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Method for electrochemically preparing graphene

An electrochemical and graphene technology, applied in the field of materials, can solve the problems of graphene sheet thickness, high cost, influence of electronic properties, etc., and achieve the effects of less defects, low cost, and environmental friendliness

Active Publication Date: 2015-09-09
苏州格瑞丰纳米科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, although the mechanical exfoliation method can obtain high-quality graphene, it cannot be used for large-scale production and cannot meet the needs of industrialization; although the graphite oxide reduction method can prepare a large amount of graphene at a relatively low cost, graphene The electronic structure and the integrity of the crystal are severely damaged by strong oxidants, which affect its electronic properties, which limits its application in devices to a certain extent.
Although the chemical deposition method can produce graphene with large area and excellent performance, the immaturity of the current process and the high cost limit its large-scale application.
In the international cutting-edge research, the preparation of graphene by electrochemical method has attracted sufficient attention in recent years. This method does not need to use strong oxidants such as potassium permanganate in the preparation process, which can avoid the damage of strong oxidants to the structure and properties of graphene; Use alkali metals (K, Na) and other flammable and explosive dangerous substances, do not introduce toxic and harmful substances, and are environmentally friendly; the preparation conditions are controllable; the cost is low, and it is suitable for large-scale production. However, graphite prepared by existing electrochemical methods The graphene sheet layer is thick, and the graphene structure made from commercial graphite electrode raw materials has many structural defects, which cannot meet the needs of practical applications well.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1 A preparation method of high-purity thin-layer graphene, its technological process is as follows:

[0043] Step S101: Press 250 mg of high-purity graphite to form a film under a pressure of 10 MPa, and use Ag glue to connect the pressed graphite disc to a copper wire to form a graphite electrode as an anode.

[0044] Step S102: 10 mL of 5 M sulfuric acid aqueous solution was used as the electrolyte, and a platinum sheet was used as the cathode, and the anodic oxidation of the graphite electrode was carried out under the condition of a constant voltage of 5 V, and the reaction time was 1 hour. The reaction product was drained and washed with water, and then dried in air for 3 hours. The dried product was subjected to microwave expansion at a power of 800 W for 30 seconds to obtain worm-like expanded graphite.

[0045] Step S103: Press 100 mg of worm-like expanded graphite to form a film under a pressure of 10 MPa, and connect it to a copper wire with Ag glue...

Embodiment 2

[0047] Example 2 A preparation method of high-purity thin-layer graphene, its technological process is as follows:

[0048] Step S101: Press 200 mg of high-purity graphite to form a film under a pressure of 20 MPa, and use Ag glue to connect the pressed graphite disc to a copper wire to form a graphite electrode as an anode.

[0049] Step S102: Use 10 mL of 10 M sulfuric acid aqueous solution as the electrolyte, and a platinum sheet as the cathode, with a constant current of 30 mA / cm 2 The anodic oxidation of the graphite electrode was carried out under the following conditions, and the reaction time was 1 hour. The reaction product was drained and washed with water, and then dried in air for 3 hours. The dried product was subjected to microwave expansion at a power of 800 W for 30 seconds to obtain worm-like expanded graphite.

[0050] Step S103: Press 100 mg of worm-like expanded graphite to form a film under a pressure of 10 MPa, and connect it to a copper wire with Ag...

Embodiment 3

[0052] Example 3 A preparation method of high-purity thin-layer graphene, its technological process is as follows:

[0053] Step S101: Press 300 mg of high-purity graphite to form a film under a pressure of 20 MPa, and use Ag glue to connect the pressed graphite disc to a copper wire to form a graphite electrode as an anode.

[0054] Step S102: Use 10 mL of sulfuric acid-acetic acid mixture (volume ratio: 5:5) as the electrolyte, and a platinum sheet as the cathode, and perform anodic oxidation of the graphite electrode under the condition of a constant voltage of 2.5 V, and the reaction time is 1 hour. After the reaction product was pumped dry, it was expanded in argon at high temperature, the gas flow rate was 200 sccm, and the temperature was 800 o C, the expansion time is 5 minutes, and the worm-like expanded graphite is obtained.

[0055] Step S103: Press 200 mg of worm-like expanded graphite to form a film under a pressure of 10 MPa, and connect it to a copper wire wi...

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Abstract

The invention discloses a method for electrochemically preparing graphene, which preferably comprises the steps of pressing a high-purity graphite raw material to form a graphite electrode, carrying out anodization through the graphite electrode by using sulfuric acid aqueous solution or acetic acid and the like mixed acid solution as an electrolyte to prepare a graphite intercalation product, and obtaining expanded graphite by high temperature or microwave and other methods; and then pressing the expanded graphite to prepare a reaction electrode, and carrying out secondary electrochemical intercalation and expansion to finally obtain laminar graphene. According to the invention, in the preparing process, potassium permanganate and other strong oxidizers are not used, and the damage of the strong oxidizers to the structure and performance of graphene are avoided; alkali metal, fuming sulfuric acid oxydol and other inflammable and explosive dangerous substances are not used, and toxic or harmful substances are not introduced, so that the production is safe and environment friendly; and at the same time, the method is simple in process flow, easy to operate, low in cost, high in yield, mild in reaction conditions and low in energy consumption, and is suitable for industrialized large-scale production.

Description

technical field [0001] The invention relates to a method for preparing graphene materials, in particular to a method for electrochemically preparing graphene, which belongs to the field of material technology. Background technique [0002] Graphene is another major discovery in the field of carbon materials after fullerene and carbon nanotubes. Graphene is composed of single layer sp 2 The honeycomb-like hexagonal planar two-dimensional crystal formed by the arrangement of hybridized carbon atoms can be stacked into 3D graphite, curled into 1D carbon nanotubes, or even wrapped into 0D fullerene. On a two-dimensional plane, sp 2 The hybridized carbon atoms are connected to the adjacent three carbon atoms through strong σ bonds, and the remaining P electron orbitals are perpendicular to the graphene plane, forming large π bonds with the surrounding atoms, making graphene have good conductivity. The theoretical specific surface area of ​​graphene can reach 2630 m 2 / g. The...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/19
Inventor 刘立伟吴丽琼李伟伟耿秀梅李鹏
Owner 苏州格瑞丰纳米科技有限公司
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