CN107117603B - It is a kind of to peel off method of the grading system for graphene using pulse ultrasonic wave - Google Patents
It is a kind of to peel off method of the grading system for graphene using pulse ultrasonic wave Download PDFInfo
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- CN107117603B CN107117603B CN201710456112.1A CN201710456112A CN107117603B CN 107117603 B CN107117603 B CN 107117603B CN 201710456112 A CN201710456112 A CN 201710456112A CN 107117603 B CN107117603 B CN 107117603B
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/02—Single layer graphene
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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
- C01B2204/04—Specific amount of layers or specific thickness
Abstract
The invention belongs to technical field of graphene preparation, there is provided a kind of to peel off method of the grading system for graphene using pulse ultrasonic wave.Natural flake graphite is dispersed in water by this method by using decentralized medium, applies high-frequency impulse ultrasonic wave, graphite slurries is produced the higher-order of oscillation, cavitation bubble is formed in liquid phase.Cavitation bubble collapse produces the high-speed micro-jet for pointing to graphite surface, produces local failure to its surface, graphite finally is isolated into graphene on upper strata to upper strata phased separation by bottom.Compared with conventional method, the invented technology is simple, and cost is low, while can overcome that graphene charge stripping efficiency is low, the time is long, the defects of being difficult to continuously peel off.
Description
Technical field
The present invention relates to the preparing technical field of graphene, and grading system is peeled off using pulse ultrasonic wave more particularly, to one kind
The method of standby graphene.
Background technology
In recent years, application of the ultrasonic wave in terms of material preparation is more and more.It is its simple to operate, efficiency high, easily controllable,
And can produce " cavitation effect ", because the life-span of cavitation bubble only has 0.1 μ s, instantaneous explosion, huge energy is discharged, it is caused micro-
Effluxvelocity is up to 110m/s, and collision density is up to 1.5kg/cm2.Therefore, ultrasonic wave can be used for peeling off preparing graphite alkene.
At present, for up-stripping prepared by ultrasonic wave into graphene to have studied.Because ultrasonic energy is impartial, when peeling off to having shelled
From graphene peel off repeatedly, to graphite, then stripping ability is inadequate, so as to directly affect charge stripping efficiency, be currently only used for auxiliary stripping
From graphite oxide.
Cai etc. is by highly oriented pyrolytic graphite（HOPG）Between being fixed on two substrates up and down with two-sided tape, ultrasound is put into
Wave producer, and be dipped in deionized water, in power 0.1 ~ 2 × 105Under J, temperature is 10 ~ 40 DEG C, starts supersonic generator,
And oscillation crosswise is carried out, it is fixed on by HOPG and upper substrate separation, and with two-sided tape under new upper substrate.Repeat 5 ~ 10
It is secondary, the graphene having good uniformity has been made.Xu etc. is prepared come graphene by the use of series compounds such as naphthalenes as intercalator first,
By the uniformly mixing in organic solvent by a certain percentage of powdered graphite and intercalator, ultrasound bath is recycled to be peeled off, one
Centrifuge, filter after fixing time, grapheme material is made.Graphene made from the technology has that fault of construction is few, impurity contains
The advantages that measuring low, excellent performance, quality balance.Wang etc. has invented ultrasonic assistant compression CO2The side of fluid preparation graphene
Method, first by CO2It is injected between graphite linings gap, then realizes that graphite is peeled off under the booster action of ultrasonic wave to form graphene,
The advantage of this method is that preparation condition is gentle, processing time is short, and required pressure is small, efficiency high, and quality is good, and energy-conserving and environment-protective can
Accomplish scale production, and protect the structural behaviour of graphene not to be destroyed.
