Method of manufacturing silver nanowires

Patent metadata

Field	Value
Publication number	US-9776249-B2
Application number	US-201514881859-A
Country	US
Kind code	B2
Filing date	Oct 13, 2015
Priority date	Oct 28, 2014
Publication date	Oct 3, 2017
Grant date	Oct 3, 2017

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 process for manufacturing high aspect ratio silver nanowires, comprising:
providing a container;
providing water;
providing a reducing sugar;
providing a polyvinyl pyrrolidone (PVP);
providing a source of copper (II) ions;
providing a source of halide ions;
providing a source of silver ions;
providing a pH adjusting agent;
adding the water, the reducing sugar, the polyvinyl pyrrolidone (PVP), the source of copper (II) ions, the source of halide ions, and the pH adjusting agent to the container to form a combination, wherein the combination has a pH of 2.0 to 4.0;
heating the combination to 110 to 160° C.;
then adding the source of silver ions to the container to form a growth mixture;
then 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; and,
wherein a total glycol concentration in the container is <0.001 wt % at all times during the process.

2. The process of claim 1 , further comprising:
dividing the source of silver ions into a first portion and a second portion;
heating the combination to 140 to 160° C.;
then adding the first portion to the container to form a creation mixture;
then cooling the creation mixture to 110 to 135° C. during a delay period;
following the delay period, adding the second portion to the container to form the growth mixture.

3. The process of claim 2 , wherein the growth mixture is maintained at 110 to 135° C. during the hold period.

4. The process of claim 3 , wherein the reducing sugar provided is glucose.

5. The process of claim 3 , wherein the polyvinyl pyrrolidone (PVP) provided has a weight average molecular weight, M W , of 40,000 to 150,000 Daltons.

6. The process of claim 3 , wherein the source of copper (II) ions provided is copper (II) chloride.

7. The process of claim 3 , wherein the source of halide ions provided is sodium chloride.

8. The process of claim 3 , wherein the source of silver ions provided is silver nitrate.

9. The process of claim 1 , further comprising:
dividing the source of silver ions into a first portion and a second portion;
heating the combination to 140 to 160° C.;
then adding the first portion to the container to form a creation mixture;
then cooling the creation mixture to 110 to 135° C. during a delay period;
following the delay period, adding the second portion to the container to form the growth mixture; and,
maintaining the growth mixture at 110 to 135° C. during the hold period;
wherein the reducing sugar provided is glucose;
wherein the polyvinyl pyrrolidone (PVP) provided has a weight average molecular weight, M W , of 40,000 to 60,000 Daltons;
wherein the source of copper (II) ions provided is copper (II) chloride;
wherein the source of halide ions provided is sodium chloride; and,
wherein the source of silver ions provided is silver nitrate.

10. The process of claim 1 , further comprising:
dividing the source of silver ions into a first portion and a second portion, wherein the first portion is 10 to 30 wt % of the source of silver ions provided;
heating the combination to 145 to 155° C.;
then adding the first portion to the container to form a creation mixture;
then cooling the creation mixture to 125 to 135° C. during a delay period of 5 to 15 minutes;
following the delay period, adding the second portion to the container to form the growth mixture; and,
maintaining the growth mixture at 125 to 135° C. during the hold period, wherein the hold period is 16 to 20 hours;
wherein the reducing sugar provided is D-glucose;
wherein the polyvinyl pyrrolidone (PVP) provided has a weight average molecular weight, M W , of 40,000 to 60,000 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; and,
wherein a weight ratio of polyvinyl pyrrolidone (PVP) to silver ions added to the container is 6:1 to 7:1; wherein a weight ratio of halide ions to copper (II) added to the container is 2.5:1 to 3.5:1; wherein the plurality of high aspect ratio silver nanowires recovered have an average diameter of 35 to 50 nm and an average length of 20 to 100 μm; and, wherein the plurality of high aspect ratio silver nanowires recovered have an average aspect ratio of >500.

Assignees

• Dow Global Technologies Llc

Inventors

• Wang Wei
• Mcgough Patrick T
• Goss Janet M
• Athens George L
• Lunn Jonathan D

Classifications

• B22F1/0547

  Nanofibres or nanotubes · CPC title

• B22F9/24 Primary

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

• B22F2301/255

  Silver or gold · CPC title

• B22F1/0025

  Operations & Transport · mapped topic

• Y10S977/896

  Chemical synthesis, e.g. chemical bonding or breaking · CPC title