CN110065938A - Structurally ordered graphene/Fe3O4The preparation method of aeroge - Google Patents
Structurally ordered graphene/Fe3O4The preparation method of aeroge Download PDFInfo
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- CN110065938A CN110065938A CN201910460382.9A CN201910460382A CN110065938A CN 110065938 A CN110065938 A CN 110065938A CN 201910460382 A CN201910460382 A CN 201910460382A CN 110065938 A CN110065938 A CN 110065938A
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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
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Abstract
The invention discloses a kind of structurally ordered graphene/Fe3O4The preparation method of aeroge, this method are with graphene oxide and Fe3O4For raw material, gel is obtained by hydro-thermal reaction, is then magnetized in magnetic field, and freezing processing is carried out using liquid nitrogen, rear dry setting obtains structurally ordered three-dimensional grapheme/Fe3O4Aeroge, in the structurally ordered three-dimensional aeroge system, graphene skeleton structure is constructing conduction pathway on the axial direction of magnetic field, promotes the conduction in the direction such as electronics, phonon.The invention solves the problems such as three-dimensional grapheme aerogel-like system degree of disorder is high, dispersion is random, conduction efficiency is low.
Description
Technical field
The present invention relates to aeroge production technical fields, more particularly to a kind of structurally ordered graphene/Fe3O4Aeroge
Preparation method.
Background technique
Graphene/Fe3O4Material as a kind of novel magnetic catalysis material, have it is environmentally friendly, it is reusable etc.
Feature.But current graphene/Fe3O4Aerogel material is mostly isotropism, the material of structural disorder；Either magnetic Fe3O4
Particle is uniformly directed distribution under magnetic fields, on graphene skeleton without influence.
Changzhou University He Guangyu et al. discloses a kind of magnetic nano ferroferric oxide-stone in patent CN102553593B
The preparation method of black alkene composite catalyst is to utilize graphite oxide and molysite at 50-90 DEG C and ammonium hydroxide is added to adjust pH as 9-
It is reacted under 11, product is subjected to Magneto separate, and dry acquisition after being washed with deionized water.Prepared by the invention
Although ferroso-ferric oxide-graphene composite material granular size is uniform, it is uniformly dispersed, point of the three-dimensional system of composite material
Cloth is still uneven.
In order to be further simplified production technology, how to use graphene oxide and ferroso-ferric oxide as raw material, prepare axis
It is aligned to direction, the modified graphene material of structurally ordered load ferroso-ferric oxide is that this seminar grinds all the time
The direction studied carefully.
Summary of the invention
The object of the present invention is to provide a kind of structurally ordered graphene/Fe3O4The preparation method of aeroge, this method are
With graphene oxide and Fe3O4For raw material, gel is obtained by hydro-thermal reaction, is then magnetized in magnetic field, and uses liquid nitrogen
Freezing processing is carried out, rear dry setting obtains structurally ordered graphene/Fe3O4Aeroge.
A kind of structurally ordered graphene/Fe3O4The preparation method of aeroge, comprising the following steps:
(1) graphene oxide and Fe that weight ratio is 0.5-1.5: 1 are weighed3O4Nanometer powder；
(2) by weighed graphene oxide and Fe3O4Nanometer powder is reacted using hydro-thermal method, be made graphene/
Fe3O4Gel；
(3) by graphene/Fe made of step (2)3O4Gel is cleaned multiple times using deionized water, until after washing
Deionized water at neutrality；
(4) by graphene/Fe after washing3O4Gel, which is placed in the magnetic field that intensity is 500-5000 Oe, to be magnetized, shape
At graphene/Fe of three-dimensional order3O4Gel；
(5) by graphene/Fe of the three-dimensional order taken out from magnetic field3O4Gel is immediately placed on freeze setting in liquid nitrogen, then
Sample is placed in freeze drier and is further dehydrated, stable structurally ordered graphene/Fe is obtained3O4Gas
Gel.
Preferably, Fe described in step (1)3O4The partial size of nanometer powder is 1-20nm.