It can be seen that ultrasonic wave prepares stage of the graphene also in up-stripping for stripping, main cause is because its energy
Amount is impartial, and impulse ultrasound wave energy overcomes this defect.At present, prepare graphene on pulse ultrasonic wave stripping and yet there are no report
Road.Some scholars are studied with regard to pulse laser scanning preparing graphite alkene, achieve certain progress.Ren etc. is by graphite
Powder mixes with solvent in reaction vessel, carries out sonic oscillation, then starts agitator, make graphite powder full and uniform in a solvent
Distribution.Then laser optical path is adjusted, laser beam is focused on successively after total reflective mirror and focus lens below liquid level at 3mm.Again
Unbalanced pulse laser, adjusting different laser energies makes laser irradiate the graphite particle in liquid environment, after reacting 1 ~ 2h, closes
Laser, the graphene of the different numbers of plies is made.Qiao etc. realizes to be prepared using pulse laser scanning graphite suspension mixed solution
Graphene, graphite suspension mixed solution is prepared first, and circulate graphite suspension mixed solution uniformly continuous using circulating pump, so
Pulse laser is focused under liquid level afterwards, scan round graphite suspension mixed solution, recycle gravitational separation process by the supernatant of acquisition
Liquid is separated and drying process, you can the graphite of the few individual layer of structural integrity, oxygen-containing functional group or few layer (being less than 6 layers) is made
Alkene.
The content of the invention
It is low that graphene charge stripping efficiency is prepared for existing ultrasonic stripping, it is difficult to which the defects of serialization volume production, the present invention proposes
It is a kind of to peel off method of the grading system for graphene using pulse ultrasonic wave.It is essentially consisted in natural squama by using decentralized medium
Piece graphite is dispersed in water, and applies high-frequency impulse ultrasonic wave, graphite slurries is produced the higher-order of oscillation, cavitation gas is formed in liquid phase
Bubble.Cavitation bubble collapse produces the high-speed micro-jet for pointing to graphite surface, local failure is produced to its surface, by graphite by bottom
To upper strata phased separation, finally graphene is continuously isolated on upper strata.Can solve conventional ultrasound stripping means and prepare graphene
Charge stripping efficiency is low, the time is long, the shortcomings that being difficult to continuously peel off, most important, and creative application pulse ultrasonic wave grading system is standby
Graphene, has broken ultrasonic wave and is only used for up-stripping and prepare the limitation of graphene, and avoids repetition stripping, obtained stone
Black alkene individual layer and 2 ~ 5 layers of content are higher.
Concrete technical scheme of the present invention is as follows：
It is a kind of to peel off method of the grading system for graphene using pulse ultrasonic wave, by using decentralized medium by natural scale
Graphite dispersion applies high-frequency impulse ultrasonic wave in water, graphite slurries is produced the higher-order of oscillation, cavitation bubble is formed in liquid phase.
Because the size of graphite is more much bigger than the size of cavitation bubble, the collapse of the cavitation bubble near graphite is asymmetrical, so that
The high-speed micro-jet for pointing to graphite surface is produced, local failure is produced to its surface, high-frequency impulse ultrasound, produces graphite slurries
The higher-order of oscillation, and because oscillating impulse frequency difference forms multilayer in a reservoir, continuously peel off graphite into graphene, and from the bottom of by
Layer progressively arrives upper strata graphite phased separation, finally continuously isolates graphene on upper strata；What is prepared comprises the following steps that：
（1）Natural scale graphite is mixed with deionized water, after sand mill grinding 10min, adds the polyethers of certain mass
Hydramine, magnetic agitation are uniformly dispersed；
（2）By step（1）The dispersion liquid of gained is placed in impulse ultrasound wave generating device, and uses cold bath, is made anti-
Temperature is answered to maintain 20 DEG C or so.Unbalanced pulse Vltrasonic device, because oscillating impulse frequency forms multilayer in a reservoir, continuously by stone
Ink is peeled off into graphene, and progressively produces high rapid fire to upper strata graphite phased separation, caused cavitation bubble rupture in by bottom
Stream, graphite phased separation is into graphene；
（3）Graphene is continuously isolated on upper strata, the solid for taking upper liquid to isolate, filtering, washing, and in 60 DEG C of temperature
Dried under degree and -0.09MPa vacuum, what is obtained is the graphene product peeled off, while steady with 20-45ml/s in bottom
Inject calmly by step（1）The graphite dispersing solution of preparation.
Preferably, step（1）The mass ratio of the polyethers hydramine and water is 1：3~1：4；
Preferably, step（1）The addition quality of the natural flake graphite be the quality summation of polyethers hydramine and water 2% ~
4%.
Preferably, step（2）The frequency of the pulse ultrasonic wave is to divide three layers, respectively 40kHz, 50kHz from bottom to top,
60kHz, power are 100 ~ 200W.
