Method of making silver-containing dispersions with nitrogenous bases

a technology of nitrogenous bases and nanoparticles, which is applied in the field of forming a silver nanoparticle composite, can solve the problems of incompatible ink with many polymeric and paper substrates, time-consuming and expensive photolithographic and electroless techniques, and inability to microfabricate electrically-conductive tracks (grids, wires, patterns) , to achieve the effect of reducing the cost of manufacturing and manufacturing

Active Publication Date: 2019-03-28
EASTMAN KODAK CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

While silver as an electrical conductor has a wide range of potential uses in the field of printed electronics, the microfabrication of electrically-conductive tracks (grids, wires, or patterns) by photolithographic and electroless techniques is time consuming and expensive, and there is an industrial need for direct digital printing to simplify the processes and to reduce manufacturing costs.
Unfortunately, even these temperatures render the ink incompatible with many polymeric and paper substrates used in flexible electronic and biomedical devices.
However, these methods require that high quantities of purchased silver particles be uniformly dispersed within the photocurable compositions so that coatings or printed patterns have a sufficiently high concentration of catalytic sites.
Scaling such curing procedures to high volume use can be difficult and hard to reproduce on a consistent scale, especially to produce fine line electrically-conductive meshes or grids where

Method used

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  • Method of making silver-containing dispersions with nitrogenous bases
  • Method of making silver-containing dispersions with nitrogenous bases
  • Method of making silver-containing dispersions with nitrogenous bases

Examples

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invention example 1

Aqueous Dispersion Containing Silver Nanoparticle-Cellulose Acetate Composite Using 2-Butyl Aminoethanol as the Nitrogenous Base

[0229]In a 2-necked round bottomed flask a mixture of cellulose acetate (0.375 g; Aldrich, mol.wt. of 50,000, acetyl content of 39%) and 2-butyl aminoethanol (0.9 g) in 2-methoxyethanol (8 ml) was heated at 95° C. with stirring until all cellulose acetate was dissolved to form a premix solution. A solution of silver nitrate (5 g) dissolved in 2-methoxyethanol (15 ml) was slowly added to form a reaction mixture over a period of 20 minutes. During this addition, the reaction mixture became dark grey in color. It was stirred at 95° C. for another 30 minutes, cooled, and poured into methanol (500 ml). The resulting precipitate (silver nanoparticle-cellulose acetate composite) was filtered and washed with methanol to yield a gray solid (yield 98% based on theoretical silver).

[0230]Particle size distribution was measured using a dynamic light scattering method (M...

invention example 2

Aqueous Dispersion Containing Silver Nanoparticle-Cellulose Acetate Propionate Composite Using 2-Methyl Aminoethanol as the Nitrogenous Base

[0233]In a 2-necked round bottomed flask. a mixture of cellulose acetate propionate (0.18 g; Eastman CAP 482-0.5, propionyl content 43%, Acetyl content 0.6%, mol. wt. of 25,000) and 2-methyl aminoethanol (1.5 g, mmol) in 2-methoxyethanol (7 ml) was heated at 95° C. with stirring until all cellulose acetate propionate was dissolved to form a premix solution. A solution of silver nitrate (5 g) dissolved in 2-methoxyethanol (15 ml) was added to the premix solution over a period of 35 minutes. The resulting reaction mixture was stirred at 95° C. for another 45 minutes, cooled, and poured into water (400 ml). The resulting precipitate was filtered and washed with methanol. A grey colored solid was obtained (yield of 97% based on silver). Particle size distribution was measured using a dynamic light scattering method (Malvern Instruments Ltd. Zetasize...

invention example 3

Aqueous Dispersion of Silver Nanoparticle-Cellulose Acetate Propionate Composite Using 1,8-Diazabicyclo[5.4.0]undec-7-ene as the Nitrogenous Base

[0235]In a 2-necked round bottomed flask, a mixture of cellulose acetate propionate (0.4 g; Eastman CAP 482-20, propionyl content 48%, Acetyl content 1.3%, Mol. wt. of 75,000) and 1,8-diazabicyclo[5.4.0]undec-7-ene (16 g, mmol) in 2-methoxyethanol (28 ml) was heated at 95° C. with stirring until all cellulose acetate propionate was dissolved to form a premix solution. A solution of silver nitrate (8.8 g) dissolved in 2-methoxyethanol (100 ml) was added to the premix solution over a period of 80 minutes. The resulting reaction mixture was stirred at 95° C. for another 20 minutes, cooled, and poured into water (800 ml). The resulting precipitate was filtered and washed with methanol. A grey colored solid was obtained (yield of 98% based on silver). Particle size distribution was measured a dynamic light scattering method (Malvern Instruments ...

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Abstract

A method is used to prepare silver nanoparticle cellulosic polymer composites. A cellulosic polymer, reducible silver ions in an amount of a weight ratio to the cellulosic polymer of 5:1 to 50:1, and an organic solvent are mixed. Each organic solvent has a boiling point at atmospheric pressure of 100° C. to 500° C. The Hansen parameter (δTPolymer) of the cellulosic polymer is less than or equal to the Hansen parameter (δTSolvent) of the organic solvent. The resulting premix solution is heated to at least 75° C., and a (d) nitrogenous base is added to provide a concentration of the nitrogenous base in an equimolar amount or in molar excess in relation to the amount of reducible silver ions, thereby forming a silver nanoparticle cellulosic polymer composite. After cooling, the silver nanoparticle cellulosic polymer composite is isolated and re-dispersed in an organic solvent to provide a non-aqueous silver-containing dispersion.

Description

CROSS-REFERENCE TO RELATED APPLICATIONS[0001]Reference is made to the following commonly assigned and copending patent application, the disclosures of all of which are incorporated herein by reference:[0002]U.S. Ser. No. 15 / 456,686, filed Mar. 13, 2017 by Shukla and Donovan;[0003]U.S. Ser. No. 15 / 456,827, filed Mar. 13, 2017 by Shukla, Donovan, and Gillmor;[0004]U.S. Ser. No. 15 / 456,868, filed Mar. 13, 2017 by Shukla and Donovan;[0005]U.S. Ser. No. 15 / ______ (filed on even date herewith by Shukla and Donovan) and entitled “Silver-containing Non-Aqueous Compositions Containing Cellulosic Polymers” (Attorney Docket K002183 / JLT);[0006]U.S. Ser. No. 15 / ______ (filed on even date herewith by Shukla, Donovan, and Klubek) and entitled “Method of Making Silver-containing Dispersion” (Attorney Docket K002190 / JLT); and[0007]U.S. Ser. No. 15 / ______ (filed on even date herewith by Shukla and Donovan) and entitled “Non-Aqueous Silver-containing Dispersions” (Attorney Docket K002192 / JLT).FIELD OF...

Claims

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Application Information

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IPC IPC(8): C08J3/09C08K5/16C08K3/08C08K3/04C08L1/12C01G5/00
CPCC08J3/095C08K5/16C08K3/08C08K3/04C08L1/12C01G5/006C08K2201/005C01P2004/64C01P2006/40C08L1/14C08K2003/0806C09D101/12
Inventor SHUKLA, DEEPAKDONOVAN, KEVIN
Owner EASTMAN KODAK CO
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