Preferably, the temperature of hydro-thermal reaction described in step (2) is 200-350 DEG C, reaction time 2-5h.
Preferably, magnetizing time described in step (4) is 10-30min.
Preferably, the time of step (5) freeze setting in liquid nitrogen be 1-2h, in freeze drier drying time be
24-48h。
Compared with prior art, the invention has the following advantages: present invention system in such a way that induced by magnetic field is orientated
For a kind of structurally ordered graphene/Fe3O4Aeroge.Make graphene and magnetic Nano ion Fe in water-heat process3O4Between
Certain interaction force is formed, the Fe under magnetic fields3O4The movement that will drive graphene sheet layer during Particles Moving, from
And entire three-dimensional system is made to obtain structurally ordered graphene/Fe along magnetic field axial direction orientations3O4Aeroge.Structure
Graphene skeleton structure in orderly three-dimensional aeroge system is constructing conduction pathway on the axial direction of magnetic field, promotes
The conduction in the direction such as electronics, phonon.The invention solves three-dimensional grapheme aerogel-like system degree of disorder height, dispersion randomly
Then, the problems such as conduction efficiency is low.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the invention
Example, for those of ordinary skill in the art, without any creative labor, can also be according to these attached drawings
Obtain other attached drawings.
Fig. 1 is the TEM of graphene oxide in the embodiment of the present invention；
Fig. 2 is the SEM of graphene oxide in the embodiment of the present invention；
Fig. 3 is graphene/Fe prepared by the embodiment of the present invention 13O4The SEM of aeroge；
Fig. 4 is graphene/Fe prepared by the embodiment of the present invention 13O4The SEM of aeroge；
Fig. 5 is graphene oxide, Fe in the embodiment of the present invention 13O4With graphene/Fe3O4The XRD of aeroge；
Fig. 6 is the graphene/Fe prepared in the embodiment of the present invention 13O4Aeroge is in compression resilience axially and longitudinally.
Specific embodiment
The invention will be further described with attached drawing combined with specific embodiments below.
Embodiment 1
(1) by 20mg graphene oxide (its TEM and SEM scheme as depicted in figs. 1 and 2) and 23.2mg Fe3O4Nanoparticle
Under ultrasonication after mixing, graphene/Fe is prepared using hydro-thermal method3O4Hydrogel, the temperature of hydro-thermal reaction are 250 DEG C,
Reaction time is 3h.
(2) structurally ordered graphene/Fe3O4The preparation of aeroge:
The sample that reaction is obtained takes out, and a large amount of deionized water is added and impregnates to wash away the monomer for having neither part nor lot in reaction, directly
To deionized water to neutrality.By the graphene/Fe3O4Hydrogel is placed in the magnetic field of 2000 Oe intensity, makes magnetic nano particle
Son is orientated 20min under magnetic fields, while driving graphene orientation arrangement, forms structurally ordered three-dimensional grapheme/Fe3O4
Hydrogel.And the material after orientation is immediately placed in freeze setting in liquid nitrogen, cooling time 1.5h, then sample is placed in cold
Further dehydration and drying 48h is carried out in lyophilizer, obtains structurally ordered graphene/Fe3O4Aeroge, different amplification
SEM it is for example as shown in Figure 3 and Figure 4.
From figure 3, it can be seen that prepared graphene/Fe3O4In aeroge, graphene surface uniform load has nanometer
Fe3O4Particle, figure 4, it is seen that prepared graphene/Fe3O4In aeroge, the skeleton of graphene oxide is in regular
Ordered structure arrangement.It can be seen that graphene/Fe of the invention3O4The nanometer Fe of aeroge not only area load3O4Particle is equal
Even orderly, the skeleton arrangement of simultaneous oxidation graphene is also regular orderly.
