JPS5912723B2 - Copper powder manufacturing method - Google Patents
Copper powder manufacturing methodInfo
- Publication number
- JPS5912723B2 JPS5912723B2 JP4007581A JP4007581A JPS5912723B2 JP S5912723 B2 JPS5912723 B2 JP S5912723B2 JP 4007581 A JP4007581 A JP 4007581A JP 4007581 A JP4007581 A JP 4007581A JP S5912723 B2 JPS5912723 B2 JP S5912723B2
- Authority
- JP
- Japan
- Prior art keywords
- copper powder
- copper
- hydrazine
- powder
- powder manufacturing
- 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
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Description
【発明の詳細な説明】
この発明は微粒子状の銅粉末の製造方法に関するもので
ある。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing finely divided copper powder.
銅粉末の製造方法としては代表的なものに溶湯の粉化法
１機械的粉砕法、あるいは電解法などがある。Typical methods for producing copper powder include molten metal pulverization method 1, mechanical pulverization method, and electrolytic method.
このうち、溶湯の粉化法は溶融金属から直接粉末を製造
する方法で、これには溶融金属を水中に流したり、ある
いは凝固のときに激しく攪拌して粗い粒子にする粒状化
法、また溶融金属の細流を小孔から流出させ、これに圧
縮ガスあるいは水流ジェットを作用させて溶融金属を細
かく分散させると同時に、冷却凝固させて粉末を製造す
る噴霧法などがある。Among these methods, the molten metal powdering method is a method for directly producing powder from molten metal.This method includes granulation methods, in which the molten metal is poured into water or violently stirred during solidification to form coarse particles. There is an atomization method in which a small stream of metal is made to flow out of a small hole, and a compressed gas or a water jet is applied to the stream to finely disperse the molten metal, and at the same time, the metal is cooled and solidified to produce a powder.
しかしながら、粉化時に被粉砕物に力が加わる時間が短
かいため、微粉を製造しにくいという欠点が見られる。However, since the time during which force is applied to the material to be ground during pulverization is short, it is difficult to produce fine powder.
機械的粉砕法は電解析出物やガス還元法で製造された金
属銅をボールミル、振動ミルなどで粉砕するというもの
であり、比較的操作が簡単であり、粉砕コストが低床で
あるという長所があるが、粉砕時に粉砕機の摩耗その他
から不純物が混入しやすいこと、粉砕中に酸化を起こし
やすく、純度の低下が免れない面がある。The mechanical pulverization method involves pulverizing copper metal produced by electrolytic precipitation or gas reduction using a ball mill, vibration mill, etc., and has the advantage of being relatively easy to operate and having low pulverization costs. However, during pulverization, impurities are likely to be mixed in due to wear of the pulverizer and other factors, and oxidation is likely to occur during pulverization, resulting in an unavoidable decrease in purity.
次に、電解法は、金属銅を陽極とし、たとえば硫酸銅か
らなる電解液を収容する電解槽中にこの陽極とさらに陰
極を浸漬し１両極間に直流電圧を印加することによって
、陰極に銅粉を析出せしめ。Next, the electrolytic method uses metallic copper as an anode, immerses the anode and the cathode in an electrolytic bath containing an electrolytic solution made of copper sulfate, and applies a DC voltage between the two electrodes. Let the powder precipitate.
この銅粉を採取し、さらに洗浄、脱水し、そののち真空
乾燥して篩分するというものである。This copper powder is collected, washed, dehydrated, vacuum dried, and sieved.
しかし、銅粉末の酸素含有量が多くなりやすいこと。However, the oxygen content of copper powder tends to increase.
電解液が粒子の間隙に残って銅粉末の経時変化が起こり
やすいこと、銅粉末の洗浄、乾燥に注意を必要とするな
どの問題があった。There were problems such as the electrolytic solution remaining in the gaps between the particles, which caused the copper powder to change easily over time, and the need to be careful in cleaning and drying the copper powder.
したがって、この発明は微粒子状の銅粉末を製造するこ
とができる方法を提供するものである。Therefore, the present invention provides a method capable of producing fine particulate copper powder.
また、この発明は純度の高い銅粉末を製造できる方法を
提供するものである。Further, the present invention provides a method for producing highly pure copper powder.
さらに、この発明は液相反応にもとづいて銅粉末を簡単
に得ることができる方法を提供するものである。Furthermore, the present invention provides a method for easily obtaining copper powder based on a liquid phase reaction.
