CN107082414A - Graphene with random and irregular three-D stomata and preparation method thereof - Google Patents
Graphene with random and irregular three-D stomata and preparation method thereof Download PDFInfo
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- CN107082414A CN107082414A CN201610353104.XA CN201610353104A CN107082414A CN 107082414 A CN107082414 A CN 107082414A CN 201610353104 A CN201610353104 A CN 201610353104A CN 107082414 A CN107082414 A CN 107082414A
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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
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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- C—CHEMISTRY; METALLURGY
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2006/11—Powder tap density
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The present invention relates to a kind of graphene with random and irregular three-D stomata and preparation method thereof.It is prepared from according to the graphene with random and irregular three-D stomata of the present invention by following methods:In the state of reducing agent is added in graphene oxide solution, it is spray-dried, so as to prepare the new construction cotton shape graphene with random and irregular three-D air hole structure, its specific surface area is high, and some strength is presented.
Description
Technical field
The present invention relates to a kind of graphene with random and irregular three-D stomata and preparation method thereof.
Background technology
At present, as the material based on carbon, such as CNT (carbon nanotube), diamond
(diamond), graphite (graphite), graphene (graphene), graphene oxide (Graphene
) etc. oxide studied in the nanotechnology research group in various field.These materials can be used in life
Thing sensor (biosensor), nano-complex (nanocomposite) or quantum devices (quantum
Device), electrode material (Electrode) etc..Graphene is a kind of two-dimensional material in carbon-based material,
It is the semi-conducting material that a kind of band gap is 0 (zero gap).In recent years, it is special with graphene electrochemistry
The relevant various researchs of property have been reported.
The hexagon that graphene is made up of sp2 carbon atoms is in the two-dimensional nano piece (2-D of honeycomb lattice
Nanosheet), the single layer structure of only one of which carbon atom thickness.
In general, graphene is as a kind of new material, with excellent physics and chemical stability,
High-specific surface area, and excellent conductive characteristic, thus get most of the attention.Also, according to these physical property,
Graphene may be used as active mold, can plate the metal oxide of nanosized.
In addition, the method for preparing existing graphene nanometer sheet mainly employs usual solwution method, i.e., in solution
Middle synthesizing graphite alkene.
According to methods described, first by graphite synthetic graphite oxide.The synthetic method of graphite oxide, leads to
Frequently with Hummers method methods.According to methods described, at normal temperatures, ordinary graphite is dipped in height
Concentration H2SO4In solution, after being sufficiently stirred for, KMnO is put into graphite impregnation solution4.Then,
To containing the KMnO4Mixed solution in add a small amount of H2O2, it occurs oxidation reaction with graphite
Form graphite oxide.Then, using whizzer, and with after distilled water and ethanol repeatedly washing,
Obtained powder is completely dried in drier, to terminate the synthesis step of graphite oxide.Then,
The graphite oxide is dispersed in water carry out ultrasonic treatment, graphite oxide is peeled off
(exfoliation) into monolithic.Then, reducing agent (such as NaBH of appropriate amount is put into solution4Deng)
It is stirred, then input reducing agent deviates from the oxy radical of graphite oxide, you can obtain monolithic
Reduction graphite oxide, i.e. graphene.
At present, graphene is as carbon-based material, can be as integrated for nano-electronic devices substantially single
Position is used, thus is got most of the attention, and as electrode material, graphene has unlimited usability.At present
Research focus focus primarily upon two-dimensional graphene and graphene oxide nanometer sheet because, it is this
Graphene oxide structure can effectively disperse in aqueous, and can change or be reduced to specific
The structure of group.
With the advantage of two-dimensional graphene nanometer sheet, three-dimensional grapheme has as sensor or electrode material
High-specific surface area and air hole structure, cause sizable concern.In order to prepare this three-dimensional grapheme structure,
Attempted to by two-dimensional slice shape graphene be converted into hollow structure capsule shape or interlayer layer structure three
Tie up shape.
The content of the invention
Technical problem
It is an object of the present invention to provide a kind of graphene with random and irregular three-D stomata and its
Preparation method.
Technical scheme
In order to solve above-mentioned technical problem, the present invention, which provides a kind of inside, has the graphene of three-dimensional stomata
Particle, it is folded by multiple graphene films and formed, and average diameter is 1~30 μm.
