Graphene powder, and preparation method therefor and application thereof

Patent metadata

Field	Value
Publication number	US-12330945-B2
Application number	US-202118555904-A
Country	US
Kind code	B2
Filing date	Sep 27, 2021
Priority date	Apr 22, 2021
Publication date	Jun 17, 2025
Grant date	Jun 17, 2025

Abstract

A graphene powder, its preparation method and application are provided. The graphene powder is a stack of graphene sheets. The graphene powder involves in its Raman spectrum a D peak and a G peak with peak heights of ID and IG respectively, where ID/IG is 0.10 or less. The graphene powder can be applied in conductive composite materials, anti-corrosion coatings, heat dissipation composite materials. In particular, when used in lithium-ion batteries, it can significantly reduce electrode internal resistance and improve battery stability at any current rates.

First claim

The invention claimed is:

1. A graphene powder comprising particles that each comprises a plurality of graphene sheets and voids disposed among the plurality of graphene sheets, wherein the graphene powder has a Raman spectrum with a D peak and a G peak having peak heights of ID and IG, respectively, wherein ID/IG is 0.03-0.10, and wherein the graphene powder has a carbon content of greater than or equal to 99.50%, a particle size of 20-35 μm, a specific surface area of 50-300 m 2 /g, and an oxygen content of 300 ppm or less.

2. The graphene powder of claim 1 , wherein based on a total mass of the graphene powder, the graphene powder has a carbon content of 99.80-99.95%.

3. The graphene powder of claim 1 , wherein the graphene powder has a specific surface area of 100-250 m 2 /g; or
the graphene powder has a tap density of 0.02-0.04 g/cm 3 ; or
the graphene powder has a conductivity of 500-5000 S/cm.

4. The graphene powder of claim 1 , wherein each of the graphene sheets comprises 1-10 layers of graphene; or each of the graphene sheets has a median particle size of 5-15 μm.

5. The graphene powder of claim 1 , having a starting temperature for thermal decomposition of greater than or equal to 600° C.; or
when subjected to a heat treatment under an air atmosphere at 800° C., the graphene powder has a thermal-loss rate of less than or equal to 10%.

6. The graphene powder of claim 1 , having a conductivity of 500-5000 S/cm.

7. A method for preparing the graphene powder of claim 1 , comprising the steps of:
(1) subjecting an expandable graphite to pre-expanding, to obtain a pre-expanded graphite;
(2) mixing the pre-expanded graphite obtained in step (1), a wetting agent and a solvent, and then subjecting the mixture to a first high-pressure homogenization and a second high-pressure homogenization, to obtain a slurry containing a graphene powder, wherein the pressure of the second high-pressure homogenization is 10-20 MPa higher than the pressure of the first high-pressure homogenization; and
(3) drying the slurry containing the graphene powder obtained in step (2), to obtain the graphene powder of claim 1 .

8. The method of claim 7 , wherein, compared to the expandable graphite before the pre-expanding, the pre-expanded graphite obtained in step (1) has an expansion ratio of 200-300 times.

9. The method of claim 7 , wherein, in step (2), the first high-pressure homogenization is operated at a pressure of 30-40 MPa for 20-60 minutes, and the second high-pressure homogenization is operated at a pressure of 40-50 MPa for 10-30 minutes.

10. The method of claim 7 , wherein the wetting agent in step (2) is fatty amine polyoxyethylene ether.

11. The method of claim 7 , wherein the pre-expanded graphite obtained in step (1) and the wetting agent are fed in a mass ratio of 1:0.01-0.1 in step (2).

12. The method of claim 7 , wherein the drying in step (3) is spray drying or freeze-drying, wherein the spray drying is operated under conditions of: the air inlet temperature being 300-350° C., the air inlet temperature being 200-250° C. higher than the air outlet temperature, the air outlet temperature being 100-130° C., and the rotating speed of the centrifugal disc of the spray drying equipment being 20000-30000 rpm; and wherein the freeze-drying is operated under conditions of: the cold trap temperature being not higher than-65° C.; the temperature of the cubical separator being not higher than −55° C.; the heating rate being 0.1-0.5° C./min; the time for heating from the temperature of the cubical separator to 0° C. being not less than 24 hours; and the vacuum degree being not higher than 10 Pa.

Assignees

• China Petroleum & Chem Corp
• Shanghai Res Inst Petrochemical Tech Sinopec

Inventors

• Sun Sai
• Zhang Siyu
• Dong Wenqian
• Gao Huanxin

Classifications

• C01P2006/11

  Powder tap density · CPC title

• C01P2004/04

  obtained by TEM, STEM, STM or AFM · CPC title

• C01P2004/03

  obtained by SEM · CPC title

• C01P2002/82

  by IR- or Raman-data · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title