JPH07107172B2 - Method for producing fine silver particles - Google Patents
Method for producing fine silver particlesInfo
- Publication number
- JPH07107172B2 JPH07107172B2 JP1196887A JP1196887A JPH07107172B2 JP H07107172 B2 JPH07107172 B2 JP H07107172B2 JP 1196887 A JP1196887 A JP 1196887A JP 1196887 A JP1196887 A JP 1196887A JP H07107172 B2 JPH07107172 B2 JP H07107172B2
- Authority
- JP
- Japan
- Prior art keywords
- silver
- particle size
- particles
- size distribution
- silver particles
- 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.)
- Expired - Lifetime
Links
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。TECHNICAL 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。(Conventional Technology and Problems Thereof) Conventionally, as a method for producing fine silver particles, a method has been used in which sodium hydroxide is added to an aqueous solution of silver nitrate to produce silver oxide, which is reduced with formalin.
ところが、この方法では、析出した微粒子同士が引き寄
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難しいという欠点を有して
いた。However, this method has a drawback that it is difficult to control the particle size because only silver particles having a wide particle size distribution, in which precipitated fine particles are attracted to each other and aggregated, can be obtained.
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粒
径コントロール可能な製造方法を提供せんとするもので
ある。The present invention has been made in order to solve the above drawbacks, and an object of the present invention is to provide a method for controlling the particle size of dispersed fine silver particles having a narrow particle size distribution.
（問題点を解決するための手段） 本発明は銀アンモニウム錯体溶液中の銀を還元して銀微
粒子を製造する方法において、還元剤としてＤ−エリソ
ルビン酸又はＤ−エリソルビン酸塩類を用いることによ
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 Problems) The present invention is a method for producing silver fine particles by reducing silver in a silver ammonium complex solution, by using D-erythorbic acid or D-erythorbates as a reducing agent. It is characterized in that dispersed silver fine particles are obtained.
而して本発明の製造方法において、Ｄ−エリソルビン酸
又は、Ｄ−エリソルビン酸塩類を用いる理由は、これら
の酸化還元電位が銀アンモニウム錯体溶液を還元するの
に適当であると同時に粒子同士の凝集を防ぐ働きがある
ためである。Thus, in the production method of the present invention, the reason for using D-erythorbic acid or D-erythorbic acid salts is that their redox potential is suitable for reducing the silver ammonium complex solution, and at the same time the particles are aggregated. This is because it has the function of preventing
また、本発明の請求範囲においてＤ−エリソルビン酸及
びＤ−エリソルビン酸塩類としては、ナトリウム塩、カ
リウム塩、アンモニウム塩等を問わない。In the claims of the present invention, the D-erythorbic acid and D-erythorbates may be sodium salts, potassium salts, ammonium salts or the like.
さらに本発明において、銀アンモニウム錯体溶液のpHは
８よりも低いと銀の酸化物が生成し、13よりも高いとア
ンモニアガスの発生が多くなり反応が遅くなるので、８
〜13の範囲がより好ましく、Ｄ−エリソルビン酸のpHは
0.1よりも低いと反応が極端に遅くなるので、0.1以上が
より好ましく、また、反応時の温度は０℃を割ると反応
が遅くなり、100℃を超えると銀微粒子が凝集してくる
とともに、粒度分布の幅が広くなってしまうので、０〜
100℃の範囲がより好ましい。Further, in the present invention, when the pH of the silver ammonium complex solution is lower than 8, silver oxide is produced, and when it is higher than 13, the ammonia gas generation is increased and the reaction is slowed.
The range of ~ 13 is more preferred, and the pH of D-erythorbic acid is
When it is lower than 0.1, the reaction becomes extremely slow, so 0.1 or more is more preferable, and when the temperature at the time of reaction falls below 0 ° C., the reaction becomes slow, and when it exceeds 100 ° C., silver fine particles agglomerate, Since the width of the particle size distribution becomes wider,
The range of 100 ° C is more preferable.
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） 硝酸銀結晶50gを水に溶解し１の水溶液とした後、28
％アンモニア水を加えて銀アンモニウム錯体溶液とし
て、そのpHを８に調整する。(Example 1) After dissolving 50 g of silver nitrate crystals in water to prepare an aqueous solution of 1, 28
% Ammonia water is added to prepare a silver ammonium complex solution, and its pH is adjusted to 8.
また、Ｄ−エリソルビン酸30gを水に溶解し、500mlの水
溶液とした後、28％のアンモニア水を加えて、pH＝１に
調整する。ここで、この２液の温度を20℃にし、銀アン
モニウム錯体溶液を撹拌しながらＤ−エリソルビン酸溶
液を添加し、２分間反応させる。Further, 30 g of D-erythorbic acid is dissolved in water to prepare an aqueous solution of 500 ml, and 28% ammonia water is added to adjust pH = 1. Here, the temperature of the two liquids is set to 20 ° C., the D-erythorbic acid solution is added to the silver ammonium complex solution while stirring, and the mixture is reacted for 2 minutes.
得られた銀微粒子は濾過、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 fine particles were filtered and washed, and the particle size distribution was measured and observed with an electron microscope.
その結果、この銀微粒子は球形で平均粒径が0.2μｍ、
粒度分布は0.17〜0.23μｍに70％が入るシャープなもの
であった。As a result, the fine silver particles were spherical and had an average particle size of 0.2 μm.
The particle size distribution was so sharp that 70% was in the range of 0.17 to 0.23 μm.
