CN107117603A - A kind of utilization pulse ultrasonic wave peels off grading system for the method for graphene - Google Patents
A kind of utilization pulse ultrasonic wave peels off grading system for the method for graphene Download PDFInfo
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- CN107117603A CN107117603A CN201710456112.1A CN201710456112A CN107117603A CN 107117603 A CN107117603 A CN 107117603A CN 201710456112 A CN201710456112 A CN 201710456112A CN 107117603 A CN107117603 A CN 107117603A
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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
Grading system is peeled off for the method for graphene there is provided a kind of utilization pulse ultrasonic wave the invention belongs to technical field of graphene preparation.Natural flake graphite is dispersed in water by this method by using decentralized medium, applies high-frequency impulse ultrasonic wave, graphite slurries is produced in the higher-order of oscillation, liquid phase and is formed cavitation bubble.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 low graphene charge stripping efficiency, time length, be difficult to the defect continuously peeled off.
Description
Technical field
The present invention relates to the preparing technical field of graphene, 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 discharges huge energy, generation it is 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 not enough, so as to directly affect charge stripping efficiency, is currently only used for auxiliary stripping
From graphite oxide.
Cai etc. is by highly oriented pyrolytic graphite（HOPG）With two-sided tape be fixed on above and below between two substrates, be put into ultrasound
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. first by the use of series compounds such as naphthalenes as intercalator preparation come graphene,
By the uniform mixing in organic solvent by a certain percentage of powdered graphite and intercalator, ultrasound bath is recycled to be peeled off, one
Centrifuged after fixing time, grapheme material is made in filtering.Graphene made from the technology has that fault of construction is few, impurity contains
The advantages of 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, and 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, and 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 is mixed with solvent in reaction vessel, is carried out sonic oscillation, is then started agitator, make graphite powder full and uniform in a solvent
Distribution.Then laser optical path is adjusted, laser beam is sequentially passed through and is focused on after total reflective mirror and focus lens below liquid level at 3mm.Again
Unbalanced pulse laser, adjusting different laser energies makes laser irradiate after the graphite particle in liquid environment, 1 ~ 2h of reaction, closes
Laser, has been made the graphene of the different numbers of plies.Qiao etc. is realized to be prepared using pulse laser scanning graphite suspension mixed solution
Graphene, prepares graphite suspension mixed solution first, and circulates 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
Graphene charge stripping efficiency is prepared for existing ultrasonic stripping low, it is difficult to the defect of serialization volume production, the present invention is proposed
A kind of utilization pulse ultrasonic wave peels off grading system for the method for graphene.It is essentially consisted in natural squama by using decentralized medium
Piece graphite is dispersed in water, and applies high-frequency impulse ultrasonic wave, produces graphite slurries and cavitation gas is formed in the higher-order of oscillation, 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.Conventional ultrasound stripping means can be solved and prepare graphene
Charge stripping efficiency is low, time length, be difficult to the shortcoming continuously peeled off, and topmost, 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：
A kind of utilization pulse ultrasonic wave peels off grading system for the method for graphene, by using decentralized medium by natural flake graphite
It is dispersed in water, applies high-frequency impulse ultrasonic wave, graphite slurries is produced in the higher-order of oscillation, liquid phase and form cavitation bubble.Due to
The size of graphite is more much bigger than the size of cavitation bubble, and the collapse of the cavitation bubble near graphite is asymmetrical, so as to produce
The high-speed micro-jet of graphite surface is pointed to, local failure is produced to its surface, high-frequency impulse ultrasound makes graphite slurries produce high frequency
Vibration, and because oscillating impulse frequency difference forms multilayer in a reservoir, continuously peels off into graphene by graphite, and from by bottom by
Walk to upper strata graphite phased separation, finally continuously isolate 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, the polyethers hydramine of certain mass is added,
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 or so.Unbalanced pulse Vltrasonic device, because oscillating impulse frequency forms multilayer in a reservoir, continuously shells graphite
Upper strata graphite phased separation, the cavitation bubble rupture generation high-speed jet of generation, stone are progressively arrived from into graphene, and in by bottom
Black 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
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.
