JPH02138492A - Production of fine copper powder - Google Patents
Production of fine copper powderInfo
- Publication number
- JPH02138492A JPH02138492A JP29185088A JP29185088A JPH02138492A JP H02138492 A JPH02138492 A JP H02138492A JP 29185088 A JP29185088 A JP 29185088A JP 29185088 A JP29185088 A JP 29185088A JP H02138492 A JPH02138492 A JP H02138492A
- Authority
- JP
- Japan
- Prior art keywords
- copper
- powder
- fine
- cathode
- copper powder
- 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.)
- Granted
Links
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000010949 copper Substances 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 18
- 229910052802 copper Inorganic materials 0.000 claims abstract description 17
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 10
- BQJTUDIVKSVBDU-UHFFFAOYSA-L copper;sulfuric acid;sulfate Chemical compound [Cu+2].OS(O)(=O)=O.[O-]S([O-])(=O)=O BQJTUDIVKSVBDU-UHFFFAOYSA-L 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 14
- 229910000365 copper sulfate Inorganic materials 0.000 abstract 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 abstract 2
- 239000002659 electrodeposit Substances 0.000 abstract 2
- 238000000034 method Methods 0.000 description 12
- 230000000694 effects Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
Landscapes
- Electrolytic Production Of Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、銅粉末の製造方法に関するものであり、より
詳しくは電解による銅微粉末の製造方法に関するもので
ある。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing copper powder, and more specifically to a method for producing fine copper powder by electrolysis.
従来、銅粉末の製造方法としては、主として噴霧法、電
解法などの方法があり、それぞれ粒状あるいは樹脂状の
形状を有する銅粉が製造されている。Conventionally, methods for producing copper powder include mainly methods such as a spraying method and an electrolytic method, each of which produces copper powder having a granular or resin-like shape.
前記製造方法のうち、噴霧法で得られるものは最も微細
なものでも平均粒径が５〜１０ｔｊｍ程度であり、また
電解法で得られる樹枝状銅粉末でも個／？の粉末の技部
の太さは１〜５μｍ１長さは５〜１０μｍで、噴霧法に
比べてやや微細になるものの、粉末全体としては１０μ
ｍ以上の大きさに達し、これより微細な銅微粉末を実用
的に量産する方法は未だ見出されていない。Among the above-mentioned manufacturing methods, even the finest particles obtained by the spraying method have an average particle diameter of about 5 to 10 tjm, and even the dendritic copper powder obtained by the electrolytic method has a particle size of about 5 to 10 tjm. The thickness of the powder part is 1 to 5 μm and the length is 5 to 10 μm, which is slightly finer compared to the spray method, but the powder as a whole is 10 μm.
A method for practical mass production of fine copper powder with a size of more than 100 m has not yet been found.
本発明者らは従来法で製造されている銅粉末に比べてよ
り微細な銅微粉末の製造方法について種々検討を行った
結果、本発明を完成させたものである。The present inventors have completed the present invention as a result of various studies on methods for producing fine copper powder, which is finer than copper powder produced by conventional methods.
（問題を解決するための手段）
本発明は、硫酸酸性硫酸銅浴にＴｔを０．１ｇ／ｆｆｉ
から５ｇ／ ｌの濃度範囲で添加した電解浴中で電解を
行うことにより、陰極上に銅を微粉状に電析させること
を特徴とする銅微粉末の製造方法である。(Means for solving the problem) The present invention provides a method for adding Tt to a sulfuric acid copper sulfate bath at a rate of 0.1 g/ffi.
This is a method for producing fine copper powder, characterized by electrodepositing copper in the form of fine powder on a cathode by electrolyzing in an electrolytic bath to which copper is added in a concentration range of 5 g/l to 5 g/l.
本発明の方法に記載の電解浴中で、電解を行うことによ
り、陰極には従来のＴｔを添加しない電解浴中で電解し
た場合に比べて著しく微細で、しかも従来の電解銅粉の
特徴時な形状である樹枝状ではなく、針状に銅微粉末が
電析する。このような銅微粉末が電析する理由は不明で
あるが、Ｔｉを添加しないと発生しないことから、Ｔｉ
が何らかの作用を及ぼしていることは明確である。By performing electrolysis in the electrolytic bath described in the method of the present invention, the cathode has significantly finer particles than when electrolyzed in a conventional electrolytic bath without Tt added, and has the characteristics of conventional electrolytic copper powder. Copper fine powder is deposited in a needle-like shape, rather than in a dendritic shape. The reason why such copper fine powder is deposited is unknown, but since it does not occur unless Ti is added, Ti
It is clear that this has some kind of effect.