It can also be seen that graphene/Fe in the XRD diagram of Fig. 53O4The characteristic peak and Fe of aeroge curve3O4Curve spy
Sign peak it is corresponding (2 θ=30.1,35.4,43.1,53.4,57.0,62.5 ° occur correspondence (220), (311), (400),
(422), the characteristic peak of (511) and (440)), it was demonstrated that successfully by Fe3O4It is supported on grapheme material surface, but at 13.2 ° of 2 θ ≈
Graphene oxide (001) characteristic peak it is unobvious, but occur a faint peak at 23.4 ° of 2 θ ≈, which is reduction
Graphene characteristic diffraction peak, graphene oxide is reduced to graphene to this explanation during the reaction.
Fig. 6 is graphene/Fe3O4The compression rebound linearity curve of aeroge axially and longitudinally, it can be seen from the figure that graphite
Alkene/Fe3O4The axial compression strength of aeroge is substantially better than longitudinal compressive strength, this is because the skeleton that graphene sheet layer is formed
Structure is in magnetic field and Fe3O4It arranges under magnetic particle effect along magnetic direction preferred orientation, forms that structure is more regular, has
Three-dimensional grapheme/Fe of sequence3O4Aeroge system.
Embodiment 2
(1) by 10mg graphene oxide (its TEM and SEM scheme as depicted in figs. 1 and 2) and 20mg Fe3O4Nanoparticle exists
Under ultrasonication after mixing, graphene/Fe is prepared using hydro-thermal method3O4Hydrogel, the temperature of hydro-thermal reaction are 200 DEG C, instead
It is 5h between seasonable.
(2) structurally ordered graphene/Fe3O4The preparation of aeroge:
The sample that reaction is obtained takes out, and a large amount of deionized water is added and impregnates to wash away the monomer for having neither part nor lot in reaction, directly
To deionized water to neutrality.By the graphene/Fe3O4Hydrogel is placed in the magnetic field of 500Oe intensity, makes magnetic nano-particle
It is orientated 30min under magnetic fields, while driving graphene orientation arrangement, forms structurally ordered three-dimensional grapheme/Fe3O4Water
Gel.And the material after orientation is immediately placed in freeze setting in liquid nitrogen, cooling time 2h, then sample is placed in freezing and is done
Further dehydration and drying is carried out in dry machine for 24 hours, obtains structurally ordered graphene/Fe3O4Aeroge.
Embodiment 3
(1) by 20mg graphene oxide (its TEM and SEM scheme as depicted in figs. 1 and 2) and 28mg Fe3O4Nanoparticle exists
Under ultrasonication after mixing, graphene/Fe is prepared using hydro-thermal method3O4Hydrogel, the temperature of hydro-thermal reaction are 350 DEG C, instead
It is 2h between seasonable.
(2) structurally ordered graphene/Fe3O4The preparation of aeroge:
The sample that reaction is obtained takes out, and a large amount of deionized water is added and impregnates to wash away the monomer for having neither part nor lot in reaction, directly
To deionized water to neutrality.By the graphene/Fe3O4Hydrogel is placed in the magnetic field of 1000 Oe intensity, makes magnetic nano particle
Son is orientated 15min under magnetic fields, while driving graphene orientation arrangement, forms structurally ordered three-dimensional grapheme/Fe3O4
Hydrogel.And the material after orientation is immediately placed in freeze setting in liquid nitrogen, cooling time 2h, then sample is placed in freezing
Further dehydration and drying 30h is carried out in drying machine, obtains structurally ordered graphene/Fe3O4Aeroge.
Embodiment 4
(1) by 30mg graphene oxide (its TEM and SEM scheme as depicted in figs. 1 and 2) and 20mg Fe3O4Nanoparticle exists
Under ultrasonication after mixing, graphene/Fe is prepared using hydro-thermal method3O4Hydrogel, the temperature of hydro-thermal reaction are 300 DEG C, instead
It is 2h between seasonable.
