JPS63186811A - Production of fine copper particles - Google Patents
Production of fine copper particlesInfo
- Publication number
- JPS63186811A JPS63186811A JP1707287A JP1707287A JPS63186811A JP S63186811 A JPS63186811 A JP S63186811A JP 1707287 A JP1707287 A JP 1707287A JP 1707287 A JP1707287 A JP 1707287A JP S63186811 A JPS63186811 A JP S63186811A
- Authority
- JP
- Japan
- Prior art keywords
- particle size
- copper
- borohydride
- soln
- 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.)
- Pending
Links
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 23
- 239000010949 copper Substances 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000002245 particle Substances 0.000 title abstract description 40
- 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 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- 229910010277 boron hydride Inorganic materials 0.000 claims description 3
- -1 boron hydride compound Chemical class 0.000 claims description 3
- 239000011859 microparticle Substances 0.000 claims 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 16
- 238000003756 stirring Methods 0.000 abstract description 6
- 239000012279 sodium borohydride Substances 0.000 abstract description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 abstract description 4
- 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 14
- 239000010419 fine particle Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
- 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
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 229960004643 cupric oxide Drugs 0.000 description 2
- 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
- 239000012736 aqueous medium Substances 0.000 description 1
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical class B UORVGPXVDQYIDP-UHFFFAOYSA-N 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
- 239000002244 precipitate Substances 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ＷＥ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 because the reduced particles are attracted to each other, it is difficult to control the width of the particle size distribution collected by WE. This method had the disadvantage that only wide 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、還元剤として水素化ホウ素化合物を
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 copper fine particles by reducing copper in an aqueous copper sulfate solution, in which monodispersed copper fine particles are obtained by using a boron hydride compound as a reducing agent. It is characterized by:
而して本発明の製造方法において、水素化ホウ素化合物
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ためである。The reason why boron hydride compounds are used in the production method of the present invention is that their redox potential is suitable for reducing an aqueous copper sulfate solution.
また、本発明の請求範囲において水素化ホウ素化合物と
しては、水素化ホウ素ナトリウム、水素化ホウ素カリウ
ム、水素化ホウ素アルミニウム等である。Further, in the scope of the claims of the present invention, examples of the borohydride compound include sodium borohydride, potassium borohydride, aluminum borohydride, and the like.
さらに本発明において、硫酸銅水溶液のｐ Ｈは０．５
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、０．５〜５の範囲がより好
ましく、水素化ホウ素化合物のｐ Ｈは３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、３〜１０の範囲が
より好ましく、また、反応時の温度は１０℃よりも低い
と反応が遅＜、６０℃を超えると！ｒｌａ粒子が凝集し
てくるので、１０〜６０℃の範囲がより好ましい。Furthermore, in the present invention, the pH of the copper sulfate aqueous solution is 0.5.
If it is lower than 5, the reaction will be slow, and if it is higher than 5, copper hydroxide will precipitate, so the range of 0.5 to 5 is more preferable, and the pH of the borohydride compound is lower than 3. The reaction will be extremely slow, and if the temperature is higher than 10, the reaction will be intense and the copper particles will aggregate, so a range of 3 to 10 is more preferable. When the temperature exceeds 60℃! Since the rla particles will aggregate, a temperature range of 10 to 60°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１２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 12, dilute sulfuric acid was added to adjust the pH to 1.
また、水素化ホウ素ナトリウム２０ｇを水に溶解し１１
の水溶液とした後、希硫酸を加えてｐ Ｈ＝８に調整す
る。ここで、この２液の温度を３０℃にし、硫酸銅水溶
液を攪拌しながら水素化ホウ素ナトリウム水溶液を添加
し、５分間反応させる。In addition, 20 g of sodium borohydride was dissolved in water and 11
After making an aqueous solution, dilute sulfuric acid is added to adjust the pH to 8. Here, the temperature of these two liquids is set to 30° C., and the sodium borohydride aqueous solution is added while stirring the copper sulfate aqueous solution, 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０．
５μｍ、粒度分布は０．２〜０．７μｍ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 0.
5 μm, and the particle size distribution was sharp with 70% falling in the range of 0.2 to 0.7 μm.
（実施例２）
硫酸銅結晶１２６ｇを水に熔解し１１の水溶液とした後
、希硫酸を加えてｐＨ＝３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 3.
