Method for preparing nanometer spherical copper powder

A copper powder and spherical technology, which is applied in the field of preparation of nano-spherical copper powder, can solve the problems of wide particle size distribution, high cost, and incomplete crystal form of copper powder

Inactive Publication Date: 2014-04-23
NINGXIA ORIENT TANTALUM IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many methods for preparing copper powder, which can be divided into liquid phase method, solid phase method and gas phase method according to the state of raw materials, but the copper powder prepared by these methods has uneven particle size, easy agglomeration, shape Irregular appearance and other characteristics
The copper powder prepared by the gas phase method has a high sphericity, but the raw material gas required is expensive, the equipment is complicated, the cost is high, and the output is low; the copper powder prepared by the solid phase method has a wide particle size distribution and is easy to introduce impurities; although the liquid phase method uses simple equipment , but the copper powder produced by this method has low crystallinity, incomplete crystal form and poor oxidation resistance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh 100g of copper sulfate, weigh 1.05 times the theoretical amount of ammonium oxalate, and configure 1mol / L copper sulfate solution and 0.75mol / L ammonium oxalate solution, mix 1.0mol / L copper sulfate and 100g / L alcohol 0.2 Add the mixed aqueous solution of L to a stirred reactor with a mixed aqueous solution of 60°C, 0.75mol / L ammonium oxalate and 0.2L, 100g / L alcohol (stirring speed is 150rpm), and after 20 minutes of reaction, copper powder is obtained The precursor copper oxalate.

[0032] Then, based on the molar amount of copper, magnesium chloride is 1.5 times, and the amount of ammonium oxalate is weighed according to the needs of the chemical reaction. Add it into the reaction container at a uniform speed, react for 30 minutes after the addition, and then wash it repeatedly with pure water for 3 times, centrifuge and dry it in an electric oven at 150°C to obtain copper oxalate wrapped with magnesium oxalate.

[0033] Next, the copper oxalate wrapped with m...

Embodiment 2

[0035] Weigh 200g of copper nitrate, weigh 1.05 times the theoretical amount of ammonium oxalate, and configure 0.75mol / L copper nitrate solution and 0.75mol / L ammonium oxalate solution, and mix 0.75mol / L copper nitrate and 30g / L PVP at 40°C The mixed aqueous solution was added at a constant speed to a stirred reactor containing a mixed aqueous solution of 0.75mol / L ammonium oxalate and 30g / L PVP at 40°C (the stirring speed was 200rpm). After the reaction was completed for 30 minutes, the copper oxalate precursor of copper powder was obtained. .

[0036] Next, based on the molar amount of copper, calcium chloride is 1.8 times as much as it is, and the amount of ammonium oxalate is weighed according to the needs of the chemical reaction, and it is configured into a 4mol / L calcium chloride aqueous solution at 40°C and 1.2mol / L oxalic acid at 60°C The ammonium aqueous solution was added into the reaction vessel at a constant speed at the same time, and reacted for 30 minutes afte...

Embodiment 3

[0039] Weigh 150g of copper chloride, weigh oxalic acid according to 1.05 times of the theoretical amount, and configure 0.5mol / L copper sulfate solution and 0.5mol / L oxalic acid solution, and mix 0.5mol / L copper chloride, 120g / L PEG The mixed aqueous solution was added at a constant speed to a stirred reactor containing a mixed aqueous solution of 0.5mol / L oxalic acid and 100g / L PEG at 35°C (the stirring speed was 100rpm). After the reaction was completed for 40 minutes, copper oxalate, a precursor of copper powder, was obtained.

[0040]Next, the copper will be based on the molar amount of copper, the magnesium chloride will be doubled, and the amount of ammonium oxalate will be weighed according to the needs of the chemical reaction. Add it into the reaction container at a constant speed, react for 40 minutes after the addition, and then wash it twice with pure water repeatedly, and then dry it in an electric oven at 150°C to obtain copper oxalate wrapped with magnesium oxal...

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Abstract

The invention relates to a method for preparing copper powder for the field of nanometer spherical electrocondution slurry, catalysts, ceramic capacitors and the like, in particular to a method for preparing nanometer spherical copper powder. The method is characterized by including the following steps that firstly, a precursor of the copper powder is prepared, wherein soluble copper salt reacts with a precipitating agent to generate precursor precipitation of the copper salt; secondly, a cladding body of the copper powder is prepared, the acquired precursor precipitation of the copper salt is used as a crystal nucleus, a cladding layer formed by a cladding agent is formed on the surface of the crystal nucleus through a physical crystallization method or a chemical crystallization method, and then centrifugal separation, filtration and drying are conducted; thirdly, acquired drying materials are kept warm for 0.5-2 hours in the reducing atmosphere or the vacuum atmosphere at the temperature ranging from 250 DEG C to 350 DEG C, and then the drying materials are processed for 2-6 hours at the high temperature ranging from 400 DEG C to 850 DEG C; fourthly, the cladding layer of the acquired materials is removed through acid washing or alkali washing, and the materials are dried and decentralized. The method for preparing the nanometer copper powder is low in cost, simple in operation, free of pollution and controllable in granularity.

Description

technical field [0001] The invention relates to a preparation method of copper powder used in the fields of nano-spherical conductive paste, catalyst, ceramic capacitor and the like, in particular to a preparation method of nano-spherical copper powder. Background technique [0002] With the rapid development of the electronics industry, Multilayer Ceramic Capacitors (MLCC), as one of the key materials, are widely used in various Oscillation, coupling, filtering and bypass circuits in electronic complete machines, especially high-frequency circuits, have made the market demand for MLCC more and more. Traditional MLCC electrodes use precious metals such as silver-palladium alloy or pure palladium metal. With the rise in the price of metal silver and palladium, the use of cheap base metal copper and copper as electrode materials has attracted widespread attention, and it is also a major trend in the development of ceramic capacitor technology. one. Copper powder for MLCC is ...

Claims

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Application Information

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IPC IPC(8): B22F9/24B82Y40/00
Inventor 李军义王东新郭顺孙本双杨国启李彬孙磊张丽
Owner NINGXIA ORIENT TANTALUM IND
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