CN108117065A - A kind of method that graphene is prepared using alternative current stripping - Google Patents
A kind of method that graphene is prepared using alternative current stripping Download PDFInfo
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Abstract
A kind of method that graphene is prepared using alternative current stripping belongs to the preparation field of graphene.It is as follows：1. prepare certain density electrolyte solution；2. using high purity graphite plate as anodic-cathodic, fixed polar plate spacing, the recirculation gas stripper in the electrolytic solution in a manner that timing exchanges electrode；3. completing to remove after a certain period of time, electrode is taken out, to electrolyte filtering and washing；4. taking solid ultrasonic disperse uniform, centrifuged supernatant is graphene.This method operating process is easy, is easy to be prepared on a large scale the low graphene of degree of oxidation.It can be reduced immediately using cathode current, the graphene degree of oxidation prepared is low, and defect is smaller after anode removes graphene by the stripping means of alternating electrode.The graphene of particular patch footpath size (100 nanometers to several microns) can be prepared after suitable alternating frequency by adjusting, and individual layer and double-deck rate are up to more than 80%, have wider purposes in bio-pharmaceuticals and composite material.
Description
Technical field
The invention belongs to the preparation fields of graphene, relate in particular to a kind of system that graphene is removed using alternative current
Preparation Method.
Background technology
Graphene is to pass through sp by carbon atom2The hexatomic ring lattice structure material that hydridization is formed, 2004 for the first time by Britain
Scientist Andre Geim and Konstantin Novoselov remove graphite using adhesive tape and are made.The graphene of individual layer is very thin,
Thickness is only about 0.335nm there are one atomic layer, is the material of known maximum intensity in the world, intensity is up to
130GP.The theoretical value of graphene specific surface area is about 2600m2/ g, room temperature thermal conductivity have reached (5.3 ± 0.48) × 103W·m-1·K-1, fracture strength and Young's modulus are up to 40N/m and 1.0TPa, have good conductive, heat conduction and mechanical property respectively.
Excellent performance determines that graphene all has broad application prospects in many fields, for example, ultracapacitor, electrochemical sensing
Device, field-effect transistor, microbiological fuel cell, dye-sensitized solar cells etc., so as to which scientific circles triggered to grind it
Study carefully upsurge.
In view of the application prospect of graphene light, how low cost prepares that mass is high, applicable graphene is existing rank
The important research contents that section scientist faces.The main method used at present has chemical method and electrochemical process, lower mask
Body introduces various stripping means and its advantage and disadvantage.
Chemical method mainly includes mechanical stripping method, graphite oxide reduction method, chemical vapour deposition technique (CVD) and epitaxial growth
Method etc..Mechanical stripping method is in graphite material, the method that graphene is therefrom stripped out using certain mechanical force.It lacks
Point is that the contingency prepared is big, and product graphene size differs and low output, it is impossible to realize large area and the scale of graphene
It prepares, but simple for process, sample quality is high, is suitable for laboratory basic research.Graphite oxide reduction method be using strong acid,
Strong oxdiative object acts on or heat treatment native graphite, obtains graphene oxide, phase is removed after ultrasonic disperse, then with reducing agent
Oxygen-containing group is closed, obtains redox graphene.The method advantage is that cost is relatively low, graphene batch production can be achieved.But it uses
Part oxygen-containing functional group cannot remove completely in graphene prepared by oxidation-reduction method, and crystal structure has a degree of broken
It is bad, it is difficult to complete graphene film layer structure to be obtained, so as to cause some physics, chemically loss of energy.CVD is in decomposable asymmetric choice net
High temperature hydrocarbon gas in, by high annealing, carbon atom is allowed to deposit to form single-layer graphene in matrix surface, this method has
Controllably, it is simple for process, can produce large area (up to number square meters) graphene the features such as.But there are crystal boundaries to lack for the graphene prepared
Sunken, pin hole, wrinkle and crackle, and have impurity generation, there is stronger dependence to facility environment, high expensive, pollution is greatly.Extension
Growth method is substantially exactly a kind of reconstruct chemical reaction of carbon atom, can be divided into SiC epitaxial growth methods and the life of metal substrate extension
Regular way.Process conditions are that high temperature is (usual>1300 DEG C), ultravacuum is (usually<10-6Pa), Si atoms are removed in SiC at this moment,
Remaining C atoms grow into graphene.The method is suitable for the preparation of large area, high-quality graphene, it can be achieved that wafer scale is extensive
The preparation of grapheme material, but graphene is influenced by substrate from when preparing matrix and being transferred to target substrate and is difficult to shift,
And use " matrix corrosion method " of high cost, it is unfavorable for scale application.