本発明の方法によって電析した銅微粉末にＴｉがほとん
ど検出されない。その理由については不明な点もあるが
、本発明者らは、次のように考える。Almost no Ti is detected in the fine copper powder deposited by the method of the present invention. Although the reason for this is unclear, the present inventors think as follows.
即ち、本発明の電解浴を用いて電解を行った場合、陰極
では、
Ｃｕ ”＋ ２ ｅ −一簀Ｃｕ −（１）なる電析
反応と
Ｃｕ”＋ ２Ｔｉ３＋→２Ｔｔ”十Ｃｕ−−ｍ−（２）
なるＴｉ”によるＣｕｚ″の還元反応が同時に進行して
いると考えられ、特に（２）で生成したＴｉ”″は陰極
で還元されて、７１３＋にもとる。したがって浴中のＴ
ｉ濃度はほとんど変化せず、また析出した銅微粉末中へ
のＴｉの混入もほとんど認められないのであろう。That is, when electrolysis is carried out using the electrolytic bath of the present invention, at the cathode, an electrodeposition reaction of Cu"+ 2e - ichitan Cu -(1) and Cu"+ 2Ti3+→2Tt"0Cu--m- (2)
It is thought that the reduction reaction of Cuz'' by Ti'' is proceeding at the same time, and in particular, Ti'' produced in (2) is reduced at the cathode and converted to 713+. Therefore, T in the bath
The i concentration hardly changes, and the incorporation of Ti into the precipitated fine copper powder is probably hardly observed.
次に、本発明の方法についてより詳しく説明する。Next, the method of the present invention will be explained in more detail.
電解浴中のＴｉ濃度はＯ，］、ｇ＃！から５ｇ／２の範
囲が適当である。Ｔｉ濃度が前記範囲以下では、析出し
てくる銅微粉末の微細針状化に対する効果が得られず、
一方、前記範囲以上にＴｉを添加しても効果が増大する
ことはなく、むしろ銅微粉末中へのＴｉの混入が増加す
るのみである。The Ti concentration in the electrolytic bath is O, ], g#! A range of 5 g/2 is appropriate. If the Ti concentration is below the above range, the effect of forming fine needles in the precipitated copper fine powder cannot be obtained,
On the other hand, even if Ti is added in an amount exceeding the above range, the effect will not increase, but rather the amount of Ti mixed into the fine copper powder will only increase.
電解浴中の硫酸濃度は高くするほど電流密度を大きくで
きるが、硫酸濃度をあまりに高くすると陰極電流効率が
低下するため、５０ｇ＃！から３００ｇ／ｌの濃度範囲
が望ましい。The higher the sulfuric acid concentration in the electrolytic bath, the higher the current density can be, but if the sulfuric acid concentration is too high, the cathode current efficiency will decrease, so 50g#! A concentration range of from to 300 g/l is preferred.
電解浴中の銅濃度は高くすると陰極電流効率が上昇する
が、Ｌｏｇ／ ｌ！、を越えると電析してくる銅微粉末
が粗大化する傾向を示すため、ｌＯｇ／ Ｑ以下に保つ
ことが望ましい。As the copper concentration in the electrolytic bath increases, the cathode current efficiency increases, but Log/l! If it exceeds , the deposited copper fine powder tends to become coarse, so it is desirable to keep it below lOg/Q.
電解時の電流密度は５Ａ／ｄｍ２から２ＯＡ／ｄｍ”の
範囲が適当で、この範囲以上では陰極電流効率が低下し
、また、この範囲以下では電析してくる銅微粉末が粗大
化し、場合によっては陰極に銅が膜状に析出することも
ある。The appropriate current density during electrolysis is in the range of 5 A/dm2 to 2 OA/dm. Above this range, the cathode current efficiency decreases, and below this range, the fine copper powder deposited becomes coarse and In some cases, copper may be deposited in the form of a film on the cathode.
