CN110002439A - A kind of alkali metal salt assisting ultrasonic removing graphene and the preparation method and application thereof - Google Patents
A kind of alkali metal salt assisting ultrasonic removing graphene and the preparation method and application thereof Download PDFInfo
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- CN110002439A CN110002439A CN201910193013.8A CN201910193013A CN110002439A CN 110002439 A CN110002439 A CN 110002439A CN 201910193013 A CN201910193013 A CN 201910193013A CN 110002439 A CN110002439 A CN 110002439A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
Abstract
The invention discloses a kind of alkali metal salt assisting ultrasonic removing graphenes and the preparation method and application thereof, are related to the preparation and application field of graphene.Preparation method is that graphite powder and alkali metal salt are added in organic solvent, and ultrasound keeps graphite powder peeling-off;The alkali metal salt is pyrophosphate or phosphate;Products therefrom is centrifuged 5min-40min under the revolving speed of 1000r/min-8000r/min, precipitating is abandoned and supernatant is taken to remove graphene suspension to get to ultrasound.The pyrophosphate is sodium pyrophosphate or potassium pyrophosphate, and the phosphate is sodium phosphate or potassium phosphate, and the organic solvent is n,N-Dimethylformamide or N-Methyl pyrrolidone.Ultrasound of the invention removes graphene obtained, improves the charge stripping efficiency of graphene, effectively reduces the thickness of graphene, while increasing the active site of graphene, improves the electrochemical sensing performance of graphene.
Description
Technical field
The present invention relates to the preparation of graphene and application fields, shell more particularly, to a kind of alkali metal salt assisting ultrasonic
From graphene and the preparation method and application thereof.
Background technique
Graphene has excellent machinery, thermodynamics, optics and electronic property, if heat transfer is fast, electron transmission is fast, than
Surface area is big etc., thus is widely used in the fields such as energy storage, catalysis, sensing.The preparation method of graphene is generally divided into " under
On and " and " from top to bottom " two kinds of routes." from bottom to top " method is mainly using silicon carbide or small organic molecule as carbon source, certain
Under the conditions of so that carbon atom is reset or is connected, to obtain graphene, including outside chemical vapour deposition technique, silicon carbide
Epitaxial growth etc.." from top to bottom " method generally weakens graphite by modes such as Mechanical Method, chemical method, electrochemical process, ultrasound removings
Van der Waals force between layers, so that the removing of block-like graphite to be become to the graphene of single layer or few layer.Wherein, ultrasound removing
Method is that graphite powder is dispersed in liquid solvent, so that solvent molecule is inserted into graphite layers by the method for ultrasound, increases graphite linings
Spacing, to separate the graphene of few layer or single layer.It is compared with other methods, ultrasonic stripping method has easy to operate, preparation
Graphene oxygen content is low, the advantages that crystal form is good.But the graphene yield of ultrasonic stripping method preparation is lower, significantly limits
It develops and application.Studies have found that adding some up-stripping reagent such as ion salts in a solvent, stone can be effectively improved
The charge stripping efficiency of black alkene.Wherein, sodium citrate is a kind of common, preferable ion salt of up-stripping graphene effect.Have perhaps
More researchs remove graphene by sodium citrate assisting ultrasonic, have developed the application of ultrasonic removing graphene.However with its other party
Method is compared, and the yield of ultrasound removing graphene is not still high, therefore how to further increase the removing effect of ultrasound removing graphene
Rate, and then the yield of removing graphene is improved, it is still of great significance and full of challenge.
Summary of the invention
The present invention solves the technical problem that the ultrasonic charge stripping efficiency for removing graphene is low in the prior art.
According to the first aspect of the invention, a kind of preparation method of alkali metal assisting ultrasonic removing graphene is provided, is contained
There are following steps:
(1) graphite powder and alkali metal salt are added in organic solvent, ultrasound keeps the graphite powder peeling-off;The alkali
Metal salt is pyrophosphate or phosphate;
(2) step (1) products therefrom is centrifuged 5min-40min under the revolving speed of 1000r/min-8000r/min, it is heavy to abandon
Shallow lake takes supernatant to remove graphene suspension to get to ultrasound.
Preferably, pyrophosphate described in step (1) is sodium pyrophosphate or potassium pyrophosphate, phosphate described in step (1)
For sodium phosphate or potassium phosphate.
