JPS61276905A - Production of fine silver particle - Google Patents
Production of fine silver particleInfo
- Publication number
- JPS61276905A JPS61276905A JP11799885A JP11799885A JPS61276905A JP S61276905 A JPS61276905 A JP S61276905A JP 11799885 A JP11799885 A JP 11799885A JP 11799885 A JP11799885 A JP 11799885A JP S61276905 A JPS61276905 A JP S61276905A
- Authority
- JP
- Japan
- Prior art keywords
- soln
- aqueous
- silver nitrate
- silver
- particle size
- 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
Abstract
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は微細な銀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 silver particles.
（従来技術とその問題点）
従来、銀微粒子の製造方法としては疎水性反応槽内てａ
死刑としてブドウ糖を用いてアンモニア性硝酸銀↑（１
体）容器を還元する方法が用いられてきた。ところが、
この方法は析出した彷ｌ！粒子同志が引き寄−已合って
凝集し、粒度分布の幅の広い銀粒子しか得られないとい
う欠点を有していた。(Prior art and its problems) Conventionally, as a method for producing fine silver particles, a
Ammoniacal silver nitrate ↑ (1
A method of reducing the container (body) has been used. However,
This method is a great success! This method has the drawback that the particles are attracted to each other and aggregate, resulting in silver particles having only a wide particle size distribution.
（発明の目的）
本発明は−１−記の欠点を解消せんがためになされたも
のであり、分１１シした粒度分布の幅の狭い微細な銀粒
子の製造方法をｂＥ ’０’、−１んとするものである
。(Objective of the Invention) The present invention has been made in order to eliminate the drawbacks listed in -1-, and provides a method for producing fine silver particles with a narrow particle size distribution of bE '0', - 1.
（問題点を解決するための手段）
本発明は疎水性反応槽内て還元剤を用いて、アンモニア
性硝酸銀↑（１体溶液を還元して銀微粒子を製造する方
法において、反応溶液中にノニオン系界面活性剤を添加
することによって１ｙ分散した銀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 uses a reducing agent in a hydrophobic reaction tank to produce silver particles by reducing an ammoniacal silver nitrate ↑ (one-body solution). This method is characterized by obtaining 1y-dispersed silver fine particles by adding a surfactant.
そして、本発明の製造方法において反応槽内面を疎水性
に保つ理由は、７１表水性の場合、析出反応が容器の壁
で起きるため、凝集した才′）度分布の幅の広い銀粒子
しか得られないが、反応槽内面を疎水性に保つことによ
って析出反応を水溶液中で均一に起こすことができるよ
うになるからである。The reason why the inner surface of the reaction tank is kept hydrophobic in the production method of the present invention is that in the case of 71 surface water, the precipitation reaction occurs on the wall of the container, so only silver particles with a wide range of agglomerated crystallinity distribution are produced. However, by keeping the inner surface of the reaction tank hydrophobic, the precipitation reaction can occur uniformly in the aqueous solution.
また、反応溶液中にカチオン系界面活性剤を添加する理
由は、アンモニア性硝酸銀↑（１体溶液を還元すること
によって、水溶液中に析出した銀微粒子が凝集しないで
中４分１１シ状態を保つようにずろためである。In addition, the reason for adding a cationic surfactant to the reaction solution is that by reducing the ammoniacal silver nitrate ↑ (one-body solution), the silver fine particles precipitated in the aqueous solution do not aggregate and maintain the medium state. It's because of the difference.
本発明において反応槽内面を疎水性に保つ方法としては
、オイルコーティング、界面活性剤コーティング、テフ
ロンコーティング等であり、反応溶液中に添加するノニ
オン系界面活性剤としてはエソマイト、エソフγソ１、
ザーフロンＳ −１４，１ザ−フロンＳ −１４５等で
ある。In the present invention, methods for keeping the inner surface of the reaction tank hydrophobic include oil coating, surfactant coating, Teflon coating, etc. Nonionic surfactants added to the reaction solution include Esomite, Esof γ So1,
These include Zaflon S-14, 1 Zaflon S-145, etc.
