CN107032339B - It is a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene - Google Patents
It is a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene Download PDFInfo
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- CN107032339B CN107032339B CN201710468321.8A CN201710468321A CN107032339B CN 107032339 B CN107032339 B CN 107032339B CN 201710468321 A CN201710468321 A CN 201710468321A CN 107032339 B CN107032339 B CN 107032339B
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- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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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
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The invention belongs to grapheme material fabricating technology field, and in particular to a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene.Its technique is that a variety of laminated crystalline graphite materials, source of ammonium, lithium source, highly basic, water are mixed into alkaline graphite slurry in the case where mechanical agitation adds ultrasound.By alkaline graphite slurry by setting the high-pressure fog mouth of sophisticated corona unit to spray, formed vaporific, vaporific slurry particles are by corona simultaneously, negative electrical charge rapid aggregation is on graphite particulate surface, electrostatic repulsion between electric charge exceedes the interlayer Van der Waals force of graphite particulate, burst, filtered after collection, wash removing inorganic ions, obtain graphene.The present invention avoids oxidation processes, is peeled off graphite into one or more layers graphene with high yield.This method can scale turn to industrial production.Compared with other graphenes preparation technology, less, electric property, mechanical property, hydrophobic performance are higher the defects of the graphene platelet of this method production.
Description
Technical field
The invention belongs to grapheme material fabricating technology field, and in particular to one kind is continuously peeled off based on electrostatic repulsion
The method for preparing graphene.
Background technology
Carbon material be material more universal and special on a kind of earth it can form the larger diamond of hardness, can also
Softer graphite is formed, in the past 20 years, carbon nanomaterial is always the Disciplinary Frontiers of scientific and technical innovation, the fullerene found in 1985
Huge repercussion is caused with the CNT found in 1991, has risen research boom, Manchester universities in 2004
Geim groups New Two Dimensional atomic crystal-graphene of individual layer or thin layer is obtained with mechanical stripping method first.Graphene
It was found that having enriched carbon material family, the fullerene from zero dimension, one-dimensional CNTs, the Buddha's warrior attendant of two-dimentional graphene to three-dimensional are formd
The integral framework of stone and graphite.
Graphene is the individual layer two-dimension plane structure by regular hexagon close-packed arrays into honeycomb crystal lattice by carbon atom.Graphite
Alkene structure is highly stable, and the connection between each carbon atom is very flexible, and when applying external mechanical force, carbon atom face just bends change
Shape so that carbon atom need not be rearranged to adapt to external force and holding structure it is stable.The lattice structure of this stabilization makes carbon former
Son has outstanding thermal conductivity 3000W/ (m*K).The maximum characteristic of graphene is that the movement velocity of its electronics has reached the light velocity
1/300, it is that to be currently known electronics conduction velocity in material most fast considerably beyond movement velocity of the electronics in general conductor
, its electron mobility at room temperature is up to 15000cm2/ (V* s).Graphene also shows perfect quantum tunneling effect
Should, the half-integer quantum hall effect of the dirac fermion behavior of zero mass and exception.Graphene or mankind's known strength
Highest material, also harder than diamond, intensity is more than 100 times of steel best in the world.In addition, single-layer graphene have it is non-
Often big specific surface area, up to 2600m2/g.Graphene possesses that translucency is good, thermal conductivity factor is high, electron mobility is high, resistance
The performance that numerous common materials such as rate is low, mechanical strength is high do not possess, future be expected to electrode, battery, transistor, touch-screen,
The various fields extensive use such as solar energy, sensor, super light material, medical treatment, desalinization, be most promising advanced material it
One.