Preferably, organic solvent described in step (1) is n,N-Dimethylformamide or N-Methyl pyrrolidone.
Preferably, the power of the ultrasound is 50W-600W, and the time of the ultrasound is 1h-40h.
Preferably, after step (1) described graphite powder is added to organic solvent, the concentration of the graphite powder is 0.5-50mg
mL-1。
Preferably, after step (1) described alkali metal salt is added to organic solvent, the concentration of the alkali metal salt is 0.5-
50mg mL-1。
It is another aspect of this invention to provide that providing the alkali metal salt assisting ultrasonic removing graphite that the method is prepared
Alkene.
It is another aspect of this invention to provide that providing the alkali metal salt assisting ultrasonic removing graphene for modifying electrification
Learn the application of sensor.
Preferably, the alkali metal salt assisting ultrasonic removes graphene modified on the working electrode (s.
Preferably, the working electrode is glass-carbon electrode.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, can obtain down and show
Beneficial effect:
(1) present invention removes graphene by adding alkali metal salt in a solvent come assisting ultrasonic, improves graphene
Charge stripping efficiency, to improve the yield of graphene.Graphene yield prepared by the present invention is 4.25%, is made than in the prior art
The yield (3.25%) that sodium citrate up-stripping obtains is higher, is the ultrasound removing graphene of no salt auxiliary
(0.9%) 4.7 times.The ultrasound removing graphene degree of oxidation that the present invention is prepared is low, and crystalline structure is complete, therefore electronics
Transmission speed is fast.
(2) present invention preferably selects alkali metal pyrophosphate salts to remove graphite powder, with other synperiodic metal ion phases
It is more maximum than the size of, alkali metal ion, be conducive to intercalation and enter graphite layers to make graphite expansion, accelerates the removing of graphene.This
Invention preferably selects N-Methyl pyrrolidone as removing solvent, which is up to 40.1mJ m-2, often with other
With solvent, (surface can generally be less than 40mJ m-2) compare, N-Methyl pyrrolidone and graphene surface can (about 70-80mJ m-2) matching degree is higher, therefore it is preferable to remove graphene effect.
(3) present invention removes graphene by adding alkali metal salt in a solvent come assisting ultrasonic, and it is smaller to have obtained thickness
Graphene, while the defect content of graphene increases, and active site increases.Therefore the ultrasound removing stone that the present invention is prepared
The glass-carbon electrode of black alkene modification has more excellent electrochemical properties, and such as bigger electrode active area and stronger electricity are urged
Change ability.Therefore the electrochemical sensing performance of graphene is improved.
(4) the ultrasound removing graphene that the present invention is prepared realizes phenols pollution for modifying electrochemical sensor
Object parachlorophenol and the quick, sensitive of p-nitrophenol detect simultaneously, and detection limit is respectively 21nM and 440nM;Biological micromolecule
Dopamine, uric acid, xanthine, it is hypoxanthic it is quick, sensitive detect simultaneously, detection limit be respectively 0.3nM, 0.4nM, 21nM,
25nM;Synthetic dyestuff famille rose and the quick, sensitive of rhodamine B detect simultaneously, and detection limit is respectively 1.7nM and 3.2nM;And
The highly sensitive detection of dyestuff malachite green, detection are limited to 23nM.
(5) one sample of the detection methods such as existing liquid chromatogram detection needs or so half an hour, based on present invention system
The electrochemical sensor of standby obtained ultrasound removing graphene can realize the direct quick detection to sample, when entire sample analysis
Between be less than 5min, meet the quick detection requirement in scene.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture for the graphene nanometer sheet that the ultrasound that embodiment 1 is prepared separates.
Fig. 2 is the scanning electron microscope (SEM) photograph for the graphene nanometer sheet that the ultrasound that embodiment 1 is prepared separates.
Fig. 3 is the graphene nanometer sheet that comparative example 1 and comparative example 2, embodiment 2, the method ultrasound of embodiment 1 separate
(being respectively labeled as GS-1, GS-2, GS-3, GS-4) dilutes the ultraviolet-visible spectrum after 30 times.
Fig. 4 is the graphene nanometer sheet that comparative example 1 and comparative example 2, embodiment 2, the method ultrasound of embodiment 1 separate
The raman spectrum of (being respectively labeled as GS-1, GS-2, GS-3, GS-4).
