# US 12,006,222 B2 · Method for the manufacture of microwave-reduced graphene oxide

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- Number: US 12,006,222 B2
- Document ID: US12006222B2
- Status: Granted
- Kind: B2
- Application number: 17/272,779
- Filed: 2019-07-09
- Published: 2021-07-15
- Granted: 2024-06-11
- Earliest claimed: 2018-09-05
- Assignees: ArcelorMittal
- Applicants: ArcelorMittal
- Inventors: Thi Tan Vu; Oscar Perez Vidal; Juan Jose Arribas; David Noriega Perez; Roberto Suarez Sanchez
- Web page: https://patentgrep.com/patent/US12006222B2

## CPC

- C01B 32/184: Preparation
- C01B 32/198: Graphene oxide
- B01J 21/18: Carbon
- C01B 32/182: Graphene
- C01B 32/194: After-treatment
- Y02E 60/13: Energy storage using capacitors
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

A method for the manufacture of microwave-reduced graphene oxide (MW-rGO) including: the provision of graphene oxide (GO), the reduction of GO into reduced graphene oxide (rGO) using a reducing agent and the reduction of rGO into MW-rGO by microwaving under air atmosphere in presence of a catalyst.

## Claims

### Claim 1

A method for manufacturing microwave-reduced graphene oxide (MW-rGO) comprising:
A. providing graphene oxide (GO) including at least one layer of graphene including at least 25% by weight of oxygen functional groups;
B. reducing the GO into reduced graphene oxide (rGO) including at least one layer of graphene having between 10 and 25% by weight of oxygen functional groups, using a reducing agent; and
C. reducing the rGO into MW-rGO, including at least one layer of graphene having less than 10% by weight of oxygen functional groups, by microwaving rGO under air atmosphere in presence of a catalyst.

### Claim 2 (depends on 1)

The method as recited in claim 1 wherein in step B), the reducing agent is at least one of the group consisting of: acid ascorbic; urea; hydrazine hydrate; alkaline solution; phenols; alcohols; glycine; sodium citrate and sodium borohydride.

### Claim 3 (depends on 1)

The method as recited in claim 1 wherein in step B), the reduction is performed a temperature between 50 and 120° C.

### Claim 4 (depends on 1)

The method as recited in claim 1 wherein in step B), the reduction is performed during less than 24 hours.

### Claim 5 (depends on 1)

The method as recited in claim 1 wherein in step C), the catalyst is at least one of the group consisting of: pristine graphene, graphene nanoplatelet(s), graphite and graphite nanoplatelets.

### Claim 6 (depends on 5)

The method as recited in claim 5 wherein in step C), the catalyst is pristine graphene.

### Claim 7 (depends on 1)

The method as recited in claim 1 wherein in step C), the ratio in weight of rGO with respect to the catalyst is as follows:
50
≤
amount
⁢
of
⁢
rGO
amount
⁢
of
⁢
catalyst
≤
15
⁢
0
.

### Claim 8 (depends on 7)

The method as recited in claim 7 wherein in step C), the ratio in weight of rGO with respect to the catalyst is as follows:
75
≤
amount
⁢
of
⁢
rGO
amount
⁢
of
⁢
catalyst
≤
12
⁢
5
.

### Claim 9 (depends on 1)

The method as recited in claim 1 wherein in step C), the microwave frequency is between 300 MHz and 100 GHz.

### Claim 10 (depends on 9)

The method as recited in claim 9 wherein in step C), the microwave frequency is between 1000 MHz and 5000 MHz.

### Claim 11 (depends on 1)

The method as recited in claim 1 wherein step C) is performed with a microwave frequency heating device.

### Claim 12 (depends on 11)

The method as recited in claim 11 wherein the microwave frequency heating device is a microwave oven.

### Claim 13 (depends on 1)

The method as recited in claim 1 wherein the microwave has a power between 100 W and 100 kW.

### Claim 14 (depends on 1)

The method as recited in claim 1 wherein in step C), the microwaving is performed for at least 2 seconds.

### Claim 15 (depends on 1)

The method as recited in claim 1 wherein the at least one layer of graphene includes a plurality of layers.

### Claim 16 (depends on 1)

The method as recited in claim 1 wherein the plurality of layers is four or fewer.