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Preparation method of nano-silver particles coated with a novel polymer protective agent

A technology of polymer protective agent and nano-silver particles, which is applied in the direction of ink, household utensils, applications, etc., can solve the problems of dissolution and shedding, failure to play the role of resin, and protection agent that cannot act as resin.

Active Publication Date: 2017-12-08
青岛纳印新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In some applications, the use of certain environmentally friendly solvents has almost no solubility for resins, and the overall performance cannot be improved through resins
The reason is that the protective agent used in the preparation process of nano-silver cannot act as a resin
[0004] The protective agents commonly used in the preparation of nano-silver particles are generally divided into two categories: water-based polymers, such as PVP, PEG, PVA, etc. These protective agents have good water solubility and poor adhesion to plastics, which limits their application in plastic substrates , will dissolve and fall off in contact with water, and cannot be stored in a high-humidity environment for a long time; small molecules, such as dodecylamine, dodecanoic acid, oleic acid, sodium hexametaphosphate, etc., such protective agents cannot play a role in the resin effect, basically no contribution to particle adhesion and aging resistance
To sum up, the silver nanoparticles prepared by the currently commonly used protective agents have various disadvantages that restrict their application after being printed into conductive lines.

Method used

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  • Preparation method of nano-silver particles coated with a novel polymer protective agent

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preparation example Construction

[0018] A preparation method of nano-silver particles coated with a novel polymer protective agent, the steps are as follows:

[0019] a) Prepare an acrylic resin solution with a temperature of 10-60°C, a concentration (mass percentage) of 1.15-4.20%, and a pH value of 9-12; the "acrylic resin" here is ethyl acrylate / methyl methacrylate copolymer , its molecular weight is 10000~100000;

[0020] b) Add the silver ammonia solution and the reducing agent solution to the above-mentioned acrylic resin solution dropwise at a rate of 5-50ml / min in equal volume; the "silver ammonia solution" here is obtained by adding the silver nitrate aqueous solution to ammonia water Mixed solution, wherein the content of silver nitrate is 300~1000g / L; the "reducing agent" here is: one or more aqueous solutions including hydrazine hydrate, sodium borohydride, sodium hypophosphite and ascorbic acid;

[0021] c) Use a stirrer to stir at a speed of 500~800r / min, and monitor the pH value of the above m...

Embodiment 1

[0023] Measure 100ml of 500g / L silver nitrate solution, under stirring, gradually add 35% ammonia water, until the mixture becomes transparent again, record the volume V1 at this time. Weigh 22g of hydrazine hydrate with a mass fraction of 85%, and add water to dilute to volume V1. Add sodium hydroxide to 300ml of deionized water to adjust the pH to 9, add 3.5g of solid acrylic resin with a molecular weight of 100,000, and keep stirring to dissolve at 10°C. The silver ammonia solution and hydrazine hydrate solution were added dropwise into the protection solution through a peristaltic pump at 50ml / min, and the stirring speed was 500r / min. The pH was monitored immediately during the reaction, and 3% sodium hydroxide solution was added to adjust the pH to ≥8. After the feeding is finished, the stirring is continued until the liquid returns to room temperature to obtain nano-silver particles.

Embodiment 2

[0025] Measure 100ml of 650g / L silver nitrate solution, under stirring, gradually add 35% ammonia water, until the mixture becomes transparent again, record the volume V2 at this time. Weigh 12g of sodium borohydride, add water to dissolve to volume V2. Add potassium hydroxide to 500ml of deionized water to adjust the pH to 10, add 12g of solid acrylic resin with a molecular weight of 65,000, and keep stirring at 25°C to dissolve. The silver ammonia solution and the hydrazine hydrate solution were added dropwise into the protection solution through a peristaltic pump at 35ml / min, and the stirring speed was 600r / min. The pH was monitored immediately during the reaction, and 4% potassium hydroxide solution was added to adjust the pH to ≥8. After the feeding is finished, the stirring is continued until the liquid returns to room temperature to obtain nano-silver particles.

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Abstract

The invention discloses a method for preparing nano-silver particles coated with a novel polymer protective agent, which belongs to the technical field of printing electronic materials. The steps are: a) preparing a polymer protective agent solution with a certain temperature, concentration and pH value; b) adding the silver ammonia solution and reducing agent solution dropwise to the above polymer protective agent solution; c) stirring and monitoring in real time The pH value of the above-mentioned mixed solution is kept greater than 7 by adding a pH regulator; the nano-silver particles can be prepared through chemical reaction. Compared with the prior art, the beneficial effect of the present invention is: the acrylic resin with polycarbonyl structure is used as a protective agent prepared by nano-silver in an alkaline environment, and there is no domestic research report on this aspect; since the acrylic resin itself has outstanding Aging resistance (strong corrosion resistance to acids, weak bases, and salts) and adhesion, so that the prepared nano-silver particles can meet the requirements for adhesion and aging resistance in applications without adding other resins.

Description

technical field [0001] The invention belongs to the technical field of printing electronic materials, and in particular relates to a method for preparing nano-silver particles coated with a novel polymer protective agent. Background technique [0002] With the extensive development of printed electronics technology at home and abroad, nano-silver conductive ink has received high attention as an upstream raw material with excellent performance. Compared with other conductive materials, nano-silver has the advantages of strong oxidation resistance, high conductivity, and mature preparation technology, and has become the main force in the industrialization of printed electronic conductive materials. [0003] Since printed electronic products belong to the electronics industry, the requirements for conductive lines printed with nano-silver are extremely high. Under normal circumstances, conductive lines need to have strong adhesion, high conductivity, good flexibility, and resi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24B22F1/02C09D11/52
Inventor 胡旭伟朱磊
Owner 青岛纳印新材料科技有限公司
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