Method for preparing ultrathin silver nanowires, and transparent conductive electrode film product thereof

Patent metadata

Field	Value
Publication number	US-9908178-B2
Application number	US-201414525334-A
Country	US
Kind code	B2
Filing date	Oct 28, 2014
Priority date	Oct 28, 2014
Publication date	Mar 6, 2018
Grant date	Mar 6, 2018

Abstract

Disclosed herein is a method for preparing ultrathin silver nanowires. It may comprise (a) dissolving a silver salt (Ag salt) and a capping agent in a reducing solvent to give a mixture solution; (b) adding a halide compound to the mixture solution to yield a silver seed; (c) heating the mixture solution and then allowing the heated mixture solution to grow ultrathin silver nanowires from the silver seed under a pressure in an inert gas atmosphere; and (d) cooling the mixture solution in which the ultrathin silver nanowires have grown, followed by purification and separation to obtain the ultrathin silver nanowires. The silver nanowires are restrained from growing in thickness under a certain pressure, so that they are 30 nm or less in thickness and have a narrow diameter distribution, which leads to an improvement in aspect ratio.

First claim

What is claimed is:

1. A method for preparing ultrathin silver nanowires, comprising performing the following steps in sequential order:
(a) dissolving a silver salt and a capping agent in a reducing solvent to give a mixture solution;
(b) adding a halide compound to the mixture solution to yield a silver seed;
(c) heating the mixture solution and then allowing the heated mixture solution to grow ultrathin silver nanowires from the silver seed under a pressure in an inert gas atmosphere, wherein the pressure is between 50 and 500 psi; and
(d) cooling the mixture solution in which the ultrathin silver nanowires have grown, followed by purification and separation to obtain the ultrathin silver nanowires.

2. A method for preparing ultrathin silver nanowires, comprising:
1) dissolving a magnetic ionic liquid containing tetrachloroferrate, and a capping agent in a reducing solvent to give a mixture solution;
2) adding a silver salt to the mixture solution to yield a silver seed;
3) heating the mixture solution and then allowing the heated mixture solution to grow ultrathin silver nanowires from the silver seed under a pressure in an inert gas atmosphere, wherein the pressure is between 100 and 1500 psi; and
4) cooling the mixture solution in which the ultrathin silver nanowires have grown, followed by purification and separation to obtain the ultrathin silver nanowires.

3. The method of claim 1 , wherein the silver salt is silver nitrate, silver acetate, or silver perchlorate.

4. The method of claim 1 , wherein the capping agent is selected from the group consisting of polyvinylpyrrolidone (PVP), polyvinylalcohol (PVA), cetyltrimethylammoniumbromide (CTAB), cetyltrimethylammoniumchloride (CTAC), polyacrylamide (PAA), and a combination thereof.

5. The method of claim 1 , wherein the capping agent is used in an amount of 1.50 to 3.50 mol per mole of the silver salt.

6. The method of claim 1 , wherein the reducing solvent is polyol.

7. The method of claim 6 , wherein the reducing solvent is selected from the group consisting of ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, glycerin, glucose, and a combination thereof.

8. The method of claim 2 , wherein the magnetic ionic liquid containing tetrachloroferrate further comprises a halide compound different from tetrachloroferrate.

9. The method of claim 1 , wherein the halide compound is a metal halide selected from the group consisting of sodium chloride (NaCl), potassium bromide (KBr), potassium iodide (KI), iron trichloride (FeCl 3 ), platinum trichloride (PtCl 3 ), gold trichloride (AuCl 3 ), and a combination thereof.

10. The method of claim 1 , wherein the halide compound is an organic halide selected from the group consisting of tetrabutylammonium chloride, tetrahexyl ammonium chloride, tetrapropylammonium chloride, tetrabutylammonium bromide, tetrahexyl ammonium bromide, tetrapropylammonium bromide, tetrabutylphosphoniumbromide, and a combination thereof.

11. The method of claim 1 , wherein the ultrathin silver nanowires obtained in step (d) have a diameter of 30 nm or less and an aspect ratio of 300 or higher.

12. The method of claim 2 , wherein the ultrathin silver nanowires obtained in step 4) have a diameter of 30 nm or less and an aspect ratio of 500 or higher.

13. The method of claim 2 , wherein the magnetic ionic liquid containing tetrachloroferrate is composed of a compound represented by the following Chemical Formula 1, with tetrachloroferrate (FeCl 4 ) as an anionic ion:

wherein R is hydrogen, an alkyl group of 1 to 15 carbon atoms, or an aromatic group.

14. The method of claim 13 , wherein the magnetic ionic liquid of Chemical Formula 1 is composed of at least one compound selected from the group consisting of 1-butyl-3-methyl-imidazolinium tetrachloroferrate, 1-ethyl-3-methyl-imidazolinium tetrachloroferrate, and 1-propyl-3-methyl-imidazolinium tetrachloroferrate.

15. The method of claim 2 , wherein the magnetic ionic liquid is used in an amount of 0.05 to 0.30 mol per mole of the silver salt.

16. The method of claim 1 , further comprising dispersing or hybridizing the ultrathin silver nanowires with a one-dimensional polymer conductor to form a two-dimensional film consisting of the ultrathin silver nanowires and one-dimensional polymer conductor hybrid, wherein the one-dimensional polymer conductor is a conductive polythiol derivative, and is contained in an amount of at least 10 weight % in the transparent, conductive electrode film, and the transparent, conductive electrode film has a light transmittance of 80 to 98%, and a surface resistance of 5 ohm/□to 150 ohm/□.

Assignees

• Univ Kookmin Ind Acad Coop Found

Inventors

• Kim Jin Yeol
• Lee Eun Jong
• Chang Min Hwa
• Cho Hyun Ah
• Kim Youn Soo

Classifications

• B22F1/0547 Primary

  Nanofibres or nanotubes · CPC title

• B22F1/054

  Nanosized particles · CPC title

• B22F9/20 Primary

  starting from solid metal compounds · CPC title

• B22F1/0025

  Operations & Transport · mapped topic

• B22F2009/245

  Reduction reaction in an Ionic Liquid [IL] · CPC title