The preparation method of graphene mainly includes micromechanics stripping method, electronation graphene oxide method, CNT
Axially cutting method, electrochemical reducing, chemical vapour deposition technique, microwave method, solvent-thermal method, arc discharge method, epitaxial growth method,
Liquid phase peels off graphite method etc..Wherein chemical vapour deposition technique can obtain the graphene of high quality, but low yield, will to substrate
Ask high, transfer exists greatly difficult；Electronation graphene oxide method can realize batch production graphene, but due to
The structure of graphene is destroyed in oxidizing process, it is difficult to obtains the graphene product of high quality；Liquid phase stripping method is suitable
Solvent in, graphite flake layer is dissociated using ultrasonic energy, however, solvent stripping method prepare graphene exist be difficult to remove
The problem of residual solvent, and solvent peels off yield and is generally less than 10%.This means 90% raw material (graphite) is not shelled yet
From, and only 10% or less raw material is reclaimed with graphene platelet, each includes one or more layers graphene.These are low
The problem of yield process is the multiple steps of their needs and is used to be processed further to produce enough products, and including will not
Tediously long multiple steps that release liner and release liner separate.Mechanical stripping method is that one kind can prepare high quality with low cost
The simple and easy method of graphene, but usually introduce organic solvent in order to improve peeling effect during mechanical stripping and insert
Layer, though intercalation efficiency and control distribution of particles can be improved to a certain extent, the solvent residues in graphene are not easy
Remove, easily cause contamination of products.And existing machinery charge stripping efficiency is low；In addition, the crunch of abrasive media can cause graphite
Rotating fields become even closer can cause peeling effect to reduce on the contrary, cause milling time length, cost very high；Furthermore mesh
Preceding grinding production graphene belongs to batch (-type), and while being peeled off to graphite, the graphene peeled off can not be sieved in time
Select, thus be difficult to the volume production of continuous-stable, it is difficult to carry out large-scale industrialized production.Arc discharge method is mainly with graphite
Bar is raw material, and graphene size prepared by arc process is larger, during as lithium ion battery negative material, lithium from migration path
Long, charge-discharge performance is bad, and yield is difficult to the demand that reaches industrial applications.
In view of the active demand of the excellent properties and every profession and trade of grapheme material to high-performance and low-cost graphene, the present invention
The purpose that continuous batch prepares grapheme material is reached using brand-new economically viable process.
The content of the invention
The present invention proposes a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene, avoids oxidation processes,
Graphite is peeled off into one or more layers graphene with high yield.This method can scale industrial production graphene.With other graphite
Alkene preparation technology compares, and less, electric property, mechanical property, hydrophobic performance be more the defects of the graphene platelet of this method production
It is high.
To achieve the above object, the concrete technical scheme used for：
It is a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene, by a variety of laminated crystalline graphite materials, source of ammonium,
Lithium source, highly basic, water are mixed into alkaline graphite slurry in the case where mechanical agitation adds ultrasound；By alkaline graphite slurry by setting
The high-pressure fog mouth of sophisticated corona unit sprays, and formation is vaporific, while vaporific slurry particles are existed by corona, negative electrical charge rapid aggregation
Graphite particulate surface, the electrostatic repulsion between electric charge exceed the interlayer Van der Waals force of graphite particulate, burst, moment stripping is stone
Black alkene, filtered after collection, wash removing inorganic ions, obtain graphene.
A variety of laminated crystalline graphite materials include one kind in native graphite, synthetic graphite, highly oriented pyrolytic graphite,
Particle size is less than 10 μm.
The source of ammonium is conventional water-soluble including ammoniacal liquor, ammonium hydrogen carbonate, urea, ammonium nitrate etc. and generates the material of ammonium ion
At least one of.
The lithium source is selected from lithium perchlorate (LiClO4), lithium hexafluoro phosphate (LiPF6), LiBF4 (LiBF4), chlorination
At least one of solvable lithium salts such as lithium (LiCl), lithium iodide (LiI), lithium borate, chelating lithium phosphate.
The highly basic is selected from least one of sodium hydroxide, potassium hydroxide.
It is a kind of to be based on the electrostatic repulsion method that continuously stripping prepares graphene, its mechanism：Laminated crystalline graphite material exists
Under alkaline environment, charge density is higher, and under electrostatic repulsion effect, carbon-coating (or being graphite interlayer) layer gap is necessarily expanded
Greatly, in the presence of ultrasound, the less cation of radius, anion diffuse into carbon-coating (or being graphite interlayer) layer gap, this
Both samples interact, and the graphene layer gap spacing for being is increased to more than 0.6nm from 0.335nm, and Van der Waals force weakens, but logical
The electrostatic interaction crossed in ion insertion and solution only allows graphite material to be expanded, also unstripped into graphene.Slurry is passed through
High-pressure fog is dispersed into small particle, under sophisticated corona unit corona, the increase of fine particles surface charge accumulation, and tiny
Grain is further differentiated into more fine particle, ultimately becomes surface and carries High Density Charge, contains a large amount of intercalating ions inside layer gap
Expanded graphite particles, the electrostatic repulsion between electric charge exceeds well over the interlayer Van der Waals force of graphene layer gap, bursts, be decomposed into
Individual layer or few layer graphene.Experiment shows that in general, the pH value of alkaline graphite slurry is higher, and peeling effect is more obvious, but ammonium
The concentration of ion is not easy excessive, and pH value can only be adjusted by sodium hydroxide, is got over by high pH value, the defects of graphene product
It is more.