すなわち、この発明の要旨とするところは、炭酸銅を含
む銅含有溶液とヒドラジンあるいはヒドラジン化合物と
混合し、これを加熱することにより銅粉末を還元析出せ
しめることを特徴とする銅粉末の製造方法である。That is, the gist of the present invention is a method for producing copper powder, which comprises mixing a copper-containing solution containing copper carbonate with hydrazine or a hydrazine compound, and heating the mixture to reduce and precipitate the copper powder. be.
炭酸銅を含む銅含有溶液とヒドラジンあるいはヒドラジ
ン化合物の混合液は加熱処理されるが。A mixture of a copper-containing solution containing copper carbonate and hydrazine or a hydrazine compound is heat-treated.
加熱適正温度は４０〜１５０℃の範囲が好ましい。The appropriate heating temperature is preferably in the range of 40 to 150°C.
これは４０℃以下では銅粉末の還元析出が不十分であり
、一方１５０℃を越えると還元析出する銅粉末の粒径が
太き（なり、微粒子状で粒径に揃ったものが得られに（
（なることによる。This is because the reduction and precipitation of copper powder is insufficient at temperatures below 40℃, while at temperatures above 150℃, the particle size of the copper powder that is reduced and precipitated becomes thick (and it becomes difficult to obtain fine particles with uniform particle size). (
(By becoming.
この発明方法を実施するに当って、銅含有溶液としては
、一般的に炭酸銅を水に溶解せしめた状態の溶液を用い
、これにヒドラジンあるいはヒドラジン化合物を添加す
る方法が通常用いられる。In carrying out the method of the present invention, a method is generally used in which a copper-containing solution is a solution in which copper carbonate is dissolved in water, and hydrazine or a hydrazine compound is added thereto.
他方１反応母液に炭酸銅とヒドラジンあるいはヒドラジ
ン化合物を同時に添加する方法もあるが。On the other hand, there is also a method in which copper carbonate and hydrazine or a hydrazine compound are added simultaneously to the reaction mother liquor.
過激な反応を避けるためには上述した方法が好ましい。The above-mentioned method is preferred in order to avoid a drastic reaction.
ここで、ヒドラジンあるいはヒドラジン化合物としては
、ヒドラジンはもちろん、ヒドラジンヒトラード、硫酸
ヒドラジン、硫酸ヒドラゾニウム。Here, examples of hydrazine or hydrazine compounds include hydrazine, hydrazine hydride, hydrazine sulfate, and hydrazonium sulfate.
塩化ヒドラゾニウムなどがある。Examples include hydrazonium chloride.
また１反応時間は特に限定されないが、１５分間では一
応銅粉末の析出は見られるものの１反応溶液に未反応物
が残る。Further, the time for one reaction is not particularly limited, but after 15 minutes, unreacted substances remain in one reaction solution, although precipitation of copper powder is observed.
１２０分間反応させることによってほぼ反応は終了し、
銅粉末を生成させるに十分な時間であることが確認でき
た。The reaction was almost completed by reacting for 120 minutes,
It was confirmed that the time was sufficient to generate copper powder.
炭酸銅とヒドラジンあるいはヒドラジン化合物の混合比
は、たとえばヒドラジン化合物にヒドラジンヒトラード
を用いた場合、炭酸銅１モルに対してヒドラジンヒトラ
ードは３〜１５モルが適当である。The mixing ratio of copper carbonate and hydrazine or a hydrazine compound is, for example, when hydrazine hittride is used as the hydrazine compound, the appropriate mixing ratio is 3 to 15 moles of hydrazine hittride per 1 mole of copper carbonate.
これは３モル未満の場合は反応速度が遅（、工業的生産
には適さないからであり、また１５モルを越えると１歩
留まり１粒径において微粒子状の銅粉末が得られないか
らである。This is because if the amount is less than 3 moles, the reaction rate is slow (and unsuitable for industrial production), and if it exceeds 15 moles, fine-grained copper powder cannot be obtained in 1 yield and 1 particle size.
以下にこの発明を実施例に従って説明する。This invention will be explained below according to examples.
実施例
炭酸銅２０ｏｚを水４０００ＣＣに溶かし、さらに抱水
ヒドラジンを加えて混合した。Example 20 oz of copper carbonate was dissolved in 4000 cc of water, and hydrazine hydrate was added and mixed.
