Non-stoichiometric nanomaterial compositions with distinctive shape and morphology

• US 7,816,006 B2
• Filed: 03/29/2004
• Issued: 10/19/2010
• Est. Priority Date: 09/03/1996
• Status: Expired due to Fees

• Current Assignee: PPG Industries Ohio Incorporated (Nouryon BV)
• Original Assignee: PPG Industries Ohio Incorporated (Nouryon BV)
• Inventors: Yadav, Tapesh, Kostelecky, Clayton
• Primary Examiner(s): LE, HOA T
• Application Number:
  US10/811,628
• Publication Number:
  US 20040180203A1
• Time in Patent Office: 2,395 Days
• Field of Search: 428/402, 428/407, 977/DIG.1, 977/762, 977/783, 977/810, 977/811, 257/E23.075, 257/E23.166
• US Class Current: 428/402
• 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 19/0046 Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays synthesis methods per se C40B50/00
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• CPC Class Codes: B01J 2219/00653 the compounds being bound to electrodes embedded in or on the solid supports
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• CPC Class Codes: B01J 2219/00745 Inorganic compounds
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• CPC Class Codes: B01J 2219/0894 : Processes carried out in the presence of a plasma
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• CPC Class Codes: B22F 1/054 : Nanosized particles
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• CPC Class Codes: B22F 2201/11 : Argon
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• 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 9/12 : 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: B82Y 5/00 : Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
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• CPC Class Codes: C01B 3/001 : characterised by the uptaking medium; Treatment thereof
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• 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
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• 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 2111/00844 : for electronic applications
• CPC Class Codes: C04B 2235/3241 : Chromium oxides, chromates, or oxide-forming salts thereof
• CPC Class Codes: C04B 2235/3262 : Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
• CPC Class Codes: C04B 2235/3275 : Cobalt oxides, cobaltates or cobaltites or oxide forming salts thereof, e.g. bismuth cobaltate, zinc cobaltite
• CPC Class Codes: C04B 2235/3279 : Nickel oxides, nickalates, or oxide-forming salts thereof
• CPC Class Codes: C04B 2235/3284 : Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
• CPC Class Codes: C04B 2235/3298 : Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate
• CPC Class Codes: C04B 2235/79 : Non-stoichiometric products, e.g. perovskites (ABO3) with an A/B-ratio other than 1
• CPC Class Codes: C04B 2235/80 : Phases present in the sintered or melt-cast ceramic products other than the main phase
• 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 35/01 : based on oxide ceramics
• CPC Class Codes: C04B 35/10 : based on aluminium oxide
• CPC Class Codes: C04B 35/265 : Compositions containing one or more ferrites of the group comprising manganese or zinc and one or more ferrites of the group comprising nickel, copper or cobalt
• CPC Class Codes: C04B 35/2666 : Other ferrites containing nickel, copper or cobalt
• CPC Class Codes: C04B 35/453 : based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
• CPC Class Codes: C04B 35/457 : based on tin oxides or stannates
• CPC Class Codes: C04B 35/56 : based on carbides or oxycarbides containing free metal binder C22C29/00
• CPC Class Codes: C04B 35/5611 : based on titanium carbides
• CPC Class Codes: C04B 35/581 : based on aluminium nitride
• 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 41/009 : characterised by the material treated
• CPC Class Codes: C04B 41/4539 : as a emulsion, dispersion or suspension
• CPC Class Codes: C04B 41/4549 : Nanometer-sized particles
• CPC Class Codes: C04B 41/5027 : Oxide ceramics in general; Specific oxide ceramics not covered by C04B41/5029 - C04B41/5051
• CPC Class Codes: C04B 41/5049 : Zinc or bismuth oxides
• CPC Class Codes: C04B 41/5059 : Silicon carbide
• CPC Class Codes: C04B 41/5116 : Ag or Au
• CPC Class Codes: C04B 41/5122 : Pd or Pt
• 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 41/524 : Multiple coatings, comprising a coating layer of the same material as a previous coating layer
• CPC Class Codes: C04B 41/87 : Ceramics
• CPC Class Codes: C04B 41/89 : for obtaining at least two superposed coatings having different compositions
• CPC Class Codes: C04B 41/90 : at least one coating being a metal
• CPC Class Codes: C08K 2201/011 : Nanostructured additives
• CPC Class Codes: C08K 2201/016 : Additives defined by their aspect ratio
• CPC Class Codes: C08K 3/01 : characterized by their specific function
• CPC Class Codes: C08K 3/08 : Metals
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• CPC Class Codes: H01C 7/112 : ZnO type
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• 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: H01F 1/36 : in the form of particles H01F1/346, H01F1/348 and H01F1/38 take precedence
• CPC Class Codes: H01F 41/0246 : Manufacturing of magnetic circuits by moulding or by pressing powder magnetic cores made by moulding or by pressing powder H01F27/255; soft magnetic particles H01F1/20, H01F1/36
• 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: H01L 23/49883 : the conductive materials containing organic materials or pastes, e.g. for thick films for printed circuits H05K1/092
• CPC Class Codes: H01L 23/5328 : containing conductive organic materials or pastes, e.g. conductive adhesives, inks
• CPC Class Codes: H01L 2924/00 : Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
• CPC Class Codes: H01L 2924/0002 : Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
• CPC Class Codes: H01L 2924/3011 : Impedance
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• CPC Class Codes: H01M 4/04 : Processes of manufacture in general
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• CPC Class Codes: Y10T 428/25 : Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
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Abstract

