Method for preparing graphene

A technology of graphene and graphene powder, applied in the field of graphene, which can solve problems such as environmental pollution, low efficiency, and large graphene sheet formation

Inactive Publication Date: 2016-10-12
GUANGZHOU TINGYU ENERGY TECH CO LTD
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Problems solved by technology

This method is low in cost, but this method reacts with strong acid and strong oxidizing substances to form graphene oxide, which will cause a large number of defects in graphene sheets during the oxidation process, resulting in the change of graphene properties, and this method uses strong acid and strong Oxidizing substances can also cause ser...

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  • Method for preparing graphene

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Embodiment 1

[0035] Using 30%wt ammonium chloride solution as intercalation agent and expanded graphite as raw material, the pretreatment time is 6 hours; the voltage of electrochemical oxidation is 10V, and the oxidation time is 30 minutes; followed by ultrasonic treatment, the time is 30 minutes , obtain a dispersion of graphene oxide, filter to obtain graphene oxide powder, use freeze drying method to dry, and heat-treat at 500° C. for 1 hour in an atmosphere protected by argon to obtain graphene powder.

[0036] In the graphene powder obtained in this example, the number of graphene sheets is 3 to 10 layers, the average thickness is 3.4 nanometers, the average sheet size is 5.3 microns, the crystallinity is good, and the ash content is <0.1%.

Embodiment 2

[0038] Using 30%wt ammonium chloride solution as intercalation agent and expanded graphite as raw material, the pretreatment time is 6 hours; the voltage of electrochemical oxidation is 10V, and the oxidation time is 30 minutes; followed by ultrasonic treatment, the time is 30 minutes , obtain a dispersion of graphene oxide, filter to obtain graphene oxide powder, use freeze-drying to dry, and heat-treat at 500° C. for 1 hour in a nitrogen-protected atmosphere to obtain graphene powder.

[0039] In the graphene powder obtained in this embodiment, the number of graphene sheets is 3 to 8 layers, the average thickness is 2.9 nanometers, the average sheet size is 5.1 microns, and the ash content is <0.1%.

Embodiment 3

[0041] Using 50%wt ammonium nitrate solution as intercalation agent, carbon paper as raw material, pretreatment time is 30 minutes; electrochemical oxidation voltage is 15V, oxidation time is 30 minutes; followed by ultrasonic treatment, time is 30 minutes, The dispersion of graphene oxide was obtained, filtered to obtain graphene oxide powder, dried by freeze-drying method, and heat-treated at 500° C. for 2 hours in an atmosphere protected by argon to obtain graphene powder.

[0042] In the graphene powder obtained in this embodiment, the number of graphene sheets is 2 to 5 layers, the average thickness is 1.9 nm, the average sheet size is 5.5 microns, and the ash content is <0.1%.

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Abstract

A kind of method for preparing graphene of the present invention, concrete process is: with halogen, hydrochloric acid, hydrogen bromide, hydrogen iodide, ammonium nitrate, zinc chloride, ferric chloride, ammonium carbonate, sodium carbonate, potassium carbonate or ammonium bicarbonate , sodium bicarbonate, potassium bicarbonate and other high-temperature, easy-to-evaporate, sublime, and easily-decomposed substances are used as intercalation agents, and the raw materials for preparing graphene, such as expanded graphite, layered graphite, and carbon paper, are pretreated. , the pretreated raw material is electrochemically oxidized under a certain voltage to obtain an oxidized precursor, and the oxidized material is further blasted and peeled off under the action of ultrasound and stirring to obtain flaky graphene oxide, and then after heat treatment Graphene oxide will be reduced to graphene. The method of the invention is simple to operate and convenient to prepare, and can prepare high-quality graphene or graphene oxide on a large scale, and can be used to solve the problems of high cost, low product quality, complicated operation and large pollution in the current graphene preparation technology.

Description

technical field [0001] The invention relates to the field of graphene, more specifically, to a method for large-scale preparation of graphene. Background technique [0002] Due to its high electrical and thermal conductivity, high light transmittance, high specific surface area, good mechanical properties and flexibility, graphene, as a new type of carbon material, has attracted people's attention in recent years. According to the content of "Made in China (2025)", graphene is expected to be widely used in the fields of lithium-ion batteries for electric vehicles, marine engineering anti-corrosion, flexible electronic devices, and electrical and thermal materials in the field of light and electricity in the future. However, large-scale preparation of high-quality graphene is still a difficult problem faced by the industry. [0003] The methods of producing graphene can be roughly divided into four types: [0004] 1. Mechanical peeling method [0005] The mechanical exfoli...

Claims

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Application Information

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IPC IPC(8): C01B31/04
CPCC01B2204/04C01B2204/30C01P2004/01
Inventor 邓惠贤
Owner GUANGZHOU TINGYU ENERGY TECH CO LTD
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