JPS61243105A - Production of pulverous silver particles - Google Patents
Production of pulverous silver particlesInfo
- Publication number
- JPS61243105A JPS61243105A JP8416485A JP8416485A JPS61243105A JP S61243105 A JPS61243105 A JP S61243105A JP 8416485 A JP8416485 A JP 8416485A JP 8416485 A JP8416485 A JP 8416485A JP S61243105 A JPS61243105 A JP S61243105A
- Authority
- JP
- Japan
- Prior art keywords
- soln
- silver nitrate
- silver
- size distribution
- ammoniac
- 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で還
元剤としてブドウ糖を用いてアンモニア性硝酸銀錯体溶
液を還元する方法が用いられてきた。ところが、この方
法は析出した微粒子同志が引き寄せ合って凝集した粒度
分布の幅の広い銀微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 silver fine particles, a method has been used in which an ammoniacal silver nitrate complex solution is reduced using glucose as a reducing agent in a hydrophobic reaction tank. However, this method has the drawback that only fine silver particles with a wide particle size distribution in which the precipitated fine particles attract each other and aggregate are obtained.
（発明の目的）
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銀粒子の製造
方法を提供せんとするものである。(Objective of the Invention) The present invention has been made to solve the above-mentioned drawbacks, and aims to provide a method for producing fine silver particles having a narrow dispersed particle size distribution.
（問題点を解決するための手段）
本発明は疎水性反応槽内で還元剤を用いて、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
おいて、反応溶液中にカチオン系界面活性剤を添ｈ口す
ることによって単分散した銀 ゛微粒子を得るこ
とを特徴とするものである。(Means for Solving the Problems) The present invention provides a method for producing silver fine particles by reducing an ammoniacal silver nitrate complex solution using a reducing agent in a hydrophobic reaction tank. This method is characterized in that monodispersed silver particles are obtained by adding an agent.
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、親水性の場合、析出反応が容器の壁で起
きるため、凝集した粒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 when the inner surface of the reaction tank is hydrophilic, the precipitation reaction occurs on the wall of the container, so only aggregated silver particles with a wide particle size distribution can be obtained. This is because 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錯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単分
散状態を保つようにするためである。Furthermore, the reason for adding a cationic surfactant to the reaction solution is to reduce the ammoniacal silver nitrate complex solution so that the silver fine particles precipitated in the aqueous solution do not aggregate and maintain a monodisperse state. .
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カチ
オン系界面活性剤としてはアーカード、エソミン、アー
マツク、サーフロンＳ−１２１、デュオミン等である。In the present invention, methods for keeping the inner surface of the reaction tank hydrophobic include oil coating, surfactant coating, Teflon coating, etc. Cationic surfactants added to the reaction solution include Alucard, Esomin, Armac, and Surflon. S-121, Duomin, 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Ｆ５０ｇを５０℃の水３００ｍｌに溶解し、この
溶液にカチオン系界面活性剤エソミンを１、Ｏｍ 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、別のビーカーで硝酸銀１０ｇを２０ ｍ
Ｉ！の水に溶解し、これに２８％アンモニア水８ ｍ
ｌを加えてアンモニア性硝酸銀錯体溶液とし、これを先
のブドウ糖＋エソミン溶液中に徐々に添加する。得られ
た銀微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なった。(Example 1) 50 g of Grape F is dissolved in 300 ml of water at 50° C., 1 Oml of the cationic surfactant Esomin is added to this solution, and the mixture is stirred in a Teflon-coated beaker. Also, in another beaker, add 10 g of silver nitrate to 20 m
I! of water, and add 8 m of 28% ammonia water to this.
1 to obtain an ammoniacal silver nitrate complex solution, which is gradually added to the above glucose + esomine 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、この銀微粒子は平均粒径１．２μｍ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, the silver fine particles had an average particle diameter of 1.2 μm, a narrow particle size distribution as shown in the figure, and a substantially spherical and monodisperse shape.
（実施例２）
ブドウ糖１００ｇを５０℃の水５００ｍｌに溶解し、こ
の溶液にカチオン系界面活性剤デュオミンを１．７ ｍ
ｊ！添加してシリコーンオイルコーティングしたビー
カーの中で攪拌しておく。また、別のビーカー中で硝酸
銀２５ｇを５０ｍ１の水に溶解し、これに２８％アンモ
ニア水２０ｍ１を加えてアンモニア性硝酸銀錯体溶液と
し、これを先のブドウ糖＋デュオミン溶液中に徐々に添
加する。(Example 2) 100 g of glucose was dissolved in 500 ml of water at 50°C, and 1.7 m of the cationic surfactant Duomin was added to this solution.
j! Add and stir in a beaker coated with silicone oil. Further, in another beaker, 25 g of silver nitrate is dissolved in 50 ml of water, and 20 ml of 28% aqueous ammonia is added thereto to obtain an ammoniacal silver nitrate complex solution, which is gradually added to the above glucose + Duomin solution.
得られた銀微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。The obtained silver particles were thoroughly washed with water by decantation, and subjected to particle size distribution measurement and electron microscopy observation.
その結果、この銀微粒子は平均粒径０．９μｍ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, the silver fine particles had an average particle diameter of 0.9 μm, had a narrow particle size distribution as shown in the figure, had a substantially spherical shape, and were monodispersed.
