METHOD OF FORMING NON-STOICHIOMETRIC NANOSCALE POWDER COMPRISING TEMPERATURE-PROCESSING OF A STOICHIOMETRIC METAL COMPOUND.

• US 20090184281A1
• Filed: 10/31/2003
• Published: 07/23/2009
• Est. Priority Date: 09/03/1996
• Status: Active Grant

• Current Assignee: PPG Industries Ohio Incorporated (Nouryon BV)
• Original Assignee: PPG Industries Ohio Incorporated (Nouryon BV)
• Inventors: Yadav, Tapesh, Alexander, John
• Granted Patent: US 7,559,494 B1
• Time in Patent Office: Days
• US Class Current: 252/62.550
• CPC Class Codes: A61L 27/06 Titanium or titanium alloys
• CPC Class Codes: A62C 31/03 adjustable, e.g. from spray to jet or vice versa
• 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 2219/00155 using insulating materials or refractories
• 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 2523/00 Constitutive chemical elements of heterogeneous catalysts
• CPC Class Codes: B01J 2523/31 Aluminium
• CPC Class Codes: B01J 2523/54 Bismuth
• CPC Class Codes: B01J 2523/67 Chromium
• CPC Class Codes: B01J 2523/72 Manganese
• CPC Class Codes: B01J 2523/845 Cobalt
• CPC Class Codes: B01J 2523/847 : Nickel
• CPC Class Codes: B01J 35/23 : in a colloidal state
• CPC Class Codes: B01J 37/18 : with gases containing free hydrogen
• CPC Class Codes: B05B 1/12 : capable of producing different kinds of discharge, e.g. either jet or spray having selectively-effective outlets B05B1/16
• CPC Class Codes: B22F 1/00 : Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
• CPC Class Codes: B22F 1/054 : Nanosized particles
• 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: 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: 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 35/04 : Metal borides
• CPC Class Codes: C01F 11/06 : of carbonates
• CPC Class Codes: C01F 17/235 : Cerium oxides or hydroxides
• 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 2002/01 : depicted by a TEM-image
• CPC Class Codes: C01P 2002/02 : Amorphous compounds
• CPC Class Codes: C01P 2002/34 : perovskite-type (ABO3)
• CPC Class Codes: C01P 2002/52 : containing elements as dopants
• CPC Class Codes: C01P 2002/54 : one element only
• 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 2004/03 : obtained by SEM
• CPC Class Codes: C01P 2004/04 : obtained by TEM, STEM, STM or AFM
• CPC Class Codes: C01P 2004/38 : cube-like
• CPC Class Codes: C01P 2004/51 : Particles with a specific particle size distribution
• CPC Class Codes: C01P 2004/54 : Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
• CPC Class Codes: C01P 2004/61 : Micrometer sized, i.e. from 1-100 micrometer
• CPC Class Codes: C01P 2004/62 : Submicrometer sized, i.e. from 0.1-1 micrometer
• 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: C01P 2006/60 : Optical properties, e.g. expressed in CIELAB-values
• 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 3/01 : characterized by their specific function
• CPC Class Codes: C08K 3/08 : Metals
• CPC Class Codes: G01N 27/127 : comprising nanoparticles
• CPC Class Codes: H01C 7/112 : ZnO type
• CPC Class Codes: H01F 1/0063 : in a non-magnetic matrix, e.g. granular solids granular films H01F10/007
• CPC Class Codes: H01F 1/401 : diluted
• 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 40/40 : Production or processing of lime, e.g. limestone regeneration of lime in pulp and sugar mills
• CPC Class Codes: Y02P 70/50 : Manufacturing or production processes characterised by the final manufactured product
• CPC Class Codes: Y10S 977/90 : having step or means utilizing mechanical or thermal property, e.g. pressure, heat

Abstract

Nanotechnology methods for creating stoichiometric and non-stoichiometric substances with unusual combination of properties by lattice level composition engineering are described. The modified properties described include electrical conductivity, dielectric constant, dielectric strength, dielectric loss, polarization, permittivity, critical current, superconductivity, piezoelectricity, mean free path, curie temperature, critical magnetic field, permeability, coercive force, magnetostriction, magnetoresistance, hall coefficient, BHmax, critical temperature, melting point, boiling point, sublimation point, phase transformation condition, vapor pressure, anisotropy, adhesion, density, hardness, ductility, elasticity, porosity, strength, toughness, surface roughness, coefficient of thermal expansion, thermal conductivity, specific heat, latent heat, refractive index, absorptivity, emissivity, dispersivity, scattering, polarization, acidity, basicity, catalysis, reactivity, energy density, activation energy, free energy, entropy, frequency factor, bioactivity, biocompatibility, thermal coefficient of any property and pressure coefficient of any property.

Claims

1-15. -15. (canceled)

16. A method of forming a non-stoichiometric nanoscale powder having one or more modified properties comprising:

selecting a powder form of a stoichiometric metal compound comprising at least one metal and at least one element selected from the group consisting of;

C, O, N, B, S, H, Se, Te, In, Sb, Al, Ni, F, P, Cl, Br, I, Si, and Ge;

adding at least one dopant element to the metal compound to form a mixture, wherein the at least one dopant element has a valency different than a valency of an electropositive element in the metal compound;

processing the mixture at a temperature greater than the solid state reaction temperature of the mixture to produce a non-stoichiometric nanoscale powder form of a substance comprising the at least one dopant element and the metal compound, wherein the at least one dopant element is combined in the lattice of the metal compound and wherein the resulting compound comprises three or more elements;

wherein combining the at least one dopant element into the lattice of the metal compound modifies at least one property of the metal compound; and

the nanoscale powder form of the substance is substantially compositionally uniform.

17. The method of claim 16 wherein the at least one metal in the metal compound is selected from the group consisting of Ti, Mn, Fe, Ni, Zn, Cu, Sr, Y, Zr, Ta, W, Se, V, Co, In, Li, Hf, Nb, Mo, Sn, Sb, Al, Ce, Pr, Be, Np, Pa, Gd, Dy, Os, Pt, Pd, Ag, Eu, Er, Yb, Ba, Ga, Cs, Na, K, Mg, Pm, Pr, Ni, Bi, Tl, Ir, Rb, Ca, La, Ac, Re, Hg, Cd, As, Th, Nd, Th, Md, and Au.

18. The method of claim 16 wherein the at least one dopant element is combined into the lattice in a concentration greater than 1% over the stoichiometric values.

19. The method of claim 16 wherein the property is selected from the group consisting of:

electrical conductivity, dielectric constant, dielectric strength, dielectric loss, polarization, permittivity, critical current, superconductivity, piezoelectricity, mean free path, curie temperature, critical magnetic field, permeability, coercive force, magnetostriction, magnetoresistance, hall coefficient, BHmax, critical temperature, melting point, boiling point, sublimation point, phase transformation condition, vapor pressure, anisotropy, adhesion, density, hardness, ductility, elasticity, porosity, strength, toughness, surface roughness, coefficient of thermal expansion, thermal conductivity, specific heat, latent heat, refractive index, absorptivity, emissivity, dispersivity, scattering, polarization, acidity, basicity, reactivity, energy density, activation energy, free energy, entropy, frequency factor, bioactivity, biocompatibility, thermal coefficient of any property and pressure coefficient of any property.

20. The method of claim 16 wherein the processing comprises one or more of steps selected from the group consisting of:

heating in inert atmosphere, heating in oxidizing atmosphere and heating in reducing atmosphere.

21. The method of claim 16 wherein the processing modifies one or more of the following characteristics of the nanoscale powders:

shape, surface area, morphology, surface characteristics, surface composition, size distribution and degree of agglomeration.