It is a kind of to be based on the electrostatic repulsion method that continuously stripping prepares graphene, its detailed process flow：
（1）Prepare alkaline graphite slurry
Now by source of ammonium, highly basic, the dissolving of lithium source mechanical agitation in deionized water, laminated crystalline graphite material is added, is opened
Vltrasonic device, ultrasonic time are 0.5 ~ 6 hour；Layered kish material is in terms of carbon, and source of ammonium is in terms of ammonium root, and lithium source is with lithium
Ionometer, the mol ratio of three is 1：0.01~0.1:0.05~0.5；The addition of the highly basic is pH value for ensureing mixed liquor etc.
In 11 ~ 14；After machinery stirs while is ultrasonically treated certain time, graphite powder even suspension forms strong basicity black lead wash in the solution
Material, now graphite linings gap spacing reaches more than 0.6nm；
（2）Corona peels off graphene
Sprayer unit is opened, atomisation pressure is 2 ~ 6MPa, and corona unit is powered, voltage is arranged to 5 ~ 20kv, opens charging
Alkaline graphite slurry high-pressure fog above corona unit discharge electrode that device prepares the first step；Graphite composite powder surface charge is high
Degree aggregation, under electrostatic repulsion effect, split into individual layer or few layer graphene；
（3）Separation, the washing of graphene
By step（2）The graphene mixture of preparation is separated, and solvent input is continuing with for the first time, mistake after collection
Filter, washing remove inorganic ions, obtain graphene.
The yield of test analysis, individual layer and few layer graphene is 55 ~ 89%, and graphene lateral dimension is 20 ~ 300nm.
The present invention is a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene, compared with prior art, the base
In the electrostatic repulsion method that continuously stripping prepares graphene, its advantage is：
1st, this process is not suffered from stone aoxidizing in the case of route (that is, not forming sp3 carbon, such as graphene oxide)
Black high yield (reaching 89%) method directly peeled off into " multilayer " (i.e. one or more layers) graphene (sp2 carbon).The application
Methods described is characterised by that it is used as reagent without using oxidant (such as nitric acid (HNO3) or sulfuric acid (H2SO4)), also saves system
The processing step of standby graphene oxide.Meanwhile these stripping graphene platelets can be by a variety of organic and inorganic constituents functionalization.
2nd, the graphene dispersion of the stripping produced by herein described method is in solution and easily from insoluble parent
Separated in compound graphite, simultaneously because whole process does not consume various inorganic constituents, separating the strong base solution after graphite can be with
It is directly recycled for the processing of graphite.
3rd, this method may act as large quantities of processing approach of high-quality graphene, so can scale turn to industrial production.With oxygen
Compound graphene is compared, less the defects of the graphene platelet of this method production, electric conductivity is higher and hydrophobicity is higher.
4th, present invention process method is simple and easy, and equipment is common equipment, no particular/special requirement, and raw material sources are wide cheap, easy
Obtain, be nontoxic.Without special protection in preparation process, easy control of reaction conditions technique is easy, is beneficial to industrialized 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
It is a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene, it is first that source of ammonium, highly basic, lithium source mechanical agitation is molten
Solution in deionized water, adds laminated crystalline graphite material, opens Vltrasonic device, after mechanical agitation adds ultrasound some time, stone
Ink powder even suspension forms strong basicity graphite slurry in the solution.Open sprayer unit and corona unit is powered, by alkaline graphite
Slurry high-pressure fog above corona unit discharge electrode.Graphite composite powder surface charge high aggregation, electrostatic repulsion in graphite particle
More than Van der Waals force between layer gap, graphene is split into rapidly.Be finally separating, wash after obtain individual layer or few layer graphene.
Wherein, layered kish material is in terms of carbon, and source of ammonium is in terms of ammonium root, and in terms of lithium ion, three's rubs lithium source
You are than being 1：0.01：0.05, the addition of the highly basic is that the pH value for ensureing mixed liquor is equal to 11；
Wherein, the ultrasound plus churned mechanically time are 0.5 hour；
Wherein, the sprayer unit, its atomisation pressure are 2MPa, and the corona unit leads to, and its operating voltage is arranged to
5kv；
Wherein, it is 55% to prepare the individual layer of gained and the output capacity of few layer graphene, and lateral dimension concentrates on 80nm.