Preferably, step（3）The bottom is with the stable injections of 35ml/s by step（1）The graphite dispersing solution of preparation.
Ultrasonic wave can produce high-frequency mechanical vibration, produce cavitation effect by vibrating, excite particulate high vibration.Ultrasound
Ripple is propagated forward density interphase in a liquid, and stretching and squeezing action are produced to liquid, makes generation in liquid ten hundreds of
Micro-bubble.These bubbles produce rapidly, and rapid closing, the instantaneous pressure of formation, superatmospheric 1000 times.Continuously not
Disconnected high pressure constantly impacts object surface, makes the superficial layer rapid deterioration of object just as a succession of small " blast ".It is former using this
Reason, so as to realize the stripping of graphene.But because ultrasonic energy is impartial, the graphene peeled off is shelled repeatedly when peeling off
From to graphite, then stripping ability is inadequate, so as to directly affect charge stripping efficiency.The present invention is using the stronger impulse ultrasound of release effect
Ripple, classification stripping is carried out to crystalline flake graphite.By introducing polyethers hydramine assisted milling, and the lamellar structure of graphene can be protected
Integrality.Because the size of crystalline flake graphite is far longer than the cavitation bubble size formed in dispersion liquid, the sky of its near surface
The rupture for changing bubble is non-spherical symmetric, and so as to produce high-speed jet, powerful impact force action is compeled in flake graphite's surface
It is set to separate graphene.Pulse ultrasonic wave continuously shells graphite because oscillating impulse frequency forms stable multilayer in a reservoir
, progressively to upper strata graphite phased separation, finally graphene is continuously isolated from into graphene, and from by bottom on upper strata；Form
Continuously prepare graphene.Different stripping ranks more preferably is in each layer graphite, by controlling bottom injection rate and upper strata
Take liquid measure so that the graphene of acquisition is quality controllable, can obtain single-layer graphene, 2-5 layer graphenes, graphene microchip.It is and each
The grapheme material of class rank is evenly distributed.In dispersion liquid, the crystalline flake graphite in lower floor is first stripped, the graphene separated
Density be less than crystalline flake graphite, its to dispersion liquid top shift.The thickness of graphene is smaller, and its density is smaller, therefore, with stripping
From progress, graphite and graphene in dispersion liquid with density distribution gradient, caused by the pulse ultrasonic wave that more lower floor is subject to
Impulsive force is stronger, more easily peelable, and so as to realize that the classification of crystalline flake graphite is peeled off, obtained graphene thickness distribution is more uniform.
Method of the grading system for graphene is peeled off using pulse ultrasonic wave the invention provides a kind of, with prior art phase
Than, its protrude the characteristics of and excellent effect be：
1. the pulse ultrasonic wave classification strip preparation method that the present invention uses compensate for ultrasonic wave can only up-stripping preparation
The defects of graphene, simplify technical process, be advantageously implemented large-scale production.
2. the classification stripping means that the present invention uses can effectively avoid peeling off the repetition for having peeled off graphene, obtained
Individual layer and 2 ~ 5 layers of content are higher in graphene product.
3. the preparation process technique of the present invention is simple, environmental protection and energy saving, cost is reduced, industrialized production can be achieved.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should not be interpreted as to the present invention
Scope be only limitted to following example.In the case where not departing from above method thought of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A kind of to peel off method of the grading system for graphene using pulse ultrasonic wave, it is classified stripping and prepares the specific of graphene
Process is as follows：
（1）Natural scale graphite is mixed with deionized water, after sand mill grinding 10min, adds the polyethers of certain mass
Hydramine, magnetic agitation are uniformly dispersed；The mass ratio of the polyethers hydramine and water is 1：3；
（2）By step（1）The dispersion liquid of gained is placed in impulse ultrasound wave generating device, the frequency of the pulse ultrasonic wave
To divide three layers, respectively 40kHz, 50kHz, 60kHz from bottom to top, power is 100W and uses cold bath rate, makes reaction temperature
Maintain 20 DEG C or so.Unbalanced pulse Vltrasonic device, because oscillating impulse frequency forms multilayer in a reservoir, continuously graphite is peeled off
Progressively high-speed jet, graphite are produced into graphene, and in by bottom to upper strata graphite phased separation, caused cavitation bubble rupture
Phased separation is into graphene；
（3）Graphene is continuously isolated on upper strata, the solid for taking upper liquid to isolate, filtering, washing, and in 60 DEG C of temperature
Dried under degree and -0.09MPa vacuum, what is obtained is the graphene product peeled off, while stable with 20ml/s in bottom
Injection is by step（1）The graphite dispersing solution of preparation.