Electrochemical process is to impose electric field force and act on to generate voltage on graphite, driving electrolyte molecule insertion graphite linings
Between, while the electrolysis of water generates O near electrode2, the boundary layer of graphite is opened in the marginal position of graphite, is further promoted
The intercalation of molecule, making graphite layers, interlayer Van der Waals force dies down, and graphene has been prepared so as to remove away from becoming larger.Electrochemistry
Method is not required the use of oxidant or reducing agent to can reach preparation purpose, has simple production process, at low cost, clean environment firendly
The advantages that, and in electrolytic process, electric current is easy to accurately control with voltage, therefore the controllable preparation of graphene easy to implement
Regulate and control with performance.Have some researchs in the technique of preparing graphene by electrochemical stripping, such as in inorganic salt solution, anode is
Graphite plate electrode, cathode are in the system of platinum electrode, choose (NH4)2SO4、Na2SO4And K2SO4Wait inorganic salts as electrolyte into
Row is removed.In the process first, cathodic reduction water is biased in using what is generated on electrode, generates strong nucleopilic reagent OH-, make it
The marginal position of attack graphite；So as to cause the depolarising and expansion at graphite edge, make hydrone andIntercalation is entered；Its electricity
Solution can generate SO2、O2Gases are waited, these gases further expand graphite flake layer spacing, so as to cause the oxidation and stripping of graphite
From.Therefore, the oxygen generated in electrochemical process preparation process can aoxidize the graphene of preparation, the oxygen content of product compared with
It is high.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, a kind of preparation side that graphene is removed using alternative current is provided
Method.
The technical solution used in the present invention comprises the following steps：
(1) certain density electrolyte solution is prepared；
(2) using high purity graphite plate as anodic-cathodic, fixed polar plate spacing, in electrolyte in a manner that timing is alternately electrolysed
In with the carry out positive and negative anodes checker recirculation gas stripper of DC current；
(3) after removing a period of time, electrode is taken out, to electrolyte filtering and washing；
(4) solid after filtering is taken, ultrasonic disperse is uniform in deionized water, and centrifuged supernatant is the water-soluble of graphene
Liquid；
(5) supernatant is dried, obtains graphene.
A kind of preparation method that graphene is removed using alternative current, the concentration of electrolyte described in preparation process
For 0.05-2mol/l；It is mixed that sodium nitrate, sodium sulphate, ammonium sulfate, one or more of sodium chloride, ammonium chloride can be used in electrolyte
Close object.
A kind of preparation method that graphene is removed using alternative current, the high purity graphite plate described in preparation process
Phosphorus content is more than 99%；Electrolysis stripping temperature is 10-90 DEG C.
A kind of preparation method that graphene is removed using alternative current, the pole plate spacing described in preparation process are excellent
Elect 3-10cm as.
A kind of preparation method that graphene is removed using alternative current, the timing described in preparation process exchange electricity
The frequency of pole is 1min-30min/ times.It is electrolysed the DC voltage used, voltage range 5-20V.
A kind of preparation method that graphene is removed using alternative current, the electrolysis time described in preparation process are
1-10h。
A kind of preparation method that graphene is removed using alternative current, the drying mode described in preparation process can
Optionally spray drying and freeze-drying.
