CN110357087A - A method of graphene oxide is prepared based on high concentration inorganic salt solution removing - Google Patents
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Abstract
The present invention provides a kind of methods for preparing graphene oxide based on high concentration inorganic salt solution removing, belong to technical field of preparation of graphene oxide.The present invention is using high concentration inorganic salt solution as electrolyte, using graphite as anode, using inertia conductive noble metal material as cathode, carries out electrochemical stripping reaction, obtains graphene oxide aggregation.The present invention uses high concentration inorganic salt solution as electrolyte, is able to suppress the fast decoupled that low-voltage is lauched, and realizes the lasting intercalation of graphite；The present invention changes destruction of traditional low concentration electrolyte to graphite electrode integrality, to realize the depth intercalation and extruding to graphite；And using anion contained by highly concentrated salt as oxidation intercalator, while intercalation and removing graphite, additionally it is possible to be aoxidized to graphite, to prepare graphene oxide；Meanwhile it is short preparation period of the present invention, at low cost, acid solution is not generated, environmental-friendly, method is simple, it is easy to accomplish industrial mass production.
Description
Technical field
The present invention relates to technical field of preparation of graphene oxide, in particular to a kind of to be shelled based on high concentration inorganic salt solution
From the method for preparing graphene oxide.
Background technique
The concept of graphene (Graphene) is proposed from the study group of the A.K.Geim leader of University of Manchester in 2004
Since, an other bright star of the graphene as carbon family has obtained the great attention of physics, chemistry and material scholar.
At present in the preparation method of graphene, preparing dilute restore as graphene of graphite oxide by graphite is considered as that a kind of realization is high-quality
Measure the large-scale preparation method of graphene.
It is the dilute derivative of graphite that graphite oxide is dilute, its structure with graphite is dilute is substantially the same, be a kind of two-dimensional surface knot
Structure, relative to graphene, it not only possesses good hydrophily and dispersibility in water, and can be made by chemical modification
It possesses wider purposes, therefore the dilute hot spot for also becoming people's research of graphite oxide.Prepare the side of graphene oxide
Method mainly has a chemical oxidization method, chemical oxidization method be by using a large amount of inorganic the strong protonic acid such as concentrated sulfuric acid, oleum or
Their mixture handles original graphite, and strong acid small molecule is inserted into graphite layers, is re-introduced into excessive strong oxidizer such as (high chlorine
Sour potassium, potassium permanganate etc.) oxidation removing is carried out to it, main preparation method includes Brodie method, Standenmaiers method
With Hummer method.However, the preparation of graphene oxide requires to introduce a large amount of acid solution and Strong oxdiative in above-mentioned preparation method
Agent is caused in purification phase, in order to remove a large amount of acid solution and strong oxidizer, water resource and the energy can be made seriously unrestrained
Take, and these strong oxidizers all have heavy metal ion, not recoverable, irreversible serious dirt is caused to environment
Dye, to hinder the mass production of graphene oxide.Therefore, in order to realize graphene oxide mass preparation, it is necessary to
A kind of method for finding clean oxidation, the technology of preparing of green energy conservation, and it can be used for the production of prepare with scale, it can just be expected to
The progress of making a breakthrough property in terms of macroscopic preparation of graphene.
Summary of the invention
Graphite oxide is prepared based on the removing of high concentration inorganic salt solution in view of this, it is an object of that present invention to provide one kind
The method of alkene.Preparation method green energy conservation provided by the invention, it is environmental-friendly, it is able to achieve the lasting intercalation of graphite.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of methods for preparing graphene oxide based on high concentration inorganic salt solution removing, including with
Lower step:
Using high concentration inorganic salt solution as electrolyte, using graphite as anode, with inertia conductive noble metal material work
For cathode, electrochemical stripping reaction is carried out, graphene oxide aggregation is obtained；
Molar concentration >=5mol/L of the high concentration inorganic salt solution；
The anion of the inorganic salts has oxidisability functional group.
Preferably, the graphite is one or more of natural flake graphite, oriented graphite, graphite paper and graphite rod.
Preferably, the material of the inertia conductive noble metal material is platinum or silver.
Preferably, the inorganic salts be one of sodium perchlorate, sodium nitrate, ammonium nitrate, Na2Fe04 and sodium chlorate or
It is several.
