Method of producing metallic nano particle colloidal dispersions
First Claim
1. A stable, fully reduced metallic nanoparticle-containing colloidal dispersion in which the nanoparticle is a reduced metal and aromatic stabilizer particle with a uniform and mean particle size less than 2.9 nm, wherein the nanoparticle comprises a metal and aromatic stabilizer with at least two nitrogen functional groups, and wherein the colloidal dispersion is synthesized by a solution phase synthesis process wherein synthesis occurs at a temperature of less than 60 degrees Celsius in a period of less than 60 minutes, comprising the steps of:
- forming a salt charge transfer complex of metal cations (CT complex) of an amino alcohol or diamine moiety with a metal salt;
reacting the CT complex with a solution comprising a two or three nitrogen atom-containing organic reducing agent to form metallic nanoparticles; and
stabilizing the metallic nanoparticles with aniline or a bi-dentate hetero atom containing a Lewis Base amine stabilizer to form the stable, fully reduced metallic nanoparticle-containing colloidal dispersion,wherein;
the CT complex results from the reaction of a metallic formate, acetate, alkoxide or citrate salt dissolved in at least two solvents selected from the group consisting of water, monoethanolamine, di-ethanolamine, tri-ethanolamine, 1,2-aminopropanol, 1,3-aminopropanol, and combinations thereof;
the two or three nitrogen atom containing reducing agent is selected from the group consisting of diethylenetriamine, 1,2-diaminocyclohexane, hydrazine, organic group substituted hydrazine molecule or phenidone molecule; and
the bi-dentate hetero atom-containing amine stabilizer is selected from the group consisting of dimethyl glyoxime, 2,2′
-bipyridine, 1,10-phenanthroline, ortho-phenylenediamine, 1,2-diaminocyclohexane, 1,4-diamino butane, urea, 8-hydroxyquinoline, substituted urea, and combinations thereof.
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Abstract
The present process provides a method for synthesizing difficult to make oxide-free nanometals and such as Zn, Sn and Ti and alloys of the period 4 and 5 transition metal elements in a free and reduced state using a solution phase synthesis process. Also provided is a method for stabilizing their associated colloidal metal and alloy dispersions under kinetic control at modest temperatures (<80 degrees Celsius). A solution of an organic reducing agent containing at least two proximal nitrogen atoms is reacted with a separate solution containing one or more metal-organic salts dissolved in the same or different low molecular weight solvent as the reducing agent. The reaction products are stabilized with Lewis bases and Lewis acids and optionally can be concentrated by removing a portion of the volatile low molecular weight solvent by either the use of a partial vacuum or by chemical extraction into another phase.
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Citations
18 Claims
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1. A stable, fully reduced metallic nanoparticle-containing colloidal dispersion in which the nanoparticle is a reduced metal and aromatic stabilizer particle with a uniform and mean particle size less than 2.9 nm, wherein the nanoparticle comprises a metal and aromatic stabilizer with at least two nitrogen functional groups, and wherein the colloidal dispersion is synthesized by a solution phase synthesis process wherein synthesis occurs at a temperature of less than 60 degrees Celsius in a period of less than 60 minutes, comprising the steps of:
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forming a salt charge transfer complex of metal cations (CT complex) of an amino alcohol or diamine moiety with a metal salt; reacting the CT complex with a solution comprising a two or three nitrogen atom-containing organic reducing agent to form metallic nanoparticles; and stabilizing the metallic nanoparticles with aniline or a bi-dentate hetero atom containing a Lewis Base amine stabilizer to form the stable, fully reduced metallic nanoparticle-containing colloidal dispersion, wherein; the CT complex results from the reaction of a metallic formate, acetate, alkoxide or citrate salt dissolved in at least two solvents selected from the group consisting of water, monoethanolamine, di-ethanolamine, tri-ethanolamine, 1,2-aminopropanol, 1,3-aminopropanol, and combinations thereof; the two or three nitrogen atom containing reducing agent is selected from the group consisting of diethylenetriamine, 1,2-diaminocyclohexane, hydrazine, organic group substituted hydrazine molecule or phenidone molecule; and the bi-dentate hetero atom-containing amine stabilizer is selected from the group consisting of dimethyl glyoxime, 2,2′
-bipyridine, 1,10-phenanthroline, ortho-phenylenediamine, 1,2-diaminocyclohexane, 1,4-diamino butane, urea, 8-hydroxyquinoline, substituted urea, and combinations thereof. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18)
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Specification