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US6746510B2 Expired / Lapsed US ⏱️ 0.0 years remaining

Processing of nanocrystalline metallic powders and coatings using the polyol process

Assignee: United States Department of the Navy
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Filing: 2002-03-29
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Granted: 2004-06-08
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Expires: 2022-03-29
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Abstract

Abstract Nanostructured metallic powders and coatings are processed by suspending a metal precursor in a glycol solution containing the constituent metal salts and using a millimeter wave beam as the heating source. The mixture is then heated to reduce the metal precursor to a metal precipitate. The precipitated metal may then be isolated.

Inventors

  • 👤 Lynn K. Kurihara
  • 👤 Ralph W. Bruce
  • 👤 Arne W. Fliflet
  • 👤 David Lewis

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-23 13:43
CPC Classifications
B; B22; B22F; B22F9/00; B22F9/16; B22F9/18; B22F9/24; B22F1/00; B22F1/05; B22F1/054; B82; B82Y; B82Y30/00; B22F2999/00

Claims Analysis

Total Claims: 17
Claim 1
Independent Claim 70 words
A method of forming a nanocrystalline metallic powder, comprising the steps of: mixing a metal salt in a glycol solvent to form a reaction mixture; applying a millimeter-wave beam to said reaction mixture; refluxing said reaction mixture so that said glycol solvent reduces said metal salt to a metal, over a time selected to produce particles of said metal having a mean diameter size of about 100 nm or less.
Claim 2
Independent Claim 70 words
A method of forming a nanocrystalline metallic powder, comprising the steps of: mixing a metal salt in a glycol solvent to form a reaction mixture; applying a millimeter-wave beam to said reaction mixture; refluxing said reaction mixture so that said glycol solvent reduces said metal salt to a metal, over a time selected to produce particles of said 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 refluxing step are performed in such a manner that said particles of said 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 metal are essentially pure.
Claim 5
Dependent Claim 27 words
The method of claim 1 , wherein said metal salt is selected from the group consisting of chlorides, acetates, acetylacetonates, oxides, carbonyls, carbonates, hydrates, hydroxides, and nitrates.
Claim 6
Dependent Claim 32 words
The method of claim 1 , wherein said glycol solvent is selected from the group consisting of ethylene glycol, propylene glycol, tetraethylene glycol, ethoxy ethanol, diethylene glycol, monoethyl ether, and mixtures thereof.
Claim 7
Dependent Claim 19 words
The method of claim 1 , wherein said mixture is filtered, centrifuged, or magnetically separated to remove said particles.
Claim 8
Dependent Claim 15 words
The method of claim 1 , wherein said millimeter-wave beam is generated by gyrotron oscillators.
Claim 9
Dependent Claim 22 words
The method of claim 1 , wherein said millimeter-wave beam has an intensity of about 10 2 -10 5 W/cm 2 .
Claim 10
Dependent Claim 17 words
The method of claim 1 , wherein said millimeter-wave beam has a frequency of about 83 GHz.
Claim 11
Dependent Claim 17 words
The method of claim 1 , wherein said millimeter-wave beam has a power of about 30-750 W.
Claim 12
Dependent Claim 12 words
The method of claim 1 , wherein said millimeter-wave beam is polarized.
Claim 13
Dependent Claim 15 words
The method of claim 1 , wherein said millimeter-wave beam is a free-space quasi-Gaussian beam.
Claim 14
Dependent Claim 17 words
The method of claim 1 , wherein said metal salt has a concentration of about 0.01-0.3 M.
Claim 15
Dependent Claim 16 words
The method of claim 1 , wherein said refluxing step is conducted for about 15 minutes.
Claim 16
Independent Claim 94 words
A method of forming a nanocrystalline metallic powder, comprising the steps of: mixing a metal salt in an alcoholic solvent to form a reaction mixture, wherein the metal salt concentration is about 0.1 M; applying a millimeter-wave beam to said reaction mixture, wherein said millimeter-wave beam has a power of about 330 W; refluxing said reaction mixture so that said alcoholic solvent reduces said metal salt to a metal; and wherein said refluxing occurs for 15 minutes to produce particles of said metal having a mean diameter size of about 80 nm or less.
Claim 17
Independent Claim 94 words
A method of forming a nanocrystalline metallic powder, comprising the steps of: mixing a metal salt in an alcoholic solvent to form a reaction mixture, wherein the metal salt concentration is about 0.1 M; applying a millimeter-wave beam to said reaction mixture, wherein said millimeter-wave beam has a power of about 330 W; refluxing said reaction mixture so that said alcoholic solvent reduces said metal salt to a metal; and wherein said refluxing occurs for 15 minutes to produce particles of said metal having a mean diameter size of about 80 nm or less.

References Cited (Backward Citations)

US5585020A Cited
US5520717A Cited
US6068800A Cited
US5759230A Cited
US6436167B1 Cited

USPTO Annuity & Maintenance Windows

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