Embodiment 2
It is a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene, it is first that source of ammonium, highly basic, lithium source mechanical agitation is molten
Solution in deionized water, adds laminated crystalline graphite material, opens Vltrasonic device, after mechanical agitation adds ultrasound some time, stone
Ink powder even suspension forms strong basicity graphite slurry in the solution.Open sprayer unit and corona unit is powered, by alkaline graphite
Slurry high-pressure fog above corona unit discharge electrode.Graphite composite powder surface charge high aggregation, electrostatic repulsion in graphite particle
More than Van der Waals force between layer gap, graphene is split into rapidly.Be finally separating, wash after obtain individual layer or few layer graphene.
Wherein, layered kish material is in terms of carbon, and source of ammonium is in terms of ammonium root, and in terms of lithium ion, three's rubs lithium source
You are than being 1：0.05：0.25, the addition of the highly basic is that the pH value for ensureing mixed liquor is equal to 12；
Wherein, the ultrasound plus churned mechanically time are 6 hours；
Wherein, the sprayer unit, its atomisation pressure are 4MPa, and the corona unit leads to, and its operating voltage is arranged to
10kv；
Wherein, it is 71% to prepare the individual layer of gained and the output capacity of few layer graphene, and lateral dimension concentrates on 120nm.
Embodiment 3
It is a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene, it is first that source of ammonium, highly basic, lithium source mechanical agitation is molten
Solution in deionized water, adds laminated crystalline graphite material, opens Vltrasonic device, after mechanical agitation adds ultrasound some time, stone
Ink powder even suspension forms strong basicity graphite slurry in the solution.Open sprayer unit and corona unit is powered, by alkaline graphite
Slurry high-pressure fog above corona unit discharge electrode.Graphite composite powder surface charge high aggregation, electrostatic repulsion in graphite particle
More than Van der Waals force between layer gap, graphene is split into rapidly.Be finally separating, wash after obtain individual layer or few layer graphene.
Wherein, layered kish material is in terms of carbon, and source of ammonium is in terms of ammonium root, and in terms of lithium ion, three's rubs lithium source
You are than being 1：0.1：0.5, the addition of the highly basic is that the pH value for ensureing mixed liquor is equal to 13；
Wherein, the ultrasound plus churned mechanically time are 2 hours；
Wherein, the sprayer unit, its atomisation pressure are 6MPa, and the corona unit leads to, and its operating voltage is arranged to
20kv；
Wherein, it is 69% to prepare the individual layer of gained and the output capacity of few layer graphene, and lateral dimension concentrates on 20nm.
Embodiment 4
It is a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene, it is first that source of ammonium, highly basic, lithium source mechanical agitation is molten
Solution in deionized water, adds laminated crystalline graphite material, opens Vltrasonic device, after mechanical agitation adds ultrasound some time, stone
Ink powder even suspension forms strong basicity graphite slurry in the solution.Open sprayer unit and corona unit is powered, by alkaline graphite
Slurry high-pressure fog above corona unit discharge electrode.Graphite composite powder surface charge high aggregation, electrostatic repulsion in graphite particle
More than Van der Waals force between layer gap, graphene is split into rapidly.Be finally separating, wash after obtain individual layer or few layer graphene.
Wherein, layered kish material is in terms of carbon, and source of ammonium is in terms of ammonium root, and in terms of lithium ion, three's rubs lithium source
You are than being 1：0.08：0.35, the addition of the highly basic is that the pH value for ensureing mixed liquor is equal to 14；
Wherein, the ultrasound plus churned mechanically time are 2 hours；
Wherein, the sprayer unit, its atomisation pressure are 4MPa, and the corona unit leads to, and its operating voltage is arranged to
15kv；
Wherein, it is 78% to prepare the individual layer of gained and the output capacity of few layer graphene, and lateral dimension concentrates on 300nm.
Embodiment 5
It is a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene, it is first that source of ammonium, highly basic, lithium source mechanical agitation is molten
Solution in deionized water, adds laminated crystalline graphite material, opens Vltrasonic device, after mechanical agitation adds ultrasound some time, stone
Ink powder even suspension forms strong basicity graphite slurry in the solution.Open sprayer unit and corona unit is powered, by alkaline graphite
Slurry high-pressure fog above corona unit discharge electrode.Graphite composite powder surface charge high aggregation, electrostatic repulsion in graphite particle
More than Van der Waals force between layer gap, graphene is split into rapidly.Be finally separating, wash after obtain individual layer or few layer graphene.