Method classification to embodiment 1 peels off the graphene being prepared and carries out testing graininess, obtains the middle grain of graphene
The data in footpath are as shown in table 1；Method classification to embodiment 1 peels off the graphene being prepared and carries out structured testing and analysis,
The content for obtaining individual layer and 2 ~ 5 layer graphenes is as shown in table 1.
Embodiment 2
A kind of to peel off method of the grading system for graphene using pulse ultrasonic wave, it is classified stripping and prepares the specific of graphene
Process is as follows：
（1）Natural scale graphite is mixed with deionized water, after sand mill grinding 10min, adds the polyethers of certain mass
Hydramine, magnetic agitation are uniformly dispersed；The mass ratio of polyethers hydramine and water is 1：4；The addition quality of natural flake graphite is polyethers
The 2% of the quality summation of hydramine and water；
（2）By step（1）The dispersion liquid of gained is placed in impulse ultrasound wave generating device, the frequency of the pulse ultrasonic wave
Rate is to divide three layers, respectively 40kHz, 50kHz, 60kHz, power 200W from bottom to top；And cold bath is used, make reaction temperature
Maintain 20 DEG C or so.Unbalanced pulse Vltrasonic device, because oscillating impulse frequency forms multilayer in a reservoir, continuously graphite is peeled off
Progressively high-speed jet, graphite are produced into graphene, and in by bottom to upper strata graphite phased separation, caused cavitation bubble rupture
Phased separation is into graphene；
（3）Graphene is continuously isolated on upper strata, the solid for taking upper liquid to isolate, filtering, washing, and in 60 DEG C of temperature
Dried under degree and -0.09MPa vacuum, what is obtained is the graphene product peeled off, while stable with 30ml/s in bottom
Injection is by step（1）The graphite dispersing solution of preparation.
Method classification to embodiment 2 peels off the graphene being prepared and carries out testing graininess, obtains the middle grain of graphene
The data in footpath are as shown in table 1；Method classification to embodiment 2 peels off the graphene being prepared and carries out structured testing and analysis,
The content for obtaining individual layer and 2 ~ 5 layer graphenes is as shown in table 1.
Embodiment 3
A kind of to peel off method of the grading system for graphene using pulse ultrasonic wave, it is classified stripping and prepares the specific of graphene
Process is as follows：
（1）Natural scale graphite is mixed with deionized water, after sand mill grinding 10min, adds the polyethers of certain mass
Hydramine, magnetic agitation are uniformly dispersed；The mass ratio of the polyethers hydramine and water is 1：3；The addition matter of the natural flake graphite
Measure 4% of the quality summation for decentralized medium and water；
（2）By step（1）The dispersion liquid of gained is placed in impulse ultrasound wave generating device, the frequency of the pulse ultrasonic wave
Rate is to divide three layers, respectively 40kHz, 50kHz, 60kHz, power 200W from bottom to top；And cold bath is used, make reaction temperature
Maintain 20 DEG C or so.Unbalanced pulse Vltrasonic device, because oscillating impulse frequency forms multilayer in a reservoir, continuously graphite is peeled off
Progressively high-speed jet, graphite are produced into graphene, and in by bottom to upper strata graphite phased separation, caused cavitation bubble rupture
Phased separation is into graphene；
（3）Graphene is continuously isolated on upper strata, the solid for taking upper liquid to isolate, filtering, washing, and in 60 DEG C of temperature
Dried under degree and -0.09MPa vacuum, what is obtained is the graphene product peeled off, while stable with 35ml/s in bottom
Injection is by step（1）The graphite dispersing solution of preparation.
Method classification to embodiment 3 peels off the graphene being prepared and carries out testing graininess, obtains the middle grain of graphene
The data in footpath are as shown in table 1；Method classification to embodiment 3 peels off the graphene being prepared and carries out structured testing and analysis,
The content for obtaining individual layer and 2 ~ 5 layer graphenes is as shown in table 1.
