IP Library Granted Patent US 10,351,429
Granted Patent B2
US 10,351,429 · App. 14/711,335 · Granted Jul 16, 2019

Direct synthesis of reduced graphene oxide films on dielectric substrates

Inventors: Anirudha V. Sumant (Plainfield, IL); Richard Gulotty (Oak Park, IL)
Assignee: UChicago Argonne, LLC
C01B31/043C01B32/23C23C16/26C23C16/4408C23C16/45557C23C16/52H01B1/04
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Quick Facts
Patent No.
US 10,351,429
App. No.
14/711,335
Granted
Jul 16, 2019
Kind
B2
Abstract

A method for coating a dielectric substrate with a R-GO film includes positioning the dielectric substrate in a chamber which is purged with a first gas to adjust a pressure of the chamber to a first pressure. A second gas at a second flow rate and a third gas at a third flow rate is inserted into the chamber to increase the chamber pressure to a second pressure greater than the first pressure. A chamber temperature is increased to a first temperature. The flow of the second gas and the third gas is stopped. The chamber is purged to a third pressure higher than the first pressure and lower than the second pressure. The pressure of the chamber is set at a fourth pressure greater than the first pressure and the third pressure. A fourth gas is inserted into the chamber at a fourth flow rate for a first time.

Claims (58)

1. A method for coating a dielectric substrate with a reduced graphene oxide film, comprising:

positioning the dielectric substrate in a chamber, the dielectric substrate being free of graphene oxide or a metallic catalyst;

depositing the reduced graphene oxide as a uniform layer directly on the dielectric substrate by:

purging the chamber with a first gas to adjust a pressure of the chamber to a first pressure;

inserting a second gas at a second flow rate and a third gas at a third flow rate into the chamber to increase the pressure inside the chamber to a second pressure, the second pressure greater than the first pressure;

increasing a temperature of the chamber to a first temperature;

stopping the flow of the second gas onto the chamber;

stopping the flow of the third gas into the chamber;

purging the chamber to a third pressure, the third pressure higher than the first pressure and lower than the second pressure;

setting the pressure of the chamber at a fourth pressure, the fourth pressure greater than the first pressure and the third pressure; and

inserting a fourth gas into the chamber at a fourth flow rate for a first time period,

wherein the reduced graphene oxide film comprises clusters of carbon having sp3 bonding in the range of 45% to 70%.

2. The method of claim 1 , further comprising:

reducing the fourth flow rate of the fourth gas to a fifth flow rate; and

maintaining the fifth flow rate for a second time period.

3. The method of claim 1 , wherein the dielectric substrate includes at least one of silicon oxide, silicon nitride, quartz, sapphire, magnesium oxide, and fused silica.

4. The method of claim 1 , wherein the first gas is nitrogen.

5. The method of claim 1 , wherein second gas is hydrogen, and wherein the third gas is argon.

6. The method of claim 1 , wherein the second pressure is in the range of 250 Torr to 350 Torr.

7. The method of claim 1 , wherein the first temperature is in the range of 800 degrees Celsius to 1,200 degrees Celsius.

8. The method of claim 1 , wherein the third pressure is about 1 Torr.

9. The method of claim 1 , wherein the fourth gas is at least one of methane, ethylene and ethane.

10. The method of claim 1 , wherein the reduced graphene oxide film has an optical transmittance of at least 80% at a thickness of up to about 5 nm.

11. The method of claim 1 , wherein the reduced graphene oxide film has a sheet resistance of 5 kOhm/square to 10 kOhm/square.

12. The method of claim 1 , wherein the reduced graphene oxide film has a thermal conductivity in the range of 60 W/m-K to 120 W/m-K.

13. A method for forming a transparent electrode, comprising:

providing a transparent dielectric substrate, the dielectric substrate being free of graphene oxide or a metallic catalyst;

positioning the transparent dielectric substrate in a chamber;

purging the chamber with nitrogen to adjust a pressure of the chamber to a first pressure;

inserting hydrogen at a second flow rate and argon at a third flow rate into the chamber to increase the pressure inside the chamber to a second pressure, the second pressure greater than the first pressure;

increasing a temperature of the chamber to a first temperature;

stopping the flow of hydrogen into the chamber;

stopping the flow of argon into the chamber;

purging the chamber to a third pressure, the third pressure higher than the first pressure and lower than the second pressure;

setting the pressure of the chamber at a fourth pressure, the fourth pressure greater than the first pressure and the third pressure; and

inserting methane into the chamber at fourth flow rate for a first time period to deposit a predetermined thickness of an electrically conductive reduced graphene oxide film as a uniform layer directly on the transparent dielectric substrate,

wherein the reduced graphene oxide film has a thermal conductivity in the range of 60 W/m-K to 120 W/m-K, and

wherein the reduced graphene oxide film comprises clusters of carbon having sp3 bonding in the range of 45% to 70%.

14. The method of claim 13 , wherein the fourth flow rate is in the range 800 sccm to 1,200 sccm and, wherein the fourth pressure is in the range of 250 Torr to 350 Torr.

15. The method of claim 13 , wherein the reduced graphene oxide film has a sheet resistance of 5 kOhm/square to 10 kOhm/square.

16. The method of claim 14 , further comprising:

reducing the flow rate of the fourth gas to a fifth flow rate; and

maintaining the fifth flow rate for a second time period to deposit the electrically conductive reduced graphene oxide film on the transparent dielectric substrate.

17. A method of enhancing heat transfer from an electronic device, comprising:

depositing a reduced graphene oxide film as a uniform layer directly on a dielectric substrate of the electronic device, the dielectric substrate being free of graphene oxide and a metallic catalyst, the reduced graphene oxide film deposited by:

positioning the electronic device in a chamber;

purging the chamber with nitrogen to adjust a pressure of the chamber to a first pressure;

inserting hydrogen at a second flow rate and argon at a third flow rate into the chamber to increase the pressure inside the chamber to a second pressure, the second pressure greater than the first pressure;

increasing a temperature of the chamber to a first temperature;

stopping the flow of hydrogen into the chamber;

stopping the flow of argon into the chamber;

purging the chamber to a third pressure, the third pressure higher than the first pressure and lower than the second pressure;

setting the pressure of the chamber at a fourth pressure, the fourth pressure greater than the first pressure and the third pressure; and

inserting methane into the chamber at fourth flow rate for a first time period to deposit a predetermined thickness of a reduced graphene oxide film on a surface of the electronic device,

wherein, the reduced graphene oxide film has a thermal conductivity in the range of 60 W/m-K to 120 W/m-K.

18. The method of claim 17 , wherein the reduced graphene oxide film has an optical transmittance of at least 80% at a thickness of up to about 5 nm.

19. The method of claim 17 , wherein the reduced graphene oxide film has a sheet resistance of 5 kOhm/square to 10 kOhm/square.

20. The method of claim 13 , wherein the reduced graphene oxide film has an optical transmittance of at least 80% at a thickness of up to about 5 nm.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 5, 2015
From: SUMANT, ANIRUDHA V.; GULOTTY, RICHARD
To: UCHICAGO ARGONNE, LLC
Reel/Frame 037054/0039 →
CONFIRMATORY LICENSE Recorded Oct 26, 2015
From: UCHICAGO ARGONNE, LLC
To: ENERGY, UNITED STATES DEPARTMENT OF
Reel/Frame 036954/0325 →
Continuity (1)
Related Publication 20160332885A1 · Nov 17, 2016