CN106744878B - A kind of scale crushes the method for preparing large stretch of footpath graphene - Google Patents

A kind of scale crushes the method for preparing large stretch of footpath graphene Download PDF

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CN106744878B
CN106744878B CN201611205525.4A CN201611205525A CN106744878B CN 106744878 B CN106744878 B CN 106744878B CN 201611205525 A CN201611205525 A CN 201611205525A CN 106744878 B CN106744878 B CN 106744878B
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graphite
graphene
mill
minute surface
large stretch
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CN106744878A (en
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陈庆
曾军堂
王镭迪
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Chengdu New Keli Chemical Science Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/04Specific amount of layers or specific thickness
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/20Graphene characterized by its properties
    • C01B2204/32Size or surface area

Abstract

The present invention proposes that a kind of scale crushes the method for preparing large stretch of footpath graphene.Graphite powder is used as raw material, graphite powder is placed in mill, the surface of fixed millstone and movable grinding disc is the ceramic minute surface of wearability, by graphite powder under the mutually opposing crisscross motion effect of minute surface mill, peeling sheet layer by layer, the reduction of radial direction in graphite linings is effectively prevent, by introducing ultrasonic dither in mill, graphite flake interlayer is torn, obtains large stretch of footpath graphene.This method realizes continuous graphene production, cleaning, the technique effect of environmental protection, has promoted the industrialization continuous production of graphene.Further, a step completes shearing stripping in mill, the scattered process of ultrasound homogenization, the deck structure of graphene is not only remained to greatest extent, and grapheme material can be prepared with continuous-stable, the surface integrity and Topological Symmetry of graphene are not destroyed, ensure that the quality of graphene product.