Preferably, the spacing between the anode and cathode is 5~15cm.
Preferably, the voltage that the electrochemical stripping reaction applies is 1~20V.
Preferably, the time of the electrochemical stripping reaction is 0.5~30h, the temperature of electrolyte when electrochemical stripping reacts
Degree is 10~35 DEG C.
It preferably, further include being post-processed to graphene oxide aggregation, after described after the electrochemical stripping reaction
Processing the following steps are included:
It is successively washed after the graphene oxide aggregation is separated, is ultrasonic and dry, obtaining graphite oxide
Alkene powder.
Preferably, the power of the ultrasound is 80~150W, and the time is 0.5~2h.
Preferably, the temperature of the drying is -40~-20 DEG C, and the time is 24~72h.
The present invention provides a kind of method for preparing graphene oxide based on high concentration inorganic salt solution removing, the present invention
Using high concentration inorganic salt solution as electrolyte, using graphite as anode, using inertia conductive noble metal material as cathode, into
Row electrochemical stripping reaction, to obtain graphene oxide aggregation.The present invention uses high concentration inorganic salt solution as electricity
Liquid is solved, the fast decoupled that low-voltage is lauched is able to suppress, realizes the lasting intercalation of graphite, the present invention changes traditional low concentration
Destruction of the electrolyte to graphite electrode integrality, to realize the depth intercalation and extruding to graphite；And it is inorganic using high concentration
Anion contained by salt is as oxidation intercalator, while intercalation and removing graphite, additionally it is possible to aoxidize, obtain to graphite
Graphene oxide；Meanwhile it is preparation method short preparation period provided by the invention, at low cost, acid solution is not generated, environmental-friendly, side
Method is simple, it is easy to accomplish industrial mass production.
Detailed description of the invention
Fig. 1 is the pictorial diagram of 1 gained graphene oxide aggregation of embodiment；
Fig. 2 is the stereoscan photograph of 1 gained graphene oxide powder of embodiment；
Fig. 3 is the X ray diffracting spectrum of 2 gained graphene oxide powder of embodiment；
Fig. 4 is the stereoscan photograph of 1 gained graphite clast of comparative example；
Fig. 5 is the X ray diffracting spectrum of 1 gained graphite clast of comparative example；
Fig. 6 is the X ray diffracting spectrum of 2 gained graphene oxide of comparative example.
Specific embodiment
The present invention provides a kind of methods for preparing graphene oxide based on high concentration inorganic salt solution removing, including with
Lower step:
Using high concentration inorganic salt solution as electrolyte, using graphite as anode, with inertia conductive noble metal material work
For cathode, electrochemical stripping reaction is carried out, graphene oxide aggregation is obtained.
In the present invention, molar concentration >=5mol/L of the high concentration inorganic salt solution, preferably >=8mol/L；It is described
The anion of inorganic salts has oxidisability functional group, is particularly preferred as sodium perchlorate, sodium nitrate, ammonium nitrate, Na2Fe04 and chlorine
One or more of sour sodium.In the present invention, the volume of the electrolyte and the mass ratio of graphite are preferably 10~40:1, more
Preferably 20~30:1.By the present invention in that using high concentration inorganic salt solution as electrolyte, it is able to suppress low-voltage and is lauched
Fast decoupled, to realize the lasting intercalation of graphite, meanwhile, anion contained by high concentration inorganic salts can be inserted as oxidation
Layer agent, while intercalation and removing graphite, additionally it is possible to be aoxidized to graphite.
In the present invention, the graphite is preferably one of natural flake graphite, oriented graphite, graphite paper and graphite rod
Or it is several；The material of the inertia conductive noble metal material is preferably platinum or silver, is particularly preferred as in platinized platinum, platinum filament and filamentary silver
It is one or more of.The present invention does not have special requirement to the source of the graphite and conductive noble metal material, normal using this field
Advise commercially available above-mentioned material.
In the present invention, the spacing between the anode and cathode is preferably 5~15cm, more preferably 8~12cm.The present invention
Pass through the spacing between control anode and cathode, the charge stripping efficiency of adjustable graphite.