Fig. 5 (a), Fig. 5 (b), Fig. 5 (c), Fig. 5 (d) and Fig. 5 (e) be respectively unmodified glass-carbon electrode, comparative example 1,
The graphite that the method ultrasound of comparative example 2, embodiment 2 and embodiment 1 (being respectively labeled as GS-1, GS-2, GS-3, GS-4) separates
On the glass-carbon electrode of alkene nanometer sheet modification, the potassium ferricyanide sweeps the cyclic voltammetry curve under speed in difference;Fig. 5 (f) is in different electricity
Extremely upper potassium ferricyanide oxidation peak and the subduplicate relationship for sweeping speed.
Fig. 6 (a), Fig. 6 (b), Fig. 6 (c), Fig. 6 (d) and Fig. 6 (e) are in unmodified rotating disk electrode (r.d.e), comparison respectively
Example 1, comparative example 2, the method ultrasound of embodiment 2 and embodiment 1 (being respectively labeled as GS-1, GS-2, GS-3, GS-4) separate
In the rotating disk electrode (r.d.e) of graphene nanometer sheet modification, linear sweep voltammetry curve of the potassium ferricyanide under different rotating speeds;Fig. 6
(f) be potassium ferricyanide current density and revolving speed inverse square root on Different electrodes relationship.
Fig. 7 (a), Fig. 7 (b), Fig. 7 (c) and Fig. 7 (d) are unmodified glass-carbon electrode, comparative example 1, comparative example 2, reality respectively
Apply example 2, graphene nanometer sheet (being respectively labeled as GS-1, GS-2, GS-3, GS-4) that the method ultrasound of embodiment 1 separates it is right
Phenolic comp ' ds pollution (parachlorophenol and p-nitrophenol), biological micromolecule (dopamine, uric acid, xanthine, hypoxanthine), synthesis
The differential pulse curve of pigment (carmine and rhodamine B) and dyestuff malachite green.
Fig. 8 (a), Fig. 8 (b), Fig. 8 (c) and Fig. 8 (d), Fig. 8 (e), Fig. 8 (f), Fig. 8 (g), Fig. 8 (h) and Fig. 8 (i) are respectively
Be the dopamine of various concentration, uric acid, xanthine, hypoxanthine, parachlorophenol, p-nitrophenol, famille rose, rhodamine B, with
And malachite green is on the electrochemical sensor for ultrasound removing graphene nanometer sheet (GS-4) modification that embodiment 1 is prepared
Differential pulse voltammetry curve, interior illustration are its linear fit curves.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
Embodiment 1
Graphite powder and sodium pyrophosphate are added in the sample bottle equipped with N-Methyl pyrrolidone, graphite powder in a solvent dense
Degree is 20mg mL-1, the concentration of sodium pyrophosphate in a solvent is 20mg mL-1.The ultrasound 2h in the ultrasonic device that power is 100W,
Obtain suspension.Resulting mixed liquor is centrifuged 20min under the centrifugal rotational speed of 2000r/min, supernatant is taken to obtain graphene
Suspension.Fig. 1 and Fig. 2 is transmission electron microscope picture and the scanning for the graphene nanometer sheet that the method ultrasound of embodiment 1 separates respectively
Electron microscope.It can be observed that thin nanometer sheet of uniform size, show graphite powder be successfully stripped for graphene.
Using the sodium salt assisting ultrasonic of above-mentioned preparation removing graphene modified glass-carbon electrode as working electrode, using common
Three-electrode system, as reference electrode, platinum column electrode is used as to electrode saturated calomel electrode, carries out electro-chemical test.
Embodiment 2
Graphite powder and sodium phosphate are added in the sample bottle equipped with N-Methyl pyrrolidone, the concentration of graphite powder in a solvent
For 20mg mL-1, the concentration of potassium phosphate in a solvent is 20mg mL-1.The ultrasound 2h in the ultrasonic device that power is 100W, obtains
Mixed liquor.Resulting mixed liquor is centrifuged 20min under the centrifugal rotational speed of 2000r/min, supernatant is taken to obtain graphene suspension
Liquid.