The beneficial effects of the invention are as follows：It can be after anode removes graphene, immediately by the stripping means for exchanging electrode
It is reduced using cathode current, the graphene degree of oxidation prepared is low, and defect is smaller, can be made after adjusting suitable alternating frequency
For the graphene for going out particular patch footpath size (100 nanometers to several microns), individual layer and double-deck rate are up to more than 80%, in bio-pharmaceuticals
With in composite material have wider purposes.
Description of the drawings
Fig. 1 prepares the experimental provision schematic diagram of graphene；
The TEM image of Fig. 2 graphenes；
Specific embodiment
Below by the technical solution that some case study on implementation further illustrate the present invention, but the present invention is not limited to following realities
Apply example.Graphite cake length and width, thickness rate 4:2:1.
Embodiment 1
(1) NaNO of 0.5mol/l is prepared3Electrolyte solution 250ml；
(2) using high purity graphite plate as anodic-cathodic, fixed polar plate spacing is 3.5cm, by way of timing alternating electrode
Recirculation gas stripper is carried out with the constant voltage of 10V in the electrolytic solution, frequency is exchanged and selects 1min/ times；
(3) after removing 5h, electrode is taken out, to electrolyte filtering and washing；
(4) solid after filtering is taken, 200ml deionized water ultrasounds 15min is added in and is uniformly dispersed, centrifuged supernatant is stone
The aqueous solution of black alkene.
(5) supernatant is freeze-dried, can obtain graphene.
The graphene solution concentration of embodiment 1 is 1.66mg/ml, and graphene phosphorus content is 90.58%, ID/IG=0.85,
Average-size size is 128nm, and individual layer and double-deck rate are 88%.
Embodiment 2
(1) (the NH of 2mol/l is prepared4)2SO4Electrolyte solution 1000ml；
(2) using high purity graphite plate as anodic-cathodic, fixed polar plate spacing be 10cm, by way of timing alternating electrode
Recirculation gas stripper is carried out with the constant voltage of 10V in electrolyte, frequency is exchanged and selects 30min/ times；
(3) after removing 10h, electrode is taken out, to electrolyte filtering and washing；
(4) solid after filtering is taken, 200ml deionized water ultrasounds 15min is added in and is uniformly dispersed, centrifuged supernatant is stone
The aqueous solution of black alkene.
(5) supernatant is freeze-dried, can obtain graphene.
The graphene solution concentration of embodiment 2 is 10.08mg/ml, and graphene phosphorus content is 72.4%, ID/IG=1.44,
Average-size size is 320nm, and individual layer and double-deck rate are 70%.
Embodiment 3
(1) the NaCl electrolyte solutions 500ml of 1mol/l is prepared；
(2) using high purity graphite plate as anodic-cathodic, fixed polar plate spacing be 5cm, by way of timing alternating electrode
Recirculation gas stripper is carried out with the constant voltage of 10V in electrolyte, frequency is exchanged and selects 20min/ times；
(3) after removing 1h, electrode is taken out, to electrolyte filtering and washing；
(4) solid after filtering is taken, 200ml deionized water ultrasounds 15min is added in and is uniformly dispersed, centrifuged supernatant is stone
The aqueous solution of black alkene.
(5) supernatant is freeze-dried, can obtain graphene.
The graphene solution concentration of embodiment 3 is 0.55mg/ml, and graphene phosphorus content is 97.07%, ID/IG=0.92,
Average-size size is 380nm, and individual layer and double-deck rate are 76%.
Embodiment 4
(1) NH of 2mol/l is prepared4Cl electrolyte solutions 250ml；
(2) using high purity graphite plate as anodic-cathodic, fixed polar plate spacing be 7cm, by way of timing alternating electrode
Recirculation gas stripper is carried out with the constant voltage of 10V in electrolyte, frequency is exchanged and selects 15min/ times；
(3) after removing 8h, electrode is taken out, to electrolyte filtering and washing；
(4) solid after filtering is taken, 200ml deionized water ultrasounds 15min is added in and is uniformly dispersed, centrifuged supernatant is stone
The aqueous solution of black alkene.
