Exfoliation of graphite to graphene by interface stabilization

Patent metadata

Field	Value
Publication number	US-12404177-B2
Application number	US-202217674389-A
Country	US
Kind code	B2
Filing date	Feb 17, 2022
Priority date	Feb 18, 2021
Publication date	Sep 2, 2025
Grant date	Sep 2, 2025

Abstract

Systems and methods are provided that may utilize a glass substrate to selectively withdraw exfoliated graphene from a high-energy interface between immiscible solvents. The exfoliated graphene preferentially adheres to the surface of the glass substrate for withdrawal from the noted high energy interface, leaving behind the graphite (which is too large to be effectively adsorbed relative to the glass substrate). The disclosed systems and methods are easily implemented and offer significant advantages for graphene production relative to conventional systems and methods, e.g., the disclosed systems/methods do not require the input of heat or mechanical energy which translates to processes that are both cheaper to run and do not result in damage to the graphene. Still further, the disclosed systems/methods do not require chemical modification of the graphene, again lowering the cost considerably and not damaging the graphene structure.

First claim

The invention claimed is:

1. A method for graphene production, comprising:
a. providing a continuous graphene recovery system that includes a glass fiber that defines a continuous loop, a first vessel containing graphite and immiscible solvents for exfoliating graphene at a high-energy interface between the immiscible solvents, and a second vessel containing a fluid for separating adsorbed graphene from the glass fiber;
b. moving a segment of the glass fiber loop through the high-energy interface within the first vessel to permit adsorption of exfoliated graphene from the high-energy interface onto the segment of the glass fiber loop;
c. moving the segment of the glass fiber loop through the second vessel to permit separation of the adsorbed exfoliated graphene from the segment of the glass fiber loop and deposit of graphene in the fluid; and
d. repeating steps (a)-(c) to recover additional graphene in the fluid.

2. The method of claim 1 , wherein the immiscible solvents define an emulsion.

3. The method of claim 1 , wherein the segment of the glass fiber loop is wetted prior to contact with the high-energy interface.

4. The method of claim 3 , wherein the segment of the glass fiber loop is wetted with water.

5. The method of claim 1 , wherein the high-energy interface is established by first and second surface/solvent constituents selected from the group consisting of:
a. first surface/solvent constituent: water; second surface/solvent constituent: heptane, pentane, or other alkane;
b. first surface/solvent constituent: glass (hydrophilic); second surface/solvent constituent: heptane, pentane or other alkane;
c. first surface/solvent constituent: chlorosilane treated glass (hydrophobic): second surface/solvent constituent: water;
d. first surface/solvent constituent: water; second surface/solvent constituent: styrene, methyl methacrylate or a comparable monomer;
e. first surface/solvent constituent: water; second surface/solvent constituent: chloroform;
f. first surface/solvent constituent: gallium; second surface/solvent constituent: heptane;
g. first surface/solvent constituent: glycerol; second surface/solvent constituent: heptane;
h. first surface/solvent constituent: heptane; second surface/solvent constituent: acetonitrile;
i. first surface/solvent constituent: PTFE; second surface/solvent constituent: water;
j. first surface/solvent constituent: gallium; second surface/solvent constituent: water;
k. first surface/solvent constituent: HDPE; second surface/solvent constituent: water;
l. first surface/solvent constituent: polypropylene; second surface/solvent constituent: water.

Assignees

• Univ Connecticut

Inventors

• Adamson Douglas H
• Parnas Richard
• Abeykoon Prabodha

Classifications

• C03C25/44

  Carbon, e.g. graphite · CPC title

• C03C2218/328

  Partly or completely removing a coating · CPC title

• C03C13/00

  Fibre or filament compositions (manufacture of fibres or filaments C03B37/00) · CPC title

• C03C12/00

  Powdered glass (C03C8/02 takes precedence); Bead compositions · CPC title

• C01B32/184

  Preparation · CPC title