Embodiment 3
Graphite powder and potassium pyrophosphate be added in the sample bottle equipped with n,N-Dimethylformamide, graphite powder is in a solvent
Concentration is 50mg mL-1, the concentration of sodium pyrophosphate in a solvent is 50mg mL-1.The ultrasound in the ultrasonic device that power is 600W
40h obtains mixed liquor.Resulting mixed liquor is centrifuged 40min under the centrifugal rotational speed of 8000r/min, supernatant is taken to obtain stone
Black alkene suspension.
Embodiment 4
Graphite powder and potassium phosphate are added in the sample bottle equipped with N-Methyl pyrrolidone, the concentration of graphite powder in a solvent
For 10mg mL-1, the concentration of sodium pyrophosphate in a solvent is 10mg mL-1.The ultrasound 1h in the ultrasonic device that power is 50W, obtains
Mixed liquor.Resulting mixed liquor is centrifuged 5min under the centrifugal rotational speed of 1000r/min, supernatant is taken to obtain graphene suspension
Liquid.
Comparative example 1
Other are with embodiment 1, the difference is that the first step does not add any alkali metal salt.By Fig. 3, comparative example 1 and comparative example
2, the graphene nanometer sheet that embodiment 2, the method ultrasound of embodiment 1 separate (is respectively labeled as GS-1, GS-2, GS-3, GS-
4) ultraviolet-visible spectrum after 30 times is diluted, it can be seen that the graphene suspension absorbance of gained the method preparation is small, explanation
Graphene concentration is low, that is, graphene removing yield is very low, and only 0.9%, and the yield of embodiment 1 has reached 4.25%,
Illustrate that the auxiliary energy of sodium pyrophosphate significantly improves the yield of ultrasound removing graphene.By Fig. 4, comparative example 1 and comparative example 2 are implemented
The drawing for the graphene nanometer sheet (being respectively labeled as GS-1, GS-2, GS-3, GS-4) that example 2, the method ultrasound of embodiment 1 separate
Graceful spectrogram, the ratio between the peak D and G peak intensity of available GS-1 (ID/IG) be only 0.30, than other methods preparation graphene all
It is smaller, illustrate that the graphene defect content of this method preparation is minimum, active site is minimum.In addition, in Fig. 4, the D ' of GS-1
Peak intensity is minimum, illustrates that the number of plies of the graphene of this method preparation is most, this conclusion is also by GS-1 relative to other graphite
The more asymmetric and broad peak 2D of alkene is confirmed.
Comparative example 2
Other are with embodiment 1, the difference is that first step alkali metal salt is sodium citrate.By Fig. 3, comparative example 1 and comparative example
2, the graphene nanometer sheet that embodiment 2, the method ultrasound of embodiment 1 separate (is respectively labeled as GS-1, GS-2, GS-3, GS-
4) ultraviolet-visible spectrum after 30 times is diluted, it can be seen that the dulling luminosity ratio GS-1 of GS-2 is significantly improved, and illustrates sodium citrate
Graphene yield can be effectively improved, can reach 3.25%.But still it is significantly less than the graphene of sodium pyrophosphate assisting ultrasonic removing
(yield is up to 4.25%).By Fig. 4, graphite that comparative example 1 and comparative example 2, embodiment 2, the method ultrasound of embodiment 1 separate
The raman spectrum of alkene nanometer sheet (being respectively labeled as GS-1, GS-2, GS-3, GS-4), the peak D and G peak intensity of available GS-2
The ratio between (ID/IG) it is 0.39, it is significantly less than the 0.49 of embodiment 1, illustrates that the defect content of GS-4 is higher.It is calculated by Fig. 5
It arrives, the electrode active area of GS-2 and GS-4 are respectively 0.81cm2And 0.85cm2, that is, the graphite that embodiment 1 is prepared
Alkene active area is bigger.It is calculated by Fig. 6, the heterogeneous electron transfer rate constant k of GS-2 and GS-4 are respectively 0.029cm
s-1With 0.084cm s-1, illustrate that the graphene that embodiment 1 is prepared has stronger electro-catalysis ability.To sum up, with right
The graphene that ratio 2 is prepared is compared, and the graphene yield that embodiment 1 is prepared is higher, and defect content is higher, electrochemistry
Active site is more, and electro-catalysis ability is stronger.