Description

A kind of scale crushes the method for preparing large stretch of footpath graphene
Technical field
The present invention relates to nano material manufacture field, and in particular to a kind of scale crushes the side for preparing large stretch of footpath graphene Method.
Background technology
The plane carbon nanomaterial that graphene is made up of one layer of carbon atom, it is to be currently known most thin two-dimensional material, its Thickness is only 0.335nm, and it is made up of the lattice of six sides.By σ key connections between carbon atom in graphene, graphene is imparted Extremely excellent mechanical property and structural rigidity.Moreover, in graphene, each carbon atom has the p electronics of a non-bonding, These p electronics can move freely in crystal, and movement velocity is up to the 1/300 of the light velocity, impart that graphene is good to lead Electrically.In optics aspect, graphene is almost fully transparent, only absorbs 2.3% light.Graphene has peculiar mechanics, light Learn and electrical properties, graphene possess very vast potential for future development.
The preparation method of graphene mainly includes chemical vapour deposition technique, oxidation intercalation restores method, liquid phase stripping method, machine Tool stripping method.Wherein chemical vapour deposition technique can obtain the graphene of high quality, but low yield, require high to substrate, turn Move and greatly difficulty be present;Oxidation intercalation, which restores method, can realize batch production graphene, but due to stone in oxidizing process The structure of black alkene is destroyed, it is difficult to obtains the graphene product of high quality;Liquid phase stripping method is in a suitable solvent, to utilize Ultrasonic energy dissociates to graphite flake layer, is difficult to remove asking for residual solvent however, solvent stripping method prepares graphene presence Topic, and solvent stripping yield is general very low.By contrast, it is high-quality to be that one kind can be prepared with low cost for mechanical-physical stripping method Measure the simple and easy method of graphene.But graphene size prepared by mechanical stripping method is generally smaller, therefore large scale stone The preparation of black alkene turns into study hotspot.
Chinese invention patent application number 201210292680.X discloses a kind of preparation method of large-size monocrystal graphene, It is characterized in that in environment more than 800 DEG C, by adjusting the flow velocity of organic gas, hydrogen and inert gas and point of flow field Cloth prepares large-size monocrystal graphene in metal surface;The organic gas includes:Alkane, alkene, alkynes, aromatic hydrocarbon etc. contains Carbon gas;The metal surface includes:The metal surfaces such as copper, platinum;The flow field includes:The flow velocity of various gases, flowing side To and air pressure;Ambient pressure during heat treatment is normal pressure, and the time is in 20min-40min;The ambient pressure during growth is 1 Between Pa-300 Pa, the time is in 1 min-2h.But this method obtains activity using metallic high temperature reduction organic gas Charcoal atom, it is costly using noble metal as growth substrates, growing film at high temperature is kept, to equipment and instrument requirement Height, be not suitable for large-scale production.
Chinese invention patent application number 201510128458.X discloses one kind and prepares large-size high-quality graphene monocrystalline Device and method.The device includes:Housing and top cover, the gas tip with gas distribution pipe is set in top cover, makes the high-purity gas of entrance Body is uniformly distributed into reaction cavity;Reaction cavity is sent out by sealed silica envelope, the graphite being plugged among two sections of sealed silica envelopes Hot body, the graphite crucible being placed on inside graphite heater composition, graphite crucible are used to place SiC wafer substrates;Graphite is sent out Heat has cooling water system, intermediate frequency coil in vitro;Housing bottom has gas outlet.The present invention also provides to be served as a contrast using the device in SiC The method that large-size high-quality graphene monocrystalline is prepared on bottom.Using the present apparatus and growing method, height is made on SiC substrates The graphene crystal of quality, graphene prepared by its mobility ratio SiC high temperature pyrolysis method improve nearly 1~2 quantity Level.But the main design thought of this method, from carbon atom is obtained, is arranged again still from the method for SiC high temperature pyrolysis Row carbon atom obtains graphene, and using decomposition reaction under high-purity hydrogen and hot environment, equipment cost is high, and equipment is endangered during working It is dangerous big.
Chinese invention patent application number 200910187298.0 discloses a kind of preparation method of big size graphene, is applicable Prepared in the magnanimity of big size graphene.This method includes:(1) large scale graphite is used as raw material, utilizes modified Hummers Method carries out weak oxide to graphite raw material;(2) graphite oxide that be will be dispersed in using weak ultrasound or oscillation method in water carries out temperature And stripping, obtain graphene oxide;(3) multiple centrifugal method is used, by controlling centrifugal rotational speed and centrifugation time to aoxidize stone Black alkene separation, obtains uniform large scale graphene oxide;(4) graphene oxide is deposited on matrix, utilizes hydrazine or hydration Hydrazine reduces, and obtains high quality, big size graphene.Large-sized graphene is obtained using the present invention, maximum area up to 3 × 104μm2, be graphene in nesa coating, display and electrode of solar battery, gas sensor, optical-electrical converter, film The application in the flexible optoelectronic function film such as electronic device field is laid a good foundation.Although The method avoids high temperature shape before The use of state and high-risk gas, still, limit there is to the size of graphene using large scale graphite as raw material in this method System, can not obtain can directly apply large-sized graphene film.The reducing agent of this method is poisonous hydrazine or hydrazine hydrate, no Only production cost is high, and environmental pollution, influences the health of operator.
In summary, at present using strong oxidizer to Graphitic pretreatment, the graphenic surface grafted polar of preparation can be made again Group, it is detrimental to health and causes environmental pollution, destroy the perfection of lattice of graphene, reduces the conductive energy of system Power.It is low that the charge stripping efficiency of graphene powder is prepared using mechanical stripping method, production process dust pollution is serious, it is impossible to realizes stone The continuous production of black alkene, and the flour mill device due to using now does not all account for the radial dimension of reservation graphite, therefore, The size of graphite prepared by mechanical stripping method is relatively small.If secondary to mill using ceramic minute surface, graphene is prepared, will be from basic On solve the above problems.Therefore, from the point of view of the extensive industrialization of big size graphene, we are with greater need for one kind operation letter List, scale, the graphene preparation method of no pollution.