(2) structurally ordered graphene/Fe3O4The preparation of aeroge:
The sample that reaction is obtained takes out, and a large amount of deionized water is added and impregnates to wash away the monomer for having neither part nor lot in reaction, directly
To deionized water to neutrality.By the graphene/Fe3O4Hydrogel is placed in the magnetic field of 5000 Oe intensity, makes magnetic nano particle
Son is orientated 20min under magnetic fields, while driving graphene orientation arrangement, forms structurally ordered three-dimensional grapheme/Fe3O4
Hydrogel.And the material after orientation is immediately placed in freeze setting in liquid nitrogen, cooling time 2h, then sample is placed in freezing
Further dehydration and drying 48h is carried out in drying machine, obtains structurally ordered graphene/Fe3O4Aeroge.
Used herein a specific example illustrates the principle and implementation of the invention, and above embodiments are said
It is bright to be merely used to help understand method and its core concept of the invention；At the same time, for those skilled in the art, foundation
Thought of the invention, there will be changes in the specific implementation manner and application range.In conclusion the content of the present specification is not
It is interpreted as limitation of the present invention.
Claims (5)
1. structurally ordered graphene/Fe3O4The preparation method of aeroge, which is characterized in that include the following steps；
(1) graphene oxide and Fe that weight ratio is 0.5-1.5: 1 are weighed3O4Nanometer powder；
(2) by weighed graphene oxide and Fe3O4Nanometer powder is reacted using hydro-thermal method, and graphene/Fe is made3O4It is solidifying
Glue；
(3) by graphene/Fe made of step (2)3O4Gel is cleaned multiple times using deionized water, until going after washing
Ionized water is at neutrality；
(4) by graphene/Fe after washing3O4Gel, which is placed in the magnetic field that intensity is 500-5000Oe, to be magnetized, and is formed three-dimensional
Orderly graphene/Fe3O4Gel；
(5) by graphene/Fe of the three-dimensional order taken out from magnetic field3O4Gel is immediately placed on freeze setting in liquid nitrogen, then by sample
Product are placed in freeze drier and are further dehydrated, and obtain stable structurally ordered graphene/Fe3O4Aeroge.
2. structurally ordered graphene/Fe according to claim 13O4The preparation method of aeroge, which is characterized in that step
(1) Fe described in3O4The partial size of nanometer powder is 1-20nm.
3. structurally ordered graphene/Fe according to claim 13O4The preparation method of aeroge, which is characterized in that step
(2) temperature of the hydro-thermal reaction described in is 200-350 DEG C, reaction time 2-5h.
4. structurally ordered graphene/Fe according to claim 13O4The preparation method of aeroge, which is characterized in that step
(4) magnetizing time described in is 10-30min.
5. structurally ordered graphene/Fe according to claim 13O4The preparation method of aeroge, which is characterized in that step
(5) time of freeze setting is 1-2h in liquid nitrogen, and drying time is 24-48h in freeze drier.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103413689A (en) * | 2013-07-19 | 2013-11-27 | 北京科技大学 | Method for preparing graphene aerogel and graphene/ metallic oxide aerogel |
| CN105000886A (en) * | 2015-07-13 | 2015-10-28 | 郑州大学 | Macroscopic three-dimensional ultralight Fe3O4 doped graphene aerogel composite material and preparation method |
| CN109320286A (en) * | 2018-11-14 | 2019-02-12 | 武汉纺织大学 | The magnetic graphite alkenyl aerogel material and preparation method thereof for having ordered structure |
-
2019
- 2019-05-30 CN CN201910460382.9A patent/CN110065938B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103413689A (en) * | 2013-07-19 | 2013-11-27 | 北京科技大学 | Method for preparing graphene aerogel and graphene/ metallic oxide aerogel |
| CN105000886A (en) * | 2015-07-13 | 2015-10-28 | 郑州大学 | Macroscopic three-dimensional ultralight Fe3O4 doped graphene aerogel composite material and preparation method |
| CN109320286A (en) * | 2018-11-14 | 2019-02-12 | 武汉纺织大学 | The magnetic graphite alkenyl aerogel material and preparation method thereof for having ordered structure |
Non-Patent Citations (1)
| Title |
|---|
| YU WANG ET AL.: "Fe3O4 nanoparticle/graphene aerogel composite with enhanced lithium storage performance", 《APPLIED SURFACE SCIENCE》 * |
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