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US5759230A Expired / Lapsed US ⏱️ 0.0 years remaining

Nanostructured metallic powders and films via an alcoholic solvent process

Assignee: NAVY United States, NAVY THE, Secretary of
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Filing: 1995-11-30
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Granted: 1998-06-02
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Expires: 2015-11-30
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Abstract

Abstract Nanostructured metal powders and films are made by dissolving or wetting a metal precursor in an alcoholic solvent. The resulting mixture is then heated to reduce the metal precursor to a metal precipitate. The precipitated metal may be isolated, for example, by filtration.

Inventors

  • 👤 Gan-Moog Chow
  • 👤 Paul E. Schoen
  • 👤 Lynn K. Kurihara

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-23 16:11
CPC Classifications
B; B22; B22F; B22F9/00; B22F9/16; B22F9/18; B22F9/24; B22F2998/00

Claims Analysis

Total Claims: 19
Claim 1
Independent Claim 103 words
A method of forming a nanocrystalline metallic powder, comprising the steps of: mixing a precursor of a refractory metal with an alcoholic solvent to form a reaction mixture, said precursor being selected from the group consisting of a metal salt, a hydrate of a metal salt, an acid including said refractory metal as part of an oxyanion, a salt of said acid, and mixtures thereof; refluxing said reaction mixture so that said alcoholic solvent reduces said precursor to said refractory metal, over a time selected to produce particles of said refractory metal having a mean diameter size of about 100 nm or less.
Claim 2
Independent Claim 103 words
A method of forming a nanocrystalline metallic powder, comprising the steps of: mixing a precursor of a refractory metal with an alcoholic solvent to form a reaction mixture, said precursor being selected from the group consisting of a metal salt, a hydrate of a metal salt, an acid including said refractory metal as part of an oxyanion, a salt of said acid, and mixtures thereof; refluxing said reaction mixture so that said alcoholic solvent reduces said precursor to said refractory metal, over a time selected to produce particles of said refractory metal having a mean diameter size of about 100 nm or less.
Claim 3
Dependent Claim 32 words
The method of claim 1, wherein said mixing step and said reacting step are performed in such a manner that said particles of said refractory metal are essentially free of non-metallic impurities.
Claim 4
Dependent Claim 29 words
The method of claim 2, wherein said mixing step and said reacting step are performed in such a manner that said particles of said refractory metal are essentially pure.
Claim 5
Dependent Claim 31 words
The method of claim 1, wherein said metal precursor is a metal acetate, a metal chloride, a metal nitrate, metal acetate hydrate, a metal chloride hydrate, or a metal nitride hydrate.
Claim 6
Dependent Claim 22 words
The method of claim 1, wherein said refractory metal is selected from the group consisting of W, Ti, Mo, Re, and Ta.
Claim 7
Dependent Claim 25 words
The method of claim 1, wherein said reaction mixture is reacted at a temperature at which said metal precursor is soluble in said alcoholic solvent.
Claim 8
Dependent Claim 16 words
The method of claim 1, wherein said reaction mixture is reacted for about 30 minutes-5 hours.
Claim 9
Dependent Claim 15 words
The method of claim 7, wherein said reaction mixture is reacted for about 1-3 hours.
Claim 10
Dependent Claim 20 words
The method of claim 1, wherein said precursor is present in said reaction mixture at a concentration of about 0.001-0.80M.
Claim 11
Independent Claim 158 words
A method of forming a nanocrystalline metallic film, comprising the steps of: mixing a precursor of a metal selected from the group consisting of Ti, V, Cr, Mn, Fe, Co, Ni, Nb, Mo, Ru, Rh, Sn, Ta, W, and mixtures thereof with an alcoholic solvent to form a reaction mixture, said precursor being selected from the group consisting of a metal salt, a hydrate of a metal salt, an acid including said refractory metal as part of an oxyanion, a salt of said acid, and mixtures thereof; physically contacting said reaction mixture with a substrate surface that is essentially free of borosilicates; refluxing said reaction mixture so that said alcoholic solvent reduces said metal precursor, while said reaction mixture is in contact with said substrate surface, for a time selected to produce an adherent metal film on said substrate surface, said film having particles of said metal with a mean diameter size of about 100 nm or less.
