# US 10,501,321 B2 · Nitride stabilized core/shell nanoparticles

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- Number: US 10,501,321 B2
- Document ID: US10501321B2
- Status: Granted
- Kind: B2
- Application number: 15/850,402
- Filed: 2017-12-21
- Published: 2018-05-17
- Granted: 2019-12-10
- Earliest claimed: 2013-11-27
- Assignees: Brookhaven Science Associates, LLC
- Applicants: Brookhaven Science Associates, LLC
- Inventors: Kurian Abraham Kuttiyiel; Kotaro Sasaki; Radoslav R. Adzic
- Web page: https://patentgrep.com/patent/US10501321B2

## CPC

- C01B 21/0622: {with iron, cobalt or nickel}
- B01D 9/0018: {Evaporation of components of the mixture to be separated}
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- H01M 4/925: {supported on carriers, e.g. powder carriers}
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2004/03: obtained by SEM
- C01P 2004/34: hollow
- Y02E 60/50: Fuel cells
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

Nitride stabilized metal nanoparticles and methods for their manufacture are disclosed. In one embodiment the metal nanoparticles have a continuous and nonporous noble metal shell with a nitride-stabilized non-noble metal core. The nitride-stabilized core provides a stabilizing effect under high oxidizing conditions suppressing the noble metal dissolution during potential cycling.

## Claims

### Claim 1

A method of forming nitride stabilized nanoparticles comprising,
a non-noble metal solid solution core with a size of less than 100 nm along at least one of three orthogonal axes, and
a continuous and nonporous noble metal shell surrounding the non-noble metal solid solution core;
wherein the non-noble metal solid solution core comprises a nitride of a non-noble metal selected from the group consisting of nickel (Ni) nitride, cobalt (Co) nitride, iron (Fe) nitride, copper (Cu) nitride and mixtures thereof;
formed by:
preparing a mixture comprising an organic solvent, a salt of a first metal, and a salt of a second metal;
evaporating the organic solvent from the mixture to leave a dry powder; and
annealing the dry powder under a nitrogen source to produce a nitride of the first metal.

### Claim 2 (depends on 1)

The method of claim 1 wherein the nitrogen source comprises a nitrogen gas (N2), an ammonium gas (NH3) or a combination thereof.

### Claim 3 (depends on 1)

The method of claim 1, wherein the annealing comprises exposing the dry powder to a temperature from between about 400 and about 700° C. under NH3 for 1 to 10 hours.

### Claim 4 (depends on 1)

The method of claim 1, wherein the mixture further comprises a carbon powder.

### Claim 5 (depends on 1)

The method of claim 1, further comprising sonicating the mixture before evaporating the organic solvent from the mixture.

### Claim 6 (depends on 1)

The method of claim 1, wherein first metal comprises at least one non-noble transition metal.

### Claim 7 (depends on 6)

The method of claim 6, wherein at least one non-noble transition metal comprises at least one of nickel (Ni), cobalt (Co), iron (Fe), copper (Cu), tungsten (W) or a combination thereof.

### Claim 8 (depends on 1)

The method of claim 1, wherein the second metal comprises at least one noble metal.

### Claim 9 (depends on 8)

The method of claim 8, wherein the at least one noble metal comprises at least one of palladium (Pd), iridium (Ir), rhenium (Re), ruthenium (Ru), rhodium (Rh), osmium (Os), gold (Au), and platinum (Pt), or a combination thereof.

### Claim 10 (depends on 1)

The method of claim 1, wherein the first metal is nickel (Ni), and the second metal is platinum (Pt).

### Claim 11 (depends on 1)

The method of claim 1, wherein the first metal is nickel (Ni), and the second metal is palladium (Pd).

### Claim 12 (depends on 1)

The method of claim 1, wherein the first metal is nickel (Ni), and the second metal is palladium (Ir).

### Claim 13 (depends on 1)

The method of claim 1, wherein the salt of the first metal is Ni(acac)2, and the salt of the second metal is Pt(acac)2.

### Claim 14 (depends on 1)

The method of claim 1, wherein the salt of the first metal is Ni(acac)2, and the salt of the second metal is Pd(acac)2.

### Claim 15 (depends on 1)

The method of claim 1, wherein the salt of the first metal is Ni(acac)2, and the salt of the second metal is Ir(acac)3.

### Claim 16 (depends on 1)

The method of claim 1, wherein the mixture further comprises a salt of a third metal.

### Claim 17 (depends on 16)

The method of claim 16, wherein the third metal is different from the first metal and the second metal, and comprises at least one of nickel (Ni), cobalt (Co), iron (Fe), copper (Cu), tungsten (W) palladium (Pd), iridium (Ir), rhenium (Re), ruthenium (Ru), rhodium (Rh), osmium (Os), gold (Au), or platinum (Pt).

### Claim 18 (depends on 16)

The method of claim 16, wherein the first metal is nickel (Ni), the second metal is palladium (Pd), and the third metal is gold (Au).

### Claim 19 (depends on 16)

The method of claim 16, wherein the salt of the first metal is Ni(acac)2, the salt of the second metal is Pd(acac)2, and the salt of the third metal is Au(CH3)2(acac).

### Claim 20 (depends on 1)

The method of claim 1, wherein the organic solvent is at least one of acetone, chloroform, benzene, cyclohexane, dichloromethane, ethanol, diethyl ether, ethyl acetate, hexane, methanol, toluene, xylene, mixtures of two or more thereof, or derivatives of one or more thereof.