A kind of preparation method of conductive ink nano copper

A technology of conductive ink and nano-copper, which is applied in the direction of ink, nanotechnology, household appliances, etc., can solve the problems of high raw material ratio and purity requirements, low reaction temperature, narrow particle size distribution, etc., and it is easy to achieve particle size and shape Control and reaction conditions are simple and mild, and the effect of high monodispersity

Active Publication Date: 2015-10-28
SHENZHEN INST OF ADVANCED TECH
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  • Application Information

AI Technical Summary

Problems solved by technology

The reaction temperature of the sol-gel method is low, the product particles are small, the particle size distribution is narrow and the purity is high, but the cost is high and it is accompanied by pollution; the particles obtained by the hydrothermal reduction method are high in purity, the particle size distribution is narrow, and the lattice growth is complete and pollution-free. However, the ratio and purity of raw materials are high, and it is not suitable for large-scale production; the preparation process of the electrolysis method is relatively simple, but the post-treatment process is relatively cumbersome; the reaction temperature of the plasma method is high, the reaction speed is fast, the operation is simple and the production speed is fast. , but consumes a lot of energy; compared with other methods, the thermal decomposition method is faster, economical and green, but it is not easy to control the particle size and shape of copper particles
The chemical reduction method can obtain nano-copper particles with different particle sizes and shapes by optimizing the process. The reducing agents used are generally sodium borohydride, formaldehyde, hydrazine hydrate or sodium hypophosphite. These reducing agents are expensive and most of them have Greater toxicity, not conducive to large-scale production
[0004] Patent 200510094614.1 discloses a method for preparing nano-copper. In this method, the reducing agent L-ascorbic acid and the compounded modifier are dissolved in water, and the copper source solution is added dropwise after heating to reflux for several hours, and then the reflux reaction is continued to obtain nano-copper. The reaction conditions are mild, but repeated reflux heating is required, and the operation is complicated and cumbersome
Patent application 200910054884.8 discloses a preparation method of nano-copper conductive ink, which is post-treated by electrodialysis and vacuum distillation, the operation process is complicated, and the preparation cycle is long
Patent 201010221315.0 discloses a method for preparing nano-copper conductive ink. Although this method does not require cumbersome post-processing, the preparation process is complicated
[0005] At present, there is no report on the preparation method of nano-copper in conductive ink that has a simple preparation process, low cost and can be applied to large-scale production.

Method used

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  • A kind of preparation method of conductive ink nano copper
  • A kind of preparation method of conductive ink nano copper
  • A kind of preparation method of conductive ink nano copper

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 0.20g of copper hydroxide to 40ml of ethanol, add 20ml of PEG-200, stir well and heat to 60°C to obtain solution a; add 3.52g of L-ascorbic acid to 40ml of ethanol, stir well and heat to 60°C to obtain solution b; add solution b to solution a, continue to stir for 5 minutes, then cool to room temperature, centrifuge and wash 4 times with 3000r / min deionized water, take the precipitate and dry it at room temperature for 6 hours under the condition of vacuum degree less than 0.01MPa, to obtain conductive ink nano-copper;

[0028] Take the above-mentioned nano-copper, use X-ray diffractometer (XRD) to analyze the phase pattern of the particles, and use the field emission scanning electron microscope (SEM) to observe the morphology of the particles, the results are as follows figure 1 and figure 2 shown. From figure 1 The characteristic peaks of copper can be seen in , without any characteristic peaks of the second phase impurities such as cuprous oxide or copper oxi...

Embodiment 2

[0030] Add 0.64g of copper sulfate to 40ml of ethylene glycol, add 15ml of PEG-400, stir well and heat to 80°C to obtain solution a; add 4.23g of L-ascorbic acid to 40ml of ethylene glycol, stir well and heat to 80°C , to obtain solution b; add solution b to solution a, continue to stir for 30 minutes, then cool to room temperature, centrifuge and wash 4 times with 5000r / min absolute ethanol, take the precipitate and dry it at room temperature for 6 hours under the condition that the vacuum degree is less than 0.01MPa to obtain conductive ink Nano copper;

[0031] The XRD pattern and SEM pattern of the prepared nano-copper are similar to those in Example 1, indicating that the phase of the nano-copper is pure copper without other second-phase impurities; the particles have good dispersion and no obvious agglomeration.

Embodiment 3

[0033] Add 2.09g of copper acetylacetonate into 40ml of diethylene glycol, add 10ml of PEG-600, stir evenly and heat to 100°C to obtain solution a; add 4.93g of L-ascorbic acid into 40ml of diethylene glycol, Stir evenly and heat to 100°C to obtain solution b; add solution b to solution a, continue to stir for 1 hour, then cool to room temperature, centrifuge and wash 4 times with acetone at 8000r / min, take the precipitate and dry it at room temperature under the condition of vacuum degree less than 0.01MPa 6h, obtain conductive ink nano-copper;

[0034] The XRD pattern and SEM pattern of the prepared nano-copper are similar to those in Example 1, indicating that the phase of the nano-copper is pure copper without other second-phase impurities; the particles have good dispersion and no obvious agglomeration.

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Abstract

The invention discloses a method for preparing conductive ink nanometer copper. The method includes the steps that a copper source is added to a solvent A at the concentration of 0.05-0.5 mol / L, 5-20ml polyethylene glycol is added, the mixture is evenly stirred and then heated to 60-160 DEG C, and a solution a is obtained; L-ascorbic acid is added to a solvent B at the concentration of 0.5-1.0mol / L, the mixture is evenly stirred and then heated to 60-160 DEG C, and a solution b is obtained; the solution B is added to the solution a, the mixture is continued to be stirred for 5min-5h and then cooled to indoor temperature, vacuum drying is performed after centrifugation, and the conductive ink nanometer copper is obtained. Ethyl alcohol or polyhydric alcohol serves as the solvent, the L-ascorbic acid which is cheap and easy to get serves as a reducing agent and a protective agent, and nanometer copper particles are prepared. Reaction conditions are simple and mild, the particle size and the morphology of the nanometer copper are easy to control, generation, agglomeration preventing and oxidation resistance of the nanometer copper are achieved synchronously, and the prepared conductive ink nanometer copper is good in dispersibility and high in single dispersity, and has oxidation resistance to a certain extent. The method can be applied to large-scale production.

Description

【Technical field】 [0001] The invention belongs to the technical field of nano metal materials, in particular to a preparation method of conductive ink nano copper. 【Background technique】 [0002] Nano-metal ink has the characteristics of small particle size, low sintering temperature (generally only 100-300°C), and high conductivity after sintering into wires. It is the main raw material for the new generation of printed electronic technology. At present, the literature has reported a variety of metal conductive inks including nano-gold, nano-silver, and nano-copper. Nano-copper has attracted the interest of many researchers due to its low price and low ion migration. [0003] Common methods for preparing nano-copper include sol-gel method, hydrothermal reduction method, electrolysis method, plasma method, gas phase steam method, thermal decomposition method, and liquid phase reduction method. The reaction temperature of the sol-gel method is low, the product particles are...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24C09D11/52B82Y40/00
Inventor 孙蓉张昱朱朋莉
Owner SHENZHEN INST OF ADVANCED TECH
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