The content of the invention
Low, the production process dust pollution for the charge stripping efficiency for preparing graphene powder with mechanical stripping method in the prior art Seriously, it is impossible to realize the continuous production of graphene, and the flour mill device due to using now does not all account for retaining stone The radial dimension of ink, therefore, the size of graphite prepared by mechanical stripping method are relatively small.The present invention proposes that a kind of scale crushes The method for preparing large stretch of footpath graphene.Use graphite powder that graphite powder is placed in mill for raw material, the table of fixed millstone and movable grinding disc Face is the ceramic minute surface of wearability, by graphite powder under minute surface mill mutually opposing crisscross motion effect, peeling sheet layer by layer, The reduction of radial direction in graphite linings is effectively prevent, by introducing ultrasonic dither in mill, tears graphite flake interlayer Split, obtain large stretch of footpath graphene.This method realizes continuous big size graphene production, cleaning, the technique effect of environmental protection, promotes The industrialization continuous production of big size graphene.Further, a step completes shearing stripping in mill, and ultrasound homogenization is scattered Process, not only remain the deck structure of graphene to greatest extent, and grapheme material can be prepared with continuous-stable, no The surface integrity and Topological Symmetry of graphene are destroyed, ensure that the quality of graphene product.
To solve the above problems, the present invention, which provides a kind of scale, crushes the method for preparing large stretch of footpath graphene, using stone Ink powder is raw material, uses the surface of fixed millstone and movable grinding disc to be used as the ceramic minute surface of wearability secondary to mill, peels off graphite layer by layer, Ultrasonic system is introduced in mill simultaneously, dither, the tear of graphite flake interlayer, forms large stretch of footpath graphene, specific steps Including:
(1)By graphite raw material, intercalation additive, water and surfactant according to mass ratio be 1:2-5:5-10:0.1-0.5 Ratio be configured to scattered suspension, 10-25min is dispersed with stirring with 300-500rpm rotating speed, to the graphite raw material molten It is uniformly dispersed in agent, obtains scattered suspension, stand 3-5 days, intercalator is entered graphite layers;
(2)Scattered suspension solution is added into ceramic minute surface mill apparatus, the rotary speed for controlling movable grinding disc is 500-1000rpm, The relative direction on the surface of fixed millstone and movable grinding disc is kept to move, graphite is by the ceramic minute surface mill mixing and peels off;
(3)While ceramic minute surface grinds and peeled off, ultrasonic dither, ultrasonic power 500-1500kW, ultrasound are introduced Frequency is 50-170kHz, under the dither effect of ultrasonic wave, tears graphite flake interlayer, interfloor distance increase, so More preferable charge stripping efficiency is obtained under inside and outside collective effect, and without reduction graphite radial dimension.
Preferably, the graphite raw material is crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide At least one of, the graphite raw material particle diameter is less than or equal to 1 millimeter.
Preferably, the intercalation additive be sodium carbonate, potassium carbonate, sodium acid carbonate, saleratus, ammonium chloride, ammonium sulfate, At least one of ammonium hydrogen sulfate, ammonium carbonate, ammonium hydrogen carbonate, ammonium phosphate.
Preferably, described surfactant is lauryl sodium sulfate, neopelex, polyvinylpyrrolidine At least one of ketone, 1- pyridine acids.
Preferably, 100-500 KW ultrasonic power is used during the standing, graphite is ultrasonically treated, promotes intercalation Additive is well into interlayer.
Preferably, the ceramic minute surface is aluminium oxide ceramics, and minute surface roughness is 0.5-2.3 μm.
Preferably, graphene collector is set in the end of ceramic minute surface mill, collects graphene.
In existing scheme mechanical stripping method prepare graphene powder charge stripping efficiency it is low, production process dust pollution is serious, The continuous production of graphene can not be realized, and the flour mill device due to using now does not all account for the footpath of reservation graphite To size, therefore, the size of graphite prepared by mechanical stripping method is relatively small.This method realizes big size graphene production and connected Continuous, cleaning, the technique effect of environmental protection, have promoted the industrialization continuous production of big size graphene.Further, a step in mill Complete shearing to peel off, the scattered process of ultrasound homogenization, not only remain the deck structure of graphene, Er Qieke to greatest extent Grapheme material is prepared with continuous-stable, does not destroy the surface integrity and Topological Symmetry of graphene, ensure that graphene produces The quality of product.
By big size graphene performance prepared by the present invention compared with tradition machinery stripping prepares graphene, in graphene matter Amount, yield etc. have the advantage that as shown in table 1.
Table 1:
Performance indications The present invention
90% graphene film radial dimension 150-180μm
90% graphene thickness 0.5-4nm
Charge stripping efficiency 85%-
The present invention proposes that a kind of scale crushes the method for preparing large stretch of footpath graphene, and compared with prior art, it is protruded The characteristics of and excellent effect be:
1st, the present invention uses graphite powder that graphite powder is placed in mill for raw material, and the surface of fixed millstone and movable grinding disc is resistance to The ceramic minute surface of mill property, by graphite powder under minute surface mill mutually opposing crisscross motion effect, peeling sheet layer by layer, effectively The reduction of radial direction in graphite linings is prevented, by introducing ultrasonic dither in mill, graphite flake interlayer is torn, obtains Large stretch of footpath graphene.
2nd, this programme is prepared in a manner of pure physics, destruction of the chemical reaction avoided to graphene-structured, not only The deck structure of graphene is remained to greatest extent, and grapheme material can be prepared with continuous-stable, does not destroy graphene Surface integrity and Topological Symmetry, further ensure the quality of graphene finished product.
3rd, scheme preparation technology disclosed by the invention is simple, and raw material sources are extensive, and cost is low, the forerunner's volume property prepared Stable, easily storage transports.
4th, operation equipment of the present invention is simple, portable high, it is easy to accomplish scale industrial production.
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
