CN108455585A - A kind of method that electric field-assisted prepares graphene - Google Patents
A kind of method that electric field-assisted prepares graphene Download PDFInfo
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Abstract
The present invention provides a kind of methods that electric field-assisted prepares graphene, including chiral molecules is added in the electrolytic solution, cathode and anode are all made of graphite foil or graphene bar electrode, connect voltage, it is pre-processed, then carries out continuing electrochemical stripping preparing graphite alkene.The present invention by chiral molecules structure to graphene electric field-assisted magnanimity remove, can efficient macroscopic preparation of graphene, realize scale.And the single-layer graphene that the product prepared is high-quality.
Description
Technical field
The present invention relates to the preparing technical fields of graphene, and in particular to a kind of method that electric field-assisted prepares graphene,
Prepared graphene has high-quality, can be widely applied to catalysis, bio-sensing, battery, ultracapacitor, functional fibre
Equal fields.
Background technology
Graphene, as a kind of presently found most thin, most hard, the strongest novel nano carbon materials of electrical and thermal conductivity performance
Material, is described as in the industry " dark fund ", is " king of new material ".Graphene not only has excellent electric property (electric at room temperature
Transport factor is up to 200000cm2/ Vs), light weight, thermal conductivity is good (5000W/mK), large specific surface area (2630m2/ g), it
Young's modulus (1100GPa) and fracture strength (125GPa), but also have some unique performances, as quantum hall effect,
Quantum tunneling effect etc..Since the Geim professors seminar of University of Manchester in 2004 successfully obtains with mechanical stripping method
1 since graphene, it just causes attracting attention for the world, the dream for having attracted countless researchers to pursue new material.Graphite
Alkene can be widely applied to lithium ion battery electrode material, ultracapacitor, electrode of solar battery material, thin film transistor (TFT)
Preparation, sensor, semiconductor devices, transparence display touch screen, functional fibre and transparent electrode etc..
Its excellent performance can be not only inherited as the graphene derived material and composite material with more application prospect,
And the more conducively regulation and control of material character and application in practice, therefore receive the concern of numerous researchers.Also just
It is to be based on the above reason, the directional assembly and functionality of novel carbon-based structure is realized using the primitive characteristic of graphene
Customization has become new a research hotspot and emphasis now, therefore prepares nano complexes material by matrix of graphene
Experiment and theoretical research widened the application range of graphene.These composite materials are in catalysis, bio-sensing, battery, super
Capacitor etc. has a wide range of applications potential, is expected to have breakthrough in energy fields such as electric vehicles in the future.
Although the synthesis and application of graphene and its composite material have been achieved for certain scientific advance, graphite
The extensive technology of preparing of alkene is still to limit the bottleneck of its practical application at present, and restrict graphene industrial market and expand
Biggest obstacle.The preparation method of graphene mainly have mechanical stripping method, chemical vapour deposition technique, crystal epitaxy method,
Chemical oxidation-reduction method, liquid phase stripping method and electric field-assisted etc..In these preparation methods, most it is expected to realize low cost, height
Efficiency, the method for environmental-friendly magnanimity production are electric field-assisteds.
Early in 20th century the seventies, people begin to prepare graphite intercalation compound using electric field-assisted.But directly
To in recent years, chemists just prepare graphene using this technology.In brief, electric field-assisted method is to utilize conduction
Electrolyte and direct current go to implement stripping to graphitic source (such as graphite rod, graphite foil and graphite flake), reach and prepare graphite
The purpose of alkene.After energization, graphite electrode can not only be used as anode again can with cathode, using the gas of electrode surface generation,
Carry out the expansion stripping of graphite.Therefore, the method that electric field-assisted stripping prepares graphene is divided into cathodic disbonding and anode stripping.
Cathodic disbonding prepares graphene and introducing Li+ or the lithium salts of some molten states, reaction temperature is required for compare mostly
It is higher, then have the production efficiency of graphene relatively low, it is more difficult to it accomplishes scale production.It is prepared by the stripping of anode graphite electric field-assisted
The problems such as graphene, also mostly there is graphene low output and not high production efficiencys.Recently, it has been reported that and utilizes organic 2,
2,6,6- tetramethyl piperidine -1- oxygroup free radicals auxiliary ammonium sulfate stripping anode graphite foil is prepared for graphene, by using double
The graphite foil for covering electrode system stripping large area, reacts 10h or more, has successfully obtained more than ten grams of graphene powder, raw
It is about 1g/h to produce efficiency, this production efficiency also has a distance from extensive actual production.
