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Preparation method of nano-silver particle coated by novel macromolecule protective agent

A technology of polymer protective agent and nano-silver particles, which is applied in ink, household utensils, applications, etc., can solve the problems of dissolution and shedding, inability to improve comprehensive performance of resin, and inability to play the role of resin, etc.

Active Publication Date: 2015-12-02
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 particle coated by novel macromolecule protective agent

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preparation example Construction

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

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

[0020] b) Add the silver ammonia solution and the reducing agent solution to the above acrylic resin solution in equal volumes at a speed of 5-50ml / min; the "silver ammonia solution" here is: the silver nitrate aqueous solution is added to the ammonia Mixed solution, in which 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 perform high-speed stirring at a speed of 500~800r / min, and monitor the pH value of the above-mentioned mixed solution i...

Embodiment 1

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

Embodiment 2

[0025] Measure 100ml of 650g / L silver nitrate solution, gradually add 35% ammonia water under stirring, and record the volume V2 at this time when the mixture becomes transparent again. Weigh 12g of sodium borohydride, add water to dissolve to volume V2. Potassium hydroxide was added to 500ml of deionized water to adjust pH=10, 12g of solid acrylic resin with a molecular weight of 65000 was added, and the mixture was stirred and dissolved at 25°C. The silver ammonia solution and the hydrazine hydrate solution were dripped into the protective solution at 35 ml / min through a peristaltic pump, and the stirring speed was 600 r / min. During the reaction, the pH was monitored immediately, and 4% potassium hydroxide solution was added to adjust the pH ≥ 8. After the feeding, continue to stir until the liquid returns to room temperature to obtain nano silver particles.

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Abstract

A preparation method of a nano-silver particle coated by a novel macromolecule protective agent belongs to the technical field of manufacture of printing electronic materials. The steps comprise that a) a solution of the macromolecule protective agent with a certain temperature, a certain concentration and a certain pH value is prepared; b) a silver ammonia solution and a reductant solution are added into the macromolecule protective agent solution; c) the mixed solution is stirred, the pH value of the mixed solution is monitored in a real time, and the pH value of the mixed solution is kept to exceed 7 by adding a pH modifier; and the nano-silver particle can be prepared through a chemical reaction. In comparison with the prior art, the preparation method of the nano-silver particle coated by the novel macromolecule protective agent provided by the invention has the beneficial effect that acrylic-based resin with a multi-carbonyl structure is taken as the protective agent for the nano-silver preparation in an alkaline environment, wherein no research report has been proposed domestically; and because of outstanding aging resistance (such as the resistance to corrosion of acids, weak alkalis and salts) and adhesive force of the acrylic-based resin, the prepared nano-silver particle can guarantee requirements in applications for the adhesive force and the aging resistance without addition of other types of resin.

Description

Technical field [0001] The invention belongs to the technical field of printed electronic material manufacturing, and specifically 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 inks have received great attention as upstream raw materials with excellent performance. Compared with other conductive materials, nano-silver has the advantages of strong oxidation resistance, high conductivity, and mature preparation technology. It has become the main force in the industrialization of printed electronic conductive materials. [0003] As printed electronic products belong to the electronics industry, the requirements for conductive circuits printed with nano-silver are extremely high. Under normal circumstances, conductive lines need to have strong adhesion, high conductivity, good flexibility, and ...

Claims

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Application Information

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Patent Type & Authority Applications(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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