Bipolar exfoliation and in-situ deposition of high-quality reduced graphene

Patent metadata

Field	Value
Publication number	US-11352703-B2
Application number	US-202117234114-A
Country	US
Kind code	B2
Filing date	Apr 19, 2021
Priority date	Jun 10, 2020
Publication date	Jun 7, 2022
Grant date	Jun 7, 2022

Abstract

Bipolar electrochemistry (BPE) concepts are used to provide a single-step and controllable process for simultaneously exfoliating a graphite source and depositing both graphene oxide and reduced graphene oxide layers on conductive substrates. A bipolar electrochemical cell can be used for a three-in-one deposition and can include two wired pieces of graphite to monitor the amount of current that passes through the bipolar electrode.

First claim

What is claimed is:

1. A system for a three-in-one in situ exfoliation, reduction, and deposition of graphene oxide and reduced graphene oxide, the system comprising:
a solution;
a negative feeding electrode and a positive feeding electrode disposed in the solution;
a first bipolar electrode and a second bipolar electrode disposed in the solution, the first bipolar electrode and the second bipolar electrode being disposed between the negative feeding electrode and the positive feeding electrode; and
a power analyzer applying a voltage across the positive feeding electrode and the negative feeding electrode,
the first bipolar electrode being a first piece of graphite,
the second bipolar electrode being a second piece of graphite,
the first bipolar electrode being disposed closer to the negative feeding electrode than is the second bipolar electrode,
the second bipolar electrode being disposed closer to the positive feeding electrode than is the first bipolar electrode,
the first bipolar electrode comprising a first surface facing the negative feeding electrode,
the second bipolar electrode comprising a second surface facing the positive feeding electrode,
a distance between the first surface of the first bipolar electrode and the second surface of the second bipolar electrode being greater than both a distance between the first surface of the first bipolar electrode and the negative feeding electrode and a distance between the second surface of the second bipolar electrode and the positive feeding electrode,
the positive feeding electrode and the negative feeding electrode being connected to a first channel of the power analyzer, and
the first bipolar electrode and the second bipolar electrode being connected to a second channel of the power analyzer different from the first channel.

2. The system according to claim 1 , the solution being water.

3. The system according to claim 1 , the solution being deionized water with no additives.

4. The system according to claim 1 , the negative feeding electrode being a stainless steel electrode.

5. The system according to claim 4 , the positive feeding electrode being a stainless steel electrode.

6. The system according to claim 1 , the positive feeding electrode being a stainless steel electrode.

7. The system according to claim 1 , the first bipolar electrode and the second bipolar electrode being configured to measure a bipolar current in the solution.

8. The system according to claim 1 , the first surface of the first bipolar electrode and the second surface of the second bipolar electrode being disposed about 7 centimeters (cm) apart from each other.

9. The system according to claim 1 , the negative feeding electrode and the positive feeding electrode being disposed about 9 cm apart from each other.

10. The system according to claim 1 , further comprising a voltage source connected to the negative feeding electrode and the positive feeding electrode and capable of supplying a direct current (DC) voltage of at least 45 Volts (V).

11. A method for simultaneously exfoliating a graphite source and depositing both graphene oxide and reduced graphene oxide layers on a conductive substrate, the method comprising:
providing a system for three-in-one in situ exfoliation, reduction, and deposition, the system comprising:
a solution;
a negative feeding electrode and a positive feeding electrode disposed in the solution;
a voltage source connected to the negative feeding electrode and the positive feeding electrode; and
a first bipolar electrode and a second bipolar electrode disposed in the solution, the first bipolar electrode and the second bipolar electrode being disposed between the negative feeding electrode and the positive feeding electrode, the first bipolar electrode being a first piece of graphite, and the second bipolar electrode being a second piece of graphite; and

supplying, by the voltage source, a voltage to the system such that: graphene oxide is exfoliated from at least one of the first bipolar electrode and the second bipolar electrode; at least some of the graphene oxide is reduced; and graphene oxide and reduced graphene oxide are deposited on at least one of the negative feeding electrode and the positive feeding electrode,
the first bipolar electrode being disposed closer to the negative feeding electrode than is the second bipolar electrode,
the second bipolar electrode being disposed closer to the positive feeding electrode than is the first bipolar electrode,
the first bipolar electrode comprising a first surface facing the negative feeding electrode,
the second bipolar electrode comprising a second surface facing the positive feeding electrode,
a distance between the first surface of the first bipolar electrode and the second surface of the second bipolar electrode being greater than both a distance between the first surface of the first bipolar electrode and the negative feeding electrode and a distance between the second surface of the second bipolar electrode and the positive feeding electrode,
the voltage source being a power analyzer,
the positive feeding electrode and the negative feeding electrode being connected to a first channel of the power analyzer, and
the first bipolar electrode and the second bipolar electrode being connected to a second channel of the power analyzer different from the first channel.

12. The method according to claim 11 , the solution being water.

13. The method according to claim 11 , the solution being deionized water with no additives.

14. The method according to claim 11 , the negative feeding electrode being a stainless steel electrode.

15. The method according to claim 14 , the positive feeding electrode being a stainless steel electrode.

16. The method according to claim 11 , the positive feeding electrode being a stainless steel electrode.

17. The method according to claim 11 , further comprising measuring, by the first bipolar electrode and the second bipolar electrode, a bipolar current in the solution.

18. The method according to claim 11 , the first surface of the first bipolar electrode and the second surface of the second bipolar electrode being disposed about 7 centimeters (cm) apart from each other, and
the negative feeding electrode and the positive feeding electrode being disposed about 9 cm apart from each other.

19. The method according to claim 11 , the graphene oxide being deposited on at least the positive feeding electrode, and the reduced graphene oxide being deposited on at least the negative feeding electrode.

20. A method for simultaneously exfoliating a graphite source and depositing both graphene oxide and reduced graphene oxide layers on a conductive substrate, the method comprising:
providing a system for three-in-one in situ exfoliation, reduction, and deposition, the system comprising:
a solution;
a negative feeding electrode and a positive feeding electrode disposed in the solution;
a voltage source connected to the negative feeding electrode and the positive feeding electrode; and
a first bipolar electrode and a second bipolar electrode disposed in the solution, the first bipolar electrode and the second bipolar electrode being disposed between the negative feeding electrode and the positive feeding electrode, the first bipolar electrode being a first piece of graphite, and the second bipolar electrode being a second piece of graphite;

supplying, by the voltage source, a voltage to the system such that: graphene oxide is exfoliated from at least on

Assignees

• Khakpour Iman
• Baboukani Amin Rabiei
• Allagui Anis
• Wang Chunlei
• The Florida International Univ Board Of Trustees

Inventors

• Khakpour Iman
• Baboukani Amin Rabiei
• Allagui Anis
• Wang Chunlei

Classifications

• C25B11/046

  Alloys · CPC title

• C25B9/17

  Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof · CPC title

• C25B11/043

  Carbon, e.g. diamond or graphene · CPC title

• C25B15/02 Primary

  Process control or regulation · CPC title

• C25B1/135 Primary

  Carbon · CPC title