Preparation method of ultrafine copper powder for conductive paste

A technology of ultra-fine copper powder and conductive paste, applied in the direction of coating, etc., can solve the problems of low tap density and crystallinity of copper powder, sintering and agglomeration of copper powder, and achieve good oxidation resistance, prevention of sintering and agglomeration, and good topographical effect

Inactive Publication Date: 2009-08-26
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

First of all, in the process of hydrogen reduction of copper oxide, a large number of oxygen vacancies are generated due to the reaction of oxygen in the oxide with hydrogen and the water generated by their reaction escapes in gaseous form and leaves a large number of pores in the copper powder particles. As a result, the tap density and crystallinity of the copper powder are very low; secondly, during the high-temperature hydrogen reduction process, the prepared copper powder is prone to sintering and agglomeration

Method used

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  • Preparation method of ultrafine copper powder for conductive paste
  • Preparation method of ultrafine copper powder for conductive paste
  • Preparation method of ultrafine copper powder for conductive paste

Examples

Experimental program
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Effect test

Embodiment 1

[0024] see figure 1 , uniformly disperse 15g of spherical cuprous oxide powder with an average particle size of 1.2μm and good dispersibility and 600mL of pure water in the reactor, and mix 6g / L MgCl 2 About 250mL of aqueous solution was slowly added to the reactor, and continued to stir, and then slowly added dropwise 2.5mol / L NaOH solution to adjust the pH value of the reaction system to above 10, and continued to stir for 30min. 2 During the generation process, it is precipitated and coated on the surface of cuprous oxide. Solid-liquid separation was performed on the suspension after the coating was completed, the coating was washed several times with pure water, and then dried with absolute ethanol. The dried cladding was placed in a porcelain boat and placed in a tube furnace, and heated with H at a temperature of 150 °C. 2 Reduction for 3 hours, and then heat preservation at 600°C for 1 hour for shrinkage and densification treatment. After the furnace temperature drop...

Embodiment 2

[0026] see figure 1 , uniformly disperse 15g of spherical copper oxide powder with an average particle size of 1μm and good dispersibility and 600mL of pure water in the reactor, and 300mL of Mg(OH) prepared in advance 2 Colloidal solution composed of water (among them, Mg(OH) 2 The content of 5g / L) was slowly added into the reactor, and the coating was continued for 30 minutes with stirring. then use H 2 The reduction temperature is 200°C, the high-temperature shrinkage temperature is 700°C, and other steps are the same as in Example 1 to obtain copper powder. As a result, the copper powder kept the original shape of copper oxide, with an average particle size of 0.8 μm, and it was confirmed that at least 80% of the particles had a particle size between 0.7 and 0.9 μm, with good dispersion and no sintering and agglomeration.

Embodiment 3

[0028] see figure 1 15g of cuprous oxide powder with an average particle size of 1.2μm and good dispersibility and 600mL of pure water were uniformly dispersed in the reactor, and the pre-prepared volume of 300mL of Fe(OH) 3 Colloidal solution composed of water (wherein, Fe(OH) 3 content of 10g / L) was slowly added into the reactor, and the coating was continued for 30 minutes with stirring. then use H 2The reduction temperature is 150°C, the high-temperature shrinkage temperature is 600°C, and other steps are the same as in Example 1 to obtain copper powder. As a result, the copper powder kept the original shape of cuprous oxide, with an average particle size of 1 μm, and it was confirmed that at least 80% of the particles had a particle size between 0.9 and 1.1 μm, with good dispersion and no sintering and agglomeration.

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Abstract

The invention discloses a preparation method of ultrafine copper powder for conductive paste. The preparation method comprises the following steps: firstly, coating copper oxide with a compound, reducing the coated copper oxide at high temperature to prepare copper powder, and finally densifying the obtained copper powder at high temperature. The preparation method overcomes preparation cost defect and product performance defect of preparing the copper powder by a gas-phase method and a liquid-phase reduction method, and help produce the ultrafine copper powder which has controllable grain size, good dispersibility, high density and mature crystal form, and meet production requirements for electrodes of multilayer ceramic capacitors. The preparation method has simple equipment and short process flow, and is applicable to industrialized production of the copper powder.

Description

technical field [0001] The invention relates to a method for preparing copper powder, in particular to a method for preparing ultrafine copper powder for conductive paste. Background technique [0002] Metal powder is an important basic raw material, which can be directly dispersed and used, or it can be pressed and sintered into a bulk material, and can also be made into a film material, etc. For example, ultra-fine copper powder can be used as high-efficiency catalysts, conductive coatings, raw materials for conductive composite materials, electrode materials, additives, etc. [0003] Taking the modern electronics industry as an example, multilayer ceramic capacitors (MLCC for short) in the modern electronics industry have become mainstream products in the capacitor industry, and are widely used in communications, computers and consumer electronics products. One of the main development directions of MLCC is the base metallization of electrodes, that is, the use of low-pri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/20B22F9/22B22F1/02
Inventor 周康根王岳俊曹艳蒋志刚
Owner CENT SOUTH UNIV
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