Low oxygen silver nanowire manufacturing method

Patent metadata

Field	Value
Publication number	US-9969005-B2
Application number	US-201514881955-A
Country	US
Kind code	B2
Filing date	Oct 13, 2015
Priority date	Oct 28, 2014
Publication date	May 15, 2018
Grant date	May 15, 2018

Abstract

A process for manufacturing high aspect ration silver nanowires is provided, 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;
sparging the source of silver ions with an inert gas to extract entrained oxygen gas from the source of silver ions and to provide a low oxygen gas concentration in a silver ion vapor space in contact with the source of silver ions, wherein the low oxygen gas concentration in the silver ion vapor space is less than or equal to 10,000 ppm;
adding the water, the reducing sugar, the polyvinyl pyrrolidone (PVP), the source of copper (II) ions and the source of halide ions to the container to form a combination;
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 2,000 ppm;
then heating the combination to 110 to 160° C.;
then adding the source of silver ions to the container to form a growth mixture, while maintaining the reduced oxygen gas concentration in the container vapor space and the low oxygen gas concentration in the silver ion vapor space;
maintaining the growth mixture at 100 to 150° C. and the reduced oxygen gas concentration in the container vapor space 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 %.

2. The process of claim 1 ,
wherein the source of silver ions is divided into a first portion and a second portion, while maintaining the low oxygen gas concentration in the silver ion vapor space;
wherein the first portion is added to the container to form a creation mixture, while maintaining the reduced oxygen gas concentration in the container vapor space and the low oxygen gas concentration in the silver ion vapor space;
wherein the creation mixture is then cooled to 100 to 150° C. during a delay period; and,
wherein, following the delay period, the second portion is added to the container to form the growth mixture, while maintaining the reduced oxygen gas concentration in the container vapor space and the low oxygen gas concentration in the silver ion vapor space;
wherein the reduced oxygen gas concentration in the container vapor space is ≤2,000 ppm.

3. The process of claim 2 , wherein the reducing sugar provided is glucose.

4. The process of claim 2 , wherein the polyvinyl pyrrolidone (PVP) provided has a weight average molecular weight, Mw, of 40,000 to 150,000 Daltons.

5. The process of claim 2 , wherein the source of copper (II) ions provided is copper (II) chloride.

6. The process of claim 2 , wherein the source of halide ions provided is sodium chloride.

7. The process of claim 2 , wherein the source of silver ions provided is silver nitrate.

8. The process of claim 2 ,
wherein the combination is heated to 140 to 155° C.;
wherein the creation mixture is cooled to 110 to 140° C. during the delay period;
wherein the growth mixture is maintained at 110 to 140° C. during the hold period;
wherein the reducing sugar provided is glucose;
wherein the polyvinyl pyrrolidone (PVP) provided has a weight average molecular weight, Mw, 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.

9. The process of claim 8 ,
wherein the first portion is 10 to 30 wt % of the source of silver ions provided;
wherein the combination is heated to 145 to 155° C. before adding the source of silver ions to the container;
wherein the creation mixture is cooled to 125 to 135° C. during the delay period, wherein the delay period is 5 to 15 minutes;
wherein the growth mixture is maintained at 125 to 135° C. during the hold period, wherein the hold period is 16 to 20 hours;
wherein the reduced oxygen gas concentration in the container vapor space is ≤400 ppm;
wherein the low oxygen gas concentration in the silver ion vapor space is ≤1,000 ppm; and,
wherein the plurality of high aspect ratio silver nanowires recovered have an average diameter of ≤40 nm with a diameter standard deviation of ≤26 nm and an average aspect ratio of >500.

Assignees

• Dow Global Technologies Llc

Inventors

• Mcgough Patrick T
• Athens George L

Classifications

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title

• B22F9/24 Primary

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

• B22F2201/03

  Oxygen · CPC title

• B22F2301/255

  Silver or gold · CPC title

• B22F2304/05

  Submicron size particles · CPC title