Claim 12
Independent Claim 158 words
A method of forming a nanocrystalline metallic film, comprising the steps of: mixing a precursor of a metal selected from the group consisting of Ti, V, Cr, Mn, Fe, Co, Ni, Nb, Mo, Ru, Rh, Sn, Ta, W, and mixtures thereof with an alcoholic solvent to form a reaction mixture, said precursor being selected from the group consisting of a metal salt, a hydrate of a metal salt, an acid including said refractory metal as part of an oxyanion, a salt of said acid, and mixtures thereof; physically contacting said reaction mixture with a substrate surface that is essentially free of borosilicates; refluxing said reaction mixture so that said alcoholic solvent reduces said metal precursor, while said reaction mixture is in contact with said substrate surface, for a time selected to produce an adherent metal film on said substrate surface, said film having particles of said metal with a mean diameter size of about 100 nm or less.
Claim 13
Dependent Claim 32 words
The method of claim 10, wherein said metal precursor is a metal acetate, a metal chloride, a metal nitrate, a metal acetate hydrate, a metal chloride hydrate, or a metal nitride hydrate.
Claim 14
Dependent Claim 12 words
The method of claim 10, wherein said metal is a refractory metal.
Claim 15
Dependent Claim 24 words
The method of claim 12, wherein said refractory metal is selected from the group consisting of W, Ti, Mo, Re, Ta, and alloys thereof.
Claim 16
Dependent Claim 32 words
The method of claim 10, wherein said mixing step and said reacting step are performed in such a manner that said particles of said refractory metal are essentially free of non-metallic impurities.
Claim 17
Independent Claim 154 words
A method of forming a nanocrystalline complex substance comprising at least 50 volume percent of first component selected from the group consisting of an elemental refractory metal or an alloy thereof, said method comprising the steps of: atomically mixing, in an alcoholic solvent, a first precursor for at least one elemental refractory metal with a second precursor for at least one second component, or with said second component, to form a reaction mixture, said first precursor being selected from the group consisting of a metal salt, a hydrate of a metal salt, an acid including said elemental refractory metal as part of an oxyanion, a salt of said acid, and mixtures thereof; refluxing said reaction mixture so that said alcoholic solvent reduces at least said first precursor to said elemental refractory metal, over a time selected to produce particles of said complex substance having a mean diameter size of about 100 nm or less.
Claim 18
Independent Claim 154 words
A method of forming a nanocrystalline complex substance comprising at least 50 volume percent of first component selected from the group consisting of an elemental refractory metal or an alloy thereof, said method comprising the steps of: atomically mixing, in an alcoholic solvent, a first precursor for at least one elemental refractory metal with a second precursor for at least one second component, or with said second component, to form a reaction mixture, said first precursor being selected from the group consisting of a metal salt, a hydrate of a metal salt, an acid including said elemental refractory metal as part of an oxyanion, a salt of said acid, and mixtures thereof; refluxing said reaction mixture so that said alcoholic solvent reduces at least said first precursor to said elemental refractory metal, over a time selected to produce particles of said complex substance having a mean diameter size of about 100 nm or less.
Claim 19
Dependent Claim 15 words
The method of claim 15, wherein said second component is a metal or a ceramic.

References Cited (Backward Citations)

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JPS63149383A Cited
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GB2236117A Cited
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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 2001-06-01 2001-12-01 2002-06-02 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 2005-06-01 2005-12-01 2006-06-02 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2009-06-01 2009-12-01 2010-06-02 $7700.00 Window Closed / Lapsed

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