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Conductive nano-copper ink and preparation method thereof

A technology of conductive nanometer and ink, applied in the directions of ink, household appliances, application, etc., can solve the problems such as no disclosure of the preparation method of conductive nanometer copper ink, large size of copper nanoparticles, unfavorable large-scale production, etc. Small size and low cost effect

Active Publication Date: 2016-07-13
SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In these methods, some need nitrogen protection, such as Chinese patent 20111036732.7 discloses a method for preparing an aqueous phase of copper nanoparticles with a particle size less than 30nm, but this method needs to be fed with nitrogen; some post-processing is complicated, such as Chinese patent 200810201967.0 discloses A preparation method of 20-50nm copper nanoparticles. This method not only has a high reaction temperature (120-160°C), but also requires post-treatment by means of electrodialysis and vacuum distillation. The process is complex and the preparation cycle is long; some use is expensive , a more toxic reducing agent, such as Chinese patent 2013105007585.1 discloses a preparation method that can mass produce copper conductive ink with a particle size of 40-100nm, but the reducing agent used in the method is borohydride, sodium hypophosphite and hydrazine hydrate, these reducing agents are easy to introduce impurities or have high toxicity during the reaction, which is not conducive to large-scale production
Chinese patent 201310252843.6 discloses a method for preparing conductive ink nano-copper. Although the method uses the green reducing agent L-ascorbic acid, the size of the obtained copper nanoparticles is relatively large, which is 100-200nm
[0005] At present, there is no disclosed preparation method of conductive nano-copper ink with a particle size of less than 100nm, which can be simple in process, does not require nitrogen protection, is green and pollution-free, and is suitable for mass production

Method used

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  • Conductive nano-copper ink and preparation method thereof
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  • Conductive nano-copper ink and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0048] (1) Dissolve 0.05mol of copper sulfate in 100ml of deionized water, slowly add 30ml, 0.1mol of ammonia water dropwise under normal temperature stirring conditions, until the formed light blue precipitate just dissolves, then add 50ml, 0.1mol of ammonia water to it Sodium hydroxide solution produces blue copper hydroxide precipitate;

[0049] (2) Precipitate the synthesized blue copper hydroxide, filter it with suction, and wash it three times with deionized water to obtain freshly prepared copper hydroxide;

[0050](3) Add 0.3g of freshly prepared copper hydroxide and 1.9g of polyvinylpyrrolidone K-30 into 30ml of absolute ethanol, and stir for 15min at room temperature;

[0051] (4) After stirring the mixed solution evenly, heat it to 60°C. After the reaction temperature stabilizes within 5 minutes, immediately add a reducing agent 1.625gL-ascorbic acid to the reaction system within 30s~60s, and react for 5 minutes to obtain copper nanoparticles Dispersions;

[0052]...

Embodiment 2

[0056] (1) Dissolve 0.05mol of copper chloride in 100ml of deionized water, and slowly add 30ml of 0.1mol of ammonia water dropwise under stirring at room temperature until the resulting light blue precipitate just dissolves, then add 50ml of 0.15mol to it Sodium hydroxide solution produces blue copper hydroxide precipitate;

[0057] (2) Precipitate the synthesized blue copper hydroxide, filter it with suction, and wash it with ethanol for 3 times to obtain freshly prepared copper hydroxide;

[0058] (3) Add 0.588g of newly prepared copper hydroxide and 2.94g of polyvinylpyrrolidone K-90 into 30ml of deionized water respectively, and stir for 10min at room temperature;

[0059] (4) After stirring the mixed solution evenly, heat it to 100°C. After the reaction temperature stabilizes within 10 minutes, immediately add a reducing agent 5.284g L-ascorbic acid to the reaction system within 30s~60s, and react for 30 minutes to obtain copper nanoparticles Dispersions;

[0060] (5) ...

Embodiment 3

[0063] (1) Dissolve 0.05mol of copper nitrate in 100ml of deionized water, and slowly add 30ml of 0.1mol of ammonia water dropwise under normal temperature stirring conditions until the formed light blue precipitate just dissolves, then add 50ml of 0.125mol of Sodium hydroxide solution produces blue copper hydroxide precipitate;

[0064] (2) Precipitate the synthesized blue copper hydroxide, filter it with suction, and wash twice with deionized water and ethanol respectively to obtain freshly prepared copper hydroxide;

[0065] (3) Add 0.513g of newly prepared copper hydroxide and 2.93g of polyvinylpyrrolidone K-30 into 40ml of ethylene glycol methyl ether, and stir for 10min at room temperature;

[0066] (4) After stirring the mixed solution evenly, heat it to 120°C. After the reaction temperature stabilizes within 15 minutes, immediately add a reducing agent 2.156g L-ascorbic acid into the reaction system for 30s~60s, and react for 40 minutes to obtain dispersed copper nanop...

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Abstract

The invention discloses a conductive nano-copper ink and a preparation method thereof. The preparation method comprises the following steps: mixing and reacting freshly prepared copper hydroxide with a protection agent in a first solvent, and adding L-ascorbic acid to obtain a copper nano-particle dispersion; and separating copper nano-particles from the copper nano-particle dispersion, washing the obtained copper nano-particles, and adding a second solvent to obtain the conductive nano-copper ink. The preparation method of the conductive nano-copper ink has the advantages of simple operation, high purity, low cost, high yield, environmental protection, and suitableness for large scale production.

Description

technical field [0001] The invention belongs to the preparation technology of conductive ink, and in particular relates to a preparation method of conductive nano-copper ink using copper nanoparticles as conductive raw materials. Background technique [0002] In recent years, a new type of manufacturing technology—printed electronics manufacturing process—is emerging all over the world. The so-called printed electronics manufacturing process is the technology of using electronic materials with conductive, dielectric or semiconductor properties to print electronic devices or circuit systems. This technology is flexible, fast, convenient, environmentally friendly and energy-saving, so it has attracted widespread attention. The key to the rapid development of this technology is the printable electronic material, here called "conductive ink". [0003] Conductive ink can be divided into inorganic conductive ink, organic conductive ink and composite conductive ink according to t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09D11/52B22F9/20
Inventor 邵霜霜陈征崔铮
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI