Silver nanowire manufacturing method

Patent metadata

Field	Value
Publication number	US-10081059-B2
Application number	US-201514881924-A
Country	US
Kind code	B2
Filing date	Oct 13, 2015
Priority date	Oct 28, 2014
Publication date	Sep 25, 2018
Grant date	Sep 25, 2018

Abstract

A process for manufacturing silver nanowires is provided, wherein the recovered silver nanowires have a high aspect ratio; and, wherein the total glycol concentration is <0.001 wt % at all times during the process.

First claim

We claim:

1. A method for manufacturing high aspect ratio silver nanowires, comprising:
providing a container;
providing water;
providing a reducing sugar;
providing a reducing agent;
providing a polyvinyl pyrrolidone (PVP), wherein the polyvinyl pyrrolidone (PVP) provided is divided into a first part of the polyvinyl pyrrolidone (PVP) and a second part of the polyvinyl pyrrolidone (PVP);
providing a source of copper (II) ions;
providing a source of halide ions;
providing a source of silver ions, wherein the source of silver ions provided is divided into a first portion of the source of silver ions and a second portion of the source of silver ions;
adding the water, the reducing sugar, the source of copper (II) ions and the source of halide ions to the container to form a combination;
heating the combination to 110 to 160 ° C.;
adding the first part of the polyvinyl pyrrolidone (PVP), the first portion of the source of silver ions and the reducing agent to the combination in the container to form a creation mixture;
then adding to the container the second part of the polyvinyl pyrrolidone (PVP) and the second portion of the source of silver ions to form a growth mixture;
maintaining the growth mixture at 110 to 160 ° C. for a hold period of 2 to 30 hours to provide a product mixture; and,
recovering a plurality of high aspect ratio silver nanowires from the product mixture;
wherein a total glycol concentration in the container is <0.001 wt % at all times.

2. The method of claim 1 , wherein the first part of the polyvinyl pyrrolidone (PVP) and the first portion of the source of silver ions are added to the container simultaneously.

3. The method of claim 1 , wherein the first portion of the source of silver ions is added to the combination below a surface of the combination in the container.

4. The method of claim 1 , further comprising:
a delay period,
wherein the delay period is interposed between adding the first portion of the source of silver ions to form the creation mixture and adding the second portion of the source of silver ions to form the growth mixture.

5. The method of claim 4 , wherein the first part of the polyvinyl pyrrolidone (PVP) is 10 to 40 wt % of the polyvinyl pyrrolidone (PVP) provided; and, wherein the first portion of the source of silver ions is 10 to 40 wt % of the source of silver ions provided.

6. The method of claim 1 , wherein the reducing agent is selected from ascorbic acid; borohydride salts; hydrazine; salts of hydrazine; hydroquinone; C 1-5 alkyl aldehyde and benzaldehyde.

7. The method of claim 1 , wherein the reducing sugar provided is glucose; and, wherein the reducing agent provided is at least one of ascorbic acid and sodium borohydride.

8. The method of claim 1 , further comprising:
providing a pH adjusting agent; and,
adding the pH adjusting agent to the combination, wherein the combination has a pH of 2.0 to 4.0 following addition of the pH adjusting agent.

9. The method of claim 1 , further comprising:
purging a container vapor space in contact with the combination in the container to provide a reduced oxygen gas concentration in the container vapor space, wherein the reduced oxygen gas concentration in the container vapor space is less than or equal to 2000 ppm;
sparging the source of silver ions provided with an inert gas to extract entrained oxygen gas from the source of silver ions provided and to provide a low oxygen gas concentration in a silver ion vapor space in contact with the source of silver ions provided, wherein the low oxygen gas concentration in the silver ion vapor space is less than or equal to 10,000 ppm;
purging a PVP vapor space in contact with the polyvinyl pyrrolidone (PVP) provided to provide a diluted oxygen gas concentration in the PVP vapor space, wherein the diluted oxygen gas concentration in the PVP vapor space is less than or equal to 10,000 ppm;
maintaining the low oxygen gas concentration in the silver ion vapor space and the diluted oxygen gas concentration in the PVP vapor space; and,
maintaining the reduced oxygen gas concentration in the container vapor space during formation of the creation mixture, during formation of the growth mixture and during the hold period.

10. The method of claim 1 ,
wherein the reducing sugar provided is glucose;
wherein the reducing agent provided is selected from ascorbic acid; borohydride salts; hydrazine; salts of hydrazine; hydroquinone; C 1-5 alkyl aldehyde and benzaldehyde;
wherein the polyvinyl pyrrolidone (PVP) provided has a weight average molecular weight, M W , of 40,000 to 150,000 Daltons;
wherein the source of copper (II) ions provided is copper (II) chloride;
wherein the source of halide ions provided is sodium chloride;
wherein the source of silver ions provided is silver nitrate;
wherein the first part of the polyvinyl pyrrolidone (PVP) is 10 to 40 wt % of the polyvinyl pyrrolidone (PVP) provided; and,
wherein the first portion of the source of silver ions is 10 to 40 wt % of the source of silver ions provided.

Assignees

• Dow Global Technologies Llc

Inventors

• Ziebarth Robin P
• Patyk Richard A
• Wang Wei
• Mcgough Patrick T
• Athens George L
• Goss Janet M
• Lunn Jonathan D

Classifications

• B22F1/0547

  Nanofibres or nanotubes · CPC title

• B22F1/062

  Fibrous particles · CPC title

• B22F9/24 Primary

  starting from liquid metal compounds, e.g. solutions · CPC title

• H01B1/02

  mainly consisting of metals or alloys · CPC title

• C22B11/04

  by wet processes (extraction of metal compounds by leaching in organic solutions C22B3/16; treatment or purification of solutions by liquid-liquid extraction C22B3/26) · CPC title