CN106744878A - The method for preparing large stretch of footpath Graphene is crushed in a kind of scale - Google Patents
The method for preparing large stretch of footpath Graphene is crushed in a kind of scale Download PDFInfo
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Abstract
The present invention proposes that the method for preparing large stretch of footpath Graphene is crushed in a kind of scale.It is raw material to use graphite powder, graphite powder is placed in mill, fixed millstone is the ceramic minute surface of wearability with the surface of movable grinding disc, by graphite powder under the mutually opposing crisscross motion effect of minute surface mill, peeling sheet, effectively prevent the reduction of radial direction in graphite linings layer by layer, by introducing ultrasonic dither in mill, graphite flake interlayer is torn, large stretch of footpath Graphene is obtained.This method realizes continuous Graphene production, cleaning, the technique effect of environmental protection, has promoted the industrialization of Graphene continuously to produce.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, it is ensured that the quality of graphene product.
Description
Technical field
The present invention relates to nano material manufacture field, and in particular to the side for preparing large stretch of footpath Graphene is crushed in a kind of scale
Method.
Background technology
The plane carbon nanomaterial that Graphene is made up of one layer of carbon atom, 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.It is bonded by σ between carbon atom in Graphene and is connect, imparts Graphene
Extremely excellent mechanical property and structural rigidity.And, in Graphene, each carbon atom has a p electronics for non-bonding,
These p electronics can be moved 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 possesses very vast potential for future development.
The preparation method of Graphene mainly includes that chemical vapour deposition technique, oxidation intercalation restore method, liquid phase stripping method, machine
Tool stripping method.Wherein chemical vapour deposition technique can obtain high-quality Graphene, however low yield, it is high to substrate requirement, turn
Move and there is greatly difficulty；Oxidation intercalation restores method and can realize producing Graphene in batches, but due to stone in oxidizing process
The structure of black alkene is destroyed, it is difficult to obtain high-quality graphene product；Liquid phase stripping method is in a suitable solvent, to utilize
Ultrasonic energy dissociates to graphite flake layer, however, solvent stripping method prepares Graphene presence to be difficult to remove asking for residual solvent
Topic, and solvent stripping yield is general very low.By contrast, to be that one kind can be prepared with low cost high-quality for mechanical-physical stripping method
Measure the method simple and easy to apply 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 adjust organic gas, hydrogen and inert gas flow velocity and flow field point
Cloth prepares large-size monocrystal graphene in metal surface；The organic gas includes：Alkane, alkene, alkynes, aromatic hydrocarbon etc. contain
Carbon gas；The metal surface includes：The metal surfaces such as copper, platinum；The flow field includes：Flow velocity, the flowing side of various gases
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 reduces organic gas using metallic high temperature, obtains activity
Charcoal atom, it is costly using noble metal as growth substrates, growing film at high temperature is kept, to equipment and instrument requirement
Height, is 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, set the gas tip with gas distribution pipe in top cover, make the high-purity gas of entrance
Body is uniformly distributed and enters reaction cavity；Reaction cavity is sent out by sealed silica envelope, the graphite being plugged in the middle of 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 is also provided and served as a contrast in SiC using the device
The method that large-size high-quality Graphene monocrystalline is prepared on bottom.Using the present apparatus and growing method, height is obtained on SiC substrates
The Graphene crystal of quality, Graphene prepared by its mobility ratio SiC high temperature pyrolysis method improves 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.The method includes：(1) it is raw material to use large scale graphite, using modified Hummers
Method carries out weak oxide to graphite raw material；(2) will be dispersed in the graphite oxide in water and carry out temperature using weak ultrasound or oscillation method
And stripping, obtain graphene oxide；(3) multiple centrifugal method is used, stone will be aoxidized by controlling centrifugal rotational speed and centrifugation time
Black alkene is separated, and obtains uniform large scale graphene oxide；(4) graphene oxide is deposited on matrix, using hydrazine or hydration
Hydrazine is reduced, and obtains high-quality, big size graphene.Large-sized Graphene is obtained using the present invention, maximum area up to 3 ×
104μm2, it is 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, but, limit there is to the size of Graphene using large scale graphite as raw material in the method
System, it is impossible to which acquisition can directly apply large-sized graphene film.The reducing agent of the method is poisonous hydrazine or hydrazine hydrate, no
Only production cost is high, and environmental pollution, and influence operator's is healthy.