In the present invention, the voltage that the electrochemical stripping reaction applies is preferably 1~20V, more preferably 5~15V；Institute
The voltage for stating application is preferably DC voltage, the voltage that the present invention is applied by control, can control graphite intercalation it is lasting when
Between and speed.In the present invention, the time of the electrochemical stripping reaction is preferably 0.5~30h, more preferably 5~20h, institute
The temperature of electrolyte is preferably 10~35 DEG C when stating electrochemical stripping reaction, and more preferably 20~30 DEG C.In the present invention, gained
Graphene oxide aggregation has complete orderly structure and big particle size, and in the present invention, the graphene oxide is poly-
Size >=300 μm of collective.
The method of Conventional electrochemical removing graphite, as electrolyte, is relied on usually using the lower water system salting liquid of concentration
The electrolysis of water generates the variation that gas causes volume, will make graphite intercalation and peeling in the shorter time, and reaction is made to terminate, this
It will cause the uncontrollable of graphene number of plies and degree of oxidation.The present invention changes traditional electrochemical stripping graphite method, for the first time
It proposes to prepare graphene oxide using high concentration inorganic salt solution as electrolyte, using high concentration inorganic salt solution to water
Constraint and high salt concentration system in lower water content, use anion contained by high salt concentration as oxidation intercalator,
Destroy it during electrochemical intercalation graphite to graphite electrode, to realize the lasting intercalation and extruding to graphite.
The present invention further preferably includes post-processing to graphene oxide aggregation after electrochemical stripping reaction,
It is described post-processing the following steps are included:
It is successively washed after the graphene oxide aggregation is separated, is ultrasonic and dry, obtaining graphite oxide
Alkene powder.
In the present invention, the isolated mode preferably filters, and the washing is preferably high purity water with detergent.This hair
It is bright to simplify traditional graphene oxide cleaning technique, using the orderly structure of preparatory phase graphene oxide aggregation and greatly
The purification to graphene oxide can be realized with most simple cheap suction filtration, washing process in size advantage.
Graphene oxide aggregation after washing is preferably placed in high purity water and carries out ultrasound by the present invention, the graphite oxide
The mass ratio of alkene aggregation and high purity water is preferably 5~10:1, more preferably 6~8:1；In the present invention, the function of the ultrasound
Rate is preferably 80~150W, more preferably 100~120W, and the time is preferably 0.5~2h, more preferably 1~1.5h；The ultrasound
It is preferably supersonic cleaning machine with equipment.In the present invention, graphene oxide aggregation becomes the oxidation of two-dimensional slice by ultrasound
Graphene dispersing solution.In the present invention, the drying is preferably freeze-dried, and the temperature of the drying is preferably -40~-20
DEG C, more preferably -35~-25 DEG C, the time is preferably 24~72h, more preferably 36~60h, the vacuum degree of the freeze-drying
Preferably 20Pa.
It is preparation method short preparation period provided by the invention, at low cost, acid solution is not generated, environmental-friendly, method is simple, easily
In realization industrial mass production.
Graphene oxide is prepared based on the removing of high concentration inorganic salt solution to provided by the invention below with reference to embodiment
Method be described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Using sodium perchlorate as electrolyte, the water for weighing 17.2g sodium perchlorate addition 5g is placed in 50 DEG C of baking ovens
30min is used for electrochemical stripping graphite as electrolyte (concentration 24.5mol/L) after solution is as clear as crystal.In electrolytic cell
Middle that prepared electrolyte is added, choosing graphite paper is that anode is connected with DC power supply, using platinized platinum as cathode and direct current
Source is connected, and two electrodes apply the DC voltage of 5V at a distance of 5cm, and electrochemical stripping reaction is carried out at 25 DEG C.After continuing 30h
Electrode does not peel off, obtains graphene oxide aggregation, and pictorial diagram is as shown in Figure 1.After filtering, washing, 80W's
Disperse 30min in supersonic cleaning machine and obtains the graphene oxide dispersion of two-dimensional slice, dispersion liquid vacuum under the conditions of -20 DEG C
20Pa is dry, and graphene oxide powder is prepared in 72h.
Electronic Speculum (SEM) analysis is scanned to gained graphene oxide powder, gained stereoscan photograph is as shown in Figure 2.
As shown in Figure 2, present invention gained graphene oxide powder piece diameter size>10 μm, thickness<5nm.
