Nano-dispersed powders and methods for their manufacture

• US 6,652,967 B2
• Filed: 12/04/2001
• Issued: 11/25/2003
• Est. Priority Date: 08/08/2001
• Status: Expired due to Term

• Current Assignee: PPG Industries Ohio Incorporated (Nouryon BV)
• Original Assignee: NanoProducts Corporation (Nouryon BV)
• Inventors: Yadav, Tapesh, Pfaffenbach, Karl
• Primary Examiner(s): LE, HOA T
• Application Number:
  US10/004,387
• Publication Number:
  US 20030102099A1
• Time in Patent Office: 721 Days
• Field of Search: 428/403, 427/212, 427/398.1, 427/398.3, 427/201, 427/229
• US Class Current: 428/403
• CPC Class Codes: A61L 27/06 Titanium or titanium alloys
• CPC Class Codes: B01J 12/005 carried out at high temperatures, e.g. by pyrolysis
• CPC Class Codes: B01J 12/02 for obtaining at least one reaction product which, at normal temperature, is in the solid state
• CPC Class Codes: B01J 19/24 Stationary reactors without moving elements inside B01J19/08, B01J19/26 take precedence; with stationary particles B01J8/02
• CPC Class Codes: B01J 2219/00094 Jackets
• CPC Class Codes: B01J 2219/00135 Electric resistance heaters
• CPC Class Codes: B01J 2219/00177 controlling the pH
• CPC Class Codes: B01J 2219/0018 controlling the conductivity
• CPC Class Codes: B01J 2219/0894 Processes carried out in the presence of a plasma
• CPC Class Codes: B01J 23/002 Mixed oxides other than spinels, e.g. perovskite
• CPC Class Codes: B01J 23/08 of gallium, indium or thallium
• CPC Class Codes: B01J 23/14 of germanium, tin or lead
• CPC Class Codes: B01J 35/23 in a colloidal state
• CPC Class Codes: B01J 37/18 with gases containing free hydrogen
• CPC Class Codes: B22F 1/054 Nanosized particles
• CPC Class Codes: B22F 1/09 Mixtures of metallic powders
• CPC Class Codes: B22F 1/12 Metallic powder containing non-metallic particles containing lubricating or binding agents or organic material B22F1/10
• CPC Class Codes: B22F 2202/13 Use of plasma
• CPC Class Codes: B22F 2999/00 Aspects linked to processes or compositions used in powder metallurgy
• CPC Class Codes: B22F 9/12 starting from gaseous material
• CPC Class Codes: B29B 2009/125 : Micropellets, microgranules, microparticles
• CPC Class Codes: B29B 9/08 : by agglomerating smaller particles
• CPC Class Codes: B29B 9/12 : characterised by structure or composition
• CPC Class Codes: B29C 70/58 : comprising fillers only , e.g. particles, powder, beads, flakes, spheres B29C70/025 takes precedence, agglomerating hollow spheres to produce synthetic foam B29C70/66; compounding ingredients per se C08K
• CPC Class Codes: B82B 1/00 : Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
• CPC Class Codes: B82Y 25/00 : Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
• CPC Class Codes: B82Y 30/00 : Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: B82Y 5/00 : Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
• CPC Class Codes: C01B 13/145 : After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
• CPC Class Codes: C01B 19/007 : Tellurides or selenides of metals C01B19/002 takes precedence
• CPC Class Codes: C01B 21/062 : with chromium, molybdenum or tungsten
• CPC Class Codes: C01B 3/001 : characterised by the uptaking medium; Treatment thereof
• CPC Class Codes: C01B 32/956 : Silicon carbide
• CPC Class Codes: C01B 32/991 : Boron carbide
• CPC Class Codes: C01B 35/04 : Metal borides
• CPC Class Codes: C01F 11/06 : of carbonates
• CPC Class Codes: C01F 5/06 : by thermal decomposition of magnesium compounds calcining magnesite or dolomite C04B2/10
• CPC Class Codes: C01G 23/006 : Alkaline earth titanates
• CPC Class Codes: C01G 41/02 : Oxides; Hydroxides
• 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: C01P 2002/60 : Compounds characterised by their crystallite size