次に、本発明の代表的な実施例について記述する。 Next, typical embodiments of the present invention will be described.
実施例■
硫酸濃度１６０ｇ／ ｉ！、、銅濃度３ｇ／尼、Ｔｉ濃
度１ｇ／ｌの電解浴中にて陰極及び陽極に銅板を用いて
電流密度］、３Ａ／ｄｍ”で電解を行い、陰極板状に銅
微粉末を電析させた。得られた銅微粉末は直径０．１〜
０．２μｍ、長さ２〜３μｍの極めて微細な針状粉末で
あった。また、粉末中へのＴｉの混入量は２０ｐｐｍ
で あ っ ノこ。Example■ Sulfuric acid concentration 160g/i! In an electrolytic bath with a copper concentration of 3 g/l and a Ti concentration of 1 g/l, electrolysis was performed using a copper plate as the cathode and anode at a current density of 3 A/dm, and fine copper powder was deposited on the cathode plate. The obtained fine copper powder had a diameter of 0.1~
It was an extremely fine needle-like powder with a diameter of 0.2 μm and a length of 2 to 3 μm. In addition, the amount of Ti mixed into the powder is 20 ppm.
De Ah Noko.
実施例■
硫酸濃度１６０ｇ／ Ｅ 、銅濃度３ｇ／ ｅ ＋ Ｔ
ｉ濃度０．１ｇ／４２の電解浴中にて陰極及び陽極に銅
板を用いて電流密度１３Ａ／ｄ＋ｓ”で電解を行い、陰
極板状に銅微粉末を電析させた。得られた銅微粉末は直
径０．５〜０．８μｍ、長さ５〜１０μｍの微細な針状
粉末であった。また、粉末中へのＴｉの混入量は１０ｐ
ｐ…以下であった。Example ■ Sulfuric acid concentration 160g/E, copper concentration 3g/e+T
Electrolysis was carried out at a current density of 13 A/d+s'' using a copper plate as the cathode and anode in an electrolytic bath with an i concentration of 0.1 g/42, and fine copper powder was electrodeposited on the cathode plate. The powder was a fine needle-like powder with a diameter of 0.5 to 0.8 μm and a length of 5 to 10 μm.The amount of Ti mixed into the powder was 10 p.
p...It was below.
実施例■
硫酸濃度１６０ｇ／ １ 、銅濃度３ｇ／ ｅ 、 Ｔ
ｉｆｉｌ、ｆ ５ｇ／ｌの電解浴中にて実施例■と同じ
条件で電解を行い陰極板状に銅微粉末を電析させた。得
られた銅微粉末は直径０．０５〜１μｍ１長さ１．５〜
２μｍの極めて微細な針状粉末であった。また、粉末中
へのＴｉの混入量は６０ ｐｐｍであった。Example ■ Sulfuric acid concentration 160g/1, copper concentration 3g/e, T
Electrolysis was carried out in an electrolytic bath containing ifil, f of 5 g/l under the same conditions as in Example (2) to deposit fine copper powder in the form of a cathode plate. The obtained fine copper powder has a diameter of 0.05-1 μm and a length of 1.5-1 μm.
It was an extremely fine needle-like powder with a diameter of 2 μm. Further, the amount of Ti mixed into the powder was 60 ppm.
以上、本発明により、従来法では得ることができなかっ
た橿めて微細な銅微粉末を電解法により大量に、かつ安
価に製造することが可能になる。As described above, according to the present invention, it becomes possible to produce extremely fine copper powder, which could not be obtained by conventional methods, in large quantities and at low cost by electrolytic method.
このような銅微粉末は電磁シールド材等の原料粉末とし
て有利に適用できる。Such fine copper powder can be advantageously applied as raw material powder for electromagnetic shielding materials and the like.