(5) supernatant is freeze-dried, can obtain graphene.
The graphene solution concentration of embodiment 4 is 2.73mg/ml, and graphene phosphorus content is 83.2%, ID/IG=1.32, it puts down
Equal size is 370nm, and individual layer and double-deck rate are 77.4%.
Embodiment 5
(1) the NaCl electrolyte solutions 250ml of 1mol/l is prepared；
(2) using high purity graphite plate as anodic-cathodic, fixed polar plate spacing be 5cm, by way of timing alternating electrode
Recirculation gas stripper is carried out with the constant voltage of 10V in electrolyte, frequency is exchanged and selects 20min/ times；
(3) after removing 1h, electrode is taken out, to electrolyte filtering and washing；
(4) solid after filtering is taken, 200ml deionized water ultrasounds 15min is added in and is uniformly dispersed, centrifuged supernatant is stone
The aqueous solution of black alkene.
(5) supernatant is freeze-dried, can obtain graphene.
The graphene solution concentration of embodiment 5 is 0.55mg/ml, and graphene phosphorus content is 97.07%, ID/IG=0.92,
Average-size size is 120nm, and individual layer and double-deck rate are 81.6%.
Embodiment 6
(1) NaNO of the NaCl and 1mol/l of 1mol/l are prepared3The common 500ml of electrolyte solution；
(2) using high purity graphite plate as anodic-cathodic, fixed polar plate spacing be 5cm, by way of timing alternating electrode
Recirculation gas stripper is carried out with the constant voltage of 10V in electrolyte, frequency is exchanged and selects 10min/ times；
(3) after removing 5h, electrode is taken out, to electrolyte filtering and washing；
(4) solid after filtering is taken, 200ml deionized water ultrasounds 15min is added in and is uniformly dispersed, centrifuged supernatant is stone
The aqueous solution of black alkene.
(5) supernatant is freeze-dried, can obtain graphene.
The graphene solution concentration of embodiment 6 is 3.74mg/ml, and graphene phosphorus content is 82.17%, ID/IG=1.11,
Average-size size is 460nm, and individual layer and double-deck rate are 82.8%.
Claims (9)
- A kind of 1. method that graphene is prepared using alternative current stripping, which is characterized in that comprise the following steps：(1) certain density electrolyte solution is prepared；(2) using high purity graphite plate as anodic-cathodic, fixed polar plate spacing, timing alternately be electrolysed by way of in the electrolytic solution with The carry out positive and negative anodes checker recirculation gas stripper of DC current；(3) after removing a period of time, electrode is taken out, to electrolyte filtering and washing；(4) solid after filtering is taken, ultrasonic disperse is uniform in deionized water, and centrifuged supernatant is the aqueous solution of graphene；(5) supernatant is dried, obtains graphene.
- 2. a kind of method that graphene is prepared using alternative current stripping described in accordance with the claim 1, which is characterized in that described Concentration of electrolyte be 0.05-2mol/l；Electrolyte is using sodium nitrate, sodium sulphate, ammonium sulfate, sodium chloride, and one in ammonium chloride The aqueous solution of kind or several mixtures.
- 3. a kind of method that graphene is prepared using alternative current stripping described in accordance with the claim 1, which is characterized in that prepare The high purity graphite plate phosphorus content is more than 99% in the process.
- A kind of 4. method that graphene is prepared using alternative current stripping described in accordance with the claim 1, which is characterized in that electrolysis Exfoliation temperature is 10-90 DEG C.
- A kind of 5. method that graphene is prepared using alternative current stripping described in accordance with the claim 1, which is characterized in that pole plate Spacing is 3-10cm.
- 6. a kind of method that graphene is prepared using alternative current stripping described in accordance with the claim 1, which is characterized in that use Timing exchanges electrode, and it is 1min-30min/ times to exchange frequency.