Wherein, layered kish material is in terms of carbon, and source of ammonium is in terms of ammonium root, and in terms of lithium ion, three's rubs lithium source
You are than being 1：0.07:0.25, the addition of the highly basic is that the pH value for ensureing mixed liquor is equal to 13；
Wherein, the ultrasound plus churned mechanically time are 2 hours；
Wherein, the sprayer unit, its atomisation pressure are 3MPa, and the corona unit leads to, and its operating voltage is arranged to
18kv；
Wherein, it is 89% to prepare the individual layer of gained and the output capacity of few layer graphene, and lateral dimension concentrates on 190nm.
Claims (5)
1. it is a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene, it is characterised by that specific preparation method is：
（1）Prepare alkaline graphite slurry
By source of ammonium, highly basic, the dissolving of lithium source mechanical agitation in deionized water, laminated crystalline graphite material is added, opens ultrasound dress
Put, ultrasonic time is 0.5~6 hour；Layered kish material is in terms of carbon, and source of ammonium is in terms of ammonium root, and lithium source is with lithium ion
Meter, the mol ratio of three is 1：0.01~0.1:0.05~0.5；The addition of the highly basic is that the pH value for ensureing mixed liquor is equal to
11~14；After machinery stirs while is ultrasonically treated certain time, graphite powder even suspension forms strong basicity graphite slurry in the solution,
Now graphite linings gap spacing reaches more than 0.6nm；
（2）Corona peels off graphene
Sprayer unit is opened, atomisation pressure is 2~6MPa, and corona unit is powered, voltage is arranged to 5~20kv, opens charging dress
Put the alkaline graphite slurry high-pressure fog above corona unit discharge electrode for preparing the first step；Graphite composite powder surface charge height
Aggregation, under electrostatic repulsion effect, split into individual layer or few layer graphene；
（3）Separation, the washing of graphene
By step（2）The graphene mixture of preparation is separated, and solvent input is continuing with for the first time, filtering, water after collection
Inorganic ions is removed in washout, obtains graphene.
It is 2. a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene according to claim 1, it is characterised in that：It is more
Kind laminated crystalline graphite material includes one kind in native graphite, synthetic graphite, highly oriented pyrolytic graphite, and particle size is less than 10
μm。
It is 3. a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene according to claim 1, it is characterised in that：Institute
State that source of ammonium includes ammoniacal liquor, ammonium hydrogen carbonate, urea, ammonium nitrate is routinely water-soluble and generates at least one of material of ammonium ion.
It is 4. a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene according to claim 1, it is characterised in that：Institute
Lithium source is stated in lithium perchlorate, lithium hexafluoro phosphate, LiBF4, lithium chloride, lithium iodide, lithium borate, chelating lithium phosphate
It is at least one.
It is 5. a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene according to claim 1, it is characterised in that：Institute
State highly basic and be selected from least one of sodium hydroxide, potassium hydroxide.
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| CN108190960B (en) * | 2018-01-23 | 2020-05-08 | 福州大学 | Method for preparing monolayer molybdenum disulfide based on hot lithium insertion stripping of electrolyte solvent |
| CN109052314B (en) * | 2018-09-17 | 2021-01-26 | 柯良节 | Method for stripping multilayer two-dimensional material |
| CN111899983B (en) * | 2020-07-15 | 2021-09-14 | 铜仁学院 | Preparation method of graphene, prepared graphene, application of graphene and super capacitor |
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| CN103451670A (en) * | 2013-09-11 | 2013-12-18 | 中南大学 | Electrochemical preparation method of graphene |
| CN103693638A (en) * | 2013-12-09 | 2014-04-02 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene by electrochemical swelling of graphite |
| CN105271205A (en) * | 2015-11-20 | 2016-01-27 | 复旦大学 | Method for preparing layer-number-controllable high-quality graphene through electrochemical process |
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| US20090022649A1 (en) * | 2007-07-19 | 2009-01-22 | Aruna Zhamu | Method for producing ultra-thin nano-scaled graphene platelets |
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| CN103693638A (en) * | 2013-12-09 | 2014-04-02 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene by electrochemical swelling of graphite |
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