JPS61276907A - Production of fine silver particle - Google Patents

Production of fine silver particle

Info

Publication number
JPS61276907A
JPS61276907A JP11800085A JP11800085A JPS61276907A JP S61276907 A JPS61276907 A JP S61276907A JP 11800085 A JP11800085 A JP 11800085A JP 11800085 A JP11800085 A JP 11800085A JP S61276907 A JPS61276907 A JP S61276907A
Authority
JP
Japan
Prior art keywords
soln
silver
aqueous
silver nitrate
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
Application number
JP11800085A
Other languages
Japanese (ja)
Inventor
Hiroshi Tamemasa
博史 為政
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tanaka Kikinzoku Kogyo KK
Original Assignee
Tanaka Kikinzoku Kogyo KK
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Tanaka Kikinzoku Kogyo KK filed Critical Tanaka Kikinzoku Kogyo KK
Priority to JP11800085A priority Critical patent/JPS61276907A/en
Publication of JPS61276907A publication Critical patent/JPS61276907A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To produce fine silver particles having a narrow particle size distribution when an aqueous soln. of an ammoniac silver nitrate complex is reduced in a hydrophobic reaction vessel to deposit fine silver particles, by specifying the ratio between the amount of silver in the aqueous soln. and the amount of a reducing agent used and adding protective colloid to the reactive soln. CONSTITUTION:An aqueous soln. of glucose as a reducing agent for a silver nitrate complex is poured into a reaction vessel after the inside of the vessel is made hydrophobic by oil coating or other method, and an aqueous gelatin soln. as protective colloid is added to the soln. and stirred. An aqueous soln. of an ammoniac silver nitrate complex prepd. by adding an aqueous ammonia soln. to an aqueous silver nitrate soln. is slowly added to the soln. in the reaction vessel. At this time, the amount of silver in the silver nitrate complex soln. is regulated to 1-200g per 1l soln. of the reducing agent. Singly dispersed fine silver particles having a narrow particle size distribution are obtd. without causing coagulation.

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硝酸銀水溶液に水酸
化ナトリウムを加えて酸化銀を作り、これをホルマリン
で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 silver fine particles, a method has been used in which silver oxide is produced by adding sodium hydroxide to an aqueous silver nitrate solution, and this is reduced with formalin.

ところが、この方法は析出した微粒子同志か引き寄せ合
って凝集した粒度分布の幅の広い銀粒子しか得られず、
粒径のコントロールがテ1(シいという欠点を有してい
た。
However, this method only yields silver particles with a wide particle size distribution in which the precipitated fine particles attract each other and aggregate.
It had the disadvantage that particle size control was poor.

(発明の目的) 本発明は一ヒ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粒
径をコンI・ロールずろ製造方法を(;を供ぜんとする
ものである。
(Objective of the Invention) The present invention has been made in order to solve the above-mentioned drawbacks, and it is an object of the present invention to improve the particle size of fine silver particles having a narrow particle size distribution by using the Con-I-Roll production method ( ;

(発明の構成) 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、還元するアンモニア性硝酸銀水溶液に含まれて
いる銀星Aを還元剤溶液1りに対して1g≦A≦200
gとし、さらに反応溶液中に保BWコロイドを添加する
ことによってfi分散した銀微粒子を得ることを特徴と
するものである。
(Structure of the Invention) 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, in which silver stars contained in an ammoniacal silver nitrate aqueous solution to be reduced are used. 1g of A for 1 liter of reducing agent solution ≦A≦200
g, and by further adding a BW retaining colloid to the reaction solution, fi-dispersed silver particles are obtained.

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 it is hydrophilic, the precipitation reaction occurs on the wall of the container, so only aggregated silver particles with a wide particle size distribution are obtained. This is because by keeping the inner surface of the tank hydrophobic, the precipitation reaction can occur uniformly in the aqueous solution.

また、還元するアンモニア性硝酸銀水ン容器に含まれて
いる銀量Aを還元剤溶液1pに対して1g≦A≦200
gとした理由は、1g以下では微細すぎるために工業的
に量産する場合に取り扱いにくい欠点を有しているため
であり、200g以上では含有量が多いため析出反応が
激しくなり、粒子同士が凝集するためである。
In addition, the amount of silver A contained in the ammoniacal silver nitrate water container to be reduced is 1g≦A≦200 for 1p of reducing agent solution.
The reason for this is that if it is less than 1g, it is too fine and difficult to handle in industrial mass production.If it is more than 200g, the precipitation reaction becomes intense and the particles agglomerate together. This is to do so.

また、反応溶液中に保護コロイドを添加する理由は、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保護コロイドとしてはゼラチン、
アラビアゴム、アルブミン、プロタルピン酸、すザルピ
ン酸等である。
In addition, the reason why a protective colloid is added 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. Methods for keeping the inner surface of the reaction tank hydrophobic include oil coating, surfactant coating, Teflon coating, etc.
Protective colloids added to the reaction solution include gelatin,
These include gum arabic, albumin, protalpic acid, and sarpic acid.

