Preparation of uniform nanoparticles of ultra-high purity metal oxides, mixed metal oxides, metals, and metal alloys

• US 20080032132A1
• Filed: 02/16/2007
• Published: 02/07/2008
• Est. Priority Date: 02/16/2006
• Status: Active Grant

• Current Assignee: Brigham Young University (The Church of Jesus Christ of Latter-Day Saints)
• Original Assignee: Brigham Young University (The Church of Jesus Christ of Latter-Day Saints)
• Inventors: Lui, Shengfeng, Woodfield, Brian, Boerio-Goates, Juliana, Liu, Qingyuan
• Granted Patent: US 8,211,388 B2
• Time in Patent Office: Days
• US Class Current: 428/402
• CPC Class Codes: B22F 1/054 Nanosized particles
• CPC Class Codes: B22F 2009/043 by ball milling
• CPC Class Codes: B22F 2009/045 by other means than ball or jet milling
• CPC Class Codes: B22F 2009/049 by pulverising at particular temperature
• CPC Class Codes: B22F 2999/00 Aspects linked to processes or compositions used in powder metallurgy
• CPC Class Codes: B22F 9/04 starting from solid material, e.g. by crushing, grinding or milling C22C1/1084 takes precedence; crushing, grinding or milling, in general, see the relevant subclasses, e.g. B02C
• CPC Class Codes: B22F 9/20 starting from solid metal compounds
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01B 13/322 of elements or compounds in the solid state
• CPC Class Codes: C01F 17/218 Yttrium oxides or hydroxides
• CPC Class Codes: C01F 17/224 Oxides or hydroxides of lanthanides
• CPC Class Codes: C01F 7/308 Thermal decomposition of nitrates
• CPC Class Codes: C01G 1/02 Oxides
• CPC Class Codes: C01G 19/02 Oxides
• CPC Class Codes: C01G 23/0536 by hydrolysing chloride-containing salts
• CPC Class Codes: C01G 25/00 Compounds of zirconium
• CPC Class Codes: C01G 25/02 Oxides
• CPC Class Codes: C01G 29/00 Compounds of bismuth
• CPC Class Codes: C01G 3/02 Oxides; Hydroxides
• CPC Class Codes: C01G 49/06 Ferric oxide [Fe2O3]
• CPC Class Codes: C01G 49/08 : Ferroso-ferric oxide [Fe3O4]
• CPC Class Codes: C01G 5/02 : Halides
• CPC Class Codes: C01G 51/00 : Compounds of cobalt
• CPC Class Codes: C01G 51/04 : Oxides; Hydroxides
• CPC Class Codes: C01G 53/00 : Compounds of nickel
• CPC Class Codes: C01G 53/006 : Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen nickelates C01G53/40
• CPC Class Codes: C01G 53/04 : Oxides; Hydroxides
• CPC Class Codes: C01G 55/002 : Compounds containing, besides ruthenium, rhodium, palladium, osmium, iridium, or platinum, two or more other elements, with the exception of oxygen or hydrogen C01G55/007 takes precedence
• CPC Class Codes: C01G 9/02 : Oxides; Hydroxides
• CPC Class Codes: C01P 2002/72 : by d-values or two theta-values, e.g. as X-ray diagram
• CPC Class Codes: C01P 2002/88 : by thermal analysis data, e.g. TGA, DTA, DSC
• CPC Class Codes: C01P 2004/04 : obtained by TEM, STEM, STM or AFM
• CPC Class Codes: C01P 2004/51 : Particles with a specific particle size distribution
• CPC Class Codes: C01P 2004/52 : highly monodisperse size distribution
• CPC Class Codes: C01P 2004/64 : Nanometer sized, i.e. from 1-100 nanometer
• CPC Class Codes: Y10S 977/84 : Manufacture, treatment, or detection of nanostructure
• CPC Class Codes: Y10S 977/896 : Chemical synthesis, e.g. chemical bonding or breaking
• CPC Class Codes: Y10T 428/2982 : Particulate matter [e.g., sphere, flake, etc.]

Abstract

In preferred embodiments, metal nanoparticles, mixed-metal (alloy) nanoparticles, metal oxide nanoparticles and mixed-metal oxide nanoparticles are provided. According to embodiments, the nanoparticles may possess narrow size distributions and high purities. In certain preferred embodiments, methods of preparing metal nanoparticles, mixed-metal nanoparticles, metal oxide nanoparticles and mixed-metal nanoparticles are provided. These methods may provide tight control of particle size, size distribution, and oxidation state. Other preferred embodiments relate to a precursor material that may be used to form nanoparticles. In addition, products prepared from such nanoparticles are disclosed.