Fig. 3 is the graphene nanometer sheet that comparative example 1 and comparative example 2, embodiment 2, the method ultrasound of embodiment 1 separate
(being respectively labeled as GS-1, GS-2, GS-3, GS-4) dilutes the ultraviolet-visible spectrum after 30 times, and absorbance is respectively 0.18mg
mL-1、0.65mg mL-1、0.75mg mL-1、0.85mg mL-1, thus calculate graphene yield be respectively 0.9%, 3.25%,
3.75%, 4.25%.Obviously, the graphene concentration obtained by embodiment 1 is maximum.That is, embodiment 1 prepares graphene
The sodium citrate up-stripping that is commonly used of productivity ratio, i.e. method auxiliaring effect in comparative example 2 is higher, does not have about
Sodium salt auxiliary, i.e. 4.7 times of the ultrasound removing graphene of method in comparative example 1.
Fig. 4 is that the graphene nanometer sheet that comparative example 1 and comparative example 2, embodiment, the method ultrasound of embodiment 1 separate (divides
Biao Ji not be, GS-2, GS-3, GS-4) raman spectrum.The peak GS-1, GS-2, GS-3, GS-4D and the peak G are calculated by Fig. 4
Intensity ratio (ID/IG) it is respectively 0.30,0.39,0.41,0.49.The wherein I of GS-4D/IGMaximum illustrates its defect content most
Height, that is, active site are most.Compared with comparative example 1, comparative example 2, embodiment 2, the peak graphene 2D peak that embodiment 1 obtains
Type is also more symmetrical, and in conjunction with the maximum intensity at its peak D ', it is less to further illustrate the graphene number of plies that embodiment 1 obtains.
Fig. 5 (a), Fig. 5 (b), Fig. 5 (c), Fig. 5 (d) and Fig. 5 (e) be respectively unmodified glass-carbon electrode, comparative example 1,
The graphite that the method ultrasound of comparative example 2, embodiment 2 and embodiment 1 (being respectively labeled as GS-1, GS-2, GS-3, GS-4) separates
On the glass-carbon electrode of alkene nanometer sheet modification, the potassium ferricyanide sweeps the cyclic voltammetry curve under speed in difference;Fig. 5 (f) is in different electricity
Extremely upper potassium ferricyanide oxidation peak and the subduplicate relationship for sweeping speed.GS-1, GS-2, GS- can be obtained by the matched curve of Fig. 5 (f)
3, the electrochemical surface area of GS-4, respectively 0.071cm2、0.081cm2、0.082cm2、0.085cm2.The wherein electricity of GS-4
Pole active area is maximum, and the graphene electro-chemical activity for illustrating that embodiment 1 obtains is good, is most suitable for the system for electrochemical sensor
It is standby.
Fig. 6 (a), Fig. 6 (b), Fig. 6 (c), Fig. 6 (d) and Fig. 6 (e) are in unmodified rotating disk electrode (r.d.e), comparison respectively
Example 1, comparative example 2, the method ultrasound of embodiment 2 and embodiment 1 (being respectively labeled as GS-1, GS-2, GS-3, GS-4) separate
In the rotating disk electrode (r.d.e) of graphene nanometer sheet modification, linear sweep voltammetry curve of the potassium ferricyanide under different rotating speeds;Fig. 6
(f) be -1/2 power of potassium ferricyanide current density and revolving speed on Different electrodes relationship.Pass through Fig. 6 (f) matched curve meter
Calculate heterogeneous electron transfer rate constant k, respectively 0.029cm s of the potassium ferricyanide on GS-1, GS-2, GS-3, GS-4-1、
0.057cm s-1、0.059cm s-1、0.084cm s-1.Wherein the k value of GS-4 is maximum, indicates its strongest catalytic capability.Explanation
The graphene electro-catalysis ability obtained by embodiment 1 is most strong, is easier to occur in the reaction of its surface oxidation reduction.
Fig. 7 (a), Fig. 7 (b), Fig. 7 (c) and Fig. 7 (d) are unmodified glass-carbon electrode, comparative example 1, comparative example 2, reality respectively
Apply example 2, the graphene nanometer sheet that the method ultrasound of embodiment 1 separates (is respectively labeled as GCE, GS-1, GS-2, GS-3, GS-
4) to biological micromolecule (dopamine, uric acid, xanthine, hypoxanthine), phenolic comp ' ds pollution (parachlorophenol and p-nitrophenol),
The differential pulse voltammetry curve of synthetic dyestuff (carmine and rhodamine B) and dyestuff malachite green.This nine kinds of small organic molecules
There is maximum oxidation peak current value on GS-4 modified electrode.That is, the graphene obtained by embodiment 1 to this nine
The electrochemistry effect of enhanced sensitivity of kind small organic molecule is best.
