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Method for preparing superfine copper powder

A technology of ultrafine copper powder and divalent copper, which is applied in the field of preparation of ultrafine metal powder, can solve the problem of high preparation cost and achieve the effect of narrow particle size distribution and good growth rate

Active Publication Date: 2008-06-11
南通麦特隆新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In addition, CN1082468A discloses a kind of superfine copper powder and preparation method thereof, described method adopts the reaction system of alcoholic solvent, and adopts the mode of two-stage heating to carry out reduction, but the reaction temperature used in this method is higher (generally 150°C or higher), the reaction system is operated under pressure (0.1-1.0MPa), and it is a non-aqueous reaction system, so the preparation cost is relatively high

Method used

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preparation example Construction

[0012] The preparation method of the ultrafine copper powder of the present invention will be described in detail below.

[0013] First, the divalent copper compound solution is subjected to a first reduction reaction with a reducing agent solution to obtain a solution containing a monovalent copper compound.

[0014] Wherein, the above-mentioned divalent copper compound may be a water-soluble inorganic acid salt or organic acid salt, such as copper sulfate, copper nitrate, copper chloride and / or copper formate, etc., preferably copper sulfate. The concentration of the divalent copper compound solution may be 0.01-0.5 mol / L, preferably 0.05-0.3 mol / L.

[0015] The reducing agent used in the above-mentioned first reduction reaction can be selected from one or more of formaldehyde, sodium hypophosphite, ascorbic acid, sodium borohydride, potassium borohydride, hydrazine hydrate, hydrazine, and sodium sulfite, preferably sodium sulfite. The concentration of the reducing agent so...

Embodiment 1

[0030] Under stirring, fully mix 0.05mol copper chloride, 0.2mol dimethylhydantoin, 0.03mol sodium sulfite and water (water is added to 1 liter of total solution), and carry out the first reduction reaction at 50°C for 15 Minutes, prepare 1 liter of solution containing monovalent copper compound.

[0031] The molecular weight of 0.02mol potassium borohydride, 0.2mol potassium hydroxide and 0.2g is polyvinylpyrrolidone (PVP) manufactured by Sinopharm Group Chemical Reagent Co., Ltd.) in the range of 50,000 to 100,000) in water and prepared into 200ml reducing agent solution, The reducing agent solution was added to the above-mentioned solution containing the monovalent copper compound, and the second reduction reaction was carried out at 50° C. under a nitrogen protective atmosphere for 20 minutes. The resulting copper powder was separated by centrifugation.

[0032] Afterwards, under nitrogen protection, the generated copper powder was washed with deionized water and absolute...

Embodiment 2

[0034] Under stirring, 0.3mol copper sulfate, 1.0mol maleimide, 60 milliliters of 36% (volume fraction) formaldehyde and water (water is added to the total solution of 1 liter) are fully mixed, and the first step is carried out at 60 ° C. The reduction reaction was performed for 10 minutes to prepare 1 liter of a solution containing a monovalent copper compound.

[0035]The 36% (volume fraction) formaldehyde of 60 milliliters and the molecular weight of 1.0g are the polyacrylamide (PAA) of 3,000,000~5,000,000 scopes (manufactured by Sinopharm Chemical Reagent Co., Ltd.) in water and are mixed with the reductant solution of 200ml, will The reducing agent solution was added into the above-mentioned solution containing the monovalent copper compound, and the second reduction reaction was carried out at 60° C. under the protection of argon for 20 minutes. The resulting copper powder was separated by centrifugation.

[0036] Afterwards, under the protection of argon, the generated...

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Abstract

The invention relates to a process for preparing ultra-fine metal powder and in particular relates to the process for preparing nanometer-grade ultra-fine copper powder. The process which is provided by the invention for preparing the ultra-fine copper powder comprises firstly, using reducing agent solution whose amount is 1-2 times of theoretical amount which is needed to reduce divalent copper compounds to one valence copper compounds to enable solution of the divalent copper compounds to carry out the first reducing reaction, preparing solution which contains the one valence copper compounds, then, using the reducing agent solution whose amount is 1-2 times of the theoretical amount which is needed to reduce the one valence copper compounds to pure copper to enable the solution which contains the one valence copper compounds to carry out the second reducing reaction, and preparing ultra-fine copper powder. According to the process for preparing the ultra-fine copper powder, reaction speed for reducing copper ions into pure copper can be increased greatly, growing speed of nucleations and crystal nucleus of copper powder can be controlled better, and thereby finer, stable, and even nanometer-grade ultra-fine copper powder with narrow distribution of particle diameters can be obtained.

Description

technical field [0001] The invention relates to a preparation method of ultrafine metal powder, in particular to a preparation method of nanoscale ultrafine copper powder. Background technique [0002] Ultrafine copper powder has the same excellent conductivity as silver (the volume resistivity of silver is 1.59×10 -6 Ω cm, the volume resistivity of copper is 1.72×10 -6 Ω cm) and cheap (1 / 20 of the price of silver), can replace precious metals such as ultra-fine silver powder, gold powder, etc., widely used in electrical fields such as conductive coatings, conductive adhesives, electrode materials, and can be used in aerospace technology, microelectronics , chemistry, biology, medicine and other fields. [0003] There are many ways to prepare ultrafine copper powder. Specifically, it can be divided into two categories: physical method and chemical method. Physical methods include ball milling method, gas phase evaporation method, plasma method, etc.; chemical methods inc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24
Inventor 陈春山周勇董俊卿
Owner 南通麦特隆新材料科技有限公司
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