IP Library Granted Patent US 8,709,126
Granted Patent B1
US 8,709,126 · App. 13/020,791 · Granted Apr 29, 2014

Generation of metal and alloy micron, submicron, or nano particles in simple, rapid process

Inventors: Claudia Catalina Luhrs (Rio Rancho, NM); Zayd Leseman (Albuquerque, NM); Jonathan Phillips (Rio Rancho, NM); Hugo Ricardo Zea-Ramirez (Bogota, CO)
Assignee: STC.UNM
B22F9/26B82Y40/00
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Quick Facts
Patent No.
US 8,709,126
App. No.
13/020,791
Granted
Apr 29, 2014
Kind
B1
Abstract

Various embodiments provide methods of forming metallic particles or carbon/graphite coated metallic particles with zero-valence from metal precursor compounds by a reductive/expansion synthesis method using nitrogen-hydrogen containing molecules.

Claims (31)

1. A method of forming a metallic particle comprising:

mixing one or more metal precursor compounds and a chemical agent that produces reducing gases upon thermal decomposition to form a physical mixture, wherein the one or more metal precursor compounds comprise one or more metals having a positive valence; and

heating the physical mixture in an inert atmosphere to a temperature ranging from 300° C. to 900° C., to form a plurality of metallic particles each comprising one or more metals corresponding to the one or more metal precursor compounds,

wherein the chemical reducing agent is urea and the one or more metal precursor compounds comprise nitrates or hydrated nitrates of a metal selected from Fe, Ni and a combination thereof.

2. The method of claim 1 , further comprising determining a heating temperature for heating the physical mixture, wherein the heating temperature ranges between a decomposition temperature of the chemical agent and 900° C.

3. The method of claim 1 , wherein the step of heating the physical mixture comprises placing the physical mixture in an oven pre-heated at a heating temperature for about 5 minutes or less.

4. The method of claim 1 , further comprising heating the physical mixture at a heating rate ranging from about 1° C./min to about 500° C./min.

5. The method of claim 1 , wherein the physical mixture comprises a ratio such that there are one or more nitrogen groups from the chemical agent for each metal atom from the one or more metal precursor compounds.

6. The method of claim 1 , wherein the heating of the physical mixture occurs for a length of time of 5 minutes or less.

7. The method of claim 1 , further comprising:

placing the physical mixture under the inert atmosphere, prior to the step of heating the physical mixture, and

cooling the plurality of metallic particles to the ambient temperature under the inert atmosphere, following the step of heating the physical mixture.

8. The method of claim 1 , wherein each of the plurality of metallic particles is zero valent and has a particle size of about 250 nm or less.

9. The method of claim 1 , wherein a portion of the plurality of metallic particles forms an agglomerated particle in the step of heating the physical mixture, wherein the agglomerated particle has an average particle size of about 2 μm or less, or an aspect ratio ranging from about 10 to about 1.

10. The method of claim 1 , further comprising controlling an average size of the plurality of metallic particles in a range between about 1 nm to about 1000 μm by controlling one or more parameters selected from a metal precursor identity, a ratio of metal atoms in the one or more metal precursor compounds to the chemical agent, a flow rate of an inert gas, an identity of the inert gas, a heating rate, and a maximum heating temperature.

11. A method of forming a metallic particle comprising:

mixing one or more metal precursor compounds and a chemical agent that produces reducing gases upon thermal decomposition to form a physical mixture, wherein the one or more metal precursor compounds comprise one or more metals having a positive valence; and

heating the physical mixture in an inert atmosphere to form a plurality of metallic particles each comprising one or more metals corresponding to the one or more metal precursor compounds, wherein each metallic particle of the plurality of metallic particles comprises a carbonaceous shell comprising carbon or graphite surrounding the metallic particle,

wherein the chemical agent that produces reducing gases upon thermal decomposition comprises one or more nitrogen-hydrogen-containing molecules.

12. The method of claim 11 , wherein the carbonaceous shell is formed by controlling at least one of an identity of the one or more metal precursor compounds, an identity of the chemical agent, a ratio of the chemical agent to the one or more metal precursor compounds, a heating rate, a maximum heating temperature, or an inert gas flow rate.

13. The method of claim 11 , wherein the carbonaceous shell is a non-conformal coating and surrounds both the metallic particle and a plurality of void spaces.

14. The method of claim 11 , wherein the chemical agent comprises one or more carbon-containing molecules.

15. The method of claim 11 , wherein the one or more nitrogen-hydrogen-containing molecules are selected from the group consisting of urea [(NH 2 ) 2 CO] and a compound containing —NH or —NH 2 .

16. The method of claim 15 , wherein the one or more metal precursor compounds comprise nitrates, hydrated nitrates, nitrides, oxides, oxide-nitrides, halogens, or hydroxides of one or more metals, and wherein each of the one or more metals are chosen from a metal in one or more of columns IB, IIB, VB, VIIB, VIIB, VIIB, IA, IIA, IIIA, or IVA of the periodic table.

17. The method of claim 16 , wherein the chemical reducing agent is urea.

18. The method of claim 17 , wherein and the one or more metal precursor compounds comprise nitrates or hydrated nitrates of a metal selected from Fe, Ni and a combination thereof.

19. The method of claim 17 , wherein the metallic particle comprises one or more metals selected from the group consisting of Fe, Ni, Sb, Co, Mg, Mn, Cr, Zn, Cu and W.

20. A method of forming a metallic particle comprising:

mixing one or more metal precursor compounds and a chemical agent that produces reducing gases upon thermal decomposition to form a physical mixture, wherein the one or more metal precursor compounds comprise one or more metals having a positive valence; and

heating the physical mixture in an inert atmosphere to a temperature ranging from about 400° C. to about 1000° C., to form a plurality of metallic particles each comprising one or more metals corresponding to the one or more metal precursor compounds,

wherein the chemical reducing agent is urea and the one or more metal precursor compounds comprise nitrates or hydrated nitrates of a metal selected from Fe, Ni and a combination thereof.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 8, 2018
From: LOS ALAMOS NATIONAL SECURITY, LLC
To: TRIAD NATIONAL SECURITY, LLC
Reel/Frame 047485/0471 →
CONFIRMATORY LICENSE Recorded Mar 26, 2015
From: LOS ALAMOS NATIONAL SECURITY
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 035258/0680 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 23, 2012
From: LESEMAN, ZAYD; LUHRS, CLAUDIA C.
To: THE REGENTS OF THE UNIVERSITY OF NEW MEXICO C/O RESEARCH & TECHNOLOGY LAW
Reel/Frame 027754/0490 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 23, 2012
From: THE REGENTS OF THE UNIVERSITY OF NEW MEXICO C/O RESEARCH & TECHNOLOGY LAW
To: STC.UNM
Reel/Frame 027754/0518 →
Continuity (1)
Provisional Application 61337495 · Feb 3, 2010