IP Library Granted Patent US 11,628,427
Granted Patent B2
US 11,628,427 · App. 17/161,114 · Granted Apr 18, 2023

Segregation induced core-shell structure

Inventors: Rongyue Wang (Naperville, IL); Vojislav Stamenkovic (Naperville, IL); Gregory K. Krumdick (Homer Glen, IL); Krzysztof Pupek (Plainfield, IL)
Assignee: UChicago Argonne, LLC
B01J23/892B01J23/42B01J35/0013B01J37/009B01J37/0072B01J37/031B01J37/04B01J37/06B01J37/14B01J37/343
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Quick Facts
Patent No.
US 11,628,427
App. No.
17/161,114
Granted
Apr 18, 2023
Kind
B2
Abstract

A process for synthesis of PtNi high surface area core/shell particles. The processing including formation of PtNi nanoparticles, exposure of the PtNi nanoparticles to oxygen to form a nickel oxide coating on the nanoparticles at the same time the segregation of Ni to surface induces a Pt-skin with PtNi core structure, removal of the nickel oxide coating to form PtNi core/Pt shell (or Pt-skin) structure.

Claims (34)

1. A method of synthesizing Pt shell PtNi core nanoparticle comprising the steps of:

forming a reaction mixture comprising a nickel precursor, a reducing agent, and a surfactant comprising one part oleic acid to two parts oleylamine, a platinum precursor, and a polar solvent;

reacting the reaction mixture at between 195° C. and 205° C. for at least 10 minutes forming a PtNi nanoparticle solution;

isolating PtNi nanoparticles from the PtNI nanoparticle solution;

exposing the PtNi nanoparticles to oxygen;

forming nickel oxide by reaction of nickel of the PtNi nanoparticles with the oxygen; and

removing the nickel oxide from at a portion of the PtNi nanoparticles.

2. The method of claim 1 , wherein isolation of the PtNi nanoparticles comprises:

sonicating the PtNi nanoparticle solution with substrate in chloroform solution;

adding hexane to the sonicated chloroform solution;

precipitating PtNi nanoparticles; and

collecting the PtNi nanoparticles by filtration.

3. The method of claim 1 , wherein exposing the PtNi nanoparticles comprises exposure at a temperature of 150° C. to 400° C.

4. The method of claim 3 , wherein exposing the PtNi nanoparticles comprises exposure at a temperature of 150° C. to 300° C.

5. The method of claim 3 , wherein the exposing the PtNi nanoparticles is for 1 to 20 hours.

6. The method of claim 1 , wherein removing the nickel oxide is by acid leaching.

7. The method of claim 6 , wherein the acid leaching is by exposure of an equal volume of acid to nanoparticle.

8. The method of claim 6 , wherein the acid leaching is by exposure to HClO 4 .

9. A method of synthesizing Pt shell PtNi core nanoparticle comprising the steps of:

forming a reaction mixture comprising a nickel precursor, a reducing agent, and a surfactant comprising one part oleic acid to two parts oleylamine, a platinum precursor, and a polar solvent;

reacting the reaction mixture at between 195° C. and 205° C. for at least 10 minutes forming a PtNi nanoparticle solution;

isolating PtNi nanoparticles from the PtNI nanoparticle solution;

exposing the PtNi nanoparticles to oxygen at a temperature of 150° C. to 400° C. for 1 to 20 hours;

forming nickel oxide on a surface of the PtNi nanoparticles by reaction of nickel of the PtNi nanoparticles with the oxygen; and

removing the nickel oxide from at a portion of the PtNi nanoparticles.

10. The method of claim 9 , wherein isolation of the PtNi nanoparticles comprises:

sonicating the PtNi nanoparticle solution with substrate in chloroform solution;

adding hexane to the sonicated chloroform solution;

precipitating PtNi nanoparticles; and

collecting the PtNi nanoparticles by filtration.

11. The method of claim 9 , wherein exposing the PtNi nanoparticles comprises exposure at a temperature of 150° C. to 300° C.

12. The method of claim 9 , wherein removing the nickel oxide is by acid leaching.

13. The method of claim 12 , wherein the acid leaching is by exposure of an equal volume of acid to nanoparticle.

14. The method of claim 12 , wherein the acid leaching is by exposure to HClO 4 .

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 16, 2021
From: PUPEK, KRZYSZTOF; KRUMDICK, GREGORY K.; WANG, RONGYUE; STAMENKOVIC, VOJISLAV
To: UCHICAGO ARGONNE, LLC
Reel/Frame 056877/0430 →
CONFIRMATORY LICENSE Recorded Mar 10, 2021
From: UCHICAGO ARGONNE LLC
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 055547/0036 →
Continuity (2)
Provisional Application 62966929 · Jan 28, 2020
Related Publication 20210252487A1 · Aug 19, 2021