次いでこの混合液を１００℃で３時間加熱すると沈澱粉
末が得られた。This mixture was then heated at 100° C. for 3 hours to obtain a precipitated powder.
これを１時間放置して冷却し、室温下でグラスフィルタ
を用いて液を沖過し、ｐＨ７の水で水洗したのちアセト
ンで洗浄して乾燥した。This was left to cool for 1 hour, and the liquid was filtered using a glass filter at room temperature, washed with water having a pH of 7, and then washed with acetone and dried.
得られた銅粉末の粒度は１μｍの微粒子状であり、また
不純物をほとんど含まない高純度のものであった。The obtained copper powder had a particle size of 1 μm and was highly pure, containing almost no impurities.
また銅粉末の粒子形状は球状であることが確認できた。It was also confirmed that the particle shape of the copper powder was spherical.
この銅粉末はガラスフリット、有機フェスとともに混合
されることによって銅ペーストとされ。This copper powder is mixed with glass frit and organic fiber to form copper paste.
セラミック基板の上に被着したのち窒素などの非酸化性
雰囲気中で焼付けされる。After being deposited on a ceramic substrate, it is baked in a non-oxidizing atmosphere such as nitrogen.
得られた電極。回路パターンは良好な半田付は性を有す
る導電部分として厚膜回路に応用できた。The resulting electrode. The circuit pattern could be applied to thick film circuits as a conductive part with good soldering properties.
上述した実施例ではヒドラジン化合物として抱水ヒドラ
ジンを用いた例について説明したが、その他のものを用
いても同様の結果が得られることはもちろんである。Although hydrazine hydrate was used as the hydrazine compound in the above-mentioned example, it goes without saying that similar results can be obtained using other compounds.
以上この発明によれば、炭酸銅を含む銅含有溶液とヒド
ラジンあるいはヒドラジン化合物と混合し、これを加熱
することにより銅粉末を還元析出せしめるものであり、
液相反応によって微粒子状の銅粉末が簡単に得られ、特
に銅粉末を得るための特別な装置、工夫を必要としない
。According to the present invention, copper powder is reduced and precipitated by mixing a copper-containing solution containing copper carbonate with hydrazine or a hydrazine compound and heating the mixture.
Copper powder in the form of fine particles can be easily obtained by liquid phase reaction, and no special equipment or devices are required to obtain copper powder.
またこの発明により得られた銅粉末は球状をなし％また
微粒子状のものが得られるため、その後の加工処理。In addition, the copper powder obtained by this invention has a spherical shape and can be obtained in the form of fine particles, so that subsequent processing is difficult.
使用に際しても取扱いが容易である。It is easy to handle during use.
したがって銅粉末を用いて銅ペーストを作成しても分散
性にすぐれた銅ペーストが得られる。Therefore, even if a copper paste is made using copper powder, a copper paste with excellent dispersibility can be obtained.
Claims (1)
ラジン化合物と混合し、これを加熱することにより銅粉
末を還元析出せしめることを特徴とする銅粉末の製造方
法。 ２ 加熱温度は４０〜１５０℃である特許請求の範囲第
１項記載の銅粉末の製造方法。[Scope of Claims] 1. A method for producing copper powder, which comprises mixing a copper-containing solution containing copper carbonate with hydrazine or a hydrazine compound, and heating the mixture to reduce and precipitate copper powder. 2. The method for producing copper powder according to claim 1, wherein the heating temperature is 40 to 150°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4007581A JPS5912723B2 (en) | 1981-03-18 | 1981-03-18 | Copper powder manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4007581A JPS5912723B2 (en) | 1981-03-18 | 1981-03-18 | Copper powder manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS57155302A JPS57155302A (en) | 1982-09-25 |
| JPS5912723B2 true JPS5912723B2 (en) | 1984-03-26 |
Family
ID=12570800
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4007581A Expired JPS5912723B2 (en) | 1981-03-18 | 1981-03-18 | Copper powder manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5912723B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997025447A1 (en) * | 1996-01-04 | 1997-07-17 | Recupyl S.A. | Method for recovering heavy metals from acid and ammonia solutions |
| CN108526490B (en) * | 2018-05-14 | 2021-05-25 | 六盘水中联工贸实业有限公司 | Method for producing copper metal powder by using copper chloride or cuprous chloride |
-
1981
- 1981-03-18 JP JP4007581A patent/JPS5912723B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS57155302A (en) | 1982-09-25 |
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