In sum, at present using strong oxidizer to Graphitic pretreatment, the graphenic surface grafted polar of preparation can be made again
Group, is detrimental to health and causes environmental pollution, destroys the perfection of lattice of Graphene, reduces the conductive energy of system
Power.The charge stripping efficiency for preparing graphene powder using mechanical stripping method is low, and production process dust pollution is serious, it is impossible to enough realize stone
The continuous prodution of black alkene, and all do not account for retaining the radial dimension of graphite due to the flour mill device for currently using, 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 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
It is low for the charge stripping efficiency for preparing graphene powder with mechanical stripping method in the prior art, production process dust pollution
Seriously, it is impossible to enough realize the continuous prodution of Graphene, and because the flour mill device for currently using all does not account for retaining stone
The radial dimension of ink, therefore, the size of graphite prepared by mechanical stripping method is relatively small.The present invention proposes that a kind of scale is crushed
The method for preparing large stretch of footpath Graphene.It is raw material to use graphite powder, and graphite powder is placed in mill, 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 of big size graphene is continuously produced.Further, a step completes shearing stripping, ultrasound homogenization dispersion in mill
Process, the deck structure of Graphene is not only remained to greatest extent, and grapheme material can be prepared with continuous-stable, no
Destroy the surface integrity and Topological Symmetry of Graphene, it is ensured that the quality of graphene product.
To solve the above problems, the present invention provides a kind of scale and crushes the method for preparing large stretch of footpath Graphene, using stone
Ink powder is raw material, uses fixed millstone with the ceramic minute surface that the surface of movable grinding disc is wearability as to mill pair, and graphite is peeled off layer by layer,
Ultrasonic system is introduced in mill simultaneously, dither, graphite flake interlayer tear 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:The ratio of 0.1-0.5
Example is configured to disperse suspension, with the rotating speed dispersed with stirring 10-25min of 300-500rpm, to the graphite raw material in a solvent
It is uniformly dispersed, obtains disperseing suspension, stand 3-5 days, intercalator is entered graphite layers；
（2）Dispersion suspension solution is added into ceramic minute surface mill apparatus, controls the rotary speed of movable grinding disc for 500-1000rpm, kept
Fixed millstone is moved with the relative direction on the surface of movable grinding disc, and graphite is by ceramic minute surface mill mixing and peels off；
（3）While ceramic minute surface grinds and peels off, ultrasonic dither is introduced, ultrasonic power is 500-1500kW, supersonic frequency
Be 50-170kHz, ultrasonic wave dither effect under, make graphite flake interlayer tear, interfloor distance increase, so including
More preferable charge stripping efficiency is obtained under outer 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
In at least one, the graphite raw material particle diameter be 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 in ammonium hydrogen sulfate, ammonium carbonate, ammonium hydrogen carbonate, ammonium phosphate.
Preferably, described surfactant is lauryl sodium sulfate, neopelex, polyvinylpyrrolidine
At least one in ketone, 1- pyridine acids.
Preferably, it is ultrasonically treated to graphite using the ultrasonic power of 100-500 KW during the standing, promote 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 prodution of Graphene can not be realized, and does not all account for retaining the footpath of graphite due to the flour mill device for currently using
To size, therefore, the size of graphite prepared by mechanical stripping method is relatively small.This method realizes big size graphene production and connects
Continuous, cleaning, the technique effect of environmental protection, have promoted the industrialization of big size graphene continuously to produce.Further, a step in mill
Complete shearing to peel off, the scattered process of ultrasound homogenization not only remains the deck structure of Graphene, Er Qieke to greatest extent
Grapheme material is prepared with continuous-stable, the surface integrity and Topological Symmetry of Graphene are not destroyed, it is ensured that Graphene is produced
The quality of product.
By big size graphene performance prepared by the present invention compared with tradition machinery stripping prepares Graphene, in Graphene matter
The aspects such as amount, yield 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 the method for preparing large stretch of footpath Graphene is crushed in a kind of scale, compared with prior art, its spy for protruding
Point and excellent effect are：
1st, it is raw material that the present invention uses graphite powder, and graphite powder is placed in mill, and fixed millstone is wearability with the surface of movable grinding disc
Ceramic minute surface, by graphite powder under minute surface mill mutually opposing crisscross motion effect, peeling sheet, effectively prevents layer by layer
The reduction of radial direction in graphite linings, by introducing ultrasonic dither in mill, tears graphite flake interlayer, obtains sheet
Footpath Graphene.
2nd, this programme is prepared in the way of pure physics, it is to avoid destruction of the chemical reaction to graphene-structured, not only
The deck structure of Graphene is remained to greatest extent, and grapheme material can be prepared with continuous-stable, do not destroy Graphene
Surface integrity and Topological Symmetry, further ensure the quality of Graphene finished product.
3rd, scheme preparation process is simple disclosed by the invention, raw material sources are extensive, low cost, the forerunner's volume property prepared
Stabilization, easily storage are transported.
4th, operation equipment of the present invention is simple, portable high, it is easy to accomplish scale industrial production.
