JPS61276906A - Production of fine silver particle - Google Patents

Production of fine silver particle

Info

Publication number
JPS61276906A
JPS61276906A JP11799985A JP11799985A JPS61276906A JP S61276906 A JPS61276906 A JP S61276906A JP 11799985 A JP11799985 A JP 11799985A JP 11799985 A JP11799985 A JP 11799985A JP S61276906 A JPS61276906 A JP S61276906A
Authority
JP
Japan
Prior art keywords
soln
aqueous
particle size
silver nitrate
size distribution
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
JP11799985A
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 JP11799985A priority Critical patent/JPS61276906A/en
Publication of JPS61276906A publication Critical patent/JPS61276906A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To produce fine silver particles having a narrow particle size distribution when the aqueous soln. of an ammoniac silver nitrate complex is reduced with glucose in a hydrophobic reaction vessel to produce fine silver particles, by adding an amphoteric surfactant to the reactive soln. CONSTITUTION:The aqueous soln. of glucose as a reducing agent is poured into a reaction vessel after the inside of the vessel is made hydrophobic by oil coating or other method, and an amphoteric surfactant such as 'Surflon-131(R)', 'Betaine(R)' or amine acrylate is added to the soln. and stirred. The 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 to reduce the silver nitrate complex with the glucose. Singly dispersed fine silver particles having a narrow particle size distribution are obtd. without causing flocculation.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明はiiM細な銀粒子の製造方法に関するものであ
る。
DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for producing iiM 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7ンモニ7性硝酸銀↑11
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萩集した
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 fine silver particles, glucose was used as a reducing agent in a hydrophobic reaction tank to produce 7-moni7-functional silver nitrate↑11.
Methods have been used to reduce body fluids. However, this method has the drawback that only fine silver particles with a wide particle size distribution can be obtained, where the precipitated fine particles are attracted to each other and clustered together.

(発明の目的) 本発明は」−記の欠点を解’/l!tせんかためになさ
れたものであり、分散した粒度分布の幅の狭い微イ、田
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 solves the drawbacks of '-'/l! The purpose of this invention was to provide a method for producing fine silver particles with a narrow dispersed particle size distribution.

(発明の構成) 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、反応溶液中に両性界面活性剤を添加するごとに
よって中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 fine silver particles by reducing an ammoniacal silver nitrate complex solution using a reducing agent in a hydrophobic reaction tank. This method is characterized by obtaining medium-dispersed silver particles.

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juられない
が、反応槽内面を伸ノ1り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 if the inner surface of the reaction tank is hydrophilic, the precipitation reaction will occur on the wall of the container, so only aggregated silver particles with a wide particle size distribution will be released. This is because by keeping the inner surface of the tank elastic, the precipitation reaction can occur uniformly in the aqueous solution.

また、反応溶液中に両性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恨1敢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。
Also, the reason for adding an amphoteric surfactant to the reaction solution is
By reducing the ammoniacal silver nitrate complex solution,
This is to ensure that the 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両性
界面活性剤としてし1リー−−フロンS’−131、ザ
ーフロンS−132、ヘタイン、アクリル酸アミン等で
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. As an amphoteric surfactant added to the reaction solution, Flon S'- 131, Zarflon S-132, hetain, acrylic acid amine, 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) ブドウ糖50gを50°Cの水300mnに溶解し、こ
の溶液に両性界面活性剤、・す“−フロンS−131を
0.7 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、別のビーカーで(il!
を酸Qm 10 gを”l Qmffの水に溶解し、こ
れに28%アンモニア水8mρを加えてアンモニア1生
硝酸丘艮↑昔体ン容ン夜とし、これを先の)゛ドウ1唐
十ザーフロンS−131溶液中に徐々に添加する。
(Example 1) 50 g of glucose was dissolved in 300 ml of water at 50°C, and 0.7 ml of an amphoteric surfactant, S-Flon S-131, was added to this solution and stirred in a Teflon-coated beaker. Also, in another beaker (il!
Dissolve 10 g of acid Qm in 1 Qmff of water, add 8 mρ of 28% ammonia water, and prepare ammonia 1 fresh nitric acid. Gradually add to Zarflon S-131 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なった
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1.3 If mて
粒度分布は図のように幅の狭いもので、形状し;口Jは
球形て争分散したものであった。
As a result, the silver fine particles had an average particle size of 1.3 If m, and the particle size distribution was narrow and shaped as shown in the figure; the mouth J was spherical and dispersed.