It is preferred that, step（1）The mass ratio of the polyethers hydramine and water is 1：3~1：4；
It is preferred that, step（1）The addition quality of the natural flake graphite is the 2% ~ 4%. of the quality summation of polyethers hydramine and water
It is preferred that, step（2）The frequency of the pulse ultrasonic wave is divides three layers from bottom to top, respectively 40kHz, 50kHz,
60kHz, power is 100 ~ 200W.
It is preferred that, 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 are produced rapidly, and rapid closing, the instantaneous pressure of formation, superatmospheric 1000 times.Continuously not
Disconnected high pressure constantly impacts object surface just as a succession of small " blast ", makes the superficial layer rapid deterioration of object.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, it is possible to protect the lamellar structure of graphene
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, 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 forms stable multilayer in a reservoir because of oscillating impulse frequency, continuously shells graphite
, 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, single-layer graphene, 2-5 layer graphenes, graphene microchip can be obtained.And it is 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, what the pulse ultrasonic wave that more lower floor is subject to was produced
Impulsive force is stronger, more easily peelable, so as to realize that the classification of crystalline flake graphite is peeled off, obtained graphene thickness distribution is more uniform.
Grading system is peeled off for the method for graphene the invention provides a kind of utilization pulse ultrasonic wave, with prior art phase
Than the characteristics of it is protruded and excellent effect are：
1. pulse ultrasonic wave that the present invention is used classification strip preparation method compensate for ultrasonic wave can only up-stripping prepare graphite
The defect of alkene, simplifies technical process, is advantageously implemented large-scale production.
The repetition for having peeled off graphene is peeled off 2. the classification stripping means that the present invention is used can be prevented effectively from, it is 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 reduce cost, and 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
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 utilization pulse ultrasonic wave peels off grading system for the method for graphene, and it is classified the detailed process that stripping prepares graphene
It is as follows：
（1）Natural scale graphite is mixed with deionized water, after sand mill grinding 10min, the polyethers hydramine of certain mass is added,
Magnetic agitation is 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, and the frequency of the pulse ultrasonic wave is
Divide three layers from bottom to top, respectively 40kHz, 50kHz, 60kHz, power is 100W and uses cold bath, maintains reaction temperature
At 20 DEG C or so.Unbalanced pulse Vltrasonic device, because oscillating impulse frequency forms multilayer in a reservoir, continuously peels off into stone by graphite
Black alkene, and in by bottom, progressively to upper strata graphite phased separation, the cavitation bubble of generation, which ruptures, produces high-speed jet, and graphite is progressively
Peel off 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
And dried under -0.09MPa vacuum, what is obtained is the graphene product peeled off, while being noted in bottom so that 20ml/s is stable
Enter by step（1）The graphite dispersing solution of preparation.
The graphene prepared progress testing graininess is peeled off in method classification to embodiment 1, obtains the middle grain of graphene
The data in footpath are as shown in table 1；The graphene prepared progress structured testing and analysis are peeled off in method classification to embodiment 1,
The content for obtaining individual layer and 2 ~ 5 layer graphenes is as shown in table 1.
Embodiment 2
A kind of utilization pulse ultrasonic wave peels off grading system for the method for graphene, and it is classified the detailed process that stripping prepares graphene
It is as follows：
（1）Natural scale graphite is mixed with deionized water, after sand mill grinding 10min, the polyethers hydramine of certain mass is added,
Magnetic agitation is uniformly dispersed；The mass ratio of polyethers hydramine and water is 1：4；The addition quality of natural flake graphite be polyethers hydramine and
The 2% of the quality summation of water；
（2）By step（1）The dispersion liquid of gained is placed in impulse ultrasound wave generating device, and the frequency of the pulse ultrasonic wave is
Divide three layers from bottom to top, respectively 40kHz, 50kHz, 60kHz, power are 200W；And cold bath is used, maintain reaction temperature
At 20 DEG C or so.Unbalanced pulse Vltrasonic device, because oscillating impulse frequency forms multilayer in a reservoir, continuously peels off into stone by graphite
Black alkene, and in by bottom, progressively to upper strata graphite phased separation, the cavitation bubble of generation, which ruptures, produces high-speed jet, and graphite is progressively
Peel off 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
And dried under -0.09MPa vacuum, what is obtained is the graphene product peeled off, while being noted in bottom so that 30ml/s is stable
Enter by step（1）The graphite dispersing solution of preparation.