Nanoscale materials with domain sizes less than 100 nanometers and unusual shapes and morphologies are disclosed. A broad approach for manufacturing oxide and non-oxide nanomaterials with aspect ratio different than 1.0 is presented. Methods for engineering and manufacturing nanomaterials'"'"' size, shape, surface area, morphology, surface characteristics, surface composition, distribution, and degree of agglomeration are discussed. The methods taught includes the use of surfactants, dispersants, emulsifying agents in order to prepare precursors, which are then processed into novel nanoscale particle morphologies.

Claims

1. A non-stoichiometric nanomaterial comprising two or more elements having a composition different than that required for stoichiometric bonding between the two or more elements, the composition represented by the formula:

M_n/pZ<sub>1−

x</sub>

wherein M comprises an element that can lower its free energy by chemically bonding with Z;

wherein Z comprises a chalcogen;

wherein n and p are integers greater than or equal to 1;

wherein 0.01<

x<

0.99; and

wherein a value for a selected material property of the non-stoichiometric nanomaterial is greater than 10% different from a value for the same property for a stoichiometric form of the nanomaterial.

2. The non-stoichiometric nanomaterial of claim 1, wherein M 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, Th, Md, and Au.

3. The non-stoichiometric nanomaterial of claim 1, wherein 0.02<

x<

0.98.

4. The non-stoichiometric nanomaterial of claim 1, wherein 0.05<

x<

0.95.

5. The non-stoichiometric nanomaterial of claim 1, wherein the domain size of the material is less than 5 times the mean free path of electrons in the material.

6. The non-stoichiometric nanomaterial of claim 1, wherein the domain size of the material is less than 100 nanometers.

7. The non-stoichiometric nanomaterial of claim 1, wherein the nanomaterial comprises two or more elements M that can lower their free energy by chemically bonding with Z.

8. The non-stoichiometric nanomaterial of claim 1, wherein the nanomaterial comprises more than one element Z.

9. The non-stoichiometric nanomaterial of claim 1, wherein the nanomaterial comprises more than one element M and more than one element Z.

10. The non-stoichiometric nanomaterial of claim 1, wherein the nanomaterial comprises a multimetallic nanopowder having an aspect ratio in a range of 1-25.

11. The non-stoichiometric nanomaterial of claim 1, wherein the nanomaterial comprises a polymetallic nanopowder comprising at least three metals and at least one chalcogen anion, and having a minimum dimension of less than 100 nm and an aspect ratio of 25 or less.

