JPH07107168B2 - Method for producing fine copper particles - Google Patents
Method for producing fine copper particlesInfo
- Publication number
- JPH07107168B2 JPH07107168B2 JP1706487A JP1706487A JPH07107168B2 JP H07107168 B2 JPH07107168 B2 JP H07107168B2 JP 1706487 A JP1706487 A JP 1706487A JP 1706487 A JP1706487 A JP 1706487A JP H07107168 B2 JPH07107168 B2 JP H07107168B2
- Authority
- JP
- Japan
- Prior art keywords
- copper
- particle size
- ascorbic acid
- aqueous solution
- particles
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は微細な銅粒子の製造方法に関するものである。TECHNICAL FIELD The present invention relates to a method for producing fine copper particles.
（従来技術とその問題点） 従来、銅微粒子の製造方法としては、酸化銅粒子を水性
媒体中でヒドラジンなどの還元剤を用いて還元する方法
が用いられてきた。(Prior art and its problems) Conventionally, as a method for producing copper fine particles, a method of reducing copper oxide particles in a water medium using a reducing agent such as hydrazine has been used.
ところが、この方法では、還元された粒子の粒径が酸化
物の粒径に依存するために粒径のコントロールが難し
く、かつ還元された粒子同士が引き寄せ合うために凝集
した粒度分布の幅の広い銅粒子しか得られないという欠
点を有していた。However, in this method, it is difficult to control the particle size because the particle size of the reduced particles depends on the particle size of the oxide, and the reduced particles are attracted to each other so that the aggregated particle size distribution has a wide range. It had a drawback that only copper particles could be obtained.
本発明は上記の欠点を解消せんがためになされたもので
あり、分散した、粒度分布の幅の狭い微細な銅粒子の粒
径コントロール可能な製造方法を提供せんとするもので
ある。The present invention has been made in order to solve the above-mentioned drawbacks, and an object of the present invention is to provide a production method capable of controlling the particle size of dispersed fine copper particles having a narrow particle size distribution.
（問題点を解決するための手段） 本発明は硫酸銅水溶液中の銅イオンを還元して銅微粒子
を製造する方法において、還元剤としてＬ−アスコルビ
ン酸又はＬ−アスコルビン酸塩類を用ることによって単
分散した銅微粒子を得ることを特徴とするものである。(Means for Solving Problems) The present invention is a method for producing copper fine particles by reducing copper ions in a copper sulfate aqueous solution, by using L-ascorbic acid or L-ascorbic acid salts as a reducing agent. It is characterized in that monodispersed copper fine particles are obtained.
而して本発明の製造方法において、Ｌ−アスコルビン酸
又は、Ｌ−アスコルビン酸塩類を用いる理由は、これら
の酸化還元電位が硫酸銅水溶液を還元するのに適当であ
ると同時に粒子同士の凝集を防ぐ働きがあるためであ
る。Thus, in the production method of the present invention, the reason for using L-ascorbic acid or L-ascorbic acid salts is that their redox potentials are suitable for reducing the copper sulfate aqueous solution and at the same time cause the aggregation of particles. This is because it has a preventive function.
また、本発明の請求範囲においてＬ−アスコルビン酸及
びＬ−アスコルビン酸塩類としては、ナトリウム塩、カ
リウム塩、アンモニウム塩等を問わない。Further, in the claims of the present invention, the L-ascorbic acid and L-ascorbic acid salts may be sodium salts, potassium salts, ammonium salts or the like.
さらに本発明において、硫酸銅水溶液のpHは0.3よりも
低いと反応が遅くなり、５よりも高いと銅の水酸化物の
沈殿が生成するので、0.3〜５の範囲がより好ましく、
Ｌ−アスコルビン酸のpHは0.5よりも低いと反応が極端
に遅くなるので、0.5以上がより好ましく、また、反応
時の温度は10℃より低いと反応が遅く、100℃を超える
と銅微粒子が凝集してくるので、10〜100℃の範囲がよ
り好ましい。Further, in the present invention, when the pH of the copper sulfate aqueous solution is lower than 0.3, the reaction becomes slow, and when it is higher than 5, precipitation of copper hydroxide is generated, so that the range of 0.3 to 5 is more preferable,
If the pH of L-ascorbic acid is lower than 0.5, the reaction becomes extremely slow, so 0.5 or more is more preferable. Also, if the temperature during the reaction is lower than 10 ° C, the reaction is slow, and if it exceeds 100 ° C, copper fine particles are generated. The range of 10 to 100 ° C. is more preferable because it causes aggregation.
