CN107032329A - A kind of three-dimensional grapheme of nano-micrometre classification pore passage structure and preparation method thereof - Google Patents
A kind of three-dimensional grapheme of nano-micrometre classification pore passage structure and preparation method thereof Download PDFInfo
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- CN107032329A CN107032329A CN201610076122.8A CN201610076122A CN107032329A CN 107032329 A CN107032329 A CN 107032329A CN 201610076122 A CN201610076122 A CN 201610076122A CN 107032329 A CN107032329 A CN 107032329A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- C01B2204/04—Specific amount of layers or specific thickness
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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Abstract
The invention provides three-dimensional grapheme of a kind of nano-micrometre classification pore passage structure and preparation method thereof, the O content of the three-dimensional grapheme is 5~30wt%, and thickness is 20 μm~10mm, and specific surface area is 400~1200m2/ g, electrical conductivity is 1~100S/cm；The nanometer and micron channel diameter of the three-dimensional grapheme are respectively 10~300nm and 0.5~50 μm；The preparation method comprises the following steps：1) mixed liquor is prepared：By graphene oxide solution made from the Hummers methods of modification and the ultrasonically treated 0.5~3h of silica；2) three-dimensional graphene oxide is prepared：Vacuum filtration step 1) made mixed liquor obtains film, successively with reducing agent and etching liquid processing gained film, vacuum or freeze-drying；3) three-dimensional grapheme is prepared：In Ar atmosphere, at a temperature of 300~1000 DEG C, reduction step 2) 0.5~20h of the three-dimensional graphene oxide of gained.The duct of gained three-dimensional grapheme porous material is stable, with high specific surface area and high electrical conductivity, has wide practical use in lithium ion battery.
Description
Technical field
The present invention relates to graphene oxide composite material preparing technical field, and in particular to a kind of nano-micrometre point
Three-dimensional grapheme of level pore passage structure and preparation method thereof.
Background technology
Graphene is the two dimensional crystal being made up of one layer of carbon atom peeled off through graphite, and it has carbon hexa-atomic
Ring group into two-dimension periodic honeycomb lattice structure, be to build other dimension carbonaceous material (such as zero dimensions
Fullerene, one-dimensional CNT and three-dimensional graphite) elementary cell.The uniqueness two dimension knot of graphene
Structure and perfect crystal structure make it have high conductivity, high mechanical properties, high-termal conductivity and peculiar
Optical property, has been widely used in the information apparatus such as transistor.In nano composite material, battery
And the field such as super capacitor, the assembling form between two dimensional surface graphene layer is particularly important.Normal conditions
Under, in drying process, because the effect of graphenic surface tension force can cause between graphene layer mutually stacking,
The self property of graphene can be remarkably decreased, and have a strong impact on the performance of its subsequent applications.
Three-dimensional porous graphene not only has the merit of graphene, and its loose structure also has it
The advantageous property such as specific surface area is big, high mechanical strength and electronic conduction ability are protruded.Ji-Lei shi et al.
Materials chemistry magazine (Ji-Lei shi, et al.Journal of Materials Chemistry, 2014,2,
10830) method for synthesizing three-dimensional grapheme using hydro-thermal method is had reported to which disclose and will aoxidize stone
Drying at room temperature obtains three-dimensional graphene oxide after being reacted 5 hours at 150 DEG C in black alkene solution addition reactor
The pore-size distribution of three-dimensional porous graphene is uneven obtained by gel, the method, and diameter is from several microns to several
Ten microns, the smaller (100~300m of specific surface area2/g).In addition, South Korea scholar (Bong Gill in 2012
Choi, et al.ACS Nano, 2012,5,4020) report by the use of PS and be used as template, assembling oxidation
The method that reducing process prepares three-dimensional porous grapheme material, the bore dia of the material obtained by the method
1-2 μm, its relatively low specific surface area (is only 194m2/ g), it is impossible to reach application requirement.
At present, the three-dimensional grapheme porous material obtained using existing method, resulting graphene
Aperture is mostly micron-sized, and porosity is relatively low, and specific surface area is smaller, and this will seriously restrict three-dimensional graphite
Application of the alkene porous material in Material Fields such as photovoltaic, energy storage device, heat accumulation devices.
