JPS61223110A - Production of ultrafine silver particle - Google Patents

Production of ultrafine silver particle

Info

Publication number
JPS61223110A
JPS61223110A JP6451285A JP6451285A JPS61223110A JP S61223110 A JPS61223110 A JP S61223110A JP 6451285 A JP6451285 A JP 6451285A JP 6451285 A JP6451285 A JP 6451285A JP S61223110 A JPS61223110 A JP S61223110A
Authority
JP
Japan
Prior art keywords
silver particles
reaction vessel
ultrafine silver
hydrophobic
reducing
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
JP6451285A
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 JP6451285A priority Critical patent/JPS61223110A/en
Publication of JPS61223110A publication Critical patent/JPS61223110A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To produce easily monodispersed ultrafine silver particles by adding a protective colloid into a reaction vessel in the stage of reducing an ammoniacal silver nitrate complex soln. in a hydrophobic reaction vessel. CONSTITUTION:The protective colloid is added into the reaction vessel in the stage of producing the ultrafine silver particles by reducing the ammoniacal silver nitrate complex soln. by using a reducing agent in the hydrophobic reaction vessel. Oil coating, surface active agent coating, etc. are used to keep hydrophobic the inside surface of the reaction vessel so that a precipitation reaction of silver is uniformly induced. Gelatin, gum arabic, etc. are used as the protective colloid so that the precipitated ultrafine silver particles maintain the monodisperse state without flocculation. The monodispersed ultrafine silver particles having a uniform grain size are thus produced in a large volume.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は、超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 Field of Application) The present invention relates to a method for producing ultrafine silver particles.

(従来技術とその問題点) 従来、銀超微粒子の製造方法としては、真空容器内で原
料の銀を溶解して、蒸発した煙状の銀微粉末を回収する
方法が用いられてきた。ところがこの方法は、発生量が
少ない上に、溶湯の温度コントロールが難かしいために
粒度分布が広くなりかつ、個々の粒子がチェーン状にな
っているために単分散粒子が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 ultrafine silver particles, a method has been used in which raw material silver is dissolved in a vacuum container and evaporated smoky fine silver powder is recovered. However, this method has the disadvantage that the amount generated is small, the particle size distribution is wide because it is difficult to control the temperature of the molten metal, and monodisperse particles cannot be obtained because the individual particles are chain-shaped. had.

(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、粒径のそろった単分散した銀超微粒子を大量に製
造する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 it is an object of the present invention to provide a method for producing a large amount of monodispersed ultrafine silver particles having uniform particle sizes.

(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超微粒子を製造する方法に
おいて、反応溶液中に保護コロイドを添加することによ
って単分散した銀超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 is a method for producing ultrafine silver particles by reducing an ammoniacal silver nitrate complex solution using a reducing agent in a hydrophobic reaction tank, in which a protective colloid is added to the reaction solution. This method is characterized by obtaining monodispersed ultrafine silver particles.

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粉末しか得ら
れないため、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
るためである。
The reason why the inner surface of the reaction tank is kept hydrophobic in the production method of the present invention is that if it is hydrophilic, the precipitation reaction will occur on the wall of the container, so only aggregated silver powder 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
液中に析出した銀超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。
Further, the reason why a protective colloid is added to the reaction solution is to prevent the ultrafine silver particles precipitated in the aqueous solution by reducing the ammoniacal silver nitrate complex solution from agglomerating and to maintain a monodisperse state.

本発明において反応槽内面を疏水性に保つ方法と1  
    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、また反応溶
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、ポリビニルアルコール等である
Method for keeping the inner surface of a reaction tank hydrophobic in the present invention, and 1
Examples include oil coating, surfactant coating, Teflon coating, etc., and protective colloids added to the reaction solution include gelatin, gum arabic, albumin, polyvinyl alcohol, etc.

(実施例) ここで本発明の実施例について説明する。(Example) Examples of the present invention will now be described.

実施例1 ブドウ1120gとゼラチン0.1gを50℃の水50
m1に溶解し、この溶液をシリコーンオイルコーティン
グしたビーカー中で攪拌してお(。また別のビーカーで
硝酸銀5gを10m1の水に溶解し、これに28%アン
モニア水4ml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+ゼラチン溶液中に1滴(約0
.05 m l )添加すると溶液の色が濃赤色に変化
し、銀超微粒子が析出した。得られた銀超微粒子を透過
型電子顕微鏡で観察した結果、平均粒径80人の単分散
した球形粒子であった。
Example 1 1120g of grapes and 0.1g of gelatin were mixed with 50℃ of water at 50°C.
This solution was stirred in a beaker coated with silicone oil.In another beaker, 5 g of silver nitrate was dissolved in 10 ml of water, and 4 ml of 28% aqueous ammonia was added thereto to prepare the ammoniacal silver nitrate complex. Make a solution and add 1 drop (approximately 0.0
.. 05 ml), the color of the solution changed to deep red and ultrafine silver particles precipitated. When the obtained ultrafine silver particles were observed using a transmission electron microscope, they were found to be monodispersed spherical particles with an average particle size of 80 mm.

