JPS63186809A - Production of fine copper particles - Google Patents
Production of fine copper particlesInfo
- Publication number
- JPS63186809A JPS63186809A JP1707087A JP1707087A JPS63186809A JP S63186809 A JPS63186809 A JP S63186809A JP 1707087 A JP1707087 A JP 1707087A JP 1707087 A JP1707087 A JP 1707087A JP S63186809 A JPS63186809 A JP S63186809A
- Authority
- JP
- Japan
- Prior art keywords
- particle size
- copper
- soln
- particles
- copper sulfate
- 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.)
- Pending
Links
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 25
- 239000010949 copper Substances 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000002245 particle Substances 0.000 title abstract description 40
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 15
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims description 7
- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- 239000011859 microparticle Substances 0.000 claims 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 8
- 238000003756 stirring Methods 0.000 abstract description 6
- 150000003839 salts Chemical class 0.000 abstract 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 abstract 1
- 229910001431 copper ion Inorganic materials 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 description 11
- 239000010419 fine particle Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000007788 liquid Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 229960004643 cupric oxide Drugs 0.000 description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 description 1
- 239000005750 Copper hydroxide Substances 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910001956 copper hydroxide Inorganic materials 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
Abstract
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。[Detailed description of the invention] (Industrial application 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 has been used in which copper oxide particles are reduced in an aqueous medium using a reducing agent such as hydrazine.
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, with 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 attract each other, resulting in agglomerated particles with a wide range of particle size distribution. It had the disadvantage 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 to solve the above-mentioned drawbacks, and aims to provide a method for producing dispersed fine copper particles having a narrow particle size distribution, in which the particle size can be controlled.
（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、還元剤として次亜リン酸又は次亜リ
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ものである。(Means for Solving the Problems) The present invention provides a method for producing fine copper particles by reducing copper in an aqueous solution of copper sulfate, in which monodispersion is achieved by using hypophosphorous acid or hypophosphites as a reducing agent. This method is characterized by obtaining fine copper particles.
而して本発明の製造方法において、次亜リン酸又は次亜
リ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。In the production method of the present invention, hypophosphorous acid or hypophosphite salts are used because their redox potential is suitable for reducing the copper sulfate aqueous solution and at the same time prevents particles from agglomerating. Because it has a function.
また、本発明の請求範囲において次亜リン酸又は次亜リ
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。Furthermore, in the scope of the claims of the present invention, hypophosphorous acid or hypophosphite 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ｐ Ｈ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、次亜リン酸のｐ Ｈは１よりも低いと反応が極
端に遅くなり、１０よりも高いと反応が激しくなり、銅
微粒子が凝集してくるので１〜１０の範囲がより好まし
く、また、反応時の温度は３０℃よりも低いと反応が起
こらず、１００℃を超えると銅微粒子が凝集してくるの
で、３０〜１００°Ｃの範囲がより好ましい。Furthermore, in the present invention, the pH of the copper sulfate aqueous solution is 0.3.
If it is lower than 5, the reaction will be slow, and if it is higher than 5, copper hydroxide will precipitate. Therefore, the range of 0.3 to 5 is more preferable, and the pH of hypophosphorous acid is lower than 1. The reaction will be extremely slow, and if it is higher than 10, the reaction will be intense and the copper fine particles will aggregate, so a range of 1 to 10 is more preferable, and if the reaction temperature is lower than 30°C, the reaction will not occur. First, if the temperature exceeds 100°C, the copper fine particles will aggregate, so a temperature range of 30 to 100°C is more preferable.
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１１の水溶液とした後
、希硫酸を加えてｐＨ＝１に調整する。(Example 1) After dissolving 197 g of copper sulfate crystals in water to make an aqueous solution of No. 11, dilute sulfuric acid was added to adjust the pH to 1.
また、次亜リン酸３０ｇを水に溶解し１βの水溶液とし
た後、水酸化ナトリウムを加えてｐ Ｈ＝ ８に調整す
る。ここで、この２液の温度を７０℃にし、硫酸銅水溶
液を攪拌しながら次亜リン酸を添加し、１０分間反応さ
せる。Further, 30 g of hypophosphorous acid is dissolved in water to obtain a 1β aqueous solution, and then sodium hydroxide is added to adjust the pH to 8. Here, the temperature of these two liquids is set to 70°C, hypophosphorous acid is added to the aqueous copper sulfate solution while stirring, and the mixture is allowed to react for 10 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, washed, and subjected to particle size distribution measurement and electron microscope observation.
その結果、この銅微粒子はほぼ球状で、平均粒径が１．
８μｍ、粒度分布は１．５〜２．０μｍに７０％が入る
シャープなものであった。As a result, the copper fine particles were almost spherical and had an average particle size of 1.
8 μm, and the particle size distribution was sharp with 70% falling between 1.5 and 2.0 μm.
（実施例２）
硫酸銅結晶１２６ｇを水に溶解し１１の水溶液とした後
、希硫酸を加えてｐＨ＝４に調整する。(Example 2) After dissolving 126 g of copper sulfate crystals in water to make an aqueous solution of No. 11, dilute sulfuric acid was added to adjust the pH to 4.
