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Preparation method and application of graphene powder

A technology of graphene powder and graphite powder, which is applied in the field of graphene powder preparation, can solve the problems of not meeting the demand for graphene powder materials, high equipment cost requirements, and large consumption of chemical reagents, and achieve good electronic conductivity and Effect of load transfer, reduction of application cost, effect of low application cost

Active Publication Date: 2020-08-21
西安稀有金属材料研究院有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mechanical exfoliation method is only suitable for laboratory research, the yield is extremely low, and special equipment is required
The redox method can be used for industrial production of graphene oxide and graphene powder, but it requires high process precision, poor controllability, high oxygen content, high consumption of chemical reagents, and difficult disposal of waste liquid; especially the reduction of graphene oxide When making graphene or reducing graphene oxide, it is necessary to use a toxic and strong reducing agent, which seriously pollutes the environment
Chemical vapor deposition can be used for large-scale graphene production and preparation, but it is mainly used for the preparation of graphene thin films, and requires high equipment costs
None of the above-mentioned existing preparation methods can meet the needs of low-cost industrial graphene powder materials

Method used

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  • Preparation method and application of graphene powder
  • Preparation method and application of graphene powder
  • Preparation method and application of graphene powder

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Experimental program
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Effect test

Embodiment 1

[0031] This embodiment includes the following steps:

[0032] Step 1. Pretreatment: Add 500g of commercially available flake graphite powder to 1000mL of acetone, use 50kW power to ultrasonically clean for 50min to remove surface oil and impurities, then let it stand until stratified, pour out the supernatant liquid, and pour out the graphite powder on the lower layer Add ethanol to the colloid for cleaning, and then vacuum freeze-dry for 15 hours at a vacuum degree of -0.1MPa and a temperature of -80°C to obtain pretreated graphite powder;

[0033] Step 2, intercalation heat treatment: the pretreated graphite powder obtained in step 1 is protected by a hydrogen-argon mixed atmosphere and subjected to an intercalation heat treatment at a temperature of 800°C for 6 hours; the volume ratio of hydrogen to argon in the hydrogen-argon mixed atmosphere 4:1, the flow rate of hydrogen-argon mixed atmosphere is 2L / min;

[0034]Step 3, ball milling and exfoliation treatment: the graphi...

Embodiment 2

[0040] This embodiment includes the following steps:

[0041] Step 1. Pretreatment: Add 10g of commercially available flake graphite powder into 100mL of acetone, use 30kW power to ultrasonically clean for 30min to remove surface oil and impurities, then let stand until stratified, pour out the supernatant liquid, and pour out the graphite powder on the lower layer Add ethanol to the colloid for cleaning, and then vacuum freeze-dry for 10 hours at a vacuum degree of -0.1MPa and a temperature of -80°C to obtain pretreated graphite powder;

[0042] Step 2, intercalation heat treatment: the pretreated graphite powder obtained in step 1 is protected by a hydrogen-argon mixed atmosphere and subjected to an intercalation heat treatment at a temperature of 600°C for 4 hours; the volume ratio of hydrogen to argon in the hydrogen-argon mixed atmosphere 4:1, the flow rate of hydrogen-argon mixed atmosphere is 10L / min;

[0043] Step 3, ball milling and exfoliation treatment: the graphit...

Embodiment 3

[0045] This embodiment includes the following steps:

[0046] Step 1. Pretreatment: Add 2000g of commercially available flake graphite powder to 2000mL of acetone, use 100kW power to ultrasonically clean for 60min to remove surface oil and impurities, then stand until stratified, pour out the supernatant liquid, and pour out the graphite powder on the lower layer Add ethanol to the colloid for cleaning, and then vacuum freeze-dry for 30 hours under the conditions of vacuum degree of -0.1MPa and temperature of -80°C to obtain pretreated graphite powder;

[0047] Step 2, intercalation heat treatment: the pretreated graphite powder obtained in step 1 is protected by a hydrogen-argon mixed atmosphere and subjected to an intercalation heat treatment at a temperature of 1000°C for 10 hours; the volume ratio of hydrogen to argon in the hydrogen-argon mixed atmosphere 4:1, the flow rate of hydrogen-argon mixed atmosphere is 5L / min;

[0048] Step 3, ball milling and exfoliation treatm...

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Abstract

The invention discloses a preparation method of graphene powder. The method comprises the following steps: 1, carrying out ultrasonic cleaning on graphite powder, and carrying out vacuum freeze dryingto obtain pretreated graphite powder; 2, carrying out intercalation heat treatment on the pretreated graphite powder under atmosphere protection; and 3, performing ball-milling stripping of high-speed vibration shearing on the graphite powder subjected to intercalation heat treatment under a low-temperature liquid nitrogen condition to obtain the graphene powder. The invention also discloses an application of the graphene powder as a reinforcement material in a metal composite material. Vacuum freeze drying, intercalation heat treatment and ball-milling stripping under the low-temperature liquid nitrogen condition are combined, the bonding force between graphite flake layers of the graphite powder is gradually weakened, the spacing between the graphite flake layers is increased, the graphene powder with low-density defects and multi-stage distribution is obtained through layer-by-layer stripping, pollution to the environment is avoided, the requirement for equipment is low, the yieldis high, and the method is suitable for large-scale industrial production of the graphene powder; and the application of the invention improves the performance of the metal composite material.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a preparation method and application of graphene powder. Background technique [0002] The development of the carbon element family has brought new opportunities for the development of modern material science. In particular, the discovery of graphene following carbon nanotubes will bring new technological revolutions in the fields of energy, chemical industry, biology, and semiconductors. In 2004, professors Andre Geim and Konstantin Novoselov in the UK discovered graphene for the first time by mechanical physical exfoliation, and won the 2010 Nobel Prize in Physics for this. So far, graphene, as the darling of the material industry, has received extensive attention from scientific researchers. [0003] In simple terms, single-layer graphene has SP 2 Hybrid monoatomic layer two-dimensional graphite microflakes. Due to its unique structure, graphene is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19C22C14/00C22C1/05C22C9/00C22C21/00
CPCC22C1/05C22C9/00C22C14/00C22C21/00C01B32/19
Inventor 董龙龙李亮刘跃卢金文霍望图张伟张于胜
Owner 西安稀有金属材料研究院有限公司
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