The graphene prepared progress testing graininess is peeled off in method classification to embodiment 2, obtains the middle grain of graphene
The data in footpath are as shown in table 1；The graphene prepared progress structured testing and analysis are peeled off in method classification to embodiment 2,
The content for obtaining individual layer and 2 ~ 5 layer graphenes is as shown in table 1.
Embodiment 3
A kind of utilization pulse ultrasonic wave peels off grading system for the method for graphene, and it is classified the detailed process that stripping prepares graphene
It is as follows：
（1）Natural scale graphite is mixed with deionized water, after sand mill grinding 10min, the polyethers hydramine of certain mass is added,
Magnetic agitation is uniformly dispersed；The mass ratio of the polyethers hydramine and water is 1：3；The addition quality of the natural flake graphite is to divide
The 4% of the quality summation of dispersion media and water；
（2）By step（1）The dispersion liquid of gained is placed in impulse ultrasound wave generating device, and the frequency of the pulse ultrasonic wave is
Divide three layers from bottom to top, respectively 40kHz, 50kHz, 60kHz, power are 200W；And cold bath is used, maintain reaction temperature
At 20 DEG C or so.Unbalanced pulse Vltrasonic device, because oscillating impulse frequency forms multilayer in a reservoir, continuously peels off into stone by graphite
Black alkene, and in by bottom, progressively to upper strata graphite phased separation, the cavitation bubble of generation, which ruptures, produces high-speed jet, and graphite is progressively
Peel off 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
And dried under -0.09MPa vacuum, what is obtained is the graphene product peeled off, while being noted in bottom so that 35ml/s is stable
Enter by step（1）The graphite dispersing solution of preparation.
The graphene prepared progress testing graininess is peeled off in method classification to embodiment 3, obtains the middle grain of graphene
The data in footpath are as shown in table 1；The graphene prepared progress structured testing and analysis are peeled off in method classification to embodiment 3,
The content for obtaining individual layer and 2 ~ 5 layer graphenes is as shown in table 1.
Embodiment 4
A kind of utilization pulse ultrasonic wave peels off grading system for the method for graphene, and it is classified the detailed process that stripping prepares graphene
It is as follows：
（1）Natural scale graphite is mixed with deionized water, after sand mill grinding 10min, the polyethers hydramine of certain mass is added,
Magnetic agitation is uniformly dispersed；The mass ratio of the polyethers hydramine and water is 1：4；The addition quality of natural flake graphite is scattered Jie
The 3% of matter and the quality summation of water；
（2）By step（1）The dispersion liquid of gained is placed in impulse ultrasound wave generating device, and the frequency of the pulse ultrasonic wave is
Divide three layers from bottom to top, respectively 40kHz, 50kHz, 60kHz, power are 150W；And cold bath is used, maintain reaction temperature
At 20 DEG C or so.Unbalanced pulse Vltrasonic device, because oscillating impulse frequency forms multilayer in a reservoir, continuously peels off into stone by graphite
Black alkene, and in by bottom, progressively to upper strata graphite phased separation, the cavitation bubble of generation, which ruptures, produces high-speed jet, and graphite is progressively
Peel off 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
And dried under -0.09MPa vacuum, what is obtained is the graphene product peeled off, while being noted in bottom so that 40ml/s is stable
Enter by step（1）The graphite dispersing solution of preparation.
The graphene prepared progress testing graininess is peeled off in method classification to embodiment 4, obtains the middle grain of graphene
The data in footpath are as shown in table 1；The graphene prepared progress structured testing and analysis are peeled off in method classification to embodiment 4,
The content for obtaining individual layer and 2 ~ 5 layer graphenes is as shown in table 1.
