Method for HF-free facile and rapid synthesis of MXenes related compounds

Patent metadata

Field	Value
Publication number	US-12344944-B2
Application number	US-202016946459-A
Country	US
Kind code	B2
Filing date	Jun 23, 2020
Priority date	Jun 24, 2019
Publication date	Jul 1, 2025
Grant date	Jul 1, 2025

Abstract

Provided herein is a method for preparing MXenes, such as Ti 2 CT x , Cr 2 CT x , and V 2 CT x , products prepared therefrom, and compositions and devices including the same.

First claim

What is claimed:

1. A method for preparing a MXene, the method comprising:
providing a composite electrode comprising at least one MAX-phase composition and a carbonaceous material, wherein the at least one MAX-phase composition has an empirical formula of M n+1 AX n , wherein M is Ti, A is Al, X is C, and n is 1;
a counter electrode; and
an aqueous electrolyte solution comprising 1 M HCl between and in contact with the composite electrode and the counter electrode; and
applying an electric current at a potential of 0.3 V between the composite electrode and the counter electrode for 9 hours resulting in electrolytic reduction of the at least one MAX-phase composition thereby forming the MXene, wherein the electrolytic reduction is conducted at a temperature between 45 to 55° C.

2. The method of claim 1 , wherein the carbonaceous material is carbon black (CB), carbon fiber cloth (CFC), or a mixture thereof.

3. The method of claim 1 , wherein the composite electrode further comprises a binder.

4. The method of claim 1 , wherein the at least one MAX-phase composition and the carbonaceous material are present in the composite electrode in a mass ratio of 80:20 to 99:1, respectively.

5. The method of claim 4 , wherein the composite electrode further comprises a binder, wherein the binder is present in the composite electrode at 0.1 to 3% by weight.

6. The method of claim 1 , wherein the at least one MAX-phase composition and the carbonaceous material are present in the composite electrode in a mass ratio of 80:20 to 99:1, respectively and the binder is present in the composite electrode 0.1 to 2% by weight.

7. A method for preparing a MXene, the method comprising:
providing a composite electrode comprising at least one MAX-phase composition; a carbonaceous material selected from the group consisting of CB, CFC, and combinations thereof; a binder, wherein the at least one MAX-phase composition has an empirical formula of M n+1 AX n , wherein each of M is Ti; A is Al; and each X is C; and n is 1; wherein the at least one MAX-phase composition and carbonaceous material are present in the composite electrode in a mass ratio of 90:10 to 99:1; and wherein the binder is present in the composite electrode in a weight ratio of 1.0-1.5% by mass;
a counter electrode; and
an electrolyte solution comprising 1 M HCl between and in contact with the composite electrode and the counter electrode; and
applying an electric current between the composite electrode and the counter electrode at a voltage 0.3 V for 9 hours resulting in the electrolytic reduction of the at least one MAX-phase composition thereby forming the MXene, wherein the electrolytic reduction is conducted at a temperature between 45 to 55° C.

Assignees

• Univ Hong Kong Polytechnic

Inventors

• Hao Jianhua
• Pang Sin Yi

Classifications

• C01B21/0617

  with vanadium, niobium or tantalum · CPC title

• C01B21/076

  with titanium or zirconium {or hafnium} · CPC title

• C25F5/00

  Electrolytic stripping of metallic layers or coatings · CPC title

• C25B1/00

  Electrolytic production of inorganic compounds or non-metals · CPC title

• C01B32/921

  Titanium carbide · CPC title