Embodiment 4
A kind of to peel off method of the grading system for graphene using pulse ultrasonic wave, it is classified stripping and prepares the specific of graphene
Process is as follows：
（1）Natural scale graphite is mixed with deionized water, after sand mill grinding 10min, adds the polyethers of certain mass
Hydramine, magnetic agitation are uniformly dispersed；The mass ratio of the polyethers hydramine and water is 1：4；The addition quality of natural flake graphite is
The 3% of the quality summation of decentralized medium and water；
（2）By step（1）The dispersion liquid of gained is placed in impulse ultrasound wave generating device, the frequency of the pulse ultrasonic wave
Rate is to divide three layers, respectively 40kHz, 50kHz, 60kHz, power 150W from bottom to top；And cold bath is used, make reaction temperature
Maintain 20 DEG C or so.Unbalanced pulse Vltrasonic device, because oscillating impulse frequency forms multilayer in a reservoir, continuously graphite is peeled off
Progressively high-speed jet, graphite are produced into graphene, and in by bottom to upper strata graphite phased separation, caused cavitation bubble rupture
Phased separation is into graphene；
（3）Graphene is continuously isolated on upper strata, the solid for taking upper liquid to isolate, filtering, washing, and in 60 DEG C of temperature
Dried under degree and -0.09MPa vacuum, what is obtained is the graphene product peeled off, while stable with 40ml/s in bottom
Injection is by step（1）The graphite dispersing solution of preparation.
Method classification to embodiment 4 peels off the graphene being prepared and carries out testing graininess, obtains the middle grain of graphene
The data in footpath are as shown in table 1；Method classification to embodiment 4 peels off the graphene being prepared and carries out structured testing and analysis,
The content for obtaining individual layer and 2 ~ 5 layer graphenes is as shown in table 1.
Embodiment 5
A kind of to peel off method of the grading system for graphene using pulse ultrasonic wave, it is classified stripping and prepares the specific of graphene
Process is as follows：
（1）Natural scale graphite is mixed with deionized water, after sand mill grinding 10min, adds the polyethers of certain mass
Hydramine, magnetic agitation are uniformly dispersed；The mass ratio for stating polyethers hydramine and water is 1：3.5；The addition matter of the natural flake graphite
Measure 4% of the quality summation for decentralized medium and water；
（2）By step（1）The dispersion liquid of gained is placed in impulse ultrasound wave generating device, the frequency of the pulse ultrasonic wave
Rate is to divide three layers, respectively 40kHz, 50kHz, 60kHz, power 200W from bottom to top；And cold bath is used, make reaction temperature
Maintain 20 DEG C or so.Unbalanced pulse Vltrasonic device, because oscillating impulse frequency forms multilayer in a reservoir, continuously graphite is peeled off
Progressively high-speed jet, graphite are produced into graphene, and in by bottom to upper strata graphite phased separation, caused cavitation bubble rupture
Phased separation is into graphene；
（3）Graphene is continuously isolated on upper strata, the solid for taking upper liquid to isolate, filtering, washing, and in 60 DEG C of temperature
Dried under degree and -0.09MPa vacuum, what is obtained is the graphene product peeled off, while stable with 45ml/s in bottom
Injection is by step（1）The graphite dispersing solution of preparation.
Method classification to embodiment 5 peels off the graphene being prepared and carries out testing graininess, obtains the middle grain of graphene
The data in footpath are as shown in table 1；Method classification to embodiment 5 peels off the graphene being prepared and carries out structured testing and analysis,
The content for obtaining individual layer and 2 ~ 5 layer graphenes is as shown in table 1.
Table 1：
| Specific embodiment | Single-layer graphene content（%） | 2 ~ 5 layer graphene contents（%） |
| Embodiment 1 | 10.5 | 84.6 |
| Embodiment 2 | 9.8 | 85.4 |
| Embodiment 3 | 8.6 | 86.2 |
| Embodiment 4 | 7.1 | 82.5 |
| Embodiment 5 | 6.5 | 83.7 |
Pass through the data to the individual layer of obtained graphene in embodiment and 2 ~ 5 layer graphene contents, it is seen that：
（1）Under preparation condition involved in the present invention, pulse ultrasonic wave is to main caused by crystalline flake graphite in dispersion liquid
It is the cavitation shock wave for acting on surface, by controlling bottom injection rate, injection rate is higher, and the graphene that upper strata is overflowed is faster,
Its single-layer graphene content can reduce.But its graphene overall distribution is uniform, 2-5 layers content keeps stable.The production of graphene
Rate is higher, and thickness distribution is more uniform.