When the average diameter of particle is below 1 μm, granularity is too low, and graphene will not form fold shape
Uniform particle, and flat or platy structure is to maintain, it is difficult to take structural advantage.When being averaged for particle
When diameter is more than 30 μm, become big from architectural characteristic volume, thus tap density reduction, exist
The problems such as being difficult to of a relatively high capacitance.Therefore, the average diameter of graphene particle of the present invention
Preferably 1~30 μm.
Graphene particle of the present invention is characterised by that it is internal with three-dimensional stomata connected, the stomata
To be closed or open.In the present invention, the stomata of the three-dimensional connection is referred to:By multiple graphite
The stomata formed during alkene piece stack fold between multiple graphene films, or graphene film formation seem paper
Open the stomata internally formed during corrugated state.
Although the stomata refers to internally generating stomata to be closed, also not with particle external connection.
The stomata refers to stomata and particle external connection to be open.
The graphene particle of the present invention can be in cotton balls shape, cotton candy shape or paper curl globulate
Shape, inside has the shape of three-dimensional stomata, is not limited to these shapes.
Graphene particle of the present invention is characterised by that the graphene particle is configured to the fold of constituent particle
The terminal part of shape graphene monolithic is formed inwardly.That is, graphene particle of the present invention is characterised by, is constituted
The end of the graphene particle of particle is formed inwardly, by being folding or bending over towards inside so that end institute shape
Into end be that edge part (edge) does not expose on the surface.
Graphene particle of the present invention is characterised by that its specific surface area is 300~900 ㎡/g.Stone of the present invention
The specific surface area of black alkene particle is more preferably 700~900 ㎡/g.When specific surface area is in 300 ㎡/below g
When, specific surface area is too low, as electrode material in use, can physical absorption due to electrolyte osmosis
Reduce with the area of desorption, it is difficult to realize high power capacity., can thing when specific surface area is in 900 ㎡/more than g
Reason absorption and the area increase of desorption, but with the increase of stomata, the size and volume of granularity also increase,
The capacity rate of per unit electrode is reduced on the contrary, therefore, and the appropriate volume of holding and granularity are critically important.
Graphene particle of the present invention is characterised by that its tap density is 0.3~1.5g/cc.Work as vibration density
Degree is in below 0.3g/cc, it is difficult to realize the high-specific surface area as particle inherent characteristic.Work as vibration density
Degree is in below 1.5g/cc, the heavier-weight of per unit area, it is difficult to keep excellent electrode characteristic.
In addition, the present invention provides a kind of preparation method of graphene particle, comprise the following steps:Prepare stone
Black alkene or graphene oxide;The graphene or graphene oxide are scattered in solvent, dispersion liquid is prepared;
And be spray-dried the dispersion liquid, form particle.
Preparation method of the present invention is characterised by, the graphene or graphene oxide are being scattered in into solution
In the step of prepared composition dispersion liquid, based on 100 parts by weight solvent (such as distilled water), comprising amount for 1~
The graphene or graphene oxide of 10 parts by weight.
Preparation method of the present invention is characterised by, the graphene or graphene oxide are being scattered in into solution
In the step of prepared composition dispersion liquid, the concentration of the dispersion liquid is 0.01~50mg/ml.
Preparation method of the present invention is characterised by that temperature is 100~150 DEG C during the spray drying.
Preparation method of the present invention is characterised by, the graphene or graphene oxide are being scattered in into solution
In the step of prepared composition dispersion liquid, reducing agent such as NaBH is added4Deng.
In addition, the present invention provides a kind of electrode active material for electrochemical element, it includes the present invention
Graphene particle.
In the present invention, the electrochemical element may each be obvious for invention technician
Electrochemical element, such as lithium rechargeable battery, lithium-sulfur cell, magnesium cell, fuel cell or capacitor,
Double-layer capacitor, ultracapacitor etc..
The electrochemical element of the present invention can be used as negative active core-shell material comprising the graphene particle of the present invention.
Technique effect
According to the present invention having the graphene of random and irregular three-D stomata by following methods preparation
Into:In the state of reducing agent is added in graphene oxide solution, it is spray-dried, so as to prepare
New construction cotton shape graphene with random and irregular three-D air hole structure, its specific surface area is high, and is in
Existing some strength.
Brief description of the drawings
Fig. 1 to Fig. 6 represents there is random and irregular three-D stomata according to prepared by one embodiment of the invention
Cotton shape graphene SEM figures measurement result.
Embodiment
Hereinafter, the present invention is further described according to embodiment.But, the present invention is not limited to
Following examples.
Embodiment 1. prepares cotton balls shape reduced graphene oxide serving
1-1. prepares graphene oxide dispersion liquid (spray liquid)
Powdered graphite (gulf carbon, SP-1) is aoxidized by the Hummers methods of amendment, graphene is prepared
Oxide.
The internal temperature of 20L double-jacket reactors is set as after 0 DEG C, 76g graphite is put into sulphur
Acid (H2SO4, 8L) in, stirring mixing 1 hour under 250rpm speed.Then, in the suspension
In with every 10 minutes add 50g speed be slowly added to 380g potassium permanganate (KMnO4), confirm outstanding
Turbid liquid becomes after dark green solution, stirs 1 hour.Then, 35 DEG C are warming up to 0.5 DEG C/min speed
Afterwards, it is stirred for 2 hours.Deionized water (DI) (12L) is slowly added in suspension, is stayed during addition
Temperature is no more than 60 DEG C when heart deionized water (DI) is added.Also, be slowly added to hydrogenperoxide steam generator (
H2O2, 50wt%, 20mL), terminate reaction when solution becomes light brown graphene solution.By reaction knot
The mixed liquor of beam is filtered, by whizzer, and is washed with deionized after 20~30 times,
By drying stage, graphene oxide powder is obtained.
Add after 15g graphene oxides, use homogenizing agent (15mg/ml) in 1000ml deionized waters
Disperse 100 minutes under 4500rpm speed.By the above method, the graphene oxygen in the aqueous solution is dipped in
Compound is peeled off as single or multiple lift, the uniform dispersion of formation graphene oxide according to stress is cut.
1-2. is prepared and reduction cotton balls shape graphene oxide
Spraying for the graphene oxide prepared in above-described embodiment 1-1 dispersion liquid to be sprayed into drop
Device, employs pan spray drier, is spray-dried by spraying dispersion liquid, and spray amount is 1
5ml/ minutes, rotating speed was 12000rpm.The graphene oxide dispersion liquid is sprayed in microlayer model shape form
Drier internal temperature be set as 100 DEG C.
In drier, it is further dried under 100 DEG C of temperature conditionss after 6 hours, by 15g graphenes
Oxide powder is added in 1L distilled water, and stirring is disperseed for 1 hour, and 1 is then put into dispersion liquid
The 5ml hydrazines aqueous solution (concentration is 35wt%), and heating stirring 12 hours at 100 DEG C.After reaction terminates,
It is dried at room temperature for, then solvent is removed using film filter, with distillation water washing 3~5 times.
By obtained powder with after distillation water washing, it is dried under 100 DEG C of temperature conditionss, prepare
A diameter of 10~15 μm of cotton balls shape reduced graphene oxide serving.
Fig. 1 to Fig. 3 shows the SEM figures of obtained cotton balls shape reduced graphene oxide serving.Such as Fig. 1 extremely
Shown in Fig. 3, it can be seen that graphene oxide prepared by embodiments in accordance with the present invention is cotton balls shape, stone
Black alkene piece end is to interior folding in collapsed shape.
Embodiment 2. prepares cotton balls shape reduced graphene oxide serving
2-1. prepares graphene oxide dispersion liquid (spray liquid)
Implemented with above-described embodiment 1-1 identicals method, it is last to obtain graphene oxide oxidate powder,
The concentration of graphene oxide mixed liquor is changed into 5mg/ml to be prepared.
2-2. is prepared and reduction cotton balls shape graphene oxide
Implemented with above-described embodiment 1-2 identicals method, a diameter of 5~30 μm of cotton balls shape is made
Reduced graphene oxide serving.
Fig. 4 shows the SEM figures of obtained cotton balls shape reduced graphene oxide serving.As shown in figure 4, can
To find out that graphene oxide prepared by embodiments in accordance with the present invention is cotton balls shape, graphene film end to
Interior folding is in collapsed shape.
Embodiment 3. prepares cotton balls shape reduced graphene oxide serving
3-1. prepares graphene oxide dispersion liquid (spray liquid)
Implemented with above-described embodiment 1-1 identicals method, it is last to obtain graphene oxide oxidate powder,
The concentration of graphene oxide mixed liquor is changed into 10mg/ml to be prepared.