（実施例２） 硝酸銀結晶40gを水に溶解し１の水溶液とした後、28
％アンモニア水を加えて銀アンモニウム錯体溶液とし
て、そのpHを12に調整する。(Example 2) After dissolving 40 g of silver nitrate crystals in water to prepare an aqueous solution of 1, 28
% Ammonia water is added to prepare a silver ammonium complex solution, and its pH is adjusted to 12.
また、Ｄ−エリソルビン酸30gを水に溶解し、500mlの水
溶液とした後、28％のアンモニア水を加えてpH＝10に調
整する。ここで、この２液の温度を10℃にし、銀アンモ
ニウム錯体溶液を撹拌しながらＤ−エリソルビン酸溶液
を添加し、４分間反応させる。Further, 30 g of D-erythorbic acid is dissolved in water to prepare a 500 ml aqueous solution, and 28% ammonia water is added to adjust the pH to 10. Here, the temperature of the two liquids is set to 10 ° C., the D-erythorbic acid solution is added to the silver ammonium complex solution while stirring, and the mixture is reacted for 4 minutes.
得られた銀微粒子は濾過、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 fine particles were filtered and washed, and the particle size distribution was measured and observed with an electron microscope.
その結果、この銀微粒子は球形で平均粒径が0.5μｍ、
粒度分布は0.3〜0.8μｍに70％が入るシャープなもので
あった。As a result, the silver particles were spherical and had an average particle size of 0.5 μm.
The particle size distribution was as sharp as 70% in 0.3 to 0.8 μm.
（実施例３） 硝酸銀結晶250gを水に溶解し１の水溶液とした後、28
％アンモニア水を加えて銀アンモニウム錯体溶液として
そのpHを12に調整する。Example 3 250 g of silver nitrate crystals was dissolved in water to give an aqueous solution of 1, and then 28
% Ammonia water is added to adjust the pH to 12 as a silver ammonium complex solution.
また、Ｄ−エリソルビン酸ナトリウム130gを水に溶解し
500mlの水溶液にする。Also, 130 g of sodium D-erythorbate was dissolved in water.
Make 500 ml of aqueous solution.
ここでこの２液を50℃にし銀アンモニウム錯体を撹拌し
ながらＤ−エリソルビン酸ナトリウムを添加し６分間反
応させる。Here, these two liquids are brought to 50 ° C. and sodium D-erythorbate is added while stirring the silver ammonium complex, and the mixture is reacted for 6 minutes.
得られた銀微粒子は濾過、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 fine particles were filtered and washed, and the particle size distribution was measured and observed with an electron microscope.
その結果、この銀微粒子は球形で平均粒径が1.5μｍ、
粒度分布は1.3〜1.7μｍに70％が入るシャープなもので
あった。As a result, the fine silver particles were spherical and had an average particle size of 1.5 μm.
The particle size distribution was so sharp that 70% was in the range of 1.3 to 1.7 μm.
（従来例） 硝酸銀15gを30mlの水に溶解し、これに48％水酸化ナト
リウム水溶液を加え酸化銀の粒子を沈殿させ、この粒子
をホルマリンで還元して銀粒子を作った。(Conventional Example) 15 g of silver nitrate was dissolved in 30 ml of water, a 48% sodium hydroxide aqueous solution was added thereto to precipitate silver oxide particles, and the particles were reduced with formalin to prepare silver particles.
得られた銀微粒子は濾過、洗浄して粒度分布及び電子顕
微鏡観察を行った。The obtained silver fine particles were filtered and washed to carry out particle size distribution and electron microscope observation.
その結果、この銀微粒子は平均粒径6.2μｍで粒度分布
の幅の広い凝集したものであった。As a result, the silver fine particles were aggregated with an average particle size of 6.2 μm and having 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銀アン
モニウウ錯体溶液を還元して銀微粒子を製造する方法に
おいて、還元剤としてＤ−エリソルビン酸又はＤ−エリ
ソルビン酸塩類を用いることにより、従来法では得られ
なかった単分散した粒度分布の幅の狭い微細な銀粒子を
粒径をコントロールして製造できるので、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 apparent from the above description, the production method of the present invention is a method of producing silver fine particles by reducing a silver ammonium complex solution, using D-erythorbic acid or D-erythorbates as a reducing agent. As a result, it is possible to manufacture fine silver particles having a narrow monodispersed particle size distribution, which cannot be obtained by the conventional method, by controlling the particle size. .
Claims (1)
子を製造する方法において、還元剤としてＤ−エリソル
ビン酸又はＤ−エリソルビン酸塩類を用いることによっ
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。1. A method for producing silver fine particles by reducing a silver ammonium complex solution, wherein monodispersed silver fine particles are obtained by using D-erythorbic acid or D-erythorbates as a reducing agent. Method for producing fine silver particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1196887A JPH07107172B2 (en) | 1987-01-21 | 1987-01-21 | Method for producing fine silver particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1196887A JPH07107172B2 (en) | 1987-01-21 | 1987-01-21 | Method for producing fine silver particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63179010A JPS63179010A (en) | 1988-07-23 |
| JPH07107172B2 true JPH07107172B2 (en) | 1995-11-15 |
Family
ID=11792417
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1196887A Expired - Lifetime JPH07107172B2 (en) | 1987-01-21 | 1987-01-21 | Method for producing fine silver particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07107172B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0363552B1 (en) * | 1988-07-27 | 1993-10-13 | Tanaka Kikinzoku Kogyo K.K. | Process for preparing metal particles |
| CN114951684A (en) * | 2022-06-01 | 2022-08-30 | 南通领跑者新材料科技有限公司 | Preparation method of nano spherical silver powder |
-
1987
- 1987-01-21 JP JP1196887A patent/JPH07107172B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63179010A (en) | 1988-07-23 |
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