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Preparation method for low-agglomeration antioxidant copper nanoparticle powder

A nano-copper powder and anti-oxidation technology, which is applied in the field of low-agglomeration and anti-oxidation nano-copper powder, can solve the problems of nano-copper powder agglomeration, oxidation, and inability to solve oxidation resistance and dispersibility well, and achieve low production cost, Great economic benefits, avoiding agglomeration and oxidation

Active Publication Date: 2013-12-25
JINGMEN GEM NEW MATERIAL +1
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  • Description
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AI Technical Summary

Problems solved by technology

However, so far, the existing various nano-copper powder preparation methods cannot well solve the problems of oxidation resistance and dispersibility in the preparation process.
Even the liquid phase reduction method that is currently reported and applied more is to first add the dispersant to the copper salt solution to form a copper salt / dispersant mixed solution, and then slowly add the reducing agent to the copper salt / dispersant mixed solution In addition, the traditional mechanical stirring method is still used, which will easily lead to agglomeration and oxidation of nano-copper powder.

Method used

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  • Preparation method for low-agglomeration antioxidant copper nanoparticle powder

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preparation example Construction

[0024] Such as figure 1 As shown in the process flow diagram, the present invention provides a method for preparing low-agglomeration anti-oxidation nano-copper powder, comprising the following steps:

[0025] The preparation step is to prepare copper salt solution and reducing agent-dispersant mixed solution respectively, wherein the copper salt solution is obtained by dissolving copper salt in water, and the concentration of Cu ions in the copper salt solution is 10-50 g / L, and the reduction The agent-dispersant mixture is obtained by adding the dispersant into the hydrazine hydrate solution with a concentration of 3-3.5mol / L, ultrasonically vibrating, and mixing uniformly. The dispersant can be any one of the following materials: poly Oxyethylene sorbitan monooleate, gelatin, sodium lauryl sulfate, fatty acid polyethylene glycol fat, etc., wherein polyoxyethylene sorbitan monooleate is preferably used, and the addition amount of the dispersant is copper 1% to 5% of the mas...

Embodiment 1

[0036] (1) Dissolve CuSO with deionized water 4 ·5H 2 O is made into copper salt solution, wherein the concentration of Cu ions is 30g / L, about 1000mL is ready for use.

[0037] (2) Add 0.3 g of polyoxyethylene sorbitan monooleate into the hydrazine hydrate solution, and ultrasonically vibrate to form a uniform reducing agent-dispersing agent mixture.

[0038] (3) According to the molar ratio Cu: N 2 h 4 =1: 1.5, add the copper salt solution dropwise to the above-mentioned reducing agent-dispersant mixed solution, adjust the pH of the solution to 11 with 10% NaOH solution by mass percentage, raise the temperature to 70°C, and Keep the reaction until the supernatant turns colorless, that is, the reaction is over, let stand, remove the supernatant, and leave the precipitate.

[0039] (4) Under nitrogen protection conditions, the precipitate obtained in step (3) was washed with deionized water and absolute ethanol in sequence, and centrifugally filtered to obtain the precipit...

Embodiment 2

[0046] (1) Dissolve copper chloride in deionized water to make a copper salt solution, in which the concentration of Cu ions is 30g / L, about 1000mL is ready for use.

[0047] (2) Add 0.6 g of polyoxyethylene sorbitan monooleate into the hydrazine hydrate solution, and ultrasonically vibrate to form a uniform reducing agent-dispersing agent mixture.

[0048] (3) According to the molar ratio Cu: N 2 h 4 = 1: 2.5 The dosage ratio of the copper salt solution is added dropwise to the above-mentioned reducing agent-dispersant mixed solution, the pH of the solution is adjusted to 12 with a 15% NaOH solution by mass percentage, and the temperature is raised to 75 ° C. Keep the reaction under the same conditions until the supernatant turns colorless, that is, the reaction ends, let stand, remove the supernatant, and leave the precipitate.

[0049] (4) Under nitrogen protection conditions, the precipitate obtained in step (3) was washed with deionized water and absolute ethanol in seq...

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Abstract

The invention discloses a preparation method for low-agglomeration antioxidant copper nanoparticle powder. The preparation method for the low-agglomeration antioxidant copper nanoparticle powder comprises the following steps of preparation: preparing copper salt solution and reductant-dispersant mixed liquor; reaction: dipping the copper salt solution into the reductant-dispersant mixed liquor, regulating the pH (potential of hydrogen) value to 10-13, keeping reaction at the temperature of 70-75DEG C under the ultrasonic oscillating condition until the reaction is finished, and standing to obtain a secondary precipitate; primary washing and filtering: obtaining the secondary precipitate; ultrasonic processing: adding surface protectant into the secondary precipitate, and standing after ultrasonic oscillating processing to obtain third precipitate; secondary washing and filtering: obtaining fourth precipitate; pre-drying: carrying out vacuum drying to the fourth precipitate to obtain copper powder; drying: adding NH4HCO3 into the obtained copper powder to be evenly mixed, putting the mixed copper powder under the flowing nitrogen atmosphere, and drying at the temperature of 70-80DEG C to obtain the copper nanoparticle powder. According to the preparation method for the low-agglomeration antioxidant copper nanoparticle powder, which is disclosed by the invention, the charging sequence is changed, ultrasonic vibration stirring is adopted, NH4HCO3 is added, and therefore the copper nanoparticle powder can be effectively prevented from being agglomerated and oxidized.

Description

technical field [0001] The invention relates to the technical field of low-agglomeration and anti-oxidation nano-copper powder, in particular to a preparation method of low-agglomeration and anti-oxidation nano-copper powder. Background technique [0002] Nano-copper powder has the characteristics of small size, large specific surface area, large number of surface active centers, small resistance, quantum size effect, macroscopic quantum tunneling effect, etc. It shows extremely important application value in metallurgy, chemical industry, electronics, aerospace and other fields. Especially as a potential substitute of noble metal nano-silver powder, nano-copper powder can be widely used in the manufacture of printed boards, the manufacture of multilayer ceramic capacitors (MLCC), conductive coatings, etc. [0003] The preparation methods of nano-copper powder mainly include: liquid phase reduction method, electrolysis method, mechanical grinding method, gas phase steam meth...

Claims

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Application Information

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IPC IPC(8): B22F9/24
Inventor 吕志张功勋王勤何显达谭翠丽
Owner JINGMEN GEM NEW MATERIAL
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