Embodiment 2
Using sodium perchlorate as electrolyte, the water for weighing 15g sodium perchlorate addition 5g places 30min in 50 DEG C of baking ovens,
Electrochemical stripping graphite is used for as electrolyte (concentration 21.4mol/L) after solution is as clear as crystal.It is added in a cell
Prepared electrolyte, choosing graphite paper is that anode is connected with DC power supply, is connected using platinum filament as cathode with DC power supply
It connects, two electrodes apply the DC voltage of 10V at a distance of 6cm, and electrochemical stripping reaction is carried out at 15 DEG C.Continue 10h after electrode not
It peels off, obtains graphene oxide aggregation, after vacuum filter, washing, disperse 1h in the supersonic cleaning machine of 100W
The graphene oxide dispersion of two-dimensional slice is obtained, oxidation is prepared in dispersion liquid vacuum 20Pa drying under the conditions of -30 DEG C for 24 hours
Graphene powder.
X-ray diffraction analysis is carried out to gained graphene oxide powder, gained X ray diffracting spectrum is as shown in Figure 3.By scheming
3 it is found that present invention gained graphene oxide powder occurs typical graphene oxide diffraction maximum, and its peak intensity at 10 degree or so
Degree illustrates that the material oxidation degree is higher, is typical graphite oxide much higher than the graphene diffraction maximum occurred at 25 degree or so
Alkene material characteristics structure.
Embodiment 3
Using sodium perchlorate as electrolyte, the water for weighing 5g sodium perchlorate addition 5g places 30min in 50 DEG C of baking ovens, to
Electrochemical stripping graphite is used for as electrolyte (concentration 7.1mol/L) after solution is as clear as crystal.It is added and prepares in a cell
Good electrolyte, choosing graphite paper is that anode is connected with DC power supply, is connected using platinum filament as cathode with DC power supply, two
Electrode applies the voltage of 15V at a distance of 10cm, and electrochemical stripping reaction is carried out at 35 DEG C.Continue 1h electrode not peel off, obtain
To graphene oxide aggregation, after vacuum filter is cleaned, disperses 2h in the supersonic cleaning machine of 150W and obtain two-dimensional slice
Graphene oxide dispersion, dispersion liquid vacuum 20Pa under the conditions of -40 DEG C is dry, and graphene oxide powder is prepared in 36h.
Electron microscope analysis and X-ray diffraction analysis be scanned to this graphene oxide powder, acquired results and embodiment 1 with
Embodiment 2 is similar.
Comparative example 1
Using sodium perchlorate as electrolyte, the water for weighing 0.5g sodium perchlorate addition 5g places 30min in 50 DEG C of baking ovens,
Electrochemical stripping graphite is used for as electrolyte (concentration 0.71mol/L) after solution is as clear as crystal.It is added in a cell
Prepared electrolyte, choosing graphite paper is that anode is connected with DC power supply, is connected using platinum filament as cathode with DC power supply
It connects, two electrodes apply the voltage of 5V at a distance of 5cm, and electrochemical stripping reaction is carried out at 25 DEG C.Then occur when carrying out 5min obvious
Electrode peel off and damage phenomenon, this is because the electrolyte of low concentration causes water electrolysis anti-due to a large amount of presence of water-soluble matter
It should be key reaction, aggravation bubble is generated, damaged to the integrality of graphite anode.
Electron microscope analysis and X-ray diffraction analysis are scanned to the graphite clast of peeling, gained stereoscan photograph is as schemed
4, X ray diffracting spectrum since the concentration of inorganic salt solution is lower as shown in figure 5, cause anode too early as seen from Figure 4
Peeling, graphite peeling effect is poor, compared to Figure 1 it can be seen that the piece diameter thickness and extent of exfoliation of 1 resulting materials of comparative example
It is all obvious poor, there is graphene diffraction maximum for 25 degree or so in Fig. 5, intensity is much higher than the graphite oxide of 10 degree or so appearance
Alkene diffraction maximum.It can be said that bright, premature graphite is peeled off in comparative example 1, and it is lower to will lead to its degree of oxidation.
Comparative example 2
Using sodium perchlorate as electrolyte, the water for weighing 15g sodium perchlorate addition 5g places 30min in 50 DEG C of baking ovens,
Electrochemical stripping graphite is used for as clear as crystal conduct electrolyte (concentration 21.4mol/L) of solution.It is added and matches in a cell
The electrolyte made, choosing graphite paper is that anode is connected with DC power supply, is connected using platinum filament as cathode with DC power supply,
Two electrodes apply the voltage of 30V at a distance of 5cm, at 25 DEG C intercalation carry out 5min when after there is apparent salting-out phenomenon.Cause
The appearance of salting-out phenomenon is because the hydrone under action of high voltage in high salt concentration water-bound, which largely reacts, generates gas, meeting
Intercalation is carried out to graphite electrode, however since the radius of gas molecule is much higher than the radius of salt ion, lead to graphite electrode structure
Integrality is by premature destruction, and being largely lost due to hydrone, and saline solution oversaturated state occurs, causes
The precipitation of salt.
Gained graphene oxide is cleaned, the structural characterization of XRD as shown in fig. 6, as seen from Figure 6, due to
Overtension leads to generation of saltouing, and anion intercalated efficiency is caused to decline, and degree of oxidation reduces.
Embodiment 4
Using sodium nitrate as electrolyte, the water for weighing 5g sodium nitrate addition 5g places 30min in 50 DEG C of baking ovens, to solution
Electrochemical stripping graphite is used for as electrolyte (concentration 11.8mol/L) after as clear as crystal.It is added and prepares in a cell
Electrolyte, choosing graphite paper is that anode is connected with DC power supply, is connected using filamentary silver as cathode with DC power supply, two is electric
Pole applies the voltage of 5V at a distance of 8cm, and electrochemical stripping reaction is carried out at 35 DEG C.Electrode does not peel off after continuing 7h, obtains
Graphene oxide aggregation disperses 30min in the supersonic cleaning machine of 80W and obtains two-dimensional slice after vacuum filter is cleaned
Graphene oxide dispersion, dispersion liquid vacuum 20Pa under the conditions of -20 DEG C is dry, and graphene oxide powder is prepared in 72h.
Electron microscope analysis and X-ray diffraction analysis be scanned to this graphene oxide powder, acquired results and embodiment 1 with
Embodiment 2 is similar.
Embodiment 5
Using ammonium nitrate as electrolyte, the water for claiming 10g ammonium nitrate that 5g is added places 30min in 50 DEG C of baking ovens, to solution
Electrochemical stripping graphite is used for as electrolyte (concentration 25mol/L) after as clear as crystal.It is added in a cell prepared
Electrolyte, choosing graphite paper is that anode is connected with DC power supply, is connected using platinum filament as cathode with DC power supply, two electrodes
At a distance of 15cm, apply the voltage of 20V, electrochemical stripping reaction is carried out at 10 DEG C.Electrode does not peel off after continuing 3h, obtains
Graphene oxide aggregation disperses 30min in the supersonic cleaning machine of 80W and obtains two-dimensional slice after vacuum filter is cleaned
Graphene oxide dispersion, dispersion liquid vacuum 20Pa under the conditions of -20 DEG C is dry, and graphene oxide powder is prepared in 72h.
Electron microscope analysis and X-ray diffraction analysis be scanned to this graphene oxide powder, acquired results and embodiment 1 with
Embodiment 2 is similar.
Embodiment 6
Using Na2Fe04 as electrolyte, the water for claiming 6g Na2Fe04 that 5g is added places 30min in 50 DEG C of baking ovens, to molten
Electrochemical stripping graphite is used for as highly concentrated saline electrolysis liquid (concentration 7.2mol/L) after liquid is as clear as crystal.In a cell plus
Enter prepared electrolyte, choosing graphite paper is that anode is connected with DC power supply, using platinum filament as cathode with DC power supply phase
Connection, two electrodes apply the voltage of 5V at a distance of 5cm, and electrochemical stripping reaction is carried out at 25 DEG C.Electrode does not occur after continuing 1h
It peels off, obtains graphene oxide aggregation, after vacuum filter is cleaned, disperse 30min in the supersonic cleaning machine of 80W and obtain
The graphene oxide dispersion of two-dimensional slice, dispersion liquid vacuum 20Pa under the conditions of -20 DEG C is dry, and graphite oxide is prepared in 72h
Alkene powder.
Electron microscope analysis and X-ray diffraction analysis be scanned to this graphene oxide powder, acquired results and embodiment 1 with
Embodiment 2 is similar.