• CPC Class Codes: C01P 2002/72 : by d-values or two theta-values, e.g. as X-ray diagram
• CPC Class Codes: C01P 2004/51 : Particles with a specific particle size distribution
• CPC Class Codes: C01P 2004/64 : Nanometer sized, i.e. from 1-100 nanometer
• CPC Class Codes: C01P 2006/10 : Solid density
• CPC Class Codes: C01P 2006/12 : Surface area
• CPC Class Codes: C01P 2006/40 : Electric properties
• CPC Class Codes: C04B 2/10 : Preheating, burning calcining or cooling decarbonation during burning of cement raw materials C04B7/43; obtaining CaO or MgO otherwise than by thermal decomposition of the corresponding carbonates C01F11/02, C01F5/02
• CPC Class Codes: C04B 20/0004 : Microcomposites or nanocomposites, e.g. composite particles obtained by polymerising monomers onto inorganic materials
• CPC Class Codes: C04B 35/00 : Shaped ceramic products characterised by their composition porous ceramic products C04B38/00; ceramic articles characterised by particular shape, see the relevant classes, e.g. linings for casting ladles, tundishes, cups or the like B22D41/02; ceramic substrates for microelectronic semi-conductors H01L23/15; Ceramics compositions containing free metal bonded to carbides, diamond, oxides, borides, nitrides, silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides or sulfides other than as macroscopic reinforcing agents C22C; shaping of ceramics B28B; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products chemical preparation of powders of inorganic compounds C01; infiltration of sintered ceramic preforms with molten metal C04B41/51
• CPC Class Codes: C04B 35/62222 : obtaining ceramic coatings coating of mortars, concrete, artificial or natural stone or ceramics C04B41/45; laminated ceramic products B32B18/00; coating metallic materials C23; coating of glass C03C17/00, applying ceramic coatings on silicon for semi-conductor purposes H01L
• CPC Class Codes: C04B 41/52 : Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
• CPC Class Codes: C04B 41/89 : for obtaining at least two superposed coatings having different compositions
• CPC Class Codes: C08K 2201/011 : Nanostructured additives
• CPC Class Codes: C08K 2201/013 : Additives applied to the surface of polymers or polymer particles
• CPC Class Codes: H01C 7/112 : ZnO type
• CPC Class Codes: H01F 1/0045 : Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use preparation of fullerenes in general C01B32/15
• CPC Class Codes: H01G 4/12 : Ceramic dielectrics H01G4/085 takes precedence
• CPC Class Codes: H01G 4/33 : Thin- or thick-film capacitors thin- or thick-film circuits H01L27/00; capacitors without a potential-jump or surface barrier specially adapted for integrated circuits, details thereof, multistep manufacturing processes therefor H01L28/40
• CPC Class Codes: H01M 4/02 : Electrodes composed of, or comprising, active material
• CPC Class Codes: H01M 4/90 : Selection of catalytic material
• CPC Class Codes: H01M 4/9066 : of metal-ceramic composites or mixtures, e.g. cermets
• CPC Class Codes: H01M 8/1213 : characterised by the electrode/electrolyte combination or the supporting material
• CPC Class Codes: H01M 8/1246 : the electrolyte consisting of oxides
• CPC Class Codes: H01M 8/1253 : the electrolyte containing zirconium oxide
• CPC Class Codes: Y02E 60/32 : Hydrogen storage
• CPC Class Codes: Y02E 60/50 : Fuel cells
• CPC Class Codes: Y02P 70/50 : Manufacturing or production processes characterised by the final manufactured product
• CPC Class Codes: Y10T 428/25 : Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
• CPC Class Codes: Y10T 428/252 : Glass or ceramic [i.e., fired or glazed clay, cement, etc.] [porcelain, quartz, etc.]
• CPC Class Codes: Y10T 428/2991 : Coated