また、水素化ホウ素カリウム１０ｇを水に溶解し１１の
水溶液とした後、希硫酸を加えてｐ ＋−１＝ ５に調
整する。ここで、この２液の温度を５０°Ｃにし、硫酸
銅水溶液を攪拌しながら、水素化ホウ素カリウム水溶液
を添加し、３分間反応させる。Further, after dissolving 10 g of potassium borohydride in water to obtain an aqueous solution of No. 11, dilute sulfuric acid was added to adjust p +-1 = 5. Here, the temperature of these two liquids is set to 50° C., and while stirring the copper sulfate aqueous solution, the potassium borohydride aqueous solution is added, and the mixture is allowed to react 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, 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０．３
μｍ、粒度分布は０．１〜０．５μｍ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 0.3.
The particle size distribution was sharp with 70% falling in the range of 0.1 to 0.5 μm.
（実施例３）
硫酸銅結晶１９７ｇを水に溶解し１ａの水溶液とした後
、希硫酸を加えてｐＨ＝４に調整する。(Example 3) After dissolving 197 g of copper sulfate crystals in water to obtain an aqueous solution of 1a, dilute sulfuric acid was added to adjust the pH to 4.
また、水素化ホウ素アルミニウム２５ｇを水に溶解し１
βの水溶液とした後、希硫酸を加えてｐ ）１＝３に調
整する。ここでこの２液の温度を２０℃にし、硫酸銅水
溶液を攪拌しながら、水素化ホウ素アルミニウム水溶液
を添加し、１０分間反応させる。In addition, 25 g of aluminum borohydride was dissolved in water and 1
After making an aqueous solution of β, dilute sulfuric acid is added to adjust p) to 1=3. Here, the temperature of these two liquids is set to 20° C., and while stirring the copper sulfate aqueous solution, an aluminum borohydride aqueous solution is added, 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０．７
μｍ、粒度分布は０．５〜１．０μｍ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 0.7.
The particle size distribution was sharp with 70% falling in the range of 0.5 to 1.0 μm.
（従来例）
水１，０ＯＯｎｊ！を攪拌しながら平均粒径５μｍの酸
化第２銅５０ｇを分散′？Ａ濁させる。(Conventional example) Water 1,0OOnj! While stirring, disperse 50 g of cupric oxide with an average particle size of 5 μm. A: Make it cloudy.
さらにこの液を攪拌しながら７０℃まで昇温し、８０％
のヒドラジンヒトラード水溶液２００ｍ Ｉ！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%.
200ml of hydrazine hittride aqueous solution I! After addition, the mixture was stirred at 70°C for 2 hours.
得られた！ＰＩｉ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。Got it! The PIi 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
μｍ１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 μm1 particle size distribution was wide, ranging from 0.5 to 10 μm, and the particles were 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
元剤として水素化ホウ素化合物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 a boron hydride compound as a reducing agent in the method of producing copper fine particles by reducing an aqueous copper sulfate solution. Since it is possible to manufacture fine copper particles with a narrow particle size distribution that are monodispersed, which was previously impossible to achieve, by controlling the particle size, it can be said to be an epoch-making method that can replace conventional manufacturing methods.
Claims (1)
て、還元剤として水素化ホウ素化合物を用いることによ
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 a boron hydride compound as a reducing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1707287A JPS63186811A (en) | 1987-01-27 | 1987-01-27 | Production of fine copper particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1707287A JPS63186811A (en) | 1987-01-27 | 1987-01-27 | Production of fine copper particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63186811A true JPS63186811A (en) | 1988-08-02 |
Family
ID=11933782
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1707287A Pending JPS63186811A (en) | 1987-01-27 | 1987-01-27 | Production of fine copper particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63186811A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| WO2012043267A1 (en) | 2010-09-30 | 2012-04-05 | Ｄｏｗａエレクトロニクス株式会社 | Copper powder for conductive paste and method for manufacturing same |
-
1987
- 1987-01-27 JP JP1707287A patent/JPS63186811A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| WO2012043267A1 (en) | 2010-09-30 | 2012-04-05 | Ｄｏｗａエレクトロニクス株式会社 | Copper powder for conductive paste and method for manufacturing same |
| US9248504B2 (en) | 2010-09-30 | 2016-02-02 | Dowa Electronics Materials Co., Ltd. | Copper powder for conductive paste and method for producing same |
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