Chirality is one of essential attribute of nature.It is chiral closely bound up with the vital movement in entire universe, nature
Basic biological phenomena and law are all made of chirality.It is found that the chiral liquid crystal phase of two-dimensional colloidal liquid crystal, it is thus identified that
The long-range orderly layered structure of standard and optical activity of graphene oxide chiral liquid crystal, explore its internal helicoid dislocation chirality knot
Structure, it is proposed that " helical lay phase " structural model explains the structure chirality source of novel chiral liquid crystal.Then, people people reports
Road graphene oxide has preferably chiral circular dichroism, and simulates its chiral arrangement architecture；Followed by chiral polymer
Polymer and amino acid molecular carry out Chiral functionalization to graphene oxide, and have inquired into the knowledge of its chiral molecule enantiomer
Other performance etc.；Recently, people induce graphene nano using the covalent effect of chiral cysteine molecule and graphene edge
The distortion of the nanoscale of piece is prepared for the graphene quantum dot of chiral mapping, but utilizes chiral molecules auxiliary electric field stripping system
The research of standby graphene has not been reported.
Invention content
For the defects in the prior art, the present invention provides a kind of preparation method of graphene, specially a kind of electric fields
The method that auxiliary prepares graphene synthesizes the chiral molecules of different structure, the chirality point of research different structure unit by design
The covalent effect difference of son and graphene edge is inquired into chiral molecules and is acted on the spiral expansion of graphite electrode interlayer, realizes it
Lower efficient, the quick and macroscopic preparation of graphene of auxiliary electric field auxiliary.
The purpose of the present invention is what is be achieved through the following technical solutions：
The present invention provides a kind of preparation methods of graphene, the described method comprises the following steps：It is added in the electrolytic solution
Chiral molecules, cathode and anode are all made of graphite foil or graphene bar electrode, connect voltage, are pre-processed, then held
Continuous electrochemical stripping preparing graphite alkene.
Preferably, the chiral molecules includes at least one of following structural formula：
Wherein, R is the alkyl of C8~20；More preferable R is the straight chained alkyl of C8~20.
It is highly preferred that the chiral molecules includes at least one of following structural formula：
Preferably, the preparation method of the chiral molecules includes the following steps：
A, it using chiral small molecule as raw material, is dissolved in the mixed solution of acetone and sodium hydroxide, stirs；
B, the acyl chlorides and sodium hydroxide solution of different alkyl chains is added dropwise into step A acquired solution systems, then persistently stirs
Reaction；
C, the pH value of regulating step B acquired solutions is 0.2-3.5 to get chiral molecules.
Preferably, in step A, the chirality small molecule structure formula isWherein R is the alkyl of C8~20；
More preferable R is the straight chained alkyl of C10~20.
Preferably, in step A, the pH value of the mixed solution is controlled 9.0~14.0.
Preferably, in step B, the time of the dropwise addition is 10-120 minutes；It is described be stirred to react the time be 0.5-5 it is small
When, the pH value for preserving the reaction system is controlled 9.0~14.0.
Preferably, the preparation method of the chiral molecules further includes the chiral molecules petroleum ether for preparing step C
Afterwards, it is placed at -30~65 DEG C and is freeze-dried.
Preferably, for the voltage used that pre-processes for 0.5~2.5V, pretreatment time is 1~10min；The electrification
The voltage that stripping graphite uses is 4~12V.
Preferably, the addition of the chiral molecules is 0.01~0.1wt%.
Preferably, the electrolyte is selected from salting liquid, acid solution, at least one of aqueous slkali.More preferable electrolyte choosing
One kind from sodium chloride solution, sulfuric acid solution, sodium hydroxide solution.
Compared with prior art, the present invention has following advantageous effect：
The present invention by chiral molecules structure to graphene electric field-assisted magnanimity remove, can efficient macroscopic preparation of graphene,
Realize scale.
Description of the drawings
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon：
Fig. 1 is that the electric field-assisted stripping of different time prepares the reaction process figure of graphene：It is using ammonium sulfate to scheme a1-a3
Electrolyte system, figure b1-b3 are using ammonium sulfate+chiral molecules electrolyte system；
Fig. 2 is that electric field-assisted removes graphene device；
Fig. 3 is chiral molecules spiral expansion graphite；
Fig. 4 is electric field-assisted stripping reaction mechanism schematic diagram；
Fig. 5 prepares the SEM under the different multiplying of graphene for chiral molecules auxiliary electric field up-stripping；
Fig. 6 is the TEM for the different zones that chiral molecules auxiliary electric field up-stripping prepares graphene：
Fig. 7 is the Raman that chiral molecules auxiliary electric field up-stripping prepares graphene.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the common skill of this field
For art personnel, without departing from the inventive concept of the premise, several changes and improvements can also be made.These belong to this
The protection domain of invention.