Embodiment 7
Using sodium chlorate as electrolyte, the water for claiming 7g sodium chlorate that 5g is added places 30min in 50 DEG C of baking ovens, clear to solution
It is clear transparent afterwards as electrolyte (concentration 13.1mol/L) for electrochemical stripping graphite.It is added in a cell prepared
Electrolyte, choosing graphite paper is that anode is connected with DC power supply, is connected using platinum filament as cathode with DC power supply, two electrodes
At a distance of 7cm, apply the voltage of 3V, electrochemical stripping reaction is carried out at 25 DEG C.Electrode does not peel off after continuing 2h, obtains oxygen
Graphite alkene aggregation disperses 30min in the supersonic cleaning machine of 80w and obtains two-dimensional slice after vacuum filter is cleaned
Graphene oxide dispersion, dispersion liquid vacuum 20Pa under the conditions of -20 DEG C is dry, and graphene oxide powder is prepared in 72h.
Electron microscope analysis and X-ray diffraction analysis be scanned to this graphene oxide powder, acquired results and embodiment 1 with
Embodiment 2 is similar.
As seen from the above embodiment, preparation method green energy conservation provided by the invention, it is environmental-friendly, in electrochemical intercalation mistake
Graphite can be destroyed in journey, realize the lasting intercalation and extruding to graphite.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of method for preparing graphene oxide based on high concentration inorganic salt solution removing, which is characterized in that including following
Step:
Using high concentration inorganic salt solution as electrolyte, using graphite as anode, using inertia conductive noble metal material as yin
Pole carries out electrochemical stripping reaction, obtains graphene oxide aggregation；
Molar concentration >=5mol/L of the high concentration inorganic salt solution；
The anion of the inorganic salts has oxidisability functional group.
2. the method according to claim 1, wherein the graphite is natural flake graphite, oriented graphite, graphite
One or more of paper and graphite rod.
3. the method according to claim 1, wherein the material of the inertia conductive noble metal material be platinum or
Silver.
4. the method according to claim 1, wherein the inorganic salts be sodium perchlorate, sodium nitrate, ammonium nitrate,
One or more of Na2Fe04 and sodium chlorate.
5. the method according to claim 1, wherein the spacing between the anode and cathode is 5~15cm.
6. the method according to claim 1, wherein the electrochemical stripping reaction apply voltage be 1~
20V。
7. the method according to claim 1, wherein the electrochemical stripping reaction time be 0.5~30h,
The temperature of electrolyte is 10~35 DEG C when electrochemical stripping reacts.
8. the method according to claim 1, wherein further including to oxidation stone after electrochemical stripping reaction
Black alkene aggregation is post-processed, it is described post-processing the following steps are included:
It is successively washed after the graphene oxide aggregation is separated, is ultrasonic and dry, obtaining graphene oxide powder
End.
9. according to the method described in claim 8, it is characterized in that, the power of the ultrasound be 80~150W, the time be 0.5~
2h。
10. according to the method described in claim 8, it is characterized in that, the temperature of the drying be -40~-20 DEG C, the time 24
~72h.
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| CN113603084A (en) * | 2021-08-24 | 2021-11-05 | 清华大学 | Method for electrochemically preparing graphene oxide |
| CN113816364A (en) * | 2021-10-20 | 2021-12-21 | 广东腐蚀科学与技术创新研究院 | Method for preparing aminosilane functionalized graphene through electrochemical stripping |
| CN113830755A (en) * | 2021-09-14 | 2021-12-24 | 广西师范大学 | Method for electrochemically preparing cobalt simple substance-graphene intercalation compound by one-step method |
| CN114408909A (en) * | 2022-03-02 | 2022-04-29 | 广西师范大学 | Method for preparing graphene by electrochemically stripping graphite |
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| CN113603084B (en) * | 2021-08-24 | 2024-01-02 | 清华大学 | Method for electrochemically preparing graphene oxide |
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| CN113830755B (en) * | 2021-09-14 | 2023-08-08 | 广西师范大学 | Method for electrochemically preparing cobalt simple substance-graphene intercalation compound by one-step method |
| CN113816364A (en) * | 2021-10-20 | 2021-12-21 | 广东腐蚀科学与技术创新研究院 | Method for preparing aminosilane functionalized graphene through electrochemical stripping |
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