Electrocatalyst for electrochemical conversion of carbon dioxide

• US 9,099,752 B2
• Filed: 07/24/2014
• Issued: 08/04/2015
• Est. Priority Date: 04/02/2012
• Status: Active Grant

• Current Assignee: King Fahd University Of Petroleum And Minerals
• Original Assignee: King Fahd University Of Petroleum And Minerals
• Inventors: Rahman, Saleem Ur, Zaidi, Syed Mohammed Javaid, Ahmed, Shakeel, Hossain, Sk Safdar
• Primary Examiner(s): MCDONOUGH, JAMES E
• Application Number:
  US14/340,222
• Publication Number:
  US 20140336036A1
• Time in Patent Office: 376 Days
• Field of Search: 204/282, 502/5, 502/100, 502/101, 502/102, 502/104
• US Class Current: 1/1
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C25B 11/04 characterised by the material
• CPC Class Codes: C25B 3/25 Reduction
• CPC Class Codes: H01M 4/8842 Coating using a catalyst salt precursor in solution followed by evaporation and reduction of the precursor
• CPC Class Codes: H01M 4/8882 Heat treatment, e.g. drying, baking
• CPC Class Codes: H01M 4/9041 Metals or alloys H01M4/92 takes precedence
• CPC Class Codes: H01M 4/9075 Catalytic material supported on carriers, e.g. powder carriers H01M4/8807, H01M4/881, H01M4/8814, H01M4/925 take precedence
• CPC Class Codes: H01M 4/925 supported on carriers, e.g. powder carriers
• CPC Class Codes: Y02E 60/50 Fuel cells

Abstract

The electrocatalyst for the electrochemical conversion of carbon dioxide includes a copper material supported on titania nanotubes. The copper material may be pure copper, copper and ruthenium, or copper and iron supported on the titania nanotubes. The electrocatalyst is prepared by first dissolving copper nitrate trihydrate in deionized water to form a salt solution. Titania nanotubes are then added to the salt solution to form a suspension, which is then heated. A urea solution is added to the suspension to form the electrocatalyst in solution. The electrocatalyst is then removed from the solution. In addition to dissolving the copper nitrate trihydrate in the volume of deionized water, either iron nitrate monohydrate or ruthenium chloride may also be dissolved in the deionized water to form the salt solution.

Claims

1. A method of making an electrocatalyst for electrochemical conversion of carbon dioxide, comprising the steps of:

dissolving copper nitrate trihydrate in deionized water to form a salt solution;

adding titania nanotubes to the salt solution to form a suspension;

heating the suspension;

adding a urea solution to the suspension to form an electrocatalyst in solution, the electrocatalyst being copper material supported on the titania nanotubes; and

removing the electrocatalyst from the solution, wherein the step of removing the electrocatalyst from the solution comprises the steps of;

cooling the solution to room temperature;

centrifuging the solution to separate the electrocatalyst out of the solution;

washing and drying the electrocatalyst at a temperature of approximately 110°

C.; and

calcining the washed and dried electrocatalyst at a temperature of approximately 450°

C. for approximately four hours in an argon gas flow.

2. The method of making an electrocatalyst as recited in claim 1, further comprising the step of sonicating the suspension for approximately one hour.

3. The method of making an electrocatalyst as recited in claim 1, wherein the step of heating the suspension comprises heating the suspension to a temperature of approximately 90°

C. with stirring.

4. The method of making an electrocatalyst as recited in claim 1, further comprising the step of maintaining the urea solution and the suspension at a temperature of approximately 90°

C. for approximately eight hours.

5. The method of making an electrocatalyst as recited in claim 1, wherein the step of removing the electrocatalyst from the solution further comprises the step of reducing the calcined electrocatalyst at a rate of approximately 100 mL/min at a temperature of approximately 450°

C. for approximately four hours in a gas flow of approximately 10% hydrogen in argon.

6. The method of making an electrocatalyst for electrochemical conversion of carbon dioxide as recited in claim 1, further comprising the step of dissolving iron nitrate monohydrate in the deionized water to form the salt solution.

7. The method of making an electrocatalyst for electrochemical conversion of carbon dioxide as recited in claim 1, further comprising the step of dissolving ruthenium chloride in the deionized water to form the salt solution.