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Polyol-based method for producing ultra-fine copper powders

a polyol-based, copper powder technology, applied in the direction of material nanotechnology, transportation and packaging, coatings, etc., can solve the problems of large consumption of organic solvents per unit weight of metallic powder produced, low concentration of metallic precursors, and wide size distribution of metallic powder produced using these procedures, etc., to achieve high crystallinity and oxidation resistance, tight size distribution, and low agglomeration degree

Inactive Publication Date: 2006-05-04
CLARKSON UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

"The present invention provides a method for producing metallic particles with desirable features such as tight size distribution, low degree of agglomeration, and high degree of crystallinity and oxidation resistance. The method involves forming a reaction mixture containing a precursor of a metal, a branched dispersing agent, and an alcoholic agent, and optionally adjusting the pH of the reaction mixture. The resulting metallic particles have been found to have improved properties when used in various applications such as coating and catalysts. The invention also provides a method for controlling the size of the metallic particles and a method for producing ultra-fine metallic particles using a concentrated reaction system."

Problems solved by technology

These procedures, however, are characterized by rather low concentrations of metallic precursors and consume large quantities of organic solvents per unit weight of metallic powder produced.
Furthermore, the metallic powders produced using these procedures have a wide size distribution, a low degree of crystallinity, and in the case of the base metals, a pronounced tendency to oxidation.

Method used

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  • Polyol-based method for producing ultra-fine copper powders
  • Polyol-based method for producing ultra-fine copper powders
  • Polyol-based method for producing ultra-fine copper powders

Examples

Experimental program
Comparison scheme
Effect test

example 1

Materials

[0048] The copper carbonate (CuCO3) was supplied by Shepherd Chemical Co. 1,2-PG and DEG were obtained from Alfa Aesar (Ward Hill, Mass.). 1,3-PG and PE were obtained from Avocado Research Chemical Ltd., while TEA was purchased from Aldrich (Milwaukee, Wis.).

example 2

Copper Particles Synthesis

[0049] All experiments were carried out in a 1 L-4-necked round flask equipped with a Dean Stark trap and a refluxing condenser. The stirring was provided by a two inch Teflon—blade connected to a variable speed mixer. The amount of cupric carbonate used in the precipitation process was in general kept at 200 g (1.62 mol) although smaller or larger amounts were occasionally used as well (i.e., 87 g and 300 g). The CuCO3 was added into 500 cm3 polyols or polyols mixture containing 15 g PE (for 200 g CuCO3). The dispersant agent (PE) was initially added in polyols and heated at low power (10%) in the heating mantle to bring the temperature to 70° C. The required amounts of CuCO3 were added into the flask at 80-85° C. after the PE was fully dissolved. The CuCO3 / polyol mixture was stirred at 500 RPM in all experiments. The mixture was then heated at 50% setting of heating power until the temperature reaches 180-185° C. The copper particles obtained were washed...

example 3

Particles Characterization

[0050] The morphology of copper particles was investigated by scanning electron microscopy (SEM) using a JEOL-JSM 6300 scanning microscope at 15 kV accelerating voltage and the magnification between 2500 and 10000. Also, the copper powders were analyzed by field emission scanning electron microscopy (FE-SEM) with 5 kV accelerating voltage and the same range of magnification using a JEOL JSM −7400F field emission scanning electron microscope.

[0051] Discussed below are results obtained by the inventors in connection with the experiments of Example 1-3:

[0052] In order to evaluate the effect of pH in the formation of Cu particles in polyols, variable amounts of triethanolamine (TEA) were added into the dispersion of CuCO3 prior to the heating as shown in Table 1. The reaction time in the presence of TEA varied between 3 and 4 hours, the addition of more base tending to speed up the reaction. The images of copper particles produced in the manner described in ...

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Abstract

The present invention provides a metallic composition, which contains a plurality of ultra-fine metallic particles (e.g., ultra-fine copper, nickel, or silver particles) having at least one desirable feature, such as, tight size distribution, low degree of agglomeration, and high degree of crystallinity and oxidation resistance. The present invention further provides a method for forming the ultra-fine metallic particles. Also provided are a substance or substrate coated with the ultra-fine metallic particles and a method of coating a substance or substrate with the ultra-fine metallic particles. Furthermore, the present invention provides a method of controlling the size of ultra-fine metal particles formed in a reducing reaction in a liquid. Also provided is a method for producing ultra-fine metallic particles, which utilizes a concentrated reaction system.

Description

CROSS REFERENCE TO RELATED APPLICATIONS [0001] The present application is a continuation application of U.S. nonprovisional application Ser. No. ______, filed Oct. 29, 2004, and is hereby incorporated by reference herein.FIELD OF THE INVENTION [0002] The present invention relates generally to ultra-fine metallic compositions and methods of making thereof. The present invention further relates to methods of depositing ultra-fine metallic compositions onto various substrates. BACKGROUND OF THE INVENTION [0003] Ultra-fine metallic particles have many unique physical and chemical characteristics, which make them ideal materials for a variety of applications, such as electronics, catalysis, metallurgy, and decorative. Compared to the various particle-producing techniques used in the art, the methods based on the chemical precipitation in solutions provide several advantages, e.g., low manufacturing cost and a very good control of the mechanism of metal particles formation. Others in the ...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): B22F9/24B22F1/05
CPCB22F1/0011B22F9/24Y10T428/12014C23C26/00B82Y30/00B22F1/05
Inventor GOIA, DAN V.ANDREESCU, DANIELFARRELL, BRENDAN P.
Owner CLARKSON UNIVERSITY
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