JPS63186807A - Production of fine copper particles - Google Patents
Production of fine copper particlesInfo
- Publication number
- JPS63186807A JPS63186807A JP1706887A JP1706887A JPS63186807A JP S63186807 A JPS63186807 A JP S63186807A JP 1706887 A JP1706887 A JP 1706887A JP 1706887 A JP1706887 A JP 1706887A JP S63186807 A JPS63186807 A JP S63186807A
- Authority
- JP
- Japan
- Prior art keywords
- copper
- particle size
- hydrazine
- particles
- soln
- 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 24
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 24
- 239000010949 copper Substances 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000002245 particle Substances 0.000 title abstract description 41
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims abstract description 19
- 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
- -1 hydrazine compound Chemical class 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- 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 12
- 238000003756 stirring Methods 0.000 abstract description 6
- 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 abstract 1
- 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
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 description 13
- 239000010419 fine particle Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- BIVUUOPIAYRCAP-UHFFFAOYSA-N aminoazanium;chloride Chemical compound Cl.NN BIVUUOPIAYRCAP-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 0.000 description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000012493 hydrazine sulfate Substances 0.000 description 3
- 229910000377 hydrazine sulfate Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229960004643 cupric oxide Drugs 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-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
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000012736 aqueous medium Substances 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
- 150000002429 hydrazines Chemical class 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
を存していた。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. The drawback was 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、還元剤としてヒドラジン化合物を用
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 is characterized in that in a method for producing fine copper particles by reducing copper in an aqueous solution of copper sulfate, monodispersed fine copper particles are obtained by using a hydrazine compound as a reducing agent. That is.
而して本発明の製造方法において、ヒドラジン化合物を
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 hydrazine compounds are used in the production method of the present invention is that their redox potential is suitable for reducing a copper sulfate aqueous solution.
また、本発明の請求範囲においてヒドラジン化合物とし
ては、ヒドラジンヒトラード、硫酸ヒドラジン、塩酸ヒ
ドラジン等を含むものである。Further, in the scope of the present invention, the hydrazine compound includes hydrazine hittride, hydrazine sulfate, hydrazine hydrochloride, and the like.
さらに本発明において、硫酸銅水溶液のｐＨは０．５よ
りも低いと反応が遅（なり、４よりも高いと銅の水酸化
物の沈殿が生成するので、０．５〜４の範囲がより好ま
しく、ヒドラジン化合物のｐＨ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°Ｃよりも低いと反
応が遅り、６０゛Ｃを超えると銅微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, if the pH of the copper sulfate aqueous solution is lower than 0.5, the reaction will be slow, and if it is higher than 4, copper hydroxide will precipitate. Preferably, if the pH of the hydrazine compound is lower than 3, the reaction will be extremely slow, and if it is higher than 10, the reaction will be intense.
Since the copper fine particles will aggregate, a range of 3 to 10 is more preferable, and if the reaction temperature is lower than 10°C, the reaction will be slow, and if it exceeds 60°C, the copper fine particles will aggregate. Therefore, 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１１の水溶液とした後
、希硫酸を加えてｐＨ＝１．５に調整する。(Example 1) After dissolving 197 g of copper sulfate crystals in water to obtain an aqueous solution of No. 11, dilute sulfuric acid was added to adjust the pH to 1.5.
また、ヒドラジンヒトラードＬｏｏｍ ｌに水を加え１
１にした後、希硫酸を加えてｐ Ｈ＝ ６に調整する。Also, add water to hydrazine Hitlerite Loom 1
After the pH is adjusted to 1, dilute sulfuric acid is added to adjust the pH to 6.
ここで、この２液の温度を３０℃にし、硫酸銅水溶液を
攪拌しながらヒドラジンヒトラードを添加し、５分間反
応させる。Here, the temperature of these two liquids is set to 30° C., hydrazine hydrogen chloride 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．
５．ｃｒｍ、粒度分布は１．０〜１．８μｍ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. crm, the particle size distribution was sharp with 70% falling in the range of 1.0 to 1.8 μm.