(1)By crystalline flake graphite, intercalation Sodium Carbonate Additive, water and Surfactant SDS according to mass ratio For 1:2:5:0.1 ratio is configured to scattered suspension, and 10min is dispersed with stirring with 300rpm rotating speed, to the graphite raw material It is uniformly dispersed in a solvent, obtains scattered suspension, stand 3 days, 100 KW ultrasonic power is used during standing, to graphite It is ultrasonically treated, promotes intercalation additive well into interlayer;
(2)Scattered suspension solution is added into ceramic minute surface mill apparatus, the rotary speed for controlling movable grinding disc is 500rpm, keeps fixed The relative direction motion on the surface of mill and movable grinding disc, graphite is by the ceramic minute surface mill mixing and peels off, the ceramic minute surface It is 2.3 μm to grind as aluminium oxide ceramics, minute surface roughness;
(3)While ceramic minute surface grinds and peeled off, ultrasonic dither, ultrasonic power 500kW are introduced, supersonic frequency is 50kHz, under the dither effect of ultrasonic wave, tear graphite flake interlayer, interfloor distance increase, so inside and outside common Effect is lower to obtain more preferable charge stripping efficiency, and without reduction graphite radial dimension.
After carrying out performance test to the graphene prepared in embodiment 1, it is as shown in table 2 to obtain data.
Embodiment 2
(1)By expanded graphite, intercalation additive potassium carbonate, water and Surfactant SDS according to mass ratio For 1:2.5:6:0.3 ratio is configured to scattered suspension, and 15min is dispersed with stirring with 350rpm rotating speed, former to the graphite Material is uniformly dispersed in a solvent, obtains scattered suspension, stands 3.5 days, and 250KW ultrasonic power is used during standing, right Graphite is ultrasonically treated, and promotes intercalation additive well into interlayer;
(2)Scattered suspension solution is added into ceramic minute surface mill apparatus, the rotary speed for controlling movable grinding disc is 650rpm, keeps fixed The relative direction motion on the surface of mill and movable grinding disc, graphite is by the ceramic minute surface mill mixing and peels off, the ceramic minute surface It is 2.0 μm to grind as aluminium oxide ceramics, minute surface roughness;
(3)While ceramic minute surface grinds and peeled off, ultrasonic dither, ultrasonic power 700kW are introduced, supersonic frequency is 70kHz, under the dither effect of ultrasonic wave, tear graphite flake interlayer, interfloor distance increase, so inside and outside common Effect is lower to obtain more preferable charge stripping efficiency, and without reduction graphite radial dimension.
After carrying out performance test to the graphene prepared in embodiment 2, it is as shown in table 2 to obtain data.
Embodiment 3
(1)By highly oriented graphite, intercalation additive saleratus, water and surfactant polyvinylpyrrolidone according to matter Amount is than being 1:4:8:0.3 ratio is configured to scattered suspension, and 20min is dispersed with stirring with 400rpm rotating speed, to the graphite Raw material is uniformly dispersed in a solvent, obtains scattered suspension, stands 4 days, and 300 KW ultrasonic power is used during standing, right Graphite is ultrasonically treated, and promotes intercalation additive well into interlayer;
(2)Scattered suspension solution is added into ceramic minute surface mill apparatus, the rotary speed for controlling movable grinding disc is 800rpm, keeps fixed The relative direction motion on the surface of mill and movable grinding disc, graphite is by the ceramic minute surface mill mixing and peels off, the ceramic minute surface It is 1.5 μm to grind as aluminium oxide ceramics, minute surface roughness;
(3)While ceramic minute surface grinds and peeled off, ultrasonic dither, ultrasonic power 1100kW, supersonic frequency are introduced For 120kHz, under the dither effect of ultrasonic wave, tear graphite flake interlayer, interfloor distance increase, so inside and outside More preferable charge stripping efficiency is obtained under collective effect, and without reduction graphite radial dimension.
After carrying out performance test to the graphene prepared in embodiment 3, it is as shown in table 2 to obtain data.
Embodiment 4
(1)By thermal cracking graphite, intercalation additive ammonium sulfate, water and surfactant sodium dodecyl base benzene sulfonic acid sodium salt according to matter Amount is than being 1:4:8:0.4 ratio is configured to scattered suspension, and 20min is dispersed with stirring with 450rpm rotating speed, to the graphite Raw material is uniformly dispersed in a solvent, obtains scattered suspension, stands 4.5 days, 400 KW ultrasonic power is used during standing, Graphite is ultrasonically treated, promotes intercalation additive well into interlayer;
(2)Scattered suspension solution is added into ceramic minute surface mill apparatus, the rotary speed for controlling movable grinding disc is 850rpm, keeps fixed The relative direction motion on the surface of mill and movable grinding disc, graphite is by the ceramic minute surface mill mixing and peels off, the ceramic minute surface It is 1.0 μm to grind as aluminium oxide ceramics, minute surface roughness;
(3)While ceramic minute surface grinds and peeled off, ultrasonic dither, ultrasonic power 1250kW, supersonic frequency are introduced For 150kHz, under the dither effect of ultrasonic wave, tear graphite flake interlayer, interfloor distance increase, so inside and outside More preferable charge stripping efficiency is obtained under collective effect, and without reduction graphite radial dimension.
After carrying out performance test to the graphene prepared in embodiment 4, it is as shown in table 2 to obtain data.
Embodiment 5
(1)By crystalline flake graphite, intercalation additive ammonium hydrogen sulfate, water and surfactant sodium dodecyl base benzene sulfonic acid sodium salt according to matter Amount is than being 1:5:10:0.5 ratio is configured to scattered suspension, and 25min is dispersed with stirring with 500rpm rotating speed, to the graphite Raw material is uniformly dispersed in a solvent, obtains scattered suspension, stands 5 days, and 500 KW ultrasonic power is used during standing, right Graphite is ultrasonically treated, and promotes intercalation additive well into interlayer;
(2)Scattered suspension solution is added into ceramic minute surface mill apparatus, the rotary speed for controlling movable grinding disc is 1000rpm, is kept The relative direction motion on the surface of fixed millstone and movable grinding disc, graphite is by the ceramic minute surface mill mixing and peels off, the ceramic mirror Face mill is aluminium oxide ceramics, and minute surface roughness is 0.5 μm;
(3)While ceramic minute surface grinds and peeled off, ultrasonic dither, ultrasonic power 1500kW, supersonic frequency are introduced For 170kHz, under the dither effect of ultrasonic wave, tear graphite flake interlayer, interfloor distance increase, so inside and outside More preferable charge stripping efficiency is obtained under collective effect, and without reduction graphite radial dimension.
After carrying out performance test to the graphene prepared in embodiment 5, it is as shown in table 2 to obtain data.
Table 2
Performance indications 90% graphene film radial dimension 90% graphene thickness Charge stripping efficiency
Embodiment one 150-160μm 0.5-2nm 81.0%
Embodiment two 160-180μm 1.5-2nm 83.4%
Embodiment three 150-178μm 0.8-1.6nm 80.8%
Example IV 155-175μm 2.9-4.0nm 79.1%
Embodiment five 160-180μm 2.5-3.7nm 85.0%

