Rapid synthesis of fuel cell catalyst using controlled microwave heating

Patent metadata

Field	Value
Publication number	US-9504999-B2
Application number	US-201314027502-A
Country	US
Kind code	B2
Filing date	Sep 16, 2013
Priority date	Jun 29, 2012
Publication date	Nov 29, 2016
Grant date	Nov 29, 2016

Abstract

Methods for the rapid synthesis of catalyst are provided, as well as catalyst formed from such methods. One method of the rapid synthesis of catalyst comprises forming a homogenous solution comprising a precious metal precursor and a catalyst substrate, reducing the precious metal precursor to precious metal nanoparticles, and depositing the precious metal nanoparticles onto the catalyst substrate to form catalyst particles. The reducing and depositing steps comprise controlling a rate of increase in temperature of the solution with microwave irradiation until the solution is a predetermined temperature and maintaining the solution at the predetermined temperature with microwave irradiation. The method further comprises detecting completion of the reduction and deposition and ceasing microwave irradiation upon detection.

First claim

What is claimed is:

1. A method of preparing catalyst comprising:
forming a homogenous solution comprising a precious metal precursor and a catalyst substrate;
reducing the precious metal precursor to precious metal nanoparticles;
depositing the precious metal nanoparticles onto the catalyst substrate to form catalyst particles, wherein reducing and depositing comprise:
controlling a rate of increase in temperature of the solution with microwave irradiation until the solution is at a predetermined temperature by, in a continuous loop, detecting a temperature of the solution with a temperature probe and adjusting the microwave irradiation, based on the temperature of the solution detected by the temperature probe, so that the temperature of the solution rises at the rate of increase until the predetermined temperature is reached; and
maintaining the solution at the predetermined temperature with microwave irradiation;

detecting completion of the reduction and deposition; and
ceasing microwave irradiation upon detection.

2. The method of claim 1 , wherein the rate of increase is between 8° C/minute to 12° C/minute.

3. The method of claim 1 , wherein the predetermined temperature is 300° C. or less.

4. A method of preparing catalyst comprising:
forming a homogenous solution comprising a precious metal precursor and a catalyst substrate;
reducing the precious metal precursor to precious metal nanoparticles;
depositing the precious metal nanoparticles onto the catalyst substrate to form catalyst particles, wherein reducing and depositing comprise:
controlling a rate of increase in temperature of the solution with microwave irradiation until the solution is at a predetermined temperature;
maintaining the solution at the predetermined temperature with microwave irradiation;
detecting completion of the reduction and deposition; and
ceasing microwave irradiation upon detection, wherein maintaining the solution at the predetermined temperature comprises, in a continuous loop:
detecting a temperature of the solution with a temperature probe;
adjusting the microwave irradiation, based on the temperature of the solution detected by the temperature probe, to maintain the solution at predetermined temperature.

5. The method of claim 1 further comprising adding stabilizer to the solution during reduction and deposition.

6. The method of claim 1 further comprising adding a second, stronger reducing agent to the solution during reduction and deposition.

7. The method of claim 1 further comprising adding one or more additional precious metal or transition metal precursors to the solution during reduction and deposition to form alloys or core-shells.

8. The method of claim 1 , wherein detecting completion of deposition comprises:
emitting light through the solution; and
measuring an amount of light emitted through the solution, wherein completion is determined when a predetermined amount of light is measured.

9. The method of claim 8 , wherein the predetermined amount of light is zero.

10. The method of claim 1 further comprising:
cooling the catalyst particles; and
washing the catalyst particles to remove impurities.

11. A method of preparing an ultra-low loading catalyst comprising:
forming a homogenous solution comprising a precious metal precursor and a catalyst substrate;
reducing the precious metal precursor to precious metal nanoparticles;
depositing the precious metal nanoparticles onto the catalyst substrate to form catalyst particles, wherein reducing and depositing comprise:
detecting a temperature of the solution with a temperature probe;
adjusting microwave irradiation of the solution, based on the temperature detected by the temperature probe, so that the temperature of the solution rises at a rate of increase until a predetermined temperature is reached, the rate of increase selected from a range of 8° C/minute to 12° C/minute; and
adjusting the microwave irradiation, based on the temperature of the solution detected by the temperature probe, to maintain the solution at predetermined temperature, wherein the predetermined temperature is 300° C. or less;

detecting completion of the reduction and deposition; and
ceasing microwave irradiation upon detection.

12. The method of claim 11 , wherein the precious metal precursor is a platinum precursor and the catalyst substrate is a non-precious metal catalyst material and the solvent, the homogenous solution further comprising a reducing agent and a stabilizer.

13. The method of claim 12 , wherein the ultra-low loading catalyst comprises less than fifteen weight percent platinum.

14. The method of claim 11 further comprising adding additional stabilizer to the solution during reduction and deposition.

15. The method of claim 11 further comprising adding one or more additional precious metal or transition metal precursors to the solution during reduction and deposition to form alloys or core-shells.

16. The method of claim 11 , wherein detecting completion of deposition comprises:
emitting light through the solution; and
measuring an amount of light emitted through the solution, wherein completion is determined when a predetermined amount of light is measured.

17. The method of claim 16 , wherein the predetermined amount of light is zero.

18. The method of claim 11 further comprising:
cooling the catalyst particles; and
washing the catalyst particles to remove impurities.

Assignees

• Nissan North America Inc

Inventors

• Niangar Ellazar V
• Han Taehee

Classifications

• H01M4/921

  Alloys or mixtures with metallic elements · CPC title

• H01M4/926

  on carbon or graphite · CPC title

• Y02E60/50

  Fuel cells · CPC title

• B01J37/346 Primary

  of microwave energy · CPC title

• H01M4/923 Primary

  Compounds thereof with non-metallic elements · CPC title