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Method for preparing antioxidated superfine copper powder

An anti-oxidation technology of ultra-fine copper powder, which is applied in the field of preparation of anti-oxidation ultra-fine copper powder, can solve the problems of poor anti-oxidation performance of copper powder, difficulty in industrial application, and difficulty in controlling the particle size of copper powder, so as to improve anti-oxidation Performance, improved shape and particle size distribution, low price effect

Inactive Publication Date: 2009-07-08
NO 52 INST OF CHINA NORTH IND GRP CORP
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because a large amount of ethanol (solvent) needs to be consumed in the reaction process, and the reaction must be carried out under high temperature and high pressure, special equipment is required, so the industrial application of this method is difficult.
[0004] Generally speaking, although there are many reports on the preparation of ultrafine copper powder by liquid phase reduction method, these methods either have difficulty in controlling the particle size of copper powder, or the obtained copper powder has poor oxidation resistance, and cannot obtain anti-oxidative properties suitable for electronic materials and other fields. Oxidation of ultra-fine copper powder requires special anti-oxidation treatment, or the preparation process requires special solvents or devices, resulting in high costs. Therefore, it is necessary to develop a new preparation method for ultra-fine, anti-oxidation copper powder to address these problems

Method used

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  • Method for preparing antioxidated superfine copper powder
  • Method for preparing antioxidated superfine copper powder
  • Method for preparing antioxidated superfine copper powder

Examples

Experimental program
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Effect test

Embodiment 1

[0028] 100ml of copper sulfate solution with a concentration of 0.02mol / L and 8ml of 20% NaOH solution were prepared respectively. in CuSO 4 Sodium dodecylbenzene sulfonate was added into the solution, fully dissolved, and its concentration reached 0.1g / L. Then add 2,2'-bipyridine so that its concentration is 10mg / L. Slowly add NaOH solution to CuSO under vigorous stirring at 300r / min 4 solution, making Cu 2+ The precipitate is light blue Cu(OH) 2 jelly. Then slowly add 0.003mol of hydrazine hydrate, the reaction proceeds vigorously, a large number of bubbles are generated, and the precipitate turns into an orange suspension. Thereafter, the reaction was incubated in two stages. In the first stage, the temperature of the suspension was raised to 30°C, and the stirring was continued until the color of the precipitate turned orange-red. Then carry out the second-stage reaction, first adjust the pH of the suspension with 20% NaOH to keep it at 11-12, raise the temperature ...

Embodiment 2

[0031] Prepare 100 ml of copper sulfate solution with a concentration of 0.1 mol / L and 40 ml of 20% NaOH solution respectively. in CuSO 4 Sodium dodecylbenzene sulfonate was added into the solution, fully dissolved, and its concentration reached 0.5g / L. Then add 2,2'-bipyridine so that its concentration is 30mg / L. Slowly add NaOH solution to CuSO under vigorous stirring at 300r / min 4 solution, making Cu 2+ Precipitate as Cu(OH) 2jelly. Then slowly add 0.02mol of hydrazine hydrate, the reaction proceeds vigorously, a large number of bubbles are generated, and the precipitate turns into an orange suspension. Thereafter, the reaction was incubated in two stages. In the first stage, the temperature of the suspension was raised to 40°C, and the stirring was continued until the color of the precipitate turned orange-red. Then carry out the second-stage reaction, first adjust the pH of the suspension with 20% NaOH to keep it at 12-13, raise the temperature to 60°C and keep it ...

Embodiment 3

[0034] 100ml of copper sulfate solution with a concentration of 0.2mol / L and 80ml of 20% NaOH solution were prepared respectively. in CuSO 4 Add PVP into the solution, fully dissolve, and make its concentration reach 1.0g / L. Then add 2,2'-bipyridine so that its concentration is 50mg / L. Slowly add NaOH solution to CuSO under vigorous stirring at 300r / min 4 solution, making Cu 2+ Precipitate as Cu(OH) 2 jelly. Then slowly add 0.05 mol of hydrazine hydrate, the reaction proceeds vigorously, a large number of bubbles are generated, and the precipitate turns into an orange suspension. Thereafter, the reaction was incubated in two stages. In the first stage, the temperature of the suspension was raised to 30°C, and the stirring was continued until the color of the precipitate turned orange-red. Then carry out the second-stage reaction, first adjust the pH of the suspension with 20% NaOH to keep it at 11-12, raise the temperature to 70°C and keep it warm until the bubbles gene...

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Abstract

A preparation method of anti-oxidation superfine copper powder belongs to the powder technical field. The process flow of the method is as follows: taking soluble divalent cupric salt as a starting material for making cupric salt solution, adding and evenly mixing a dispersant and a trace additive, then adding NaOH solution to the cupric salt solution with the NaOH / Cu mol ratio being 2 to cause the Cu to precipitate as Cu(OH)2, adding a hydrazine hydrate as a reducing agent to obtained jelly with the N2H4 / Cu mol ratio being 1.5-2.5 and obtaining pure copper powder by two-stage heat preserving reaction: (1) a first stage: preserving at the temperature of 30-50 DEG C, and converting the Cu(OH)2 into Cu2O after reaction; and (2) a second stage: adjusting pH value of the solution with NaOH to 11-13, heating suspending liquid obtained from the first stage to 60-70 DEG C, keeping the temperature until the reaction is finished to obtain the pure copper powder, and then cleaning and drying the copper powder by centrifugal separation. The raw materials used in the method are cheap and available, and the superfine copper powder with the average particle size below 0.5 micron prepared by the method does not need any anti-oxidation treatment, does not discolor after being kept in the air for more than one year, has anti-oxidation temperature of more than 100 DEG C proved by thermogravimetric analysis and is especially suitable for being used as an electronic material.

Description

technical field [0001] The invention relates to the technical field of powder preparation, in particular to a preparation method of anti-oxidation ultrafine copper powder. Background technique [0002] As a functional material, ultrafine copper powder has broad application prospects in powder metallurgy, electronic paste, lubrication, catalysis and other fields. Especially when it is used as a conductive filler, because of its low price and no material "migration" problem of silver powder, it has great potential value in the fields of electromagnetic shielding and electronic paste. The copper powder used as a conductive filler must not only have high purity, but also its particle size, shape, and oxidation resistance (that is, weather resistance) when stored at room temperature are also important basis for evaluating its quality. For example, the copper powder used in the conductive adhesive used for the external electrodes of ceramic capacitors is required to have a relati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24
Inventor 王尚军方晓祖
Owner NO 52 INST OF CHINA NORTH IND GRP CORP
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