Hydrothermal method for manufacturing filtered silver nanowires

Patent metadata

Field	Value
Publication number	US-10081020-B2
Application number	US-201615158297-A
Country	US
Kind code	B2
Filing date	May 18, 2016
Priority date	Jun 12, 2015
Publication date	Sep 25, 2018
Grant date	Sep 25, 2018

Abstract

A method for manufacturing filtered high aspect ratio silver nanowires is provided, wherein a total glycol concentration is <0.001 wt % at all times.

First claim

We claim:

1. A method for manufacturing filtered high aspect ratio silver nanowires, comprising:
providing a container;
providing an initial volume of water;
providing an initial reducing sugar;
providing an initial polyvinyl pyrrolidone (PVP), wherein the initial polyvinyl pyrrolidone (PVP) provided is dividable into a first part of the initial polyvinyl pyrrolidone (PVP) and a second part of the initial polyvinyl pyrrolidone (PVP);
providing an initial source of copper (II) ions;
providing an initial source of halide ions;
providing an initial source of silver ions, wherein the initial source of silver ions provided is dividable into a first portion of the initial source of silver ions and a second portion of the initial source of silver ions;
adding the initial volume of water, the initial reducing sugar, the initial source of copper (II) ions and the initial source of halide ions to the container to form a combination;
heating the combination to 110 to 160° C.;
comingling the first part of the initial polyvinyl pyrrolidone (PVP) with the first portion of the initial source of silver ions to form a comingled polyvinyl pyrrolidone/source of silver ions;
adding the comingled polyvinyl pyrrolidone/source of silver ions to the combination in the container to form a creation mixture; then, following a delay period, adding to the container the second part of the initial polyvinyl pyrrolidone (PVP) and the second portion of the initial 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 produce a raw feed wherein a total glycol concentration in the container is <0.001 wt %; wherein the raw feed produced comprise a mother liquor and silver solids; wherein the mother liquor comprises the initial volume of water; and wherein the silver solids in the raw feed include high aspect ratio silver nanowires and low aspect ratio silver particles;
providing a dynamic filtration device, wherein the dynamic filtration device, comprises:
a housing, comprising: a cavity having a first side and a second side;
wherein there is at least one inlet to the first side of the cavity, at least one product outlet from the first side of the cavity and at least one permeate outlet from the second side of the cavity; and,
a porous element disposed within the cavity;
a turbulence inducing element disposed within the cavity; and,
a pressure source;
wherein the porous element is interposed between the first side of the cavity and the second side of the cavity; wherein the porous element has a plurality of passages that traverse from the first side of the cavity to the second side of the cavity; wherein the plurality of passages are large enough to permit transfer of the mother liquor and low aspect ratio silver particles and small enough to block transfer of the high aspect ratio silver nanowires;
wherein the porous element and the turbulence inducing element cooperate to form a filtration gap, FG; and,
wherein at least one of the porous element and the turbulence inducing element is moveable;

providing a transport fluid, wherein the transport fluid comprises a supplemental volume of water and a supplemental polyvinyl pyrrolidone (PVP);
transferring the raw feed to the dynamic filtration device through the at least one inlet to the first side of the cavity;
transferring a volume of the transport fluid to the dynamic filtration device through the at least one inlet to the first side of the cavity;
wherein the filtration gap, FG, is filled by water; wherein the porous element and the turbulence inducing element disposed within the cavity are both in contact with the water;
pressurizing the first side of the cavity using the pressure source resulting in a first side pressure, FS P , in the first side of the cavity; wherein the first side pressure, FS P , is higher than a second side pressure, SS P , in the second side of the cavity, whereby there is created a pressure drop (PE Δ ) across the porous element from the first side of the cavity to the second side of the cavity; wherein the pressure source provides a primary motive force for inducing a flow from the first side of the cavity through the porous element to the second side of the cavity providing a permeate;
moving at least one of the porous element and the turbulence inducing element whereby a shear stress is generated in the water in the filtration gap, FG; wherein the shear stress generated in the water in the filtration gap, FG, operates to reduce fouling of the porous element;
withdrawing the permeate from the at least one permeate outlet from the second side of the cavity, wherein the permeate comprises a second cut of the mother liquor and a second fraction of the silver solids; wherein the second fraction of the silver solids is rich in low aspect ratio silver particles; and,
withdrawing a product from the at least one product outlet from the first side of the cavity, wherein the product comprises a first cut of the mother liquor and a first fraction of the silver solids; wherein the first fraction of the silver solids is depleted in low aspect ratio silver particles; and,
wherein the shear stress generated in the water in the filtration gap, FG, and the pressure drop (PE Δ ) across the porous element from the first side of the cavity to the second side of the cavity are decoupled.

2. The method of claim 1 , wherein the transport fluid further comprises:
a supplemental source of halide ions.

3. The method of claim 2 , wherein the transport fluid further comprises:
a supplemental reducing sugar.

4. The method of claim 1 , further comprising:
removing the silver solids from the permeate to provide a cleaned permeate; and,
recycling the cleaned permeate to the dynamic filtration device through the at least one inlet to the first side of the cavity.

5. The method of claim 4 , wherein the silver solids are removed from the permeate using centrifugation to provide the cleaned permeate.

6. The method of claim 4 , wherein the transport fluid comprises the cleaned permeate.

7. The method of claim 1 , wherein the first part of the initial polyvinyl pyrrolidone (PVP) is 10 to 40 wt % of the initial polyvinyl pyrrolidone (PVP) provided; and, wherein the first portion of the initial source of silver ions is 10 to 40 wt % of the initial source of silver ions provided.

8. The method of claim 7 , further comprising:
providing a pH adjusting agent;
adding the pH adjusting agent to the combination before adding the comingled polyvinyl pyrrolidone/source of silver ions; wherein the combination has a pH of 2.0 to 4.0 before adding the comingled polyvinyl pyrrolidone/source of silver ions to the container.

9. The method of claim 7 , further comprising:
providing a reducing agent;
adding the reducing agent to the creation mixture.

10. 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;
sparging the initial source of silver ions provided with an inert gas to extract entrained oxygen gas from the initial source of silver ions provided and to provide a low oxygen gas concentration in a silver ion vapor space in contact with the initial 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 initial 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;

Assignees

• Dow Global Technologies Llc

Inventors

• Athens George L
• Collins Raymond M
• Bauer William R
• Mcgough Patrick T
• Goss Janet M
• Frycek George J
• Wang Wei
• Lunn Jonathan D
• Ziebarth Robin P
• Patyk Richard A

Classifications

• B22F1/0547 Primary

  Nanofibres or nanotubes · CPC title

• B22F9/24 Primary

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

• B03B5/66 Primary

  of the hindered settling type · 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

• B22F3/003

  Apparatus, e.g. furnaces (in general F27B) · CPC title