The content of the invention
It is an object of the invention to provide a kind of nano-micrometre classification pore passage structure three-dimensional grapheme and its
Preparation method, overcomes the deficiencies in the prior art, spherical by graphene oxide solution coated silica
Into film, the film after etching is handled through drying with high temperature reduction, obtains the stable nano-micrometre in duct
Duct three-dimensional graphite porous material is classified, the duct classification of the material is obvious, and specific surface area is big, leads
Electrical property is good, prepares with low cost, it is adaptable to field of lithium ion battery.
To achieve these goals, the present invention uses following technical scheme：
A kind of nano-micrometre is classified the three-dimensional grapheme of pore passage structure, and the O of the three-dimensional grapheme contains
Measure as 5~30wt%, thickness is 20 μm~10mm, specific surface area is 400~1200m2/ g, electrical conductivity
For 1~100S/cm；The nanometer and micron channel diameter of the three-dimensional grapheme are respectively 10~300nm
With 0.5~50 μm.
First optimal technical scheme of described three-dimensional grapheme, constitutes the graphite of the three-dimensional grapheme
The alkene piece number of plies is 1~300, and lateral dimension is 0.5~500 μm.
Second optimal technical scheme of described three-dimensional grapheme, the O of three-dimensional grapheme content
For 9~15wt%；The number of plies of the graphene film is 1~40.
A kind of preparation method of the three-dimensional grapheme, the described method comprises the following steps：
1) mixed liquor is prepared：By graphene oxide solution and dioxy made from the Hummers methods of modification
Ultrasonically treated 0.5~the 3h of SiClx；
2) three-dimensional graphene oxide is prepared：Vacuum filtration step 1) made mixed liquor obtains film, successively
With reducing agent and etching liquid processing gained film, vacuum or freeze-drying；
3) three-dimensional grapheme is prepared：In Ar atmosphere, at a temperature of 300~1000 DEG C, reduction step 2)
0.5~20h of gained three-dimensional graphene oxide.
First optimal technical scheme of the preparation method, the silica is including mass ratio
0.1~10 diameter is respectively 20~300nm and 1~60 μm of silica spheres.
Second optimal technical scheme of the preparation method, step 2) described in reducing agent for hydration
Hydrazine, sodium borohydride, vitamin C or HI.
3rd optimal technical scheme of the preparation method, step 2) described in etching liquid be hydrogen fluorine
The aqueous solution of acid.
4th optimal technical scheme of the preparation method, it is 1 that the silica, which includes mass ratio,
Diameter is respectively 20~160nm and 1~20 μm of silica spheres.
5th optimal technical scheme of the preparation method, the step 3) it is, at 900 DEG C, to go back
Former 2h.
The three-dimensional grapheme of the nano-micrometre classification pore passage structure is used for lithium ion battery electrode material
Application.
With immediate prior art ratio, the present invention has the advantages that：
1) pore passage structure of the three-dimensional grapheme of nano-micrometre of the invention classification pore passage structure is stable,
With high-specific surface area, high conductivity, it can be used as the electrode material of lithium ion battery；
2) preparation method technique of the invention is simple, and course of reaction is easily controlled, and equipment investment is few,
It need not be carried out under the conditions of vacuum high-pressure, large-scale production can be achieved.
Brief description of the drawings
Fig. 1：The scanning electron microscope (SEM) photograph of the three-dimensional grapheme of embodiment 1.
Embodiment
With reference to embodiment and accompanying drawing, the present invention will be described in more detail, but application of the present invention
It is not limited thereto.
Embodiment 1
20nm silica spheres and 1 μm of silica spheres are equal for 1 ratio according to mass ratio
Even mixing, is added to by mutually being mixed in graphene oxide solution made from the Hummers methods of modification
Close, then ultrasonic 1 hour；Mixed solution is filtered by vacuum, you can obtain film, then at 60 DEG C
Under the conditions of reduction treatment 10min is carried out to film with hydrazine hydrate steam, then with acetone remove filter membrane, then
Film is transferred in the etching liquid being made up of hydrofluoric acid and water and performed etching, silica mould is removed
Three-dimensional graphene oxide film after etching, is then freeze-dried 12 hours by plate；Finally three
Dimension graphene oxide film is put into reacting furnace, and is passed through Ar (300sccm), while heated to
900 DEG C of 0.5 hours of reaction, then it is cooled to room temperature.
The three-dimensional grapheme that nano-micrometre is classified pore passage structure is obtained, material specific surface area is 680m2/ g,
Electrical conductivity is 35S/cm.