ここで本発明の実施例について説明する。Examples of the present invention will now be described.
（実施例１） 硫酸銅結晶197gを水に溶解し１の水溶液とした後、希
硫酸を加えてpH＝１に調整する。Example 1 197 g of copper sulfate crystal is dissolved in water to form an aqueous solution of 1, and then diluted sulfuric acid is added to adjust the pH to 1.
また、Ｌ−アスコルビン酸200gを水に溶解し１の水溶
液とした後、水酸化ナトリウムを加えてpH＝７に調整す
る。ここで、この２液の温度を30℃にし、硫酸銅水溶液
を撹拌しながらＬ−アスコルビン酸溶液を添加し、５分
間反応させる。Further, 200 g of L-ascorbic acid is dissolved in water to form an aqueous solution of 1, and then sodium hydroxide is added to adjust the pH to 7. Here, the temperature of the two liquids is set to 30 ° C., the L-ascorbic acid solution is added while stirring the copper sulfate aqueous solution, and the reaction is allowed to proceed for 5 minutes.
得られた銅微粒子は濾過、洗浄して、粒度分布測定及び
電子顕微鏡観察を行った。The obtained copper fine particles were filtered and washed, and the particle size distribution was measured and observed with an electron microscope.
その結果、この銅微粒子はほぼ球状で、平均粒径が1.2
μｍ、粒度分布は0.8〜1.5μｍに70％が入るシャープな
ものであった。As a result, the fine copper particles were almost spherical and had an average particle size of 1.2.
The particle size distribution was as sharp as 70% in 0.8 to 1.5 μm.
（実施例２） 硫酸銅結晶126gを水に溶解し１の水溶液とした後、希
硫酸を加えてpH＝３に調整する。(Example 2) 126 g of copper sulfate crystals was dissolved in water to form an aqueous solution of 1, and then diluted sulfuric acid was added to adjust the pH to 3.
また、Ｌ−アスコルビン酸128gを水に溶解し１の水溶
液とした後、水酸化ナトリウムを加えてpH＝５に調整す
る。ここで、この２液の温度を70℃にし、硫酸銅水溶液
を撹拌しながらＬ−アスコルビン酸溶液を添加し、３分
間反応させる。Further, 128 g of L-ascorbic acid is dissolved in water to form an aqueous solution of 1, and then sodium hydroxide is added to adjust the pH to 5. Here, the temperature of the two liquids is set to 70 ° C., the L-ascorbic acid solution is added while stirring the copper sulfate aqueous solution, and the reaction is carried out for 3 minutes.
得られた銅微粒子は濾過、洗浄して、粒度分布測定及び
電子顕微鏡観察を行った。The obtained copper fine particles were filtered and washed, and the particle size distribution was measured and observed with an electron microscope.
その結果、この銅微粒子は多面体で平均粒径が1.8μ
ｍ、粒度分布は1.5〜2.5μｍに70％が入るシャープなも
のであった。As a result, these copper particles are polyhedral and have an average particle size of 1.8μ.
The particle size distribution was as sharp as 70% in 1.5 to 2.5 μm.
（実施例３） 硫酸銅結晶197gを水に溶解し１の水溶液とした後、希
硫酸を加えてpH＝１に調整する。Example 3 197 g of copper sulfate crystal is dissolved in water to form an aqueous solution of 1, and then diluted sulfuric acid is added to adjust the pH to 1.
また、Ｌ−アスコルビン酸ナトリウム200gを水に溶解し
１の水溶液にする。ここでこの２液の温度を20℃にし
硫酸銅水溶液を撹拌しながらＬ−アスコルビン酸ナトリ
ウムを添加し５分間反応させる。Further, 200 g of sodium L-ascorbate is dissolved in water to prepare an aqueous solution of 1. Here, the temperature of the two liquids is adjusted to 20 ° C., sodium L-ascorbate is added to the aqueous solution of copper sulfate while stirring, and the mixture is reacted for 5 minutes.
得られた銅微粒子は濾過、洗浄して、粒度分布測定及び
電子顕微鏡観察を行った。The obtained copper fine particles were filtered and washed, and the particle size distribution was measured and observed with an electron microscope.
その結果、この銅微粒子はほぼ球状で平均粒径が1.0μ
ｍ、粒度分布は0.7〜1.3μｍに70％が入るシャープなも
のであった。As a result, the copper fine particles are almost spherical and have an average particle size of 1.0 μ.
m, and the particle size distribution was a sharp one with 70% in 0.7 to 1.3 μm.