Claims

1. A composition comprising nanoparticles having an average particle size, wherein the average particle size is between about 1 nm and about 100 nm, a size distribution, wherein the size distribution is within about 1% to about 15% of the average particle size, and a substantially pre-determined stoichiometry.

2. The composition according to claim 1, wherein the nanoparticles comprise at least one compound selected from the group consisting of a metal, a metal oxide, a mixed-metal, and a mixed-metal oxide.

3. The composition according to claim 2, wherein the metal is selected from the group consisting of alkali metals, alkali earth metals, transition metals, lanthanide series metals, actinide series metals, aluminum, gallium, indium, thallium, germanium, tin, lead, antimony, bismuth, and polonium.

4. The composition according to claim 2, wherein the mixed-metal or mixed-metal oxide comprises two or more metals selected from the group consisting of alkali metals, alkali earth metals, transition metals, lanthanide series metals, actinide series metals, aluminum, gallium, indium, thallium, germanium, tin, lead, antimony, bismuth, and polonium.

5. The composition according to claim 1, wherein the oxidation state of the nanoparticles is substantially uniform among the nanoparticles.

6. The composition according to claim 1, wherein the nanoparticles have a pre-determined oxidation state.

7. The composition according to claim 1, wherein the nanoparticles comprise metal nanoparticles in a zero oxidation state.

8. A method of forming nanoparticles comprising:

providing a metal salt;

providing a base;

mixing the metal salt and the base to form a precursor material; and

heating the precursor material to a pre-determined temperature, at a pre-determined rate, in a pre-determined atmosphere, and for a pre-determined length of time, wherein the nanoparticles have an average particle size, wherein the average particle size is between about 1 nm and about 100 nm, a size distribution, wherein the size distribution is within about 1% to about 15% of the average particle size, and a substantially pre-determined stoichiometry.

9. The method according to claim 8, wherein the nanoparticles comprise at least one compound selected from the group consisting of a metal, a metal oxide, a mixed-metal, and a mixed-metal oxide.

10. The method according to claim 9, wherein the metal is selected from the group consisting of alkali metals, alkali earth metals, transition metals, lanthanide series metals, actinide series metals, aluminum, gallium, indium, thallium, germanium, tin, lead, antimony, bismuth, and polonium.

11. The method according to claim 8, wherein the mixing is performed, at least in part, by an apparatus selected from the group consisting of a mortar and pestle, a ball mill, a roller mill, and a counter rotator.

12. The method according to claim 8, wherein the mixing comprises adding a pre-determined amount of energy to the metal salt and the base to form the precursor material.

13. The method according to claim 8, wherein the atmosphere is an inert atmosphere.

14. The method according to claim 8, wherein the atmosphere is a reductive atmosphere.

15. The method according to claim 8, further comprising the step of drying the precursor material at a pre-determined temperature and for a pre-determined length of time.

17. The precursor material according to claim 15, wherein the metal comprises a metal selected from the group consisting of alkali metals, alkali earth metals, transition metals, lanthanide series metals, actinide series metals, aluminum, gallium, indium, thallium, germanium, tin, lead, antimony, bismuth, and polonium.

18. The precursor material according to claim 15, wherein the base comprises a compound selected from the group consisting of ammonium bicarbonate, ammonium sesquicarbonate, ammonium hydroxide, lithium hydroxide, sodium hydroxide, potassium hydroxide, magnesium hydroxide, calcium hydroxide, and mixtures thereof.

19. The precursor material according to claim 15, wherein the mixing is performed, at least in part, by an apparatus selected from the group consisting of a mortar and pestle, a ball mill, a roller mill, and a counter rotator.

16. A precursor material comprising:

a metal hydroxide; and

a salt compound, wherein the metal hydroxide and the salt compound are formed, at least in part, from mixing a metal salt and a base, and wherein the precursor material can be heated to a pre-determined temperature, at a pre-determined rate, in a pre-determined atmosphere, and for a pre-determined length of time to form nanoparticles having an average particle size, wherein the average particle size is between about 1 nm and about 100 nm, a size distribution, wherein the size distribution is within about 1% and about 15% of the average particle size, and a substantially pre-determined stoichiometry.

20. A precursor material comprising a complex mixture comprising a metal hydroxide and a salt compound, wherein the precursor material can be heated to a pre-determined temperature, in a pre-determined atmosphere, and for a pre-determined length of time to form nanoparticles having an average particle size, wherein the average particle size is between about 1 nm and about 100 nm, a size distribution, wherein the size distribution is within about 1% and about 15% of the average particle size, and a substantially pre-determined stoichiometry.