Embodiment 2
It is respectively 40nm and 5 μm of silica spheres from diameter, remaining condition is same as Example 1,
The three-dimensional grapheme that nano-micrometre is classified pore passage structure is obtained, material specific surface area is 592m2/ g, electricity
Conductance is 43S/cm.
Embodiment 3
It is respectively 80nm and 10 μm of silica spheres, remaining condition and the phase of embodiment 1 from diameter
Together, the three-dimensional grapheme that nano-micrometre is classified pore passage structure is obtained, material specific surface area is 565m2/ g,
Electrical conductivity is 38S/cm.
Embodiment 4
It is respectively 160nm and 20 μm of silica spheres, remaining condition and the phase of embodiment 1 from diameter
Together, the three-dimensional grapheme that nano-micrometre is classified pore passage structure is obtained, material specific surface area is 496m2/ g,
Electrical conductivity is 32S/cm.
Embodiment 5
It is respectively 300nm and 40 μm of silica spheres, remaining condition and the phase of embodiment 1 from diameter
Together, the three-dimensional grapheme that nano-micrometre is classified pore passage structure is obtained, material specific surface area is 450m2/ g,
Electrical conductivity is 18S/cm.
Embodiment 6
It is respectively 300nm and 60 μm of silica spheres, remaining condition and the phase of embodiment 1 from diameter
Together, the three-dimensional grapheme that nano-micrometre is classified pore passage structure is obtained, material specific surface area is 410m2/ g,
Electrical conductivity is 8S/cm.
Comparative example 1
Graphene oxide solution made from Hummers methods by modification is added to hydrothermal reaction kettle
In, after 150 DEG C of reactions 5 hours, allowing reactor to be cooled to room temperature, just to can obtain three-dimensional grapheme more
Gel sample, is then made film by hole sol sample, then under freeze-drying, so that it may obtain three
Tie up graphene porous film material.
The bore dia of the three-dimensional grapheme porous material of gained is 2~4 μm, and specific surface area is 150m2/ g,
Electrical conductivity is 3S/cm.
Comparative example 2
2 μm of silica spheres are added in above-mentioned graphene oxide solution and are mutually mixed, then
Uniform mixing 1 hour is carried out under ultrasonication, then is filtered by vacuum, then graphene oxide
Film is added in the etching liquid of hydrofluoric acid and water, to remove silica spheres, then is freeze-dried
12 hours, finally graphene film is put into reacting furnace, and is passed through Ar (300sccm),
While heated to 900 DEG C of 1 hours of reaction, three-dimensional grapheme film can be obtained by being then cooled to room temperature
Material.
The bore dia of resulting three-dimensional grapheme porous material is 1~2 μm, and specific surface area is 200
m2/ g, electrical conductivity is 2.6S/cm.
Contrast finds that nano-micrometre of the invention is classified the three-dimensional grapheme material (Kong Zhi of pore passage structure
Footpath is 10~300nm and 0.5~50 μm) with the institute by hydro-thermal method and by template of micron silica
Three-dimensional grapheme porous material compare, specific surface area and electrical conductivity are all greatly improved and more had
Beneficial to its application in lithium ion battery electrode material.
The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof, art it is common
It will be appreciated by the skilled person that with reference to above-described embodiment can to the present invention embodiment modify or
Person's equivalent substitution, these any modifications or equivalent substitution without departing from spirit and scope of the invention are in application
Within pending claims.
Claims (10)
1. a kind of nano-micrometre is classified the three-dimensional grapheme of pore passage structure, it is characterised in that described three
The O content for tieing up graphene is 5~30wt%, and thickness is 20 μm~10mm, and specific surface area is
400~1200m2/ g, electrical conductivity is 1~100S/cm；The nanometer of the three-dimensional grapheme and micron duct
Diameter is respectively 10~300nm and 0.5~50 μm.