- A kind of 7. method that graphene is prepared using alternative current stripping described in accordance with the claim 1, which is characterized in that electrolysis The DC voltage of use, voltage range 5-20V.
- A kind of 8. method that graphene is prepared using alternative current stripping described in accordance with the claim 1, which is characterized in that electrolysis Time is 1-10h.
- 9. a kind of method that graphene is prepared using alternative current stripping described in accordance with the claim 1, which is characterized in that dry Mode is spray drying and freeze-drying.
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| CN109128148A (en) * | 2018-07-20 | 2019-01-04 | 新疆烯金石墨烯科技有限公司 | A kind of preparation method of graphene aluminum matrix composite |
| CN109231185A (en) * | 2018-10-24 | 2019-01-18 | 深圳大学 | A kind of preparation method of nano-sized carbon onion |
| CN109574355A (en) * | 2018-12-25 | 2019-04-05 | 浙江大学 | A kind of method of resource of the high containing sulfate Acid Dye Wastewater of high concentration |
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| CN109128148A (en) * | 2018-07-20 | 2019-01-04 | 新疆烯金石墨烯科技有限公司 | A kind of preparation method of graphene aluminum matrix composite |
| CN109231185A (en) * | 2018-10-24 | 2019-01-18 | 深圳大学 | A kind of preparation method of nano-sized carbon onion |
| CN109678142A (en) * | 2018-12-24 | 2019-04-26 | 华中科技大学 | A kind of function dough porous graphene and preparation method thereof |
| CN109678142B (en) * | 2018-12-24 | 2021-01-19 | 华中科技大学 | Functionalized porous graphene and preparation method thereof |
| CN109574355B (en) * | 2018-12-25 | 2022-12-09 | 浙江大学 | Recycling method of high-concentration high-sulfur-content hydrochloric acid dye wastewater |
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| CN112978721A (en) * | 2019-12-02 | 2021-06-18 | 中国科学院上海硅酸盐研究所 | Method for preparing high-quality graphene by double-pulse electrochemical technology |
| CN111470499A (en) * | 2020-04-07 | 2020-07-31 | 中钢集团南京新材料研究院有限公司 | Method for electrochemically preparing graphene |
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| CN112225206A (en) * | 2020-10-20 | 2021-01-15 | 陕西理工大学 | Method for preparing water-soluble graphene by electric field driving of double graphite electrodes |
| CN113563760A (en) * | 2021-07-22 | 2021-10-29 | 桂林清研皓隆新材料有限公司 | Electrothermal ink, preparation method thereof and electrothermal product |
| CN114497493A (en) * | 2022-01-21 | 2022-05-13 | 华中科技大学 | Electrically-stripped graphene silicon carbon composite material and preparation method and application thereof |
| CN114540656A (en) * | 2022-02-25 | 2022-05-27 | 南京工程学院 | Preparation method of high-quality electronic aluminum foil |
| CN114604864A (en) * | 2022-04-11 | 2022-06-10 | 东北大学 | Method for preparing graphene by stripping graphite material by virtue of confined electrochemical method |
| CN114604864B (en) * | 2022-04-11 | 2023-08-22 | 东北大学 | Method for preparing graphene by stripping graphite material through limited-area electrochemical method |
| CN115536014A (en) * | 2022-09-21 | 2022-12-30 | 石家庄铁道大学 | Method for electrochemically preparing graphene |
| CN115536014B (en) * | 2022-09-21 | 2023-11-21 | 石家庄铁道大学 | Method for electrochemically preparing graphene |
| CN115784216A (en) * | 2023-01-05 | 2023-03-14 | 沈阳理工大学 | Preparation method of graphene applied to lead-carbon battery negative electrode material |
| CN115784216B (en) * | 2023-01-05 | 2024-03-19 | 沈阳理工大学 | Preparation method of graphene applied to lead-carbon battery anode material |
| CN116395680A (en) * | 2023-04-10 | 2023-07-07 | 中钢集团南京新材料研究院有限公司 | Integrated device and method for preparing graphene by electrochemical method |
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