essential changes and modifications made by the person skilled in the art according to the above disclosure are all within the scope of the present invention.
Example 1:
(1) at a concentration of 10mgg-1The graphene oxide dispersion liquid (2) was subjected to film scraping to obtain a film thickness of 0.5 mm.
(2) Soaking the obtained graphene oxide film in a coagulating bath for 0.5h, wherein the coagulating bath is a ferric trichloride hydrochloric acid solution with the mass fraction of 0.1%, and the concentration of hydrochloric acid is 0.1mol L-1
(3) And (3) soaking the graphene oxide membrane fully crosslinked by iron ions in a hydrothermal kettle filled with 28wt% ammonia water for hydrothermal treatment at the temperature of 120 ℃ for 0.5 hour.
(4) And (3) washing with deionized water, drying, transferring to an aerobic environment, and calcining at 300 ℃ for 0.5-1 h to obtain the graphene-ferrite magnetic composite membrane.
As shown in FIG. 2, the obtained graphene-ferrite magnetic composite film has an obvious layered structure, the ferrite content is only 3.3% by mass, and the crystal size is about 1-2 nm. The graphene-ferrite magnetic composite film in the embodiment has only the magnetic field intensity of about 0.01 Tesla, but has good flexibility, can be bent greatly without cracking, and has the conductivity of 1500S m-1
Example 2:
(1) at a concentration of 12mgg-1The graphene oxide dispersion liquid (2) was subjected to film scraping, and the film thickness was 1 mm.
(2) Soaking the obtained graphene oxide film in a coagulating bath for 1h, wherein the coagulating bath is a ferric trichloride hydrochloric acid solution with the mass fraction of 0.5%, and the hydrochloric acid concentration is 0.5mol L-1
(3) And (3) soaking the graphene oxide membrane fully crosslinked by iron ions in a hydrothermal kettle filled with 28wt% ammonia water for hydrothermal treatment at the temperature of 150 ℃ for 1 hour.
(4) And washing with deionized water and drying to obtain the graphene-ferrite magnetic composite membrane.
Through the steps, the obtained graphene-ferrite magnetic composite film has an obvious layered structure, the ferrite content is only 16.4% by mass, and the crystal size is about 2-5 nm. The graphene-ferrite magnetic composite film in the embodiment has only the magnetic field intensity of about 0.03 Tesla, but has good flexibility, can be bent greatly without cracking, and has the conductivity of 1300S m-1
Example 3:
(1) at a concentration of 15mg g-1The graphene oxide dispersion liquid (2) was subjected to film scraping, and the film thickness was 2 mm.
(2) Soaking the obtained graphene oxide film in a coagulating bath for 2h, wherein the coagulating bath is a ferric trichloride hydrochloric acid solution with the mass fraction of 1%, and the hydrochloric acid concentration is 1mol L-1
(3) And (3) soaking the graphene oxide membrane fully crosslinked by iron ions in a hydrothermal kettle filled with 28wt% ammonia water for hydrothermal treatment at 180 ℃ for 2 hours.
(4) And (3) washing with deionized water, drying, transferring to an aerobic environment, and calcining at 300 ℃ for 0.5-1 h to obtain the graphene-ferrite magnetic composite membrane.
As shown in FIG. 3, the obtained graphene-ferrite magnetic composite film has an obvious layered structure, the ferrite content reaches 29.7% by mass, and the crystal size is about 5-10 nm. The graphene-ferrite magnetic composite film under the embodiment has the magnetic field intensity of about 0.11 Tesla, has certain flexibility, can be bent in a small range without cracking, and has the conductivity of 1000S m-1
Example 4:
(1) at a concentration of 20mgg-1The graphene oxide dispersion liquid (2) was subjected to film scraping, and the film thickness was 6 mm.
(2) Soaking the obtained graphene oxide film in a coagulating bath for 5h, wherein the coagulating bath is a ferric trichloride hydrochloric acid solution with the mass fraction of 5%, and the hydrochloric acid concentration is 5mol L-1
(3) And (3) soaking the graphene oxide membrane fully crosslinked by iron ions in a hydrothermal kettle filled with 28wt% ammonia water for hydrothermal treatment, wherein the temperature of the hydrothermal treatment is 200 ℃, and the time is 18 hours.
(4) And (3) washing with deionized water, drying, transferring to an aerobic environment, and calcining at 300 ℃ for 0.5-1 h to obtain the graphene-ferrite magnetic composite membrane.
Through the steps, the obtained graphene-ferrite magnetic composite film has an obvious layered structure, the ferrite content reaches 64.3% by mass, and the crystal size is about 10-50 nm. The graphene-ferrite magnetic composite film in this example achieves a magnetic field strength of about 0.31 tesla, but is not flexible enough to undergo only a small deformation without breaking the conductivity of only 600S m-1
Example 5:
(1) at a concentration of 15mgg-1The graphene oxide dispersion liquid (2) was subjected to film scraping, and the film thickness was 2 mm.
(2) Soaking the obtained graphene oxide film in a coagulating bath for 4h, wherein the coagulating bath is a ferric trichloride hydrochloric acid solution with the mass fraction of 10%, and the hydrochloric acid concentration is 1mol L-1
(3) And (3) soaking the graphene oxide membrane fully crosslinked by iron ions in a hydrothermal kettle filled with 25 wt% ammonia water for hydrothermal treatment at 180 ℃ for 2 hours.
(4) And (3) washing with deionized water, drying, transferring to an aerobic environment, and calcining at 300 ℃ for 0.5-1 h to obtain the graphene-ferrite magnetic composite membrane.
As shown in FIG. 4, the concentration of ferric chloride and hydrochloric acid in the coagulation bath is high, so that the obtained graphene-ferrite magnetic composite film has an obvious layered structure, the ferrite content reaches 86.5% by mass, and the crystal size is about 100-200 nm. The graphene-ferrite magnetic composite film in this example has a magnetic field strength of about 0.5 tesla, but has little flexibility and cannot be strongly bent, and the electric conductivity is only 200S m-1

Claims (4)

1. A preparation method of a graphene-ferrite magnetic composite film is characterized by comprising the following steps:
(1) the concentration is 10-20 mg g-1Scraping the graphene oxide dispersion liquid to form a film with the thickness of 0.5-6 mm;
(2) transferring the obtained graphene oxide film into a coagulating bath, and soaking for more than 0.5 hours; the coagulating bath is hydrochloric acid solution of ferric chloride, and the concentration of hydrochloric acid is less than 5mol L-1The mass fraction of the ferric chloride is 0.1-10 wt%;
(3) carrying out hydrothermal treatment on the graphene oxide membrane subjected to iron ion crosslinking in a hydrothermal kettle filled with ammonia water with the concentration of 25-28 wt%, wherein the temperature of the hydrothermal treatment is 120-200 ℃, and the time is 0.5-24 hours;
(4) and (3) washing with deionized water, drying, transferring to an aerobic environment, and calcining at 300 ℃ for 0.5-1 h to obtain the graphene-ferrite magnetic composite membrane.
2. The method according to claim 1, wherein the mass fraction of ferric chloride in the coagulation bath of step (2) is 0.5wt% or less.
3. A graphene-ferrite magnetic composite film prepared by the method of claim 1.
4. The composite film of claim 3, wherein ferrite crystals are uniformly distributed between graphene layers, graphene forms a conductive network, and a pi-pi bonding effect is formed between two adjacent graphene layers; the ferrite crystal has a grain size of 1-200nm, wherein the ferrite crystal has a mass content of 3-87%.
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