3-2. is prepared and reduction cotton balls shape graphene oxide
Implemented with above-described embodiment 1-2 identicals method, a diameter of 5~10 μm of cotton balls shape is made
Reduced graphene oxide serving.
Fig. 5 shows the SEM figures of obtained cotton balls shape reduced graphene oxide serving.As shown in figure 5, can
To find out that graphene oxide prepared by embodiments in accordance with the present invention is cotton balls shape, graphene film end to
Interior folding is in collapsed shape.
Embodiment 4. prepares cotton balls shape reduced graphene oxide serving
4-1. prepares graphene oxide dispersion liquid (spray liquid)
Implemented with above-described embodiment 1-1 identicals method, it is last to obtain graphene oxide oxidate powder,
The concentration of graphene oxide mixed liquor is changed into 20mg/ml to be prepared.
4-2. is prepared and reduction cotton balls shape graphene oxide
Implemented with above-described embodiment 1-2 identicals method, a diameter of 10~35 μm of cotton balls shape is made
Reduced graphene oxide serving.
Fig. 6 shows the SEM figures of obtained cotton balls shape reduced graphene oxide serving.As shown in fig. 6, can
To find out that graphene oxide prepared by embodiments in accordance with the present invention is cotton balls shape, graphene film end to
Interior folding is in collapsed shape.
Comparative example prepares flat graphene oxide
Comparative example 1-1. prepares graphene oxide powder
Implemented with embodiment 1-1 identicals method, obtain graphene oxide oxide powder.
Comparative example 1-2. prepares flat reduced graphene oxide serving
Graphene oxide described in 15g is added after 1000ml deionized waters, using homogenizing agent 4500
Disperse 100 minutes under rpm speed.
The 15ml hydrazines aqueous solution (concentration is 35wt%) is put into dispersion liquid, and heats and stirs at 100 DEG C
Mix 12 hours.
After reaction terminates, removed using film filter after solvent with distillation water washing.Make it at 100 DEG C
Dried under temperature conditionss, be prepared for flat reduced graphene oxide serving.
Claims (12)
1. a kind of inside has the graphene particle of three-dimensional stomata, it is folded by multiple graphene films and formed,
And average diameter is 1~30 μm.
2. graphene particle according to claim 1, wherein, the stomata is closed or open
Formula.
3. graphene particle according to claim 1, wherein, the graphene particle is configured to pleat
The terminal part of wrinkle shape graphene film is formed inwardly.
4. graphene particle according to claim 1, wherein, the graphene particle in cotton balls shape,
The shape of cotton candy shape or paper curl globulate.
5. graphene particle according to claim 1, wherein, the ratio surface of the graphene particle
Product is 300~900 ㎡/g.
6. graphene particle according to claim 1, wherein, the vibration density of the graphene particle
Spend for 0.3~1.5g/cc.
7. a kind of method of the graphene particle prepared described in claim 1, comprises the following steps:
Prepare graphene or graphene oxide;
The graphene or graphene oxide are scattered in solvent, dispersion liquid is prepared;And
The dispersion liquid is spray-dried, particle is formed.
8. the preparation method of graphene particle according to claim 7, wherein, by the graphite
In the step of alkene or graphene oxide are scattered in solution prepared composition dispersion liquid, based on 100 parts by weight solvent,
Include the graphene or graphene oxide of the amount for 1~10 parts by weight.
9. the preparation method of graphene particle according to claim 7, wherein, by the graphite
In the step of alkene or graphene oxide are scattered in solution prepared composition dispersion liquid, the concentration of the dispersion liquid is
0.01~50mg/ml.
10. the preparation method of graphene particle according to claim 7, wherein, the spraying is dry
Temperature is 100~250 DEG C when dry.
11. the preparation method of the graphene particle according to claim 7 with wrinkled surface, its
In, in the step of graphene or graphene oxide are scattered in solution prepared composition dispersion liquid, addition
Reducing agent.
12. a kind of electrode active material for electrochemical element, it includes the stone described in claim 1
Black alkene particle.
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CN114163712A (en) * | 2021-12-27 | 2022-03-11 | 杭州耕鑫生物科技有限公司 | Graphene composite PE material and preparation method thereof |
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KR20210090483A (en) * | 2020-01-10 | 2021-07-20 | 주식회사 엘지에너지솔루션 | Porous reduced graphene oxide, manufacturing method thereof, sulfur-carbon composite and lithium secondary battery comprising the same |
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