Fig. 8 (a), Fig. 8 (b), Fig. 8 (c) and Fig. 8 (d), Fig. 8 (e), Fig. 8 (f), Fig. 8 (g), Fig. 8 (h) and Fig. 8 (i) are respectively
Be the dopamine of various concentration, uric acid, xanthine, hypoxanthine, parachlorophenol, p-nitrophenol, famille rose, rhodamine B, with
And malachite green is on the electrochemical sensor for ultrasound removing graphene nanometer sheet (GS-4) modification that embodiment 1 is prepared
Differential pulse voltammetry curve, interior illustration are its linear fit curves.It is 0.02-10.00 μM that the dopamine range of linearity, which is calculated,
Detection is limited to 0.3nM, and the uric acid range of linearity is 0.025-20.00 μM, and detection is limited to 0.4nM, and the xanthine range of linearity is 0.05-
20.00 μM, detection is limited to 21nM, and the hypoxanthine range of linearity is 0.10-50.00 μM, and detection is limited to 25nM.Parachlorophenol is linear
Range is 0.20-10.00 μM, and detection is limited to 21nM, and the p-nitrophenol range of linearity is 1.00-25.00 μM, and detection is limited to
440nM.The carmine range of linearity is 0.005-1.00 μM, and detection is limited to 1.7nM, and the rhodamine B range of linearity is 0.01-2.00 μ
M, detection is limited to 3.2nM and the malachite green range of linearity is 0.10-2.00 μM, and detection is limited to 22nM.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of alkali metal salt assisting ultrasonic removing graphene, which is characterized in that contain following steps:
(1) graphite powder and alkali metal salt are added in organic solvent, ultrasound keeps the graphite powder peeling-off;The alkali metal
Salt is pyrophosphate or phosphate;
(2) step (1) products therefrom is centrifuged under the revolving speed of 1000r/min-8000r/min 5min-40min, abandons precipitating and takes
Supernatant removes graphene suspension to get to ultrasound.
2. the preparation method of alkali metal salt assisting ultrasonic removing graphene as described in claim 1, which is characterized in that step
(1) pyrophosphate described in is sodium pyrophosphate or potassium pyrophosphate, and phosphate described in step (1) is sodium phosphate or potassium phosphate.
3. the preparation method of alkali metal salt assisting ultrasonic removing graphene as described in claim 1, which is characterized in that step
(1) organic solvent described in is N,N-dimethylformamide or N-Methyl pyrrolidone.
4. the preparation method of alkali metal salt assisting ultrasonic removing graphene as described in claim 1, which is characterized in that described super
The power of sound is 50W-600W, and the time of the ultrasound is 1h-40h.
5. the preparation method of alkali metal salt assisting ultrasonic removing graphene as described in claim 1, which is characterized in that step
(1) after the graphite powder is added to organic solvent, the concentration of the graphite powder is 0.5-50mg mL-1。
6. the preparation method of alkali metal salt assisting ultrasonic removing graphene as described in claim 1, which is characterized in that step
(1) after the alkali metal salt is added to organic solvent, the concentration of the alkali metal salt is 0.5-50mg mL-1。
7. the alkali metal salt assisting ultrasonic that any the method for claim 1-6 is prepared removes graphene.
8. the application that the removing graphene of alkali metal salt assisting ultrasonic described in claim 7 is used to modify electrochemical sensor.
9. application as claimed in claim 8, which is characterized in that the alkali metal salt assisting ultrasonic removing graphene modified is in work
Make on electrode.
10. application as claimed in claim 9, which is characterized in that the working electrode is glass-carbon electrode.
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Cited By (1)
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CN115403036A (en) * | 2022-08-30 | 2022-11-29 | 中钢集团南京新材料研究院有限公司 | Device and method for continuous electrochemical stripping and application |
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US10081551B2 (en) * | 2016-07-15 | 2018-09-25 | Nanotek Instruments, Inc. | Supercritical fluid process for producing graphene from coke or coal |
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