Claims (7)

1. a kind of scale crushes the method for preparing large stretch of footpath graphene, graphite powder is used as raw material, using fixed millstone and dynamic mill The surface of disk is used as to mill pair for the ceramic minute surface of wearability, peels off graphite layer by layer, while ultrasonic system is introduced in mill, high Frequency vibration, graphite flake interlayer tear, forms large stretch of footpath graphene, specific steps include:
(1)By graphite raw material, intercalation additive, water and surfactant according to mass ratio be 1:2-5:5-10:0.1-0.5 ratio Example is configured to scattered suspension, and 10-25min is dispersed with stirring with 300-500rpm rotating speed, to the graphite raw material in a solvent It is uniformly dispersed, obtains scattered suspension, stand 3-5 days, intercalator is entered graphite layers;
(2)Scattered suspension solution is added into ceramic minute surface mill apparatus, the rotary speed for controlling movable grinding disc is 500-1000rpm, is kept The relative direction motion on the surface of fixed millstone and movable grinding disc, graphite is by the ceramic minute surface mill mixing and peels off;
(3)While ceramic minute surface grinds and peeled off, ultrasonic dither, ultrasonic power 500-1500kW, supersonic frequency are introduced For 50-170kHz, under the dither effect of ultrasonic wave, tear graphite flake interlayer, interfloor distance increase, so including More preferable charge stripping efficiency is obtained under outer collective effect, and without reduction graphite radial dimension.
2. a kind of scale according to claim 1 crushes the method for preparing large stretch of footpath graphene, it is characterised in that described Graphite raw material is crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, at least one of graphite oxide, the stone Black raw material particle size is less than or equal to 1 millimeter.
3. a kind of scale according to claim 1 crushes the method for preparing large stretch of footpath graphene, it is characterised in that described Intercalation additive is sodium carbonate, potassium carbonate, sodium acid carbonate, saleratus, ammonium chloride, ammonium sulfate, ammonium hydrogen sulfate, ammonium carbonate, carbon At least one of sour hydrogen ammonium, ammonium phosphate.
4. a kind of scale according to claim 1 crushes the method for preparing large stretch of footpath graphene, it is characterised in that described Surfactant be lauryl sodium sulfate, neopelex, polyvinylpyrrolidone, in 1- pyridine acids at least It is a kind of.
5. a kind of scale according to claim 1 crushes the method for preparing large stretch of footpath graphene, it is characterised in that described 100-500 KW ultrasonic power is used during standing, graphite is ultrasonically treated, promotes intercalation additive well into interlayer.
6. a kind of scale according to claim 1 crushes the method for preparing large stretch of footpath graphene, it is characterised in that described Ceramic minute surface is aluminium oxide ceramics, and minute surface roughness is 0.5-2.3 μm.
7. a kind of scale according to claim 1 crushes the method for preparing large stretch of footpath graphene, it is characterised in that is making pottery The end of porcelain minute surface mill sets graphene collector, collects graphene.
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CN110078062A (en) * 2019-05-22 2019-08-02 大同墨西科技有限责任公司 A kind of graphene energetic catalytic physics strip preparation method
CN110203914B (en) * 2019-07-13 2021-07-23 武汉中科先进技术研究院有限公司 Device and method for preparing few-layer graphene composite material
CN115924996A (en) * 2022-12-30 2023-04-07 化学与精细化工广东省实验室潮州分中心 One-step synthesis-stripping method of nickel-iron layered double hydroxide

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104401971A (en) * 2014-10-23 2015-03-11 江阴碳谷科技有限公司 Graphene grinding and stripping device, graphene production system and production method
CN104609413A (en) * 2015-02-11 2015-05-13 合肥微晶材料科技有限公司 Machine-like stripping device for ton-scale production of graphene and production method of machine-like stripping device
CN105905888A (en) * 2016-05-06 2016-08-31 成都新柯力化工科技有限公司 Graphene composite microchips stripped by using turbine sander and preparation method for graphene composite microchips
CN106044761A (en) * 2016-08-01 2016-10-26 邓仟菀 High-shearing-force wear-resistant rubber grinding pan for preparing graphene and preparation method and application of high-shearing-force wear-resistant rubber grinding pan

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015184555A1 (en) * 2014-06-06 2015-12-10 Group Nanoxplore Inc. Large scale production of thinned graphite, graphene, and graphite-graphene composites

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104401971A (en) * 2014-10-23 2015-03-11 江阴碳谷科技有限公司 Graphene grinding and stripping device, graphene production system and production method
CN104609413A (en) * 2015-02-11 2015-05-13 合肥微晶材料科技有限公司 Machine-like stripping device for ton-scale production of graphene and production method of machine-like stripping device
CN105905888A (en) * 2016-05-06 2016-08-31 成都新柯力化工科技有限公司 Graphene composite microchips stripped by using turbine sander and preparation method for graphene composite microchips
CN106044761A (en) * 2016-08-01 2016-10-26 邓仟菀 High-shearing-force wear-resistant rubber grinding pan for preparing graphene and preparation method and application of high-shearing-force wear-resistant rubber grinding pan

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