22. The method of claim 16 wherein the processing comprises plasma processing.

23. The method of claim 16 wherein the processing comprises a quench step after the mixture reaches the solid state reaction temperature.

24. The method of claim 16 wherein the at least one dopant element has a valency different than at least two metals in the metal compound.

25. The method of claim 16 wherein the nanoscale powder has an aspect ratio greater than 1.

53. The method of claim 16 wherein the processing comprises a combustion step.

26. A method of forming a non-stoichiometric nanoscale powder comprising:

selecting a powder form of a stoichiometric metal compound comprising at least one metal and at least one element selected from the group consisting of C, O, N, B, S, H, Se, Te, In, Sb, Al, Ni, F, P, Cl, Br, I, Si, and Ge;

adding at least one dopant element to the metal compound to form a mixture, wherein the at least one dopant element has a valency different than a valency of an electropositive element in the metal compound;

processing the mixture at a temperature greater than the solid state reaction temperature of the mixture to produce a non-stoichiometric nanoscale powder form of a substance comprising the at least one dopant element and the metal compound, wherein the at least one dopant element is combined in the lattice of the metal compound and wherein the resulting compound comprises three or more elements;

wherein combining the at least one dopant element into the lattice of the metal compound modifies at least one property of the metal compound; and

the nanoscale powder form of the substance exhibits a gradient composition.

27. The method of claim 26 wherein the at least one metal in the metal compound is selected from the group consisting of Ti, Mn, Fe, Ni, Zn, Cu, Sr, Y, Zr, Ta, W, Sc, V, Co, In, Li, Hf, Nb, Mo, Sn, Sb, Al, Ce, Pr, Be, Np, Pa, Gd, Dy, Os, Pt, Pd, Ag, Eu, Er, Yb, Ba, Ga, Cs, Na, K, Mg, Pm, Pr, Ni, Bi, Tl, Ir, Rb, Ca, La, Ac, Re, Hg, Cd, As, Th, Nd, Tb, Md, and Au.

28. The method of claim 26 wherein the at least one dopant element is combined into the lattice in a concentration greater than 1% over the stoichiometric values.

29. The method of claim 26 wherein the property is selected from the group consisting of:

electrical conductivity, dielectric constant, dielectric strength, dielectric loss, polarization, permittivity, critical current, superconductivity, piezoelectricity, mean free path, curie temperature, critical magnetic field, permeability, coercive force, magnetostriction, magnetoresistance, hall coefficient, BHmax, critical temperature, melting point, boiling point, sublimation point, phase transformation condition, vapor pressure, anisotropy, adhesion, density, hardness, ductility, elasticity, porosity, strength, toughness, surface roughness, coefficient of thermal expansion, thermal conductivity, specific heat, latent heat, refractive index, absorptivity, emissivity, dispersivity, scattering, polarization, acidity, basicity, reactivity, energy density, activation energy, free energy, entropy, frequency factor, bioactivity, biocompatibility, thermal coefficient of any property and pressure coefficient of any property.

30. The method of claim 26 wherein the processing comprises one or more of steps selected from the group consisting of heating in inert atmosphere, heating in oxidizing atmosphere and heating in reducing atmosphere.

31. The method of claim 26 wherein the processing comprises a combustion step.

32. The method of claim 26 wherein the processing comprises plasma processing.

33. The method of claim 26 wherein the processing comprises a quench step after the mixture reaches the solid state reaction temperature.

34. The method of claim 26 wherein the at least one dopant element has a valency different than at least two metals in the metal compound.

35. The method of claim 26 wherein the nanoscale powder has an aspect ratio greater than 1.

40. The method of claim 26 wherein the processing modifies one or more of the following characteristics of the nanoscale powders:

shape, surface area, morphology, surface characteristics, surface composition, size distribution and degree of agglomeration.

36-39. -39. (canceled)

41-52. -52. (canceled)