Claims (1)
濃度範囲で添加した電解浴中で電解を行うことにより、
陰極上に銅を微粉状に電析させることを特徴とする銅微
粉末の製造方法。By performing electrolysis in an electrolytic bath in which Ti was added in a concentration range of 0.1 g/l to 5 g/l to a sulfuric acid copper sulfate bath,
A method for producing fine copper powder, characterized by electrodepositing copper in the form of fine powder on a cathode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29185088A JP2706110B2 (en) | 1988-11-18 | 1988-11-18 | Production method of copper fine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29185088A JP2706110B2 (en) | 1988-11-18 | 1988-11-18 | Production method of copper fine powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02138492A true JPH02138492A (en) | 1990-05-28 |
| JP2706110B2 JP2706110B2 (en) | 1998-01-28 |
Family
ID=17774227
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP29185088A Expired - Fee Related JP2706110B2 (en) | 1988-11-18 | 1988-11-18 | Production method of copper fine powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2706110B2 (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MD4031C2 (en) * | 2008-10-30 | 2010-12-31 | Институт Прикладной Физики Академии Наук Молдовы | Process for the galvanic obtaining of copper powder |
| CN102873322A (en) * | 2011-07-13 | 2013-01-16 | 三井金属矿业株式会社 | Dendritic crystal-shaped copper powder |
| JP2013053347A (en) * | 2011-09-05 | 2013-03-21 | Mitsui Mining & Smelting Co Ltd | Dendritic copper powder |
| JP2013089576A (en) * | 2011-10-21 | 2013-05-13 | Mitsui Mining & Smelting Co Ltd | Silver-coated copper powder |
| JP2013100592A (en) * | 2011-10-21 | 2013-05-23 | Mitsui Mining & Smelting Co Ltd | Silvered copper powder |
| WO2014021037A1 (en) * | 2012-08-02 | 2014-02-06 | 三井金属鉱業株式会社 | Electroconductive film |
| EA021884B1 (en) * | 2009-03-20 | 2015-09-30 | Нано-Тек Сп. З.О.О. | Method for obtaining copper powders and nanopowders from industrial electrolytes including waste industrial electrolytes |
| CN111593373A (en) * | 2020-07-13 | 2020-08-28 | 重庆有研重冶新材料有限公司 | Production method of electrolytic copper powder for perforating charge |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104928724B (en) * | 2015-07-07 | 2017-07-07 | 昆明理工大学 | A kind of method of the electrolytic preparation dendroid fine copper powder in ethanedioic acid |
-
1988
- 1988-11-18 JP JP29185088A patent/JP2706110B2/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MD4031C2 (en) * | 2008-10-30 | 2010-12-31 | Институт Прикладной Физики Академии Наук Молдовы | Process for the galvanic obtaining of copper powder |
| EA021884B1 (en) * | 2009-03-20 | 2015-09-30 | Нано-Тек Сп. З.О.О. | Method for obtaining copper powders and nanopowders from industrial electrolytes including waste industrial electrolytes |
| CN102873322A (en) * | 2011-07-13 | 2013-01-16 | 三井金属矿业株式会社 | Dendritic crystal-shaped copper powder |
| JP2013019034A (en) * | 2011-07-13 | 2013-01-31 | Mitsui Mining & Smelting Co Ltd | Dendritic copper powder |
| JP2013053347A (en) * | 2011-09-05 | 2013-03-21 | Mitsui Mining & Smelting Co Ltd | Dendritic copper powder |
| JP2013089576A (en) * | 2011-10-21 | 2013-05-13 | Mitsui Mining & Smelting Co Ltd | Silver-coated copper powder |
| JP2013100592A (en) * | 2011-10-21 | 2013-05-23 | Mitsui Mining & Smelting Co Ltd | Silvered copper powder |
| WO2014021037A1 (en) * | 2012-08-02 | 2014-02-06 | 三井金属鉱業株式会社 | Electroconductive film |
| JP5503813B1 (en) * | 2012-08-02 | 2014-05-28 | 三井金属鉱業株式会社 | Conductive film |
| CN111593373A (en) * | 2020-07-13 | 2020-08-28 | 重庆有研重冶新材料有限公司 | Production method of electrolytic copper powder for perforating charge |
| CN111593373B (en) * | 2020-07-13 | 2022-06-17 | 重庆有研重冶新材料有限公司 | Production method of electrolytic copper powder for perforating charge |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2706110B2 (en) | 1998-01-28 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |