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Preparation method of small-sized nanosilver for water-based conductive printing ink

A conductive ink, small size technology, applied in the field of preparation of small size nano-silver, can solve problems such as environmental pollution and safety hazards, and achieve the effects of friendly process environment, inhibition of agglomeration and high conductivity

Active Publication Date: 2018-08-07
UNIV OF ELECTRONICS SCI & TECH OF CHINA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Prior art CN102504646A discloses a stable nano-silver ink-jet conductive ink and a preparation method thereof. The method uses alkyl mercaptans which have a strong effect on nano-silver and alkylamines which have a weak effect together as protective agents to prepare particles Nano-silver particles with a diameter less than 10nm can obtain solvent-based inks with low post-treatment temperature and good stability; but this technology uses toluene, phenylhydrazine toluene, methanol, cyclohexane, alkane as a solvent, there are huge safety hazards and environmental pollution problems

Method used

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  • Preparation method of small-sized nanosilver for water-based conductive printing ink
  • Preparation method of small-sized nanosilver for water-based conductive printing ink
  • Preparation method of small-sized nanosilver for water-based conductive printing ink

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preparation example Construction

[0024] A method for preparing small-size nano silver used in water-based conductive ink includes the following steps:

[0025] Step 1. Add the nucleation promoting stabilizer A, the water-soluble organic protective agent B and the reducing agent to deionized water in sequence, stir and mix uniformly, to obtain the mixed solution A; among them, the nucleation promoting stabilizer A in the mixed solution A The concentration is 0.1-0.6 mol / L, the concentration of the water-soluble organic protective agent B is 0.5-1.0 mol / L, the concentration of the reducing agent is 5-10 mol / L, and the stirring speed is 400-800 rpm;

[0026] Step 2. Prepare a water-soluble silver salt solution with a concentration of 5-12 mol / L, and add it to the mixed solution A obtained in step 1 at a rate of 15-25 drops / min, stir and mix uniformly to obtain mixed solution B; The molar ratio of the silver salt in solution B to the reducing agent in step 1 is 1: (3-7);

[0027] Step 3. The mixture B obtained in step ...

Embodiment 1

[0034] Add 4.3g of trisodium citrate, 3g of polyacrylic acid, and 25g of ethanolamine to 50mL of deionized water in turn, and magnetically stir at 600rpm for 30min at room temperature to obtain mixture A; add 20 drops / min to the above mixture A Add 10mL 10mol / L silver nitrate solution dropwise, magnetically stir for 10min to obtain mixed solution B; the obtained mixed solution B is reacted for 30min under the condition of 30℃ water bath, then the temperature is raised to 45℃ at 1.0℃ / min, and the water bath reacts for 10min , Then heat up to 65°C at a heating rate of 1.0°C / min, and react in a water bath for 30 minutes to obtain a gray-green solution; add 250ml of absolute ethanol to the reacted solution system. During the addition, keep the magnetic stirring and then stand still. The nano-metal silver particles in the solution settled after standing, and the precipitated solids were collected; the collected precipitated solids were washed in a mixture of deionized water and absol...

Embodiment 2

[0040] Add 3.2g of chitosan, 5.8g of polyglutamic acid, and 30g of diethanolamine to 50mL of deionized water in turn, and magnetically stir at 600rpm for 25min at room temperature to obtain mixed solution A; mix to the above at a speed of 20 drops / min Add 10mL of 8mol / L silver nitrate solution dropwise to solution A, and magnetically stir for 10 minutes to obtain mixed solution B; the obtained mixed solution B is reacted for 20 minutes in a water bath at 30°C, and then heated to 40°C at a heating rate of 1.0°C / min , The water bath reacts for 10 minutes, and then the temperature is increased to 70°C at a heating rate of 1.0°C / min, and the water bath reacts for 40 minutes to obtain a gray-green solution; 400ml of absolute ethanol is added to the reacted solution system. During the addition, keep magnetic stirring. Then stand still, the nano-metal silver particles in the solution all settle after standing, and the precipitated solids are collected; the collected precipitated solids...

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Abstract

The invention provides a preparation method of small-sized nanosilver for water-based conductive printing ink, and relates to the technical field of preparation of nanosilver. According to the preparation method provided by the invention, one of trisodium citrate, tripotassium citrate, carboxymethyl cellulose, sodium dodecyl sulfate and chitosan is added as a nucleation promoting stabilizer A, andone of polyglutamic acid, polyacrylic acid, polymethylacrylic acid, polyoxypropylene and polyacrylamide is added as a water-soluble organic protective agent B, so that caking of the nanosilver can beeffectively inhibited; nanosilver particles prepared through the preparation method are small in size and uniform in distribution, and the caking cannot be caused after long-term storage; the contentof an organic cladding agent on the surfaces of the nanosilver particles is less, and high conductivity can be realized; during preparation of the water-based conductive printing ink, the nanosilvercan be quickly and fully dispersed in a waterborne solvent, has excellent dispersity and can be applied to the technical field of ink jet printing.

Description

Technical field [0001] The invention belongs to the technical field of nano metal material preparation, and specifically relates to a method for preparing small-size nano silver used in water-based conductive inks. Background technique [0002] In recent years, the increasing complexity of silicon-based integrated circuit manufacturing technology and the huge investment required have promoted the use of traditional printing technology to manufacture various electronic devices and systems. As the basis and key of using printing technology to manufacture electronic devices, conductive ink has attracted much attention in its research and preparation. Conductive inks are mainly divided into gold-based conductive inks, silver-based conductive inks, copper-based conductive inks, and carbon-based conductive inks. Compared with gold, silver is inexpensive and has excellent conductivity compared to copper and carbon. Based on the consideration of conductivity and production cost of condu...

Claims

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Application Information

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IPC IPC(8): B22F9/24B82Y40/00C09D11/52
CPCB22F9/24B82Y40/00C09D11/52
Inventor 陈金菊刘书丽冯哲圣王焱王小明
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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