（従来例）
ブドウ糖７０ｇを５０℃の水４００ｍｌに溶解し、この
溶液をテフロンコーティングしたビーカー中で攪拌して
おく。また別のビーカー中で硝酸銀１５ｇを３０ｍｌ！
の水に溶解し、これに２８％アンモニア水１３ｍ１を加
えてアンモニア性硝酸銀錯体溶液とし、これを先のブド
ウ糖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。その結果、この銀粒子は平
均粒径６．２μｍで粒度分布は図のように幅の広い凝集
したものであった。(Conventional Example) 70 g of glucose is dissolved in 400 ml of water at 50° C., and this solution is stirred in a Teflon-coated beaker. In another beaker, add 15g of silver nitrate to 30ml!
of water, add 13 ml of 28% ammonia water to obtain an ammoniacal silver nitrate complex solution, and gradually add this to the glucose solution. The obtained silver particles were thoroughly washed with water by decantation, and subjected to particle size distribution measurement and electron microscopic observation. As a result, the silver particles were agglomerated with an average particle size of 6.2 μm and a wide particle size distribution 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
溶液中にカチ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微
細な根粒を製造できるので、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 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 cationic surfactant to the reaction solution,
Since it is possible to produce fine root nodules with a narrow, monodisperse particle size distribution that could not be obtained using conventional methods, it can be said to be an epoch-making 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微粒子の粒
度分布を測定した結果を横軸に粒径、縦軸に累積パーセ
ントを取って示したものである。The figure shows the results of measuring the particle size distribution of each fine silver particle using a light transmission type particle size distribution measuring device, with the horizontal axis representing the particle diameter and the vertical 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
応溶液中にカチ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 cationic surfactant to the reaction solution. A method for producing silver fine particles characterized by obtaining
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8416485A JPS61243105A (en) | 1985-04-19 | 1985-04-19 | Production of pulverous silver particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8416485A JPS61243105A (en) | 1985-04-19 | 1985-04-19 | Production of pulverous silver particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS61243105A true JPS61243105A (en) | 1986-10-29 |
Family
ID=13822852
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8416485A Pending JPS61243105A (en) | 1985-04-19 | 1985-04-19 | Production of pulverous silver particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61243105A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013073607A1 (en) * | 2011-11-18 | 2013-05-23 | 住友金属鉱山株式会社 | Silver powder, method for producing silver powder, and conductive paste |
| CN103506631A (en) * | 2013-09-22 | 2014-01-15 | 天津大学 | Method for preparing small-size nano-silver with chitosan as reducing agent |
| CN105880626A (en) * | 2016-05-13 | 2016-08-24 | 浙江光达电子科技有限公司 | Preparation method of sphere-like shaped superfine silver powder for front silver paste of solar cell |
| WO2021106171A1 (en) | 2019-11-28 | 2021-06-03 | エム・テクニック株式会社 | Method for producing fine particles of silver |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5236104A (en) * | 1975-09-17 | 1977-03-19 | Taihoo Kogyo Kk | Hydrocarbon fuel |
-
1985
- 1985-04-19 JP JP8416485A patent/JPS61243105A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5236104A (en) * | 1975-09-17 | 1977-03-19 | Taihoo Kogyo Kk | Hydrocarbon fuel |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013073607A1 (en) * | 2011-11-18 | 2013-05-23 | 住友金属鉱山株式会社 | Silver powder, method for producing silver powder, and conductive paste |
| JP5310967B1 (en) * | 2011-11-18 | 2013-10-09 | 住友金属鉱山株式会社 | Silver powder manufacturing method |
| CN103506631A (en) * | 2013-09-22 | 2014-01-15 | 天津大学 | Method for preparing small-size nano-silver with chitosan as reducing agent |
| CN105880626A (en) * | 2016-05-13 | 2016-08-24 | 浙江光达电子科技有限公司 | Preparation method of sphere-like shaped superfine silver powder for front silver paste of solar cell |
| WO2021106171A1 (en) | 2019-11-28 | 2021-06-03 | エム・テクニック株式会社 | Method for producing fine particles of silver |
| KR20220106128A (en) | 2019-11-28 | 2022-07-28 | 엠. 테크닉 가부시키가이샤 | Method for producing fine silver particles |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Shankar et al. | Synthesis of gold nanospheres and nanotriangles by the Turkevich approach | |
| US4863510A (en) | Reduction process for preparing copper, silver, and admixed silver-palladium metal particles | |
| US20110262646A1 (en) | Surfactant-Assisted Inorganic Nanoparticle Deposition on a Cellulose Nanocrystals | |
| CN113369491A (en) | Spherical and flaky mixed silver powder and manufacturing method thereof | |
| JPH04333504A (en) | Continuous production of monodisperse fine silver powder | |
| JPS61243105A (en) | Production of pulverous silver particles | |
| JP2004068072A (en) | Manufacturing method of silver particulate colloid dispersion solution | |
| JPS61276907A (en) | Production of fine silver particle | |
| JPH0920903A (en) | Production of monodisperse gold grain powder | |
| CN112264629A (en) | Preparation method and application of low-cost high-dispersion silver powder | |
| JPS61276905A (en) | Production of fine silver particle | |
| JPH08176620A (en) | Production of silver powder | |
| JPS61276906A (en) | Production of fine silver particle | |
| JP3820018B2 (en) | Method for producing granular silver powder | |
| JPS61276904A (en) | Production of fine silver particle | |
| JPS63186803A (en) | Production of fine copper particles | |
| JPS61223110A (en) | Production of ultrafine silver particle | |
| JPS6277406A (en) | Production of fine copper particle | |
| CN110181038A (en) | A kind of gold nanorods self-assembly and its preparation method and application | |
| JPH01290706A (en) | Production of fine copper powder | |
| JPS63186805A (en) | Production of fine copper particles | |
| CN117300147B (en) | Superfine gold powder and preparation method thereof | |
| JPS6240302A (en) | Production of pulverous copper particle | |
| JPS6277408A (en) | Production of fine copper particles | |
| JPH0211707A (en) | Production of silver fine particle |