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Preparation method of low-temperature sintering nano copper conductive ink

A conductive ink, low temperature sintering technology, applied in the direction of ink, conductive pattern formation, household appliances, etc., can solve the problems of limiting the choice of printed substrates, high sintering temperature, reducing ink conductivity, etc., to achieve large-scale production, simple process , the effect of high conductivity

Inactive Publication Date: 2013-05-08
TIANJIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent 200910054884.8 The nano-copper particles (20-70nm) produced by the chemical reduction method are uneven, and generally the particles exceeding 50nm are easy to block the nozzle; the use of electrodialysis to remove impurities will not only infiltrate a large amount of water to reduce the concentration of solid solution, but also Oxygen dissolved in the solvent oxidizes the nano-copper partially or locally, reducing the conductivity of the ink
On the other hand, the current common printed patterns require a higher sintering temperature (>250°C), which limits the choice of printed substrates, such as substrates such as plastics and paper with low temperatures, which cannot be applied.
The international patent WO2004 / 005413 reports the preparation method of metal conductive ink that can be sintered at low temperature, but the particles prepared by it are all above the micron level, which can only be used for smearing instead of inkjet printing, which limits its application in the field of fine printed electronics Application; In addition, excessive addition of binders, additives, polymers, buffers, etc. reduces the conductivity of the ink

Method used

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  • Preparation method of low-temperature sintering nano copper conductive ink
  • Preparation method of low-temperature sintering nano copper conductive ink

Examples

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Embodiment 1

[0027] A preparation method of low-temperature sintering nano-copper conductive ink, comprising the steps of:

[0028] 1) Dissolve 20mmol of copper sulfate pentahydrate and 1mmol of polyvinylpyrrolidone with a molar mass of 40,000g / mol in 100ml of diethylene glycol, gradually raise the temperature to 80°C, and adjust its Ph value with ammonia water with a concentration of 25% by mass After completely dissolving, add 50ml of sodium borohydride dropwise at a rate of 8ml / min with a concentration of 8mol / L sodium borohydride in the solution to be reacted and continue stirring. After reacting for 30 minutes, stop heating and continue stirring for 60 minutes, then cool naturally;

[0029] 2) Add ethanol to the above-mentioned cooled solution to wash, centrifuge, and dry to obtain nano-copper powder with high oxidation resistance;

[0030] figure 1 This is the TEM photo of the nano-copper powder, which shows that the nano-copper particles are 5-30nm in size.

[0031] figure 2 It ...

Embodiment 2

[0035] A preparation method of low-temperature sintering nano-copper conductive ink, comprising the steps of:

[0036] 1) Mix 0.2mol copper nitrate, 0.2molC 16 TAB was dissolved in 1L of ethylene glycol, and the temperature was gradually raised to 80°C. The Ph value was adjusted to 10.5 with ammonia water with a mass percent concentration of 25%. L hydrazine hydrate in the solution to be reacted and continued to stir, reacted for 30 minutes, stopped heating and continued to stir for 90 minutes, then naturally cooled;

[0037] 2) adding deionized water to the above-mentioned cooled solution to wash, centrifuge, and dry to obtain high oxidation-resistant nano-copper powder;

[0038] 3) Take 10g of nano-copper powder and dissolve it in 7.25g of the prepared mixed solvent. The mixed solvent is composed of ethanol, diethylene glycol, ethylene glycol and glycerol. The volume ratio of each component is ethanol: 1 to 2 Ethylene glycol: ethylene glycol: glycerol is 35:25:30:10, and f...

Embodiment 3

[0041] A preparation method of low-temperature sintering nano-copper conductive ink, comprising the steps of:

[0042] 1) Dissolve 0.5 mol copper octadecenoate and 3 mol oleic acid in 3 L of glycerol, gradually raise the temperature to 120°C, adjust the Ph value with 25% ammonia water with a mass percentage concentration of 25% After being completely dissolved, add 1 L of sodium hypophosphite with a concentration of 5 mol / L dropwise at a rate of 9.6 ml / min to the solution to be reacted and continue to stir. After 30 minutes of reaction, stop heating and continue to stir for 150 minutes. Then cool naturally;

[0043] 2) adding methanol to the above-mentioned cooled solution to wash, centrifuge, and dry to obtain high oxidation-resistant nano-copper powder;

[0044] 3) Dissolve 30g of nano-copper powder in 37.5g of ethylene glycol and fully ultrasonicate to obtain a stable nano-copper conductive ink.

[0045] The prepared nano-copper conductive ink was inkjet printed on the po...

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Abstract

The invention provides a preparation method of low-temperature sintering nano copper conductive ink. The preparation method comprises the steps of: dissolving a copper salt and a protective agent in an organic solvent, heating until the copper salt and the protective agent are completely dissolve, regulating the pH value to be 8.6-10.5 by using ammonia water, dropping a reducing agent in a reaction system, reacting for 10-60minutes and continuously stirring, gradually cooling; carrying out centrifuging, washing and vacuum drying to obtain high-purity nano copper particles; and dispersing the nano copper particles in solvents with different proportions to obtain stable nano copper conductive ink. The preparation method has the advantages that the particle size of nano copper powder in the prepared nano copper conductive ink is 5-30nm, and the prepared nano copper conductive ink has high oxidization resistance and can not be oxidized after stored for above one year in air; the nano copper conductive ink has high conductivity, the resistivity of the sintered electronic device is only 2-5 times that of the conventional copper wire and can be kept unchangeable after being placed for a long time in air; and the preparation method is suitable for preparing various printed electronic devices, is simple in process, and can realize massive production.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a method for preparing low-temperature sintered nanometer copper conductive ink. Background technique [0002] Printed electronics technology refers to the printing of various conductive inks on various substrates to prepare large-area, flexible, and low-cost electronic products and devices. Conductive ink can be used in many fields such as: wireless intelligent identification electronic tags (RFID), printed circuit boards (PCB), flexible printed circuit boards (FPCB), etc. With the rapid development of printed electronic technology and the social and economic development trend of green production, energy saving and emission reduction, conductive ink will surely become the key material of the new generation of fully printed electronic technology in the electronics industry. [0003] Conductive ink is mainly composed of nano-metal particles or non-metal fillers, ...

Claims

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Application Information

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IPC IPC(8): C09D11/02H05K3/12C09D11/52
Inventor 陈民芳李伟魏军李文江
Owner TIANJIN UNIVERSITY OF TECHNOLOGY
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