A kind of preparation method of graphene described in following embodiment is a kind of method that electric field-assisted prepares graphene,
It the described method comprises the following steps：Chiral molecules is added in the electrolytic solution, cathode and anode are all made of graphite foil or graphene
Bar electrode is connected voltage, is pre-processed, and then carries out continuing electrochemical stripping preparing graphite alkene.
The chiral molecules includes at least one of following structural formula：
Wherein, R is the alkyl of C8~20.
The preparation method of the chiral molecules includes the following steps：
A, it using chiral small molecule as raw material, is dissolved in the mixed solution of acetone and sodium hydroxide, stirs；
B, acyl chlorides and sodium hydroxide solution are added dropwise into step A acquired solution systems, then is persistently stirred to react；
C, the pH value of regulating step B acquired solutions is 0.2-3.5 to get chiral molecules.
4, the preparation method of graphene according to claim 3, which is characterized in that in step A, the small molecule
Structural formula isWherein R is the alkyl of C8~20.
In step A, the pH value of the mixed solution is controlled 9.0~14.0.
In step B, the time of the dropwise addition is 10-120 minutes；It is described be stirred to react the time be 0.5-5 hour, preservation
The pH value of the reaction system is controlled 9.0~14.0.
The preparation method of the chiral molecules further includes placement after the chiral molecules petroleum ether for preparing step C
It is freeze-dried at -30~65 DEG C.
For the voltage used that pre-processes for 0.5~2.5V, pretreatment time is 1~10min；The electrochemical stripping stone
The voltage that ink uses is 4~12V.
The addition of the chiral molecules is 0.01-0.1wt%.
The electrolyte is selected from salting liquid, acid solution, at least one of aqueous slkali.
Embodiment 1
By being starting point from existing chiral small molecule, as shown in table 1, it is dissolved in the mixed of acetone and sodium hydroxide
It closes in solution (pH=11.5 or so of control solution).Quickly stirring at room temperature, while being added dropwise simultaneously not into the system
With the acyl chlorides and sodium hydroxide solution of alkyl chain, and maintain pH value between 11.5-12.0.Above two liquid is slowly added dropwise,
After 60 minutes or so are added dropwise, reaction system is kept persistently to be stirred to react again about 1 hour in pH=12.0 or so.Then,
Concentrated hydrochloric acid is added and is adjusted to system pH=1.0 or so, is made the chiral molecules of 6 kinds of solids, then with petroleum ether 3 times, placement-
It is freeze-dried at 60 DEG C, it is then spare.
Chiral molecules obtained (0.01wt%) is added in the electrolyte of ammonium sulfate, cathode uses graphite foil electrode, sun
Pole also uses graphite foil electrode (it is as shown in Figure 2 that electric field-assisted removes graphene device), external constant-voltage is connected, first in 2V
3min is pre-processed under voltage, mainly carries out chiral molecules and the spiral expansion of graphite electrode interlayer is handled, as shown in Figure 3.With
Voltage is adjusted to 10V afterwards and carries out sustained electric field up-stripping preparing graphite alkene.Electric field-assisted stripping reaction mechanism such as Fig. 4
It is shown.The electric field-assisted stripping of different time prepares the reaction process of graphene as shown in Figure 1, wherein a1-a3 is to be not added with to start with
The reaction process figure of property molecule；Figure b1-b3 is the reaction process figure that chiral molecules is added.As seen from Figure 1, it is deposited in chiral molecules
When, graphene can be quickly from graphite foil sur-face peeling.
The structure of the chiral molecules and its raw material of use are as shown in table 1.
Table 1
Embodiment 2
By being starting point from existing chiral small molecule, it is dissolved in the mixed solution of acetone and sodium hydroxide
(pH=11.0 or so of control solution).Quickly stirring at room temperature, while different alkyl chains are added dropwise simultaneously into the system
Acyl chlorides and sodium hydroxide solution, and maintain pH value between 11.0-11.5.Above two liquid, 30 minutes left sides is slowly added dropwise
After the right side is added dropwise, reaction system is kept persistently to be stirred to react about 1.5 again in pH=11.0 or so.Then, concentrated hydrochloric acid is added
It is adjusted to system pH=1.0 or so, is made the chiral molecules of 6 kinds of solids, then with petroleum ether 3 times, is freezed at -60 DEG C of placement
It is dry, it is then spare.
It is added in the electrolyte of ammonium sulfate using the different structure unit chiral molecules (0.05wt%) of design synthesis, cathode
Using graphite foil electrode, anode also uses graphite foil electrode, connects external constant-voltage, is first pre-processed under 2.5V voltages
5min mainly carries out chiral molecules and handles the spiral expansion of graphite electrode interlayer, then holds voltage modulated 11V
Continuous electric field-assisted removes preparing graphite alkene.
The structure of the chiral molecules and its raw material of use are as shown in table 1.
Embodiment 3
By being starting point from existing chiral small molecule, it is dissolved in the mixed solution of acetone and sodium hydroxide
(pH=10.0 or so of control solution).Quickly stirring at room temperature, while different alkyl chains are added dropwise simultaneously into the system
Acyl chlorides and sodium hydroxide solution, and maintain pH value between 10.0-10.5.Above two liquid, 30 minutes left sides is slowly added dropwise
After the right side is added dropwise, keep reaction system when pH=10.0 is persistently stirred to react about 2 again.Then, concentrated hydrochloric acid is added to be adjusted to
System pH=2.0 or so, is made the chiral molecules of solid, then with petroleum ether 3 times, is freeze-dried at -60 DEG C of placement, so
It is spare afterwards.
It is added in the electrolyte of ammonium sulfate using the different structure unit chiral molecules (0.1wt%) of design synthesis, cathode
Using graphite foil electrode, anode also uses graphite foil electrode, connects external constant-voltage, is first pre-processed under 1.5V voltages
10min mainly carries out chiral molecules and handles the spiral expansion of graphite electrode interlayer, then holds voltage modulated 10V
Continuous electric field-assisted removes preparing graphite alkene.
The structure of the chiral molecules and its raw material of use are as shown in table 1.
Embodiment 4
It is added in the electrolyte of sodium chloride using chiral molecules (0.1wt%) prepared by embodiment 3, cathode uses graphene
Bar electrode, anode also use graphene bar electrode, connect external constant-voltage, first pre-process 10min under 0.5V voltages, main
If carrying out chiral molecules to handle the spiral expansion of graphite electrode interlayer, it is auxiliary that voltage modulated 4V is then subjected to sustained electric field
Help stripping preparing graphite alkene.
Embodiment 5
It is added in the electrolyte of sodium hydroxide using chiral molecules (0.1wt%) prepared by embodiment 3, cathode uses graphite
Foil electrode, anode also use graphite foil electrode, connect external constant-voltage, first pre-process 1min under 2.5V voltages, mainly
It carries out chiral molecules to handle the spiral expansion of graphite electrode interlayer, voltage modulated 12V is then subjected to sustained electric field auxiliary stripping
From preparing graphite alkene.
Graphene prepared by the various embodiments described above carries out experimental verification：Pass through electronic scanner microscope, high-resolution transmission
Electron microscope, Raman spectrum carry out pattern, thickness and quality characterization to graphite ene product and pass through electronics as illustrated in figs. 5-7
Flying-spot microscope, high resolution transmission electron microscopy can clearly show that prepared graphene is equal single-layer graphene,
And surface does not have fault of construction.Raman spectrum shows that the carbon graphene degree in the graphene prepared is high, compound with regular structure.
Therefore, it is somebody's turn to do the result shows that the product prepared by the embodiment of the present invention is the single-layer graphene of high-quality.
Comparative example 1
This comparative example use structure forChiral molecules auxiliary electric field stripping prepare graphite
Alkene, in addition to the chiral molecules structure of use is different from embodiment 3, other steps are same as Example 3.
Graphene made from this comparative example compares embodiment 3, and graphene single layer rate is low made from this comparative example, and graphene
There is fault of construction on surface.
Comparative example 2
The method of this comparative example and embodiment 3 is essentially identical, the difference is that only：In this comparative example, chiral molecules
Addition is 0.2wt%.
Graphene made from this comparative example compares embodiment 3, and graphene single layer rate is low made from this comparative example, most of
For multi-layer graphene.
Comparative example 3
The method of this comparative example and embodiment 3 is essentially identical, the difference is that only：In this comparative example, without locating in advance
The step of reason.