2. three-dimensional grapheme according to claim 1, it is characterised in that the composition three-dimensional
The graphene film number of plies of graphene is 1~300, and lateral dimension is 0.5~500 μm.
3. three-dimensional grapheme according to claim 2, it is characterised in that the three-dimensional graphite
The O of alkene content is 9~15wt%；The number of plies of the graphene film is 1~40.
4. the preparation method of three-dimensional grapheme described in a kind of claim 1, it is characterised in that described
Method comprises the following steps：
1) mixed liquor is prepared：By graphene oxide solution and dioxy made from the Hummers methods of modification
Ultrasonically treated 0.5~the 3h of SiClx；
2) three-dimensional graphene oxide is prepared：Vacuum filtration step 1) made mixed liquor obtains film, successively
With reducing agent and etching liquid processing gained film, vacuum or freeze-drying；
3) three-dimensional grapheme is prepared：In Ar atmosphere, at a temperature of 300~1000 DEG C, reduction step 2)
0.5~20h of gained three-dimensional graphene oxide.
5. preparation method according to claim 4, it is characterised in that the silica bag
Include the silica spheres that the diameter that mass ratio is 0.1~10 is respectively 20~300nm and 1~60 μm.
6. preparation method according to claim 4, it is characterised in that step 2) described in
Reducing agent is hydrazine hydrate, sodium borohydride, vitamin C or HI.
7. preparation method according to claim 4, it is characterised in that step 2) described in
Etching liquid is the aqueous solution of hydrofluoric acid.
8. preparation method according to claim 5, it is characterised in that the silica bag
Include the silica spheres that the diameter that mass ratio is 1 is respectively 20~160nm and 1~20 μm.
9. preparation method according to claim 4, it is characterised in that the step 3) be in
At 900 DEG C, reductase 12 h.
10. a kind of three-dimensional grapheme of the nano-micrometre classification pore passage structure described in claim 1 is used for
The application of lithium ion battery electrode material.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107689271A (en) * | 2017-08-22 | 2018-02-13 | 京东方科技集团股份有限公司 | Preparation method, porous graphene film and the electronic product of porous graphene film |
| CN109867277A (en) * | 2017-12-04 | 2019-06-11 | 武汉大学 | A kind of preparation method of big size graphene three-dimensional material |
| CN111864204A (en) * | 2020-05-28 | 2020-10-30 | 武汉理工大学 | Self-supporting graphene carbon conductive network material and preparation method and application thereof |
| CN112622357A (en) * | 2020-12-02 | 2021-04-09 | 成都飞机工业（集团）有限责任公司 | Multilayer porous graphene film with high conductivity and manufacturing method thereof |
| CN113583336A (en) * | 2021-07-23 | 2021-11-02 | 江阴市海江高分子材料有限公司 | Heat-resistant flexible semiconductive shielding PP cable material and preparation method thereof |
| CN116281986A (en) * | 2023-04-17 | 2023-06-23 | 华能新能源股份有限公司 | Preparation method, drafting device and application of three-dimensional graphene |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107689271A (en) * | 2017-08-22 | 2018-02-13 | 京东方科技集团股份有限公司 | Preparation method, porous graphene film and the electronic product of porous graphene film |
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| CN109867277A (en) * | 2017-12-04 | 2019-06-11 | 武汉大学 | A kind of preparation method of big size graphene three-dimensional material |
| CN111864204A (en) * | 2020-05-28 | 2020-10-30 | 武汉理工大学 | Self-supporting graphene carbon conductive network material and preparation method and application thereof |
| CN112622357A (en) * | 2020-12-02 | 2021-04-09 | 成都飞机工业（集团）有限责任公司 | Multilayer porous graphene film with high conductivity and manufacturing method thereof |
| CN113583336A (en) * | 2021-07-23 | 2021-11-02 | 江阴市海江高分子材料有限公司 | Heat-resistant flexible semiconductive shielding PP cable material and preparation method thereof |
| CN116281986A (en) * | 2023-04-17 | 2023-06-23 | 华能新能源股份有限公司 | Preparation method, drafting device and application of three-dimensional graphene |
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Application publication date: 20170811 |