実施例2 ブドウW500gとポリビニルアルコール0.5gを5
0℃の水1.000m1に溶解し、この溶液を界面活性
剤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’f: 10 m lの水
に溶解し、これに28%アンモニア水8ml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+
ポリビニルアルコール溶液中に1滴(約0.1 m l
 )添加すると溶液の色が濃赤色に変化し、銀超微粒子
が析出した。
Example 2 500g of grape W and 0.5g of polyvinyl alcohol
Dissolve in 1.000 ml of water at 0° C. and stir this solution in a surfactant-coated beaker. Also,
In another beaker, dissolve 10 g'f of silver nitrate in 10 ml of water, add 8 ml of 28% ammonia water to make an ammoniacal silver nitrate complex solution, and add this to the glucose +
1 drop (approximately 0.1 ml
) When added, the color of the solution changed to deep red, and ultrafine silver particles precipitated.

得られた銀超微粒子を透過型電子顕微鏡で観察した結果
、平均粒径100人の単分散した球形粒子であった。
As a result of observing the obtained ultrafine silver particles using a transmission electron microscope, they were found to be monodispersed spherical particles with an average particle size of 100.

(従来例) ガラス製の真空容器内に設置しであるバスケット型タン
グステンヒーターの上に原料の銀を置きこの真空容器内
を5X10−’Torrまで真空に引いた後、バスケッ
ト型タングステンヒーターに通電し、銀を溶解すると溶
湯の表面から煙状の銀微粉末が発生した。
(Conventional example) After placing the raw material silver on top of a basket-type tungsten heater installed in a glass vacuum container and evacuating the inside of this vacuum container to 5 x 10-' Torr, electricity is applied to the basket-type tungsten heater. When silver was melted, fine smoke-like silver powder was generated from the surface of the molten metal.

得られた銀超微粒子を透過型電子顕微鏡で観察した結果
、平均粒径150人で粒度分布の広いチェーン状の粒子
であった。
When the obtained ultrafine silver particles were observed using a transmission electron microscope, they were found to be chain-shaped particles with an average particle size of 150 mm and a wide particle size distribution.

(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、疏水
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
液を還元して銀超微粒子を製造する方法において、反応
溶液中に保護コロイド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根部徽粒子を簡単に製造で
きるので、従来の製造方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 ultrafine silver particles by reducing an ammoniacal silver nitrate complex solution using a reducing agent in a hydrophobic reaction tank. By adding a protective colloid to the solution, it is possible to easily produce monodispersed root particles that cannot be obtained using conventional methods, so it can be said to be an epoch-making method that can replace conventional production methods.

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
体溶液を還元し銀超微粒子を製造する方法において、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
散した銀超微粒子を得ることを特徴とする銀超微粒子の
製造方法
In a method for producing ultrafine silver particles by reducing an ammoniacal silver nitrate complex solution using a reducing agent in a hydrophobic reaction tank, it is possible to obtain monodispersed ultrafine silver particles by adding a protective colloid to the reaction solution. Characteristic method for producing ultrafine silver particles
JP6451285A 1985-03-28 1985-03-28 Production of ultrafine silver particle Pending JPS61223110A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP6451285A JPS61223110A (en) 1985-03-28 1985-03-28 Production of ultrafine silver particle

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP6451285A JPS61223110A (en) 1985-03-28 1985-03-28 Production of ultrafine silver particle

Publications (1)

Publication Number Publication Date
JPS61223110A true JPS61223110A (en) 1986-10-03

Family

ID=13260329

Family Applications (1)

Application Number Title Priority Date Filing Date
JP6451285A Pending JPS61223110A (en) 1985-03-28 1985-03-28 Production of ultrafine silver particle

Country Status (1)

Country Link
JP (1) JPS61223110A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005053885A1 (en) * 2003-12-01 2005-06-16 Kojima Chemicals Co., Ltd. Process for producing metal micropowder having particle diameter uniformalized
CN110592959A (en) * 2019-08-27 2019-12-20 台州市旭泓服饰有限公司 Self-cleaning textile material for automotive interior and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005053885A1 (en) * 2003-12-01 2005-06-16 Kojima Chemicals Co., Ltd. Process for producing metal micropowder having particle diameter uniformalized
JPWO2005053885A1 (en) * 2003-12-01 2007-06-28 小島化学薬品株式会社 Method for producing fine metal powder with uniform particle size
JP4861701B2 (en) * 2003-12-01 2012-01-25 小島化学薬品株式会社 Method for producing fine metal powder with uniform particle size
CN110592959A (en) * 2019-08-27 2019-12-20 台州市旭泓服饰有限公司 Self-cleaning textile material for automotive interior and preparation method thereof

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