Graphene made from this comparative example compares embodiment 3, speed of this comparative example graphene from graphite foil sur-face peeling
Slowly, the efficiency for preparing graphene is low.
Comparative example 4
The method of this comparative example and embodiment 5 is essentially identical, the difference is that only：In this comparative example, using in 3V electricity
Pressure carries out sustained electric field up-stripping preparing graphite alkene.
Graphene made from this comparative example compares embodiment 5, and graphene surface fault of construction is apparent made from this comparative example.
Although it should be noted that provided only in embodiment 1-5 the chiral molecules of the alkyl structure for using R for C15 into
Row battery up-stripping preparing graphite alkene, but according to the common knowledge of those skilled in the art, use R for C15 other than
The chiral molecules of the alkyl structure of C8-20 of the present invention similarly has identical with the chiral molecules of structure in embodiment
Effect can be realized and be removed to graphene electric field-assisted magnanimity.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make a variety of changes or change within the scope of the claims, this not shadow
Ring the substantive content of the present invention.In the absence of conflict, the feature in embodiments herein and embodiment can arbitrary phase
Mutually combination.
Claims (10)
1. a kind of preparation method of graphene, which is characterized in that the described method comprises the following steps：It is added in the electrolytic solution chiral
Molecule, cathode and anode are all made of graphite foil or graphene bar electrode, connect voltage, are pre-processed, and then carry out continuing electricity
Chemical stripping preparing graphite alkene.
2. the preparation method of graphene according to claim 1, which is characterized in that the chiral molecules includes with lower structure
At least one of formula：
Wherein, R is the alkyl of C8~20.
3. the preparation method of graphene according to claim 2, which is characterized in that the preparation method packet of the chiral molecules
Include following steps：
A, it using chiral small molecule as raw material, is dissolved in the mixed solution of acetone and sodium hydroxide, stirs；
B, acyl chlorides and sodium hydroxide solution are added dropwise into step A acquired solution systems, then is persistently stirred to react；
C, the pH value of regulating step B acquired solutions is 0.2-3.5 to get chiral molecules.
4. the preparation method of graphene according to claim 3, which is characterized in that in step A, the small molecule structure formula
ForWherein R is the alkyl of C8~20.
5. the preparation method of graphene according to claim 3, which is characterized in that in step A, the pH of the mixed solution
Value control is 9.0~14.0.
6. the preparation method of graphene according to claim 3, which is characterized in that in step B, the time of the dropwise addition is
10-120 minutes；It is described be stirred to react the time be 0.5-5 hour, preserve the reaction system pH value control 9.0~14.0.
7. the preparation method of graphene according to claim 3, which is characterized in that the preparation method of the chiral molecules is also
Include being placed at -30~65 DEG C and being freeze-dried after the chiral molecules petroleum ether for preparing step C.
8. the preparation method of graphene according to claim 1, which is characterized in that it is described pre-process the voltage that uses for
0.5~2.5V, pretreatment time are 1~10min；The voltage that the electrochemical stripping graphite uses is 4~12V.
9. the preparation method of graphene according to claim 1, which is characterized in that the addition of the chiral molecules is
0.01-0.1wt%.
10. the preparation method of graphene according to claim 1, which is characterized in that the electrolyte is selected from salting liquid, acid
Solution, at least one of aqueous slkali.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114684814A (en) * | 2022-04-24 | 2022-07-01 | 江苏大学 | Preparation method of self-supporting flexible graphene film and application of self-supporting flexible graphene film to flexible supercapacitor |
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| CN102206388A (en) * | 2011-05-12 | 2011-10-05 | 商丘师范学院 | Preparation method of graphene composite by industrialized electrolytic stripping |
| WO2016203388A1 (en) * | 2015-06-15 | 2016-12-22 | Graphene Nanotechnologies Hub S.R.L. | Process for the production of functionalized graphene |
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| CN102206388A (en) * | 2011-05-12 | 2011-10-05 | 商丘师范学院 | Preparation method of graphene composite by industrialized electrolytic stripping |
| WO2016203388A1 (en) * | 2015-06-15 | 2016-12-22 | Graphene Nanotechnologies Hub S.R.L. | Process for the production of functionalized graphene |
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| CN114684814A (en) * | 2022-04-24 | 2022-07-01 | 江苏大学 | Preparation method of self-supporting flexible graphene film and application of self-supporting flexible graphene film to flexible supercapacitor |
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