（従来例） 水1,000mlを撹拌しながら平均粒径５μｍの酸化第２銅5
0gを分散懸濁させる。(Conventional example) Cupric oxide 5 with an average particle size of 5 μm while stirring 1,000 ml of water
Disperse and suspend 0 g.
さらにこの液を撹拌しながら70℃まで昇温し、80％の抱
水ヒドラジン水溶液200mlを添加後、70℃で２時間撹拌
した。The temperature of this solution was further raised to 70 ° C. with stirring, 200 ml of an 80% aqueous hydrazine hydrate solution was added, and the mixture was stirred at 70 ° C. for 2 hours.
得られた銅微粒子は濾過、洗浄して粒度分布測定及び電
子顕微鏡観察を行った。The obtained copper fine particles were filtered and washed, and the particle size distribution was measured and observed with an electron microscope.
その結果、この銅微粒子は不定形で、平均粒径が3.5μ
ｍ、粒度分布は0.5〜10μｍと幅が広く、凝集したもの
であった。As a result, these copper particles are amorphous and have an average particle size of 3.5μ.
m, the particle size distribution was as wide as 0.5 to 10 μm, and they were aggregated.
（発明の効果） 上記の説明で明らかなように本発明の製造方法は硫酸銅
水溶液を還元して銅微粒子を製造する方法において、還
元剤としてＬ−アスコルビン酸又はＬ−アスコルビン酸
塩類を用いることにより、従来法では得られなかった単
分散した粒度分布の幅の狭い微細な銅粒子を粒径をコン
トロールして製造できるので、従来の製造方法にとって
代わることのできる画期的なものと言える。(Effect of the invention) As is clear from the above description, the production method of the present invention uses L-ascorbic acid or L-ascorbic acid salts as a reducing agent in the method of producing copper fine particles by reducing an aqueous solution of copper sulfate. Thus, since it is possible to produce finely dispersed fine copper particles having a narrow width of particle size distribution, which cannot be obtained by the conventional method, by controlling the particle size, it can be said to be an epoch-making thing that can replace the conventional manufacturing method.
Claims (1)
る方法において、還元剤としてＬ−アスコルビン酸又は
Ｌ−アスコルビン酸塩類を用いることによって単分散し
た銅微粒子を得ることを特徴とする銅微粒子の製造方
法。1. A method for producing copper fine particles by reducing an aqueous solution of copper sulfate, wherein copper fine particles monodispersed are obtained by using L-ascorbic acid or L-ascorbic acid salts as a reducing agent. Method for producing fine particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1706487A JPH07107168B2 (en) | 1987-01-27 | 1987-01-27 | Method for producing fine copper particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1706487A JPH07107168B2 (en) | 1987-01-27 | 1987-01-27 | Method for producing fine copper particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63186803A JPS63186803A (en) | 1988-08-02 |
| JPH07107168B2 true JPH07107168B2 (en) | 1995-11-15 |
Family
ID=11933551
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1706487A Expired - Lifetime JPH07107168B2 (en) | 1987-01-27 | 1987-01-27 | Method for producing fine copper particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07107168B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101522738B1 (en) * | 2008-04-01 | 2015-05-26 | 도와 일렉트로닉스 가부시키가이샤 | Copper Powder For Conductive Paste and Method For Preparation Thereof |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1300381C (en) * | 2003-06-16 | 2007-02-14 | 昆明理工恒达科技有限公司 | Preparing method for conductive composite bronze powder and composite bronze conductive sizing agent |
| KR20050003164A (en) * | 2003-06-30 | 2005-01-10 | 나노솔루션주식회사 | Method for manufacturing copper powder |
| JP5820202B2 (en) | 2010-09-30 | 2015-11-24 | Ｄｏｗａエレクトロニクス株式会社 | Copper powder for conductive paste and method for producing the same |
| CN102601383A (en) * | 2012-03-30 | 2012-07-25 | 电子科技大学 | Method for preparing ultrafine copper powder at room temperature |
| JP6181368B2 (en) * | 2012-12-14 | 2017-08-16 | ユニチカ株式会社 | Aggregates of fibrous silver particles |
| JP6181367B2 (en) * | 2012-12-14 | 2017-08-16 | ユニチカ株式会社 | Coated fibrous copper particulate aggregate |
-
1987
- 1987-01-27 JP JP1706487A patent/JPH07107168B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101522738B1 (en) * | 2008-04-01 | 2015-05-26 | 도와 일렉트로닉스 가부시키가이샤 | Copper Powder For Conductive Paste and Method For Preparation Thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63186803A (en) | 1988-08-02 |
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