ここで、本発明の実施例について説明ずろ。Examples of the present invention will now be described.

(実施例1) フ゛ト“つ!M50 gを50°Cの水300m1にン
容11イし、この溶液にセラチン水溶液を17rr+j
l!添力11シてテフロンコーチインクしたビーカー中
で攪拌しておく。また、別のヒーツ−で硝酸銀]Ogを
20m(lの水に溶解し、これに28%アンモニア水8
mRを加えてアンモニア性硝酸銀↑1i′体溶液とし、
これを先の)゛ドウIJ!!+セラチン?容ン夜中に徐
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) Add 50 g of Phyto"!
l! Stir in a beaker coated with Teflon coated ink with 11 additions. In addition, in a separate heat, dissolve silver nitrate]Og in 20ml (l) of water, and add 8% of 28% ammonia water to this.
Add mR to make an ammoniacal silver nitrate ↑1i' body solution,
This is the first)゛Do IJ! ! + Seratin? Add it gradually during the night. 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0.7μmで粒度分
布は図のように幅の狭いもので、形状番、スはぼ球形で
単分散したものであった。
As a result, the silver fine particles had an average particle size of 0.7 μm, a narrow particle size distribution as shown in the figure, and a monodisperse shape with a spherical shape.

(実施例2) フ゛ドウ+jJM 100 gを50°Cの水500m
6に?容解し、この?客演にアラビアゴム水)容ン夜を
30mρ添加してシリコーンオイルコーティングしたヒ
−カーの中でI貼拌しておく。また、別のピーカー中で
硝酸銀25gを50mj!の水に溶解し、これに28%
アンモニア水2Q rn R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11g+アラビアゴ
J、溶液中に徐々に添加する。得られた銀微粒子はデカ
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った。
(Example 2) 100 g of Fido+jJM was poured into 500 m of water at 50°C.
To 6? Understood, this? Add 30 mρ of gum arabic water and stir in a silicone oil-coated silicone oil heater. Also, in another peaker, 25g of silver nitrate was added to 50mj! dissolved in water and added 28%
Add ammonia water 2Q rn R to obtain an ammoniacal silver nitrate complex solution, and gradually add this to the above 11 g of grapes + Arabico J solution. The obtained fine silver particles were thoroughly washed with water using a decane solution, 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1.4μm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分散
したものであった。
As a result, the silver fine particles had an average particle size of 1.4 μm, had a narrow particle size distribution as shown in the figure, and was approximately spherical in shape and dispersed.

(従来例) 硝酸銀]、 5 gを30mρの水に溶解し、これに4
8%水酸化ナトリウム水溶液を加え酸化銀の粒子を沈澱
させ、この粒子をポルマリンで還元して銀粒子を作った
。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) Dissolve 5 g of silver nitrate in 30 mρ water, and add 4 g of silver nitrate to this solution.
An 8% aqueous sodium hydroxide solution was added to precipitate silver oxide particles, and the particles were reduced with Polmarine to produce silver particles. 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、この根粒子は平均粒径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。
As a result, the root particles were aggregated 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番:1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j1.:、に粒子を製造ずろ方法
において、還元するアンモニア=Iノl硝酸銀水溶液に
含まれている銀量Aを還元剤溶液11に対して1g≦A
≦200gとし、さらに反応溶液中に保護コロイド 得られなかった単分散した粒度分布の狭い微細な銀粒子
を粒径コントロールしてできるので、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 description, the production method number of the present invention is as follows: 1 A reducing agent is used in a hydrophobic reaction tank to reduce an ammoniacal silver nitrate complex solution to produce silver j1. : In the process of producing particles, the amount A of silver contained in the ammonia=I nitrate silver nitrate aqueous solution to be reduced is 1 g ≦ A with respect to the reducing agent solution 11.
≦200g, and because it is possible to control the particle size of monodispersed fine silver particles with a narrow particle size distribution that could not be obtained as a protective colloid in the reaction solution, it is an epoch-making product that can replace conventional manufacturing methods. I can say it.

【図面の簡単な説明】[Brief explanation of drawings]

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%’+’)径、#iit
軸に累積パーセン1〜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 particle size distribution measuring device, and the horizontal axis shows the %'+') diameter, #iit
The cumulative percentage is shown on the axis from 1 to 1.

