# US 11,305,350 B2 · Method for preparing silver powder by using micro-nano bubbles as crystal seeds

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- Number: US 11,305,350 B2
- Document ID: US11305350B2
- Status: Granted
- Kind: B2
- Application number: 16/078,164
- Filed: 2017-06-15
- Published: 2019-02-07
- Granted: 2022-04-19
- Earliest claimed: 2016-05-04
- Assignees: Suzhou Smart Advanced Coating Technologies Co., Ltd.
- Applicants: Suzhou Smart Advanced Coating Technologies Co., Ltd.
- Inventors: Qiang Gong
- Web page: https://patentgrep.com/patent/US11305350B2

## CPC

- B22F 9/24: starting from liquid metal compounds, e.g. solutions
- C22C 5/06: Alloys based on silver
- B22F 1/05: Metallic powder characterised by the size or surface area of the particles
- B22F 1/056: {Submicron particles having a size above 100 nm up to 300 nm}
- B22F 1/07: Metallic powder characterised by particles having a nanoscale microstructure (nanosized particles B22F1/054)
- B22F 2998/10: Processes characterised by the sequence of their steps
- B22F: WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER (making alloys by powder metallurgy C22C); APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- C22C: ALLOYS (treatment of alloys C21D, C22F)

## Abstract

A preparation method using micro-nano bubbles as crystal seeds to induce spherical or spherical-type silver power production, said method specifically comprising the steps of: pre-adding a prepared dispersing agent solution to a reaction vessel, within the reaction vessel, simultaneously adding a prepared oxidizing solution (an aqueous solution containing silver ions or a silver ammonia solution) and a reducing solution (an aqueous solution containing one or a plurality of hydroxylamine compounds, vitamin C, formaldehyde or hydrazine hydrate), performing a reduction reaction under vigorous stirring, and using the pre-generated micro-nano bubbles within the dispersing agent solution as crystal seeds, the micro-nano bubbles crystal seeds effectively controlling the particle size of reduced silver particles throughout the reduction reaction. The method effectively controls the particle size of the silver powder during production, and also controls the crystal nucleus growth rate and dispersibility.

## Claims

### Claim 1

A method for preparing silver powder, comprising the following steps:
(1) preparing an oxidant solution, the oxidant solution including silver nitrate or silver sulfate, having a silver concentration of 0.1-10 mol/L, and being kept at 10° C. to 50° C.;
(2) preparing a reductant solution, the reductant solution including a reductant selected from the group consisting of a hydroxylamine compound, vitamin C, a 37% to 40% formaldehyde solution, and hydrazine hydrate, having a reductant concentration of 0.1-10 mol/L, and being kept at 10° C. to 50° C., a volume of the reductant solution being 0.5-5 times a volume of the oxidant solution;
(3) preparing a dispersant solution, the dispersant solution including a dispersant selected from the group consisting of polyvinylpyrrolidone (PVP), poly(ethylene glycol) 400 (PEG), polyoxyethylenesorbitan monopalmitate, and glycerol and being kept at 10° C. to 50° C., a weight of the dispersant in the dispersant solution being 0.01-5 times a weight of the silver in the oxidant solution;
(4) preparing a flocculant solution, the flocculant solution including alcohol and a flocculant selected from the group consisting of oleic acid and an oleate, a weight of the flocculant is 0.01% to 10% of the silver in the oxidant solution;
(5) adding the dispersant solution in a reaction vessel, generating controllable micro-nano bubbles in the dispersant solution by using a micro-nano bubble generator, the micro-nano bubbles being introduced as crystal seeds, adding the oxidant solution and the reductant solution simultaneously to the dispersant solution at a flow rate of 0.1-100 L/min; and
(6) discharging a mixture of the dispersant solution, the oxidant solution and the reductant solution from step (5) into a flocculation sedimentation tank, adding the flocculant solution, stirring for 1-60 min, and standing for precipitation to obtain nearly spherical silver powder having an average particle size of 0.1-10 μm,
wherein in step (5), the oxidant solution and the reductant solution are simultaneously sprayed through micropores into the dispersant solution at a flow rate of 50 L/min and stirred at 120 rpm.

### Claim 2 (depends on 1)

The method of claim 1, wherein the reductant is the hydroxylamine compound is selected from the group consisting of hydroxylamine, hydroxylamine sulfate, and hydroxylamine nitrate.

### Claim 3 (depends on 1)

The method of claim 1, wherein the silver powder particles have an internal loose structure that aids an activity of the silver powder particles.