# US 12,002,967 B1 · Cobalt and copper-doped nickel ferrite nanoparticles as catalyst for direct methanol fuel cells

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- Number: US 12,002,967 B1
- Document ID: US12002967B1
- Status: Granted
- Kind: B1
- Application number: 18/391,192
- Filed: 2023-12-20
- Granted: 2024-06-04
- Earliest claimed: 2023-03-22
- Assignees: King Faisal University
- Applicants: King Faisal University
- Inventors: Hany Mohamed Abd El-Lateef Ahmed; Mai Mustafa Khalaf Ali; Ibrahim Abdelhamid Mohamed Elsayed Elshaer; Hadyl Hany Mohamed Abd El-Lateef
- Web page: https://patentgrep.com/patent/US12002967B1

## CPC

- H01M 4/9016: {Oxides, hydroxides or oxygenated metallic salts}
- H01M 8/1011: Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
- H01M 2008/1095: {Fuel cells with polymeric electrolytes}
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY

## Abstract

Cobalt and copper-doped nickel Cu/Co—Ni-ferrite nanoparticles having a general formula CuxCoxNi(1-x)Fe2O4 can be a catalyst for electrooxidation of methanol in direct methanol fuel cells (DMFC). The catalyst can be an efficient anode for DMFC in alkaline electrolytes. The Cu/Co—Ni-ferrite nanoparticles can have a sponge-like structure with irregular pores. A diameter of the Cu/Co—Ni-ferrite nanoparticles can range from about 8 nm to about 30 nm.

## Claims

### Claim 1

Cobalt and copper-doped nickel ferrite nanoparticles prepared according to a method comprising:
preparing a gel including iron nitrate, cobalt nitrate, nickel nitrate, copper nitrate, and a capping agent;
drying the gel to provide a dried gel;
burning the dried gel to provide a brittle mass;
reducing the brittle mass to a powder; and
calcining the powder to provide cobalt and copper-doped nickel ferrite nanoparticles;
wherein the cobalt and copper-doped nickel ferrite nanoparticles have the general formula CuxCoxNi(1-x)Fe2O4;
wherein x equals about 0.03 to about 0.05; and
wherein the cobalt and copper-doped nickel ferrite nanoparticles are sponge-like with irregularly shaped pores.

### Claim 2 (depends on 1)

The cobalt and copper-doped nickel ferrite nanoparticles of claim 1, wherein x equals 0.05.

### Claim 3 (depends on 1)

The cobalt and copper-doped nickel ferrite nanoparticles of claim 1, wherein the capping agent is citric acid.

### Claim 4 (depends on 1)

The cobalt and copper-doped nickel ferrite nanoparticles of claim 1, wherein drying the gel comprises heating the gel to a temperature ranging from about 90° C. to about 110° C. for a period of time ranging from about 8 hours to about 12 hours.

### Claim 5 (depends on 1)

The cobalt and copper-doped nickel ferrite nanoparticles of claim 1, wherein burning the dried gel can include heating the dried gel at a temperature ranging from about 165° C. to about 175° C. for a period of time ranging from about 30 minutes to about 2 hours.

### Claim 6 (depends on 1)

The cobalt and copper-doped nickel ferrite nanoparticles of claim 1, wherein the brittle mass is reduced to a powder by grinding.

### Claim 7 (depends on 1)

The cobalt and copper-doped nickel ferrite nanoparticles of claim 1, wherein the powder is calcined for about two hours to about five hours at a temperature ranging from about 400° C. to about 500° C.

### Claim 8 (depends on 1)

The cobalt and copper-doped nickel ferrite nanoparticles of claim 1, wherein the powder is calcined for about three hours at about 420° C.

### Claim 9

Cobalt and copper-doped nickel ferrite nanoparticles prepared according to a method comprising:
preparing a gel including iron nitrate, cobalt nitrate, nickel nitrate, copper nitrate, and citric acid;
drying the gel to provide a dried gel;
burning the dried gel to provide a brittle mass;
reducing the brittle mass to a powder; and
calcining the powder to provide cobalt and copper-doped nickel ferrite nanoparticles; and
wherein the gel is prepared by:
dissolving iron nitrate in water to provide an iron nitrate solution;
dissolving cobalt nitrate in water to provide a cobalt nitrate solution;
dissolving nickel nitrate in water to provide a nickel nitrate solution;
combining the iron nitrate solution, the cobalt nitrate solution, and the nickel nitrate solution to provide a first mixture;
adding copper nitrate to the first mixture to provide a second mixture;
adding a capping agent to the second mixture to provide a third mixture;
adjusting a pH of the third mixture to provide an alkaline solution;
heating the alkaline solution to provide a heated solution; and
sealing the heated solution to provide a gel;
wherein the cobalt and copper-doped nickel ferrite nanoparticles have the general formula CuxCoxNi(1-x)Fe2O4;
wherein x equals about 0.03 to about 0.05; and
wherein the cobalt and copper-doped nickel ferrite nanoparticles are sponge-like with irregularly shaped pores.

### Claim 10 (depends on 9)

The cobalt and copper-doped nickel ferrite nanoparticles of claim 9, wherein x equals 0.05.

### Claim 11 (depends on 9)

The cobalt and copper-doped nickel ferrite nanoparticles of claim 9, wherein the capping agent is citric acid.

### Claim 12 (depends on 9)

The cobalt and copper-doped nickel ferrite nanoparticles of claim 9, wherein drying the gel comprises heating the gel to a temperature ranging from about 90° C. to about 110° C. for a period of time ranging from about 8 hours to about 12 hours.

### Claim 13 (depends on 9)

The cobalt and copper-doped nickel ferrite nanoparticles of claim 9, wherein burning the dried gel can include heating the dried gel at a temperature ranging from about 165° C. to about 175° C. for a period of time ranging from about 30 minutes to about 2 hours.

### Claim 14 (depends on 9)

The cobalt and copper-doped nickel ferrite nanoparticles of claim 9, wherein the brittle mass is reduced to a powder by grinding.

### Claim 15 (depends on 9)

The cobalt and copper-doped nickel ferrite nanoparticles of claim 9, wherein the powder is calcined for about two hours to about five hours at a temperature ranging from about 400° C. to about 500° C.

### Claim 16 (depends on 9)

The cobalt and copper-doped nickel ferrite nanoparticles of claim 9, wherein the powder is calcined for about three hours at about 420° C.