Claims (4)
1. a kind of peel off method of the grading system for graphene using pulse ultrasonic wave, by using decentralized medium by natural scale stone
Ink is dispersed in water, and applies high-frequency impulse ultrasonic wave, graphite slurries is produced the higher-order of oscillation, cavitation bubble is formed in liquid phase, by
More much bigger than the size of cavitation bubble in the size of graphite, the collapse of the cavitation bubble near graphite is asymmetrical, so as to produce
The raw high-speed micro-jet for pointing to graphite surface, local failure is produced to its surface, high-frequency impulse ultrasound, produces graphite slurries high
Frequency vibration is swung, and because of oscillating impulse frequency difference, multilayer is formed in a reservoir, continuously by graphite stripping into graphene, and from the bottom of by
Layer progressively arrives upper strata graphite phased separation, finally continuously isolates graphene on upper strata；What is prepared comprises the following steps that：
（1）Natural scale graphite is mixed with deionized water, after sand mill grinding 10min, adds the polyethers hydramine of certain mass,
Magnetic agitation is uniformly dispersed；
（2）By step（1）The dispersion liquid of gained is placed in impulse ultrasound wave generating device, and uses cold bath, makes reaction temperature
Degree maintains 20 DEG C, unbalanced pulse Vltrasonic device, because oscillating impulse frequency forms multilayer in a reservoir, continuously by graphite peel off into
Graphene, and upper strata graphite phased separation is progressively arrived in by bottom, the rupture generation high-speed jet of caused cavitation bubble, graphite by
Step is peeled off into graphene；The frequency of the pulse ultrasonic wave is to divide three layers, respectively 40kHz, 50kHz, 60kHz from bottom to top,
Power is 100~200W；
（3）Graphene is continuously isolated on upper strata, the solid for taking upper liquid to isolate, filtering, washing, and in 60 DEG C of temperature
And dried under -0.09MPa vacuum, what is obtained is the graphene product peeled off, while stable with 20-45ml/s in bottom
Injection is by step（1）The graphite dispersing solution of preparation.
2. a kind of according to claim 1 peel off method of the grading system for graphene using pulse ultrasonic wave, it is characterised in that：
Step（1）The mass ratio of the polyethers hydramine and water is 1：3~1：4.
3. a kind of according to claim 1 peel off method of the grading system for graphene using pulse ultrasonic wave, it is characterised in that：
Step（1）The addition quality of the natural flake graphite is the 2%~4% of the quality summation of decentralized medium polyethers hydramine and water.
4. a kind of according to claim 1 peel off method of the grading system for graphene using pulse ultrasonic wave, it is characterised in that：
Step（3）The bottom is with the stable injections of 35ml/s by step（1）The graphite dispersing solution of preparation.
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| CN107601480B (en) * | 2017-10-20 | 2023-07-25 | 南通富莱克流体装备有限公司 | Graphene production equipment |
| CN108622888B (en) * | 2018-03-08 | 2019-03-22 | 北京地泽科技有限公司 | A kind of method, apparatus of high-volume scale continuous production graphene and graphene prepared therefrom |
| RU2723172C1 (en) * | 2019-12-30 | 2020-06-09 | Общество с ограниченной ответственностью "Артпол Холдинг" | Device for production of graphene with different number of atomic layers |
| CN111440470A (en) * | 2020-04-24 | 2020-07-24 | 南京同诚节能环保装备研究院有限公司 | Preparation method of nickel-coated graphene |
| CN112919457A (en) * | 2021-02-26 | 2021-06-08 | 中科雷舜智能科技(宁波)有限公司 | Nano material and preparation method thereof |
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| CN103466612A (en) * | 2013-10-08 | 2013-12-25 | 东南大学 | Method for preparing native grapheme by means of frequency mixing ultrasound |
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| CN103991863A (en) * | 2014-04-28 | 2014-08-20 | 南京航空航天大学 | Method and device for preparing graphene or graphene oxide by controlled vibration |
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