12. The non-stoichiometric nanomaterial of claim 1, wherein the nanomaterial comprises a nanofiller dispersed in a polymer matrix, thereby forming a nanostructured composite material.

13. A coating composition comprising the non-stoichiometric nanomaterial of claim 1.

14. A nanostructured composite material comprising:

a polymer matrix; and

a nanofiller dispersed in the polymer matrix;

wherein the nanofiller comprises a non-stoichiometric nanomaterial comprising two or more elements having a composition different than that required for stoichiometric bonding between the two or more elements, the composition represented by the formula;

M_n/pZ<sub>1−

x</sub>

wherein M comprises an element that can lower its free energy by chemically bonding with Z;

wherein Z comprises a chalcogen;

wherein n and p are integers greater than or equal to 1; and

wherein 0.01<

x<

0.99; and

wherein a value for a selected material property of the nanostructured composite material comprising the nanofiller is at least 20% different from a value for the same property for an otherwise identical composite material comprising a micron-scale filler.

15. The nanostructured composite material of claim 14, wherein the nanofiller comprises a polymer coated nanofiller.

16. The nanostructured composite material of claim 14, wherein the nanofiller comprises a monomer coated nanofiller.

17. The nanostructured composite material of claim 14, wherein the composite material comprises a coating composition.

18. The nanostructured composite material of claim 14, wherein M 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, Th, Md, and Au.

19. The nanostructured composite material of claim 14, wherein 0.02<

x<

0.98.

20. The nanostructured composite material of claim 14, wherein 0.05<

x<

0.95.

21. The nanostructured composite material of claim 14, wherein the domain size of the material is less than 5 times the mean free path of electrons in the material.

22. The nanostructured composite material of claim 14, wherein the domain size of the material is less than 100 nanometers.

23. The nanostructured composite material of claim 14, wherein the nanomaterial comprises two or more elements M that can lower their free energy by chemically bonding with Z.

24. The nanostructured composite material of claim 14, wherein the nanomaterial comprises more than one element Z.

25. The nanostructured composite material of claim 14, wherein the nanomaterial comprises more than one element M and more than one element Z.

26. The nanostructured composite material of claim 14, wherein the nanomaterial comprises a multimetallic nanopowder having an aspect ratio in a range of 1-25.

27. The nanostructured composite material of claim 14, wherein the nanomaterial comprises a polymetallic nanopowder comprising at least three metals and at least one anion, and having a minimum dimension of less than 100 nm and an aspect ratio of 25 or less.

28. A non-stoichiometric nanomaterial comprising two or more elements having a composition different than that required for stoichiometric bonding between the two or more elements, the composition represented by the formula:

M_n/pZ<sub>1−

x</sub>

wherein M comprises an element that can lower its free energy by chemically bonding with Z;

wherein Z comprises an element selected from the group consisting of B, C, Si, N, P, O, S, Se, Te, and H;

wherein n and p are integers greater than or equal to 1;

wherein 0<

x<

1; and

wherein a value for a selected material property of the non-stoichiometric nanomaterial is greater than 10% different from a value for the same property for a stoichiometric form of the nanomaterial.

29. A nanostructured composite material comprising:

a polymer matrix; and

a nanofiller dispersed in the polymer matrix;

wherein the nanofiller comprises a non-stoichiometric nanomaterial comprising two or more elements having a composition different than that required for stoichiometric bonding between the two or more elements, the composition represented by the formula;

M_n/pZ<sub>1−

x</sub>

wherein M comprises an element that can lower its free energy by chemically bonding with Z;

wherein Z comprises an element selected from the group consisting of B, C, Si, N, P, O, S, Se, Te, and H;

wherein n and p are integers greater than or equal to 1;

wherein 0<

x<

1; and

wherein a value for a selected material property of the nanostructured composite material comprising the nanofiller is at least 20% different from a value for the same property for an otherwise identical composite material comprising a micron-scale filler.