（実施例２）
硫酸銅結晶１２６ｇを水に溶解し１７！の水溶液とした
後、希硫酸を加えてｐＨ＝３に調整する。(Example 2) 126g of copper sulfate crystals were dissolved in water and 17! After making an aqueous solution, dilute sulfuric acid is added to adjust the pH to 3.
また、硫酸ヒドラジン６０ｇを水に溶解し１１の水溶液
とした後、水酸化ナトリウムを加えてｐ Ｈ＝４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、硫酸ヒドラジン水溶液を添加し
、７分間反応させる。Further, 60 g of hydrazine sulfate was dissolved in water to obtain an aqueous solution of No. 11, and then sodium hydroxide was added to adjust the pH to 4. Here, the temperature of these two liquids is set to 50°C, and while stirring the copper sulfate aqueous solution, the hydrazine sulfate aqueous solution is added, and the mixture is allowed to react for 7 minutes.
得られたｍｉ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 mi particles were filtered and 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１ｘの水溶液とした後
、希硫酸を加えてｐＨ＝１に調整する。(Example 3) After dissolving 197 g of copper sulfate crystals in water to make a 1x aqueous solution, dilute sulfuric acid is added to adjust the pH to 1.
また、塩酸ヒドラジンン１００ｇを水に溶解し１ｉの水
溶液とした後、２８％のアンモニア水を加えてｐＨ＝８
に調整する。ここでこの２液の温度を２０°Ｃにし、硫
酸銅水溶液を攪拌しながら、塩酸ヒドラジン水溶液を添
加し５分間反応させる。In addition, after dissolving 100 g of hydrazine hydrochloride in water to make a 1i aqueous solution, 28% ammonia water was added to the solution to pH = 8.
Adjust to. Here, the temperature of these two liquids is set to 20°C, and while stirring the copper sulfate aqueous solution, the hydrazine hydrochloride aqueous solution is added and 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１．８
μｍ、粒度分布は１．５〜２．３μｍに７０％が入るシ
ャープなものであった。As a result, the copper particles were almost spherical and had an average particle size of 1.8.
The particle size distribution was sharp with 70% falling between 1.5 and 2.3 μm.
（従来例）
水１．ＯＯＯｍｆ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 OOOmf, 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
元剤としてヒドラジン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 hydrazine compound as a reducing agent in the method of producing copper fine particles by reducing an aqueous copper sulfate solution. It is possible to manufacture fine, monodispersed copper particles with a narrow particle size distribution by controlling the particle size.
It can be said to be an epoch-making method that can replace conventional manufacturing methods.
Claims (1)
て、還元剤としてヒドラジン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。1. A method for producing copper microparticles by reducing an aqueous copper sulfate solution, the method comprising obtaining monodispersed copper microparticles by using a hydrazine compound as a reducing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1706887A JPS63186807A (en) | 1987-01-27 | 1987-01-27 | Production of fine copper particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1706887A JPS63186807A (en) | 1987-01-27 | 1987-01-27 | Production of fine copper particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63186807A true JPS63186807A (en) | 1988-08-02 |
Family
ID=11933668
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1706887A Pending JPS63186807A (en) | 1987-01-27 | 1987-01-27 | Production of fine copper particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63186807A (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 |
| CN113549948A (en) * | 2021-07-28 | 2021-10-26 | 中国科学技术大学 | Surface amino modified Cu @ NH2Nano catalyst, preparation method and application thereof |
-
1987
- 1987-01-27 JP JP1706887A patent/JPS63186807A/en active Pending
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 |
| CN113549948A (en) * | 2021-07-28 | 2021-10-26 | 中国科学技术大学 | Surface amino modified Cu @ NH2Nano catalyst, preparation method and application thereof |
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