Embodiment 5
A kind of utilization pulse ultrasonic wave peels off grading system for the method for graphene, and it is classified the detailed process that stripping prepares graphene
It is as follows：
（1）Natural scale graphite is mixed with deionized water, after sand mill grinding 10min, the polyethers hydramine of certain mass is added,
Magnetic agitation is uniformly dispersed；The mass ratio for stating polyethers hydramine and water is 1：3.5；The addition quality of the natural flake graphite is to divide
The 4% of the quality summation of dispersion media and water；
（2）By step（1）The dispersion liquid of gained is placed in impulse ultrasound wave generating device, and the frequency of the pulse ultrasonic wave is
Divide three layers from bottom to top, respectively 40kHz, 50kHz, 60kHz, power are 200W；And cold bath is used, maintain reaction temperature
At 20 DEG C or so.Unbalanced pulse Vltrasonic device, because oscillating impulse frequency forms multilayer in a reservoir, continuously peels off into stone by graphite
Black alkene, and in by bottom, progressively to upper strata graphite phased separation, the cavitation bubble of generation, which ruptures, produces high-speed jet, and graphite is progressively
Peel off 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
And dried under -0.09MPa vacuum, what is obtained is the graphene product peeled off, while being noted in bottom so that 45ml/s is stable
Enter by step（1）The graphite dispersing solution of preparation.
The graphene prepared progress testing graininess is peeled off in method classification to embodiment 5, obtains the middle grain of graphene
The data in footpath are as shown in table 1；The graphene prepared progress structured testing and analysis are peeled off in method classification to embodiment 5,
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 individual layer and the data of 2 ~ 5 layer graphene contents to obtained graphene in embodiment, it is seen that：
（1）Under preparation condition involved in the present invention, what pulse ultrasonic wave was produced to crystalline flake graphite in dispersion liquid mainly makees
For the cavitation shock wave on surface, by controlling bottom injection rate, injection rate is higher, and the graphene that upper strata is overflowed is faster, its list
Layer graphene content can be reduced.But its graphene overall distribution is uniform, 2-5 layers of content keep stable.The yield of graphene compared with
Height, thickness distribution is more uniform.
Claims (5)
1. a kind of utilization pulse ultrasonic wave peels off grading system for the method for graphene, by using decentralized medium by natural scale stone
Ink is dispersed in water, and applies high-frequency impulse ultrasonic wave, graphite slurries is produced in the higher-order of oscillation, liquid phase and is formed cavitation bubble,
Because the size of graphite is more much bigger than the size of cavitation bubble, the collapse of the cavitation bubble near graphite be it is asymmetrical,
So as to produce the high-speed micro-jet for pointing to graphite surface, local failure is produced to its surface, high-frequency impulse ultrasound makes graphite slurries
The higher-order of oscillation is produced, and because of oscillating impulse frequency difference, forms multilayer in a reservoir, graphite is continuously peeled off into graphene, and
, progressively to upper strata graphite phased separation, finally graphene is continuously isolated from by bottom 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, the polyethers hydramine of certain mass is added,
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 or so, and unbalanced pulse Vltrasonic device, because oscillating impulse frequency forms multilayer in a reservoir, is continuously shelled graphite
Upper strata graphite phased separation, the cavitation bubble rupture generation high-speed jet of generation, stone are progressively arrived from into graphene, and in by bottom
Black 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
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 utilization pulse ultrasonic wave peels off grading system for the method for graphene according to claim 1, 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 utilization pulse ultrasonic wave peels off grading system for the method for graphene according to claim 1, 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 utilization pulse ultrasonic wave peels off grading system for the method for graphene according to claim 1, it is characterised in that：
Step（2）The frequency of the pulse ultrasonic wave is divides three layers from bottom to top, respectively 40kHz, and 50kHz, 60kHz, power are 100
~200W。
5. a kind of utilization pulse ultrasonic wave peels off grading system for the method for graphene according to claim 1, 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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| 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 |
| WO2021137734A1 (en) * | 2019-12-30 | 2021-07-08 | Общество с ограниченной ответственностью "Артпол Холдинг" | Method and device for producing graphene with different numbers of atomic layers |
| WO2021212774A1 (en) * | 2020-04-24 | 2021-10-28 | 南京同诚节能环保装备研究院有限公司 | Preparation method for 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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| CN107117603B (en) | 2018-03-27 |
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