Method for producing dispersed, crystalline, stable to oxidation copper particles
View Patent ↗Dispersed, crystalline, stable to oxidation copper particles are prepared in the absence of polymeric dispersants by rapidly reducing a Cu(I) salt with an Fe(II) carboxylic acid complex in water. The resulting microns sized copper powders contain only organics which decompose at temperatures low enough not to interfere with sintering processes and the formation of conductive copper structures.
1. A method for the manufacture of easily dispersed, stable to oxidation, crystalline, copper powders in the absence of polymeric dispersants comprising the sequential steps:
a. forming a Cu(I) solution by dissolving a Cu(I) salt in deionized water, wherein the Cu(I) salt is selected from the group consisting of cuprous chloride, cuprous acetate and cuprous bromide;
b. forming a Fe(II) salt solution by dissolving a Fe(II) salt in deionized water;
c. forming a carboxylic acid solution by dissolving a carboxylic acid or a salt of a carboxylic acid in deionized water,
d. forming a reducing Fe (II) carboxylic acid complex solution by adding the Fe (II) salt solution to the carboxylic acid solution
e. rapidly adding the reducing Fe(II) carboxylic acid complex solution to the Cu(I) solution
f. continuing to stir the solution until all of the copper has been precipitated and copper particles have been formed;
g. allowing the copper particles to settle followed by removal of a supernatant, washing the copper particles, collecting them, and then drying them.
2. The method of claim 1 wherein the Fe(II) salt is selected from the group consisting of ferrous sulfate, ferrous chloride, ferrous citrate and ferrous thiocyanate.
3. The method of claim 1 wherein the carboxylic acid solution is a deionized water solution of citric acid, oxalic acid, malonic acid, or succinic acid.
4. The method of claim 1 wherein the carboxylic acid solution is a deionized water solution of citric acid.
5. The method of claim 1 where the Fe (II) salt solution is added to the copper (I) solution at an operating temperature between 20° C. and 60° C.
6. A method for the manufacture of copper particles comprising the sequential steps:
a. providing a Cu(I) solution, wherein the solution comprises water, and a Cu(I) salt is selected from the group consisting of cuprous chloride, cuprous acetate and cuprous bromide;
b. providing a Fe(II) solution, wherein the solution comprises water;
c. providing a carboxylic acid solution, wherein the solution comprises water;
d. combining the Fe (II) solution and the carboxylic acid solution, forming a reducing Fe (II) carboxylic acid complex solution; and
e. combining the reducing Fe(II) carboxylic acid complex solution and the Cu(I) solution to form copper particles.