Specific embodiment
Below by way of specific embodiment, the present invention is described in further detail, but this should not be interpreted as into the present invention
Scope be only limitted to following example.In the case where above method thought of the present invention is not departed from, 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
（1）By crystalline flake graphite, intercalation Sodium Carbonate Additive, water and Surfactant SDS according to mass ratio be 1:
2:5:, into dispersion suspension, with the rotating speed dispersed with stirring 10min of 300rpm, the extremely graphite raw material is molten for 0.1 proportions
It is uniformly dispersed in agent, obtains disperseing suspension, stand 3 days, using the ultrasonic power of 100 KW during standing, to graphite ultrasound
Treatment, promotes intercalation additive well into interlayer；
（2）Dispersion suspension solution is added into ceramic minute surface mill apparatus, controls the rotary speed of movable grinding disc for 500rpm, keep fixed millstone
Relative direction with the surface of movable grinding disc is moved, and graphite is by ceramic minute surface mill mixing and peels off, and the ceramic minute surface mill is
Aluminium oxide ceramics, minute surface roughness is 2.3 μm；
（3）While ceramic minute surface grinds and peels off, ultrasonic dither is introduced, ultrasonic power is 500kW, and supersonic frequency is
50kHz, under the dither effect of ultrasonic wave, tears graphite flake interlayer, and interfloor distance increases, so inside and outside common
Effect is lower to obtain more preferable charge stripping efficiency, and without reduction graphite radial dimension.
After Graphene to being prepared in embodiment 1 carries out performance test, data are obtained as shown in table 2.
Embodiment 2
（1）By expanded graphite, intercalation additive potassium carbonate, water and Surfactant SDS according to mass ratio be 1:
2.5:6:0.3 proportions, with the rotating speed dispersed with stirring 15min of 350rpm, exist into dispersion suspension to the graphite raw material
It is uniformly dispersed in solvent, obtains disperseing suspension, 3.5 days is stood, using the ultrasonic power of 250KW during standing, to graphite
It is ultrasonically treated, promote intercalation additive well into interlayer；
（2）Dispersion suspension solution is added into ceramic minute surface mill apparatus, controls the rotary speed of movable grinding disc for 650rpm, keep fixed millstone
Relative direction with the surface of movable grinding disc is moved, and graphite is by ceramic minute surface mill mixing and peels off, and the ceramic minute surface mill is
Aluminium oxide ceramics, minute surface roughness is 2.0 μm；
（3）While ceramic minute surface grinds and peels off, ultrasonic dither is introduced, ultrasonic power is 700kW, and supersonic frequency is
70kHz, under the dither effect of ultrasonic wave, tears graphite flake interlayer, and interfloor distance increases, so inside and outside common
Effect is lower to obtain more preferable charge stripping efficiency, and without reduction graphite radial dimension.
After Graphene to being prepared in embodiment 2 carries out performance test, data are obtained as shown in table 2.
Embodiment 3
（1）By highly oriented graphite, intercalation additive saleratus, water and surfactant polyvinylpyrrolidone according to mass ratio
It is 1:4:8:0.3 proportions into dispersion suspension, with the rotating speed dispersed with stirring 20min of 400rpm, to the graphite raw material
It is uniformly dispersed in a solvent, obtains disperseing suspension, 4 days is stood, using the ultrasonic power of 300 KW during standing, to graphite
It is ultrasonically treated, promote intercalation additive well into interlayer；
（2）Dispersion suspension solution is added into ceramic minute surface mill apparatus, controls the rotary speed of movable grinding disc for 800rpm, keep fixed millstone
Relative direction with the surface of movable grinding disc is moved, and graphite is by ceramic minute surface mill mixing and peels off, and the ceramic minute surface mill is
Aluminium oxide ceramics, minute surface roughness is 1.5 μm；
（3）While ceramic minute surface grinds and peels off, ultrasonic dither is introduced, ultrasonic power is 1100kW, and supersonic frequency is
120kHz, under the dither effect of ultrasonic wave, tears graphite flake interlayer, and interfloor distance increases, so inside and outside common
More preferable charge stripping efficiency is obtained under same-action, and without reduction graphite radial dimension.
After Graphene to being prepared in embodiment 3 carries out performance test, data are obtained as shown in table 2.
Embodiment 4
（1）By thermal cracking graphite, intercalation additive ammonium sulfate, water and surfactant sodium dodecyl base benzene sulfonic acid sodium salt according to mass ratio
It is 1:4:8:0.4 proportions into dispersion suspension, with the rotating speed dispersed with stirring 20min of 450rpm, to the graphite raw material
It is uniformly dispersed in a solvent, obtains disperseing suspension, 4.5 days is stood, using the ultrasonic power of 400 KW during standing, to stone
Ink is ultrasonically treated, promotes intercalation additive well into interlayer；
（2）Dispersion suspension solution is added into ceramic minute surface mill apparatus, controls the rotary speed of movable grinding disc for 850rpm, keep fixed millstone
Relative direction with the surface of movable grinding disc is moved, and graphite is by ceramic minute surface mill mixing and peels off, and the ceramic minute surface mill is
Aluminium oxide ceramics, minute surface roughness is 1.0 μm；
（3）While ceramic minute surface grinds and peels off, ultrasonic dither is introduced, ultrasonic power is 1250kW, and supersonic frequency is
150kHz, under the dither effect of ultrasonic wave, tears graphite flake interlayer, and interfloor distance increases, so inside and outside common
More preferable charge stripping efficiency is obtained under same-action, and without reduction graphite radial dimension.