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）
ブドウｔＪＩＷ ５０ ｇを５０°Ｃの水３００ｍ＋８
に熔解し、この溶液にノニオン系界面活性剤エソマイ［
を１．２ ｍ （ｌ添加してテフロンコーティングした
ビーカー中で攪拌しておく。また、別のビーカーてｆｉ
ｌ“ｊ酸銀１． Ｏｇを２０ｍＡの水乙こ熔解し、これ
に２８％アンモニア水８ｍｐを加えてアン干ニア性硝酸
８Ｎ １ｇ体溶液とし、これを先のブドウ糖＋エソマイ
ト溶液中に徐々に添加する。得られた銀微粒子ｉｆｔデ
カンチーシコンにより充分に水で洗浄して、粒度分布測
定及び電子顕微鏡観察を行なった。(Example 1) 50 g of grape tJIW was added to 300 m of water at 50°C +8
and add the nonionic surfactant Esomy to this solution.
Add 1.2 m (l) of water and stir in a Teflon-coated beaker.
Melt 1.0 g of silver acid at 20 mA in water, add 8 mp of 28% ammonia water to make a solution of 1 g of 8N ammonia nitric acid, and gradually add this to the glucose + esomite solution. The obtained silver particles were thoroughly washed with water and subjected to particle size distribution measurement and electron microscopic observation.
その結果、この銀微粒子は平均粒径１．５ ｔ！ｍで粒
度分布は図のように幅の）ノニい４）ので、形状はほぼ
ｆＦ、形て分散したものてあ−２た。As a result, the average particle size of these silver particles was 1.5 tons! As shown in the figure, the particle size distribution was wide (as shown in the figure), so the shape was approximately fF, and the shape was dispersed.
（実施例２）
ブドウ１Ｉ７ｉ １００ 、、を５０ ’ｒ：の水５０
０ｍｐｌこン１゛ζ解し、この溶液にノニオン系界面活
＋４１剤、−り゛−フロンＳ−１／ＩＩを０．７ ｒｎ
ρ添加してシリ：１−ンオイルコーティングしたビーカ
ーの中で攪拌して」９く。また、別のビーカー中で硝酸
銀２５ｇを５０ｍ１．の水に溶解し、ごれに２８％アン
モニア水２０ｍ１を加えてアンモニア性硝酸１門１１体
溶液とし、これを先のフ゛トつ本１ｉＨ→−“リーーフ
１１ンＳ−１４１／ｌン１奴中に徐々々に添加する。１
ゴられた銀微粒子も３１′デカンテーシヨンにより充分
に水で’ｔｊＩ＝ ？’／’ シて、１′）”Ｌ度分布
測定及び電子顕／、５鏡観察を行った。(Example 2) Grape 1I7i 100, 50'r: water 50
Dissolve 0 ml of this solution and add 0.7 rn of nonionic surfactant +41 agent and -Ri-Freon S-1/II to this solution.
Add ρ and stir in a beaker coated with silicone oil. Also, in a separate beaker, 50 ml of 25 g of silver nitrate was added. of water, add 20ml of 28% ammonia water to the dirt to make an ammoniacal nitric acid solution. Gradually add to 1.
The crushed silver particles are also thoroughly soaked with water by 31' decantation. 1')"L power distribution measurement and electron microscopy/5 mirror observation were performed.
その結果、この銀微粒子は丁均才′◇径０．９ ｔｔ
ｍで、粒度分布は図のように幅の狭いもので形状はほぼ
球形で単分散したものであった。As a result, these fine silver particles had a diameter of 0.9 tt.
m, the particle size distribution was narrow as shown in the figure, and the shape was almost spherical and monodisperse.
（従来例）
フ゛トウ！Ｆｉ ７０ ｇを５０℃の水４００ｍ４に？
８角了し、この溶液をテフロンコーティングしたビーカ
一中で１景拌しておく。また別のビーカー中で硝酸１尺
１５ｇを３０ｍｆｆの水に？容解し、これに２８％アン
モニア水１３ｍｎを加えてアンモニア性硝酸銀銘体溶液
とし、これを先のブドウＩＪ、’ｉ溶液中に徐々に添加
する。得られた銀粒子はデカンテーションにより充分に
水で洗浄して、粒度分布測定及び電子顕微鏡観察を行っ
た。(Conventional example) Fight! 70 g of Fi in 400 m4 of water at 50℃?