また、次亜リン酸２０ｇを水に溶解し１β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。Further, 20 g of hypophosphorous acid is dissolved in water to obtain a 1β aqueous solution, and then sodium hydroxide is added to adjust the pH to 5.
ここで、この２液の温度を５０℃にし、硫酸銅水溶液を
攪拌しながら次亜リン酸を添加し、５分間反応させる。Here, the temperature of these two liquids is set to 50°C, hypophosphorous acid is added to the aqueous copper sulfate solution while stirring, and the mixture is allowed to react 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, washed, and subjected to particle size distribution measurement and electron microscope observation.
その結果、この銅微粒子はほぼ球状で平均粒径が１．１
μｍ、粒度分布は０．７〜１．５μｍに７０％が入るシ
ャープなものであった。As a result, the copper fine particles were almost spherical and had an average particle size of 1.1
The particle size distribution was sharp with 70% falling in the range of 0.7 to 1.5 μm.
（実施例３）
硫酸銅結晶１９７ｇを水に溶解し１１の水溶液とした後
、希硫酸を加えてｐ Ｈ＝ ２に調整する。(Example 3) After dissolving 197 g of copper sulfate crystals in water to make an aqueous solution of No. 11, dilute sulfuric acid was added to adjust the pH to 2.
また、次亜リン酸ナトリウム５０ｇを水に溶解し１βの
水溶液にする。ここでこの２液の温度を８０℃にし硫酸
銅水溶液を攪拌しながら次亜リン酸ナトリウムを添加し
１５分間反応させる。Further, 50 g of sodium hypophosphite is dissolved in water to make a 1β aqueous solution. Here, the temperature of these two liquids is set to 80°C, and sodium hypophosphite is added while stirring the copper sulfate aqueous solution, and the mixture is allowed to react for 15 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, washed, and subjected to particle size distribution measurement and electron microscope observation.
その結果、この銅微粒子はほぼ球状で平均粒径が１．５
μｍ、粒度分布は１．２〜１．８μｍに７０％が入るシ
ャープなものであった。As a result, the copper fine particles were almost spherical and had an average particle size of 1.5.
The particle size distribution was sharp with 70% falling within the range of 1.2 to 1.8 μm.
（従来例）
水１．ＯＯＯｍｊ２を攪拌しながら平均粒径５μｍの酸
化第２銅５０ｇを分散懸濁させる。(Conventional example) Water 1. While stirring OOOmj2, 50 g of cupric oxide having an average particle size of 5 μm is dispersed and suspended.
さらにこの液を攪拌しながら７０℃まで昇温し、８０％
の抱水ヒドラジン水溶液２００ｍ ｌを添加後、７０℃
で２時間攪拌した。Furthermore, the temperature of this liquid was raised to 70℃ while stirring, and the temperature was increased to 80%.
After adding 200ml of hydrazine hydrate aqueous solution of
The mixture was stirred 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, washed, and subjected to particle size distribution measurement and electron microscope observation.
その結果、この銅微粒子は不定形で、平均粒径が３．５
μｍ、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, the copper particles were irregularly shaped and had an average particle size of 3.5.
The particle size distribution was wide, ranging from 0.5 to 10 μm, and was agglomerated.
（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
元剤として次亜リン酸又は次亜リ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。(Effects of the Invention) As is clear from the above explanation, the production method of the present invention uses hypophosphorous acid or hypophosphites as a reducing agent in the method of producing copper fine particles by reducing an aqueous copper sulfate solution. By using this method, it is possible to manufacture monodisperse fine copper particles with a narrow particle size distribution, which cannot be obtained using conventional methods, by controlling the particle size, so it can be said to be an epoch-making method that can replace conventional manufacturing methods.
Claims (1)
て、還元剤として次亜リン酸又次亜リン酸塩類を用いる
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。A method for producing copper microparticles by reducing an aqueous copper sulfate solution, the method comprising obtaining monodispersed copper microparticles by using hypophosphorous acid or hypophosphites as a reducing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1707087A JPS63186809A (en) | 1987-01-27 | 1987-01-27 | Production of fine copper particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1707087A JPS63186809A (en) | 1987-01-27 | 1987-01-27 | Production of fine copper particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63186809A true JPS63186809A (en) | 1988-08-02 |
Family
ID=11933723
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1707087A Pending JPS63186809A (en) | 1987-01-27 | 1987-01-27 | Production of fine copper particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63186809A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02294417A (en) * | 1989-05-10 | 1990-12-05 | Seidou Kagaku Kogyo Kk | Production of superfine copper powder |
| JP2008019503A (en) * | 2006-07-10 | 2008-01-31 | Samsung Electro-Mechanics Co Ltd | Method for manufacturing copper nanoparticle, and copper nanoparticle obtained by the method |
-
1987
- 1987-01-27 JP JP1707087A patent/JPS63186809A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02294417A (en) * | 1989-05-10 | 1990-12-05 | Seidou Kagaku Kogyo Kk | Production of superfine copper powder |
| JP2008019503A (en) * | 2006-07-10 | 2008-01-31 | Samsung Electro-Mechanics Co Ltd | Method for manufacturing copper nanoparticle, and copper nanoparticle obtained by the method |
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