(実施例2) フ゛トつ1店100gを50℃の水500 m +2に
?容解し、この溶液に両性7面活性剤、アクリル酸アミ
ンを1.、 Om A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i%拌しでおく。また、別の
ビーカー中で硝酸tP25gを50m/7の水に溶解し
、これに28%アンモニア水20mρを加えてアンモニ
ア性硝酸銀811体?8液とし、これを先のブドウ糖」
−アクリル酸ア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った。
(Example 2) 100g of one fish in 500m+2 of water at 50℃? Dissolve the solution and add 1. , OmA and stir in a silicone oil coated beaker. Also, in another beaker, 25g of nitric acid tP was dissolved in 50m/7 water, and 20mρ of 28% ammonia water was added to it to obtain 811 ammoniacal silver nitrate bodies. Make 8 liquids and add this to the glucose.
- Add gradually into the amine acrylate solution. 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$、l、径0.85 /
1 mて、粒度分布し、1図のように幅の狭いもので形
状シJはぼ球形でii’+分散したものであった。
As a result, these silver particles had an average $, l, diameter of 0.85/
1 m, the particle size distribution was narrow as shown in Figure 1, and the shape J was spherical and ii'+ dispersed.

(従来例) ブドウiji 70 gを50°Cの氷400汀1ρに
溶解し、この溶液をテフロン:2−ティングしたし一カ
一中てR111’l’ L、ておく。また別のビーカー
中で硝酸銀15gを30m12の水に溶解し、これに2
8%アンモニア水] 3 mρを加えてアユ/モニア性
硝酸銀錯体溶液とし、これを先のブドウ糖熔l夜中に徐
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) Dissolve 70 g of grapes in 400°C of ice at 50°C, and pour this solution into a Teflon-2-filled cup and set aside. In another beaker, dissolve 15 g of silver nitrate in 30 m12 of water, add 2
Add 3 mρ of 8% ammonia water to obtain a sweetfish/moniacal silver nitrate complex solution, and gradually add this to the glucose melt overnight. 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 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
溶ン佼を還元して銀微粒子を製造する方法に於いて、反
応溶液中に両性界面活性剤を添j>t+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、(it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 ammoniacal silver nitrate complex solution using a reducing agent in a hydrophobic reaction tank. By adding an amphoteric surfactant to the reaction solution, it is possible to produce fine root nodules with a narrow particle size distribution that is monodisperse, which could not be obtained by conventional methods. It can be said that this is an epoch-making thing that can be done.

【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](へ軸に粒径、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 silver particle using a light transmission type particle size distribution measuring device] (particle size is plotted on the horizontal axis and cumulative percentage is plotted on the vertical axis)

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於いて、反
応溶液中に両性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 obtained by adding an amphoteric surfactant to the reaction solution. A method for producing silver fine particles, characterized by:
JP11799985A 1985-05-31 1985-05-31 Production of fine silver particle Pending JPS61276906A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP11799985A JPS61276906A (en) 1985-05-31 1985-05-31 Production of fine silver particle

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP11799985A JPS61276906A (en) 1985-05-31 1985-05-31 Production of fine silver particle

Publications (1)

Publication Number Publication Date
JPS61276906A true JPS61276906A (en) 1986-12-06

Family

ID=14725535

Family Applications (1)

Application Number Title Priority Date Filing Date
JP11799985A Pending JPS61276906A (en) 1985-05-31 1985-05-31 Production of fine silver particle

Country Status (1)

Country Link
JP (1) JPS61276906A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6660058B1 (en) * 2000-08-22 2003-12-09 Nanopros, Inc. Preparation of silver and silver alloyed nanoparticles in surfactant solutions
EP2409762A1 (en) * 2010-07-20 2012-01-25 Rohm and Haas Electronic Materials LLC A composition of nanoparticles

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6660058B1 (en) * 2000-08-22 2003-12-09 Nanopros, Inc. Preparation of silver and silver alloyed nanoparticles in surfactant solutions
EP2409762A1 (en) * 2010-07-20 2012-01-25 Rohm and Haas Electronic Materials LLC A composition of nanoparticles

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