Abstract

Dispersed powders are disclosed that comprise fine nanoscale powders dispersed on coarser carrier powders. The composition of the dispersed fine powders may be oxides, carbides, nitrides, borides, chalcogenides, metals, and alloys. Fine powders discussed are of sizes less than 100 microns, preferably less than 10 micron, more preferably less than 1 micron, and most preferably less than 100 nanometers. Methods for producing such powders in high volume, low-cost, and reproducible quality are also outlined. Such powders are useful in various applications such as catalysts, sensor, electronic, electrical, photonic, thermal, biomedical, piezo, magnetic, catalytic and electrochemical products.

Claims

1. A method for producing a dispersed powder comprising nano-sized particles dispersed on and attached to the surface of carrier particles, the method comprising:

providing a slurry precursor comprising a mixture of a metal-containing precursor and carrier particles;

heating the slurry precursor to a temperature greater than 3000°

C., wherein the slurry precursor is converted to the vapor phase; and

cooling the vapor phase to produce the dispersed powder.

2. The method of claim 1, where the temperature is greater than 4000°

C.

3. The method of claim 1, wherein the carrier particle comprises a sub-micron powder.

4. The method of claim 1, wherein the carrier particle comprises a nanoscale powder.

5. The method of claim 1, wherein the metal-containing precursor is selected from the group consisting of oxides, carbides, nitrides, borides, metals, and alloys.

6. The method of claim 1, wherein the metal-containing precursor is of multi-metal composition.

7. The method of claim 1, wherein the metal-containing precursor comprises a non-stoichiometric ceramic composition.

8. The method of claim 1, wherein the metal-containing precursor comprises a mixture of at least two different metal-containing precursors.

9. The method of claim 1, further comprising quenching the dispersed powder.

10. The method of claim 1, further comprising adding a reactive fluid to said slurry precursor prior to completion of said heating step.

11. A method for producing a dispersed powder comprising nano-sized particles dispersed on and attached to the surface of carrier particles, the method comprising:

combining nano-scale powders and carrier particles to form a slurry precursor;

heating the slurry precursor to a temperature greater than 3000°

C., wherein the slurry precursor is converted to the vapor phase; and

cooling the vapor phase to produce the dispersed powder.

12. A method for producing a dispersed powder comprising nano-sized particles dispersed on and attached to the surface of carrier particles, the method comprising:

providing a slurry precursor comprising a mixture of a metal-containing precursor and carrier particles; and

mechanically milling said mixture to produce said dispersed powder.

13. A dispersed powder comprising:

a sub-micron carrier particle having a first composition; and

nano-scale particles of a second composition that are dispersed on and attached to the surface of the carrier particle in a mechanically stable state, wherein the attached particles are smaller than the carrier particle and wherein at least two neighboring attached particles on the surface of said carrier particle do not touch each other at 300 Kelvin.

14. The dispersed powder of claim 13, wherein the distance between the at least two neighboring attached particles on the surface of the carrier that do not touch each other is at least 2 Angstroms.

15. The dispersed powder of claim 14, wherein said distance is greater than 5 Angstroms.

16. The dispersed powder of claim 14, wherein said distance is greater than 10 Angstroms.

17. The dispersed powder of claim 14, wherein said distance is greater than 50 Angstroms.

18. The dispersed powder of claim 13, wherein the ratio of the average diameter of the carrier particles and the average diameter of the attached particles is greater than or equal to 2.

19. The dispersed powder of claim 18, wherein said ratio is greater than 10.

20. The dispersed powder of claim 18, wherein said ratio is greater than 25.

21. The dispersed powder of claim 18, wherein said ratio is greater than 100.

22. The dispersed powder of claim 13, wherein the surfaces of the attached particle and carrier particle interact physically, chemically, electrochemically.

23. The dispersed powder of claim 13, wherein the carrier particle is nanoscale particle.

24. The dispersed powder of claim 13, wherein the composition of the attached particle is selected from the group consisting of oxides, carbides, nitrides, borides, metals, and alloys.

25. The dispersed powder of claim 13, wherein the attached particle is a multi-metal composition.

26. The dispersed powder of claim 13, wherein the attached particle is a non-stoichiometric ceramic composition.

27. The dispersed powder of claim 13, wherein the composition of said nano-sized particles is the same as the composition of said carrier particles.

28. The dispersed powder of claim 13, wherein the composition of said nano-sized particles is different than the composition of said carrier particles.

29. A product containing a dispersed powder of claim 13.

30. The dispersed powder of claim 13, wherein the dispersed powder has been post-processed.