Claims (1)

【特許請求の範囲】[Claims] 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、還
元するアンモニア性硝酸銀錯体溶液中に含まれている銀
量Aを還元剤溶液1lに対して1g≦A≦200gとし
さらに反応溶液中に保護コロイド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 particles by reducing an ammoniacal silver nitrate complex solution using a reducing agent in a hydrophobic reaction tank, the amount A of silver contained in the ammoniacal silver nitrate complex solution to be reduced is added to 1 liter of the reducing agent solution. 1g≦A≦200g, and further adding a protective colloid to the reaction solution to obtain monodispersed silver particles.
JP11800085A 1985-05-31 1985-05-31 Production of fine silver particle Pending JPS61276907A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP11800085A JPS61276907A (en) 1985-05-31 1985-05-31 Production of fine silver particle

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP11800085A JPS61276907A (en) 1985-05-31 1985-05-31 Production of fine silver particle

Publications (1)

Publication Number Publication Date
JPS61276907A true JPS61276907A (en) 1986-12-06

Family

ID=14725565

Family Applications (1)

Application Number Title Priority Date Filing Date
JP11800085A Pending JPS61276907A (en) 1985-05-31 1985-05-31 Production of fine silver particle

Country Status (1)

Country Link
JP (1) JPS61276907A (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001049309A (en) * 1999-08-13 2001-02-20 Dowa Mining Co Ltd Silver powder, its production and production of flaky silver powder
WO2007043664A1 (en) 2005-10-14 2007-04-19 Toyo Ink Mfg. Co., Ltd. Method for producing metal particle dispersion, conductive ink using metal particle dispersion produced by such method, and conductive coating film
WO2007126012A1 (en) 2006-04-28 2007-11-08 Toyo Ink Mfg. Co., Ltd. Method for producing conductive coating film
WO2006050248A3 (en) * 2004-10-29 2009-04-09 Nanodynamics Inc Aqueous-based method for producing ultra-fine metal powders
US7785392B2 (en) 2006-07-06 2010-08-31 Samsung Electro-Mechanics Co., Ltd. Method for manufacturing metal nanoparticles
JP2012021232A (en) * 2011-09-01 2012-02-02 Dowa Holdings Co Ltd Silver powder and method for production thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001049309A (en) * 1999-08-13 2001-02-20 Dowa Mining Co Ltd Silver powder, its production and production of flaky silver powder
WO2006050248A3 (en) * 2004-10-29 2009-04-09 Nanodynamics Inc Aqueous-based method for producing ultra-fine metal powders
WO2007043664A1 (en) 2005-10-14 2007-04-19 Toyo Ink Mfg. Co., Ltd. Method for producing metal particle dispersion, conductive ink using metal particle dispersion produced by such method, and conductive coating film
US7981327B2 (en) 2005-10-14 2011-07-19 Toyo Ink Mfg. Co. Ltd. Method for producing metal particle dispersion, conductive ink using metal particle dispersion produced by such method, and conductive coating film
US8440110B2 (en) 2005-10-14 2013-05-14 Toyo Ink Mfg Co., Ltd. Method for producing metal particle dispersion, conductive ink using metal particle dispersion produced by such method, and conductive coating film
WO2007126012A1 (en) 2006-04-28 2007-11-08 Toyo Ink Mfg. Co., Ltd. Method for producing conductive coating film
US8313800B2 (en) 2006-04-28 2012-11-20 Toyo Ink Mfg. Co., Ltd. Method for producing conductive coating film
US7785392B2 (en) 2006-07-06 2010-08-31 Samsung Electro-Mechanics Co., Ltd. Method for manufacturing metal nanoparticles
JP2012021232A (en) * 2011-09-01 2012-02-02 Dowa Holdings Co Ltd Silver powder and method for production thereof

Similar Documents

Publication Publication Date Title
US4944985A (en) Method for electroless plating of ultrafine or colloidal particles and products produced thereby
US5134039A (en) Metal articles having a plurality of ultrafine particles dispersed therein
US4863510A (en) Reduction process for preparing copper, silver, and admixed silver-palladium metal particles
WO2017190712A9 (en) Preparation method using micro-nano bubbles as crystal seeds to induce silver powder production
JPS61276907A (en) Production of fine silver particle
JPH04333504A (en) Continuous production of monodisperse fine silver powder
JPH0920903A (en) Production of monodisperse gold grain powder
JP3973236B2 (en) Method for producing monodisperse noble metal powder
JPS61243105A (en) Production of pulverous silver particles
JPS61276906A (en) Production of fine silver particle
JPH0225431B2 (en)
JPS61276905A (en) Production of fine silver particle
JPS61223110A (en) Production of ultrafine silver particle
JPS63179009A (en) Production of fine silver particles
JPS63186803A (en) Production of fine copper particles
JP7003668B2 (en) Manufacturing method of copper nano ink and copper nano ink
JPS61276904A (en) Production of fine silver particle
JPS61223111A (en) Production of fine silver powder
JPS63186805A (en) Production of fine copper particles
JPS6277406A (en) Production of fine copper particle
JPH0885807A (en) Monodispersed silver-palladium composite powder and its prodution
JPH01290706A (en) Production of fine copper powder
JPS63293107A (en) Production of gold particle
JPS63179011A (en) Production of fine silver particles
JP3122148B2 (en) Method for producing palladium powder