After 8 hours, stir this solution in a Teflon-coated beaker. In another beaker, add 15g of nitric acid to 30mff of water? Dissolve and add 13 ml of 28% ammonia water to obtain an ammoniacal silver nitrate solution, which is gradually added to the grape IJ,'i solution. The obtained silver particles were thoroughly washed with water by decantation, and subjected to particle size distribution measurement and electron microscopic observation.
その結果、この銀粒子ＩＩ平均粒径５，２μｍで粒度分
布は図のように幅の広い擬集したものであった。As a result, the average particle diameter of the silver particles II was 5.2 μm, and the particle size distribution was agglomerated with a wide range as shown in the figure.
（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疎水性
反応槽内で還元剤を使用して、アンモニア性硝酸銀錯体
溶液を還元して銀微粒子を製造する方法に於いて、反応
溶液中にノニオン系界面活性剤を添加することにより、
従来法では得られなかった単分散した粒度分布の狭いｉ
故細な銀粒子を製造できるので、従来の製造法にとって
代わることのできる画ｊｊＪｌ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 is a method for producing silver fine particles by reducing an ammoniacal silver nitrate complex solution using a reducing agent in a hydrophobic reaction tank. , by adding a nonionic surfactant to the reaction solution,
Monodisperse and narrow particle size distribution that cannot be obtained with conventional methods
Since it is possible to produce fine silver particles, it can be said to be a method that can replace conventional production methods.
図は光透過式粒度分布測定装置を用いて各銀ｉ故粒子の
１′１ｊ度分布を測定した結果を横軸に粒径、８１子軸
に累積パーセントを取って示したものである。The figure shows the results of measuring the 1'1j degree distribution of each silver i particle using a light transmission type particle size distribution measuring device, with the horizontal axis representing the particle diameter and the 81 minor axis representing the cumulative percentage.
Claims (1)
体溶液を還元して銀微粒子を製造する方法に於いて、反
応溶液中にノニオン系界面活性剤を添加することによっ
て単分散した銀微粒子を得ることを特徴とする銀微粒子
の製造方法。In a method for producing silver fine particles by reducing an ammoniacal silver nitrate complex solution using a reducing agent in a hydrophobic reaction tank, monodispersed silver fine particles are produced by adding a nonionic surfactant to the reaction solution. A method for producing fine silver particles, characterized in that:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11799885A JPS61276905A (en) | 1985-05-31 | 1985-05-31 | Production of fine silver particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11799885A JPS61276905A (en) | 1985-05-31 | 1985-05-31 | Production of fine silver particle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS61276905A true JPS61276905A (en) | 1986-12-06 |
Family
ID=14725509
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11799885A Pending JPS61276905A (en) | 1985-05-31 | 1985-05-31 | Production of fine silver particle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61276905A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6425910A (en) * | 1987-04-07 | 1989-01-27 | Norddeutsche Affinerie | Production of non-ferrous metal powder or non-ferrous metal powder mixture |
| JP2000129318A (en) * | 1998-10-22 | 2000-05-09 | Dowa Mining Co Ltd | Silver powder and its production |
| US6660058B1 (en) * | 2000-08-22 | 2003-12-09 | Nanopros, Inc. | Preparation of silver and silver alloyed nanoparticles in surfactant solutions |
| CN103785853A (en) * | 2014-01-24 | 2014-05-14 | 太原理工大学 | Preparation method of hybrid carbon silver composite material |
-
1985
- 1985-05-31 JP JP11799885A patent/JPS61276905A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6425910A (en) * | 1987-04-07 | 1989-01-27 | Norddeutsche Affinerie | Production of non-ferrous metal powder or non-ferrous metal powder mixture |
| JP2000129318A (en) * | 1998-10-22 | 2000-05-09 | Dowa Mining Co Ltd | Silver powder and its production |
| US6660058B1 (en) * | 2000-08-22 | 2003-12-09 | Nanopros, Inc. | Preparation of silver and silver alloyed nanoparticles in surfactant solutions |
| CN103785853A (en) * | 2014-01-24 | 2014-05-14 | 太原理工大学 | Preparation method of hybrid carbon silver composite material |
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