After Graphene to being prepared in embodiment 4 carries out performance test, data are obtained as shown in table 2.
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 mass ratio
It is 1:5:10:0.5 proportions into dispersion suspension, with the rotating speed dispersed with stirring 25min of 500rpm, to the graphite raw material
It is uniformly dispersed in a solvent, obtains disperseing suspension, 5 days is stood, using the ultrasonic power of 500 KW during standing, to graphite
It is ultrasonically treated, promote intercalation additive well into interlayer；
（2）Dispersion suspension solution is added into ceramic minute surface mill apparatus, the rotary speed of movable grinding disc is controlled for 1000rpm, fixed mill is kept
Disk is moved with the relative direction on the surface of movable grinding disc, and graphite is by ceramic minute surface mill mixing and peels off, the ceramic minute surface mill
It is aluminium oxide ceramics, minute surface roughness is 0.5 μm；
（3）While ceramic minute surface grinds and peels off, ultrasonic dither is introduced, ultrasonic power is 1500kW, and supersonic frequency is
170kHz, under the dither effect of ultrasonic wave, tears graphite flake interlayer, and interfloor distance increases, so inside and outside common
More preferable charge stripping efficiency is obtained under same-action, and without reduction graphite radial dimension.
After Graphene to being prepared in embodiment 5 carries out performance test, data are obtained as shown in table 2.
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. the method for preparing large stretch of footpath Graphene is crushed in a kind of scale, and it is raw material to use graphite powder, using fixed millstone and dynamic mill
The surface of disk is the ceramic minute surface of wearability as secondary to mill, and graphite is peeled off layer by layer, while ultrasonic system is introduced in mill, it is high
Frequency vibration, graphite flake interlayer tear forms large stretch of footpath Graphene, and specific steps include：
（1）By graphite raw material, intercalation additive, water and surfactant according to mass ratio be 1:2-5:5-10:The ratio of 0.1-0.5
Example is configured to disperse suspension, with the rotating speed dispersed with stirring 10-25min of 300-500rpm, to the graphite raw material in a solvent
It is uniformly dispersed, obtains disperseing suspension, stand 3-5 days, intercalator is entered graphite layers；
（2）Dispersion suspension solution is added into ceramic minute surface mill apparatus, controls the rotary speed of movable grinding disc for 500-1000rpm, kept
Fixed millstone is moved with the relative direction on the surface of movable grinding disc, and graphite is by ceramic minute surface mill mixing and peels off；
（3）While ceramic minute surface grinds and peels off, ultrasonic dither is introduced, ultrasonic power is 500-1500kW, supersonic frequency
Be 50-170kHz, ultrasonic wave dither effect under, make graphite flake interlayer tear, interfloor distance increase, so including
More preferable charge stripping efficiency is obtained under outer collective effect, and without reduction graphite radial dimension.
2. the method that a kind of microwave radiation technology stirring according to claim 1 quickly prepares Graphene, it is characterised in that described
Graphite raw material is at least one in crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide, the stone
Black raw material particle size is less than or equal to 1 millimeter.
3. the method that a kind of microwave radiation technology stirring according to claim 1 quickly prepares 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 in sour hydrogen ammonium, ammonium phosphate.
4. the method that a kind of microwave radiation technology stirring according to claim 1 quickly prepares Graphene, it is characterised in that described
Surfactant in lauryl sodium sulfate, neopelex, polyvinylpyrrolidone, 1- pyridine acids at least
It is a kind of.
5. the method that a kind of microwave radiation technology stirring according to claim 1 quickly prepares Graphene, it is characterised in that described
It is ultrasonically treated to graphite using the ultrasonic power of 100-500 KW during standing, promote intercalation additive well into interlayer.
6. the method that a kind of microwave radiation technology stirring according to claim 1 quickly prepares 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. the method that a kind of microwave radiation technology stirring according to claim 1 quickly prepares Graphene, it is characterised in that in pottery
The end of porcelain minute surface mill sets Graphene collector, collects Graphene.
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN110203914A (en) * | 2019-07-13 | 2019-09-06 | 武汉中科先进技术研究院有限公司 | It is a kind of to prepare few layer of graphene composite material device and method |
| 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 |
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