JPS63179010A - Production of fine silver particles - Google Patents
Production of fine silver particlesInfo
- Publication number
- JPS63179010A JPS63179010A JP1196887A JP1196887A JPS63179010A JP S63179010 A JPS63179010 A JP S63179010A JP 1196887 A JP1196887 A JP 1196887A JP 1196887 A JP1196887 A JP 1196887A JP S63179010 A JPS63179010 A JP S63179010A
- Authority
- JP
- Japan
- Prior art keywords
- silver
- particle size
- soln
- erythorbic acid
- 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.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000002245 particle Substances 0.000 title abstract description 43
- 239000010946 fine silver Substances 0.000 title abstract description 7
- CIWBSHSKHKDKBQ-DUZGATOHSA-N D-isoascorbic acid Chemical compound OC[C@@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-DUZGATOHSA-N 0.000 claims abstract description 18
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052709 silver Inorganic materials 0.000 claims abstract description 18
- 239000004332 silver Substances 0.000 claims abstract description 18
- NGBNXJUWQPLNGM-UHFFFAOYSA-N silver;azane Chemical compound N.[Ag+] NGBNXJUWQPLNGM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 150000003839 salts Chemical class 0.000 claims abstract 3
- 239000010419 fine particle Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 229940026231 erythorbate Drugs 0.000 claims description 3
- 235000010350 erythorbic acid Nutrition 0.000 claims description 3
- 239000011859 microparticle Substances 0.000 claims 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 abstract description 15
- 238000009826 distribution Methods 0.000 abstract description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 abstract description 3
- 229910052708 sodium Inorganic materials 0.000 abstract description 3
- 150000003863 ammonium salts Chemical class 0.000 abstract description 2
- 229910021529 ammonia Inorganic materials 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 229910001961 silver nitrate Inorganic materials 0.000 description 6
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910001923 silver oxide Inorganic materials 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 238000001493 electron microscopy Methods 0.000 description 2
- 239000004318 erythorbic acid Substances 0.000 description 2
- 229940026239 isoascorbic acid Drugs 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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、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 the disadvantage that only silver particles with a wide particle size distribution in which the precipitated fine particles are attracted to each other and aggregate are obtained, and that it is difficult to control the particle size.
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 to solve the above-mentioned drawbacks, and aims to provide a method for producing fine, dispersed silver particles having a narrow particle size distribution, in which the particle size can be controlled.
（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、遷元剤として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 the Problems) The present invention provides a method for producing silver fine particles by reducing silver in a silver ammonium complex solution, by using D-erythorbic acid or D-erythorbic acid salts as a transition agent. This method is characterized by obtaining monodispersed silver particles.
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。The reason why D-erythorbic acid or D-erythorbic acid salts are used in the production method of the present invention is that their redox potential is suitable for reducing the silver ammonium complex solution, and at the same time, it prevents the aggregation of particles. This is because it works to prevent
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。Further, in the scope of the present invention, D-erythorbic acid and D-erythorbic acid salts include sodium salts, potassium salts, ammonium salts, and 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。Furthermore, in the present invention, the pH of the silver ammonium complex solution
If it is lower than 8, silver oxide will be produced, and if it is higher than 13, ammonia gas will be generated more and the reaction will be slow, so a range of 8 to 13 is more preferable, and the pH of D-erythorbic acid is 0. If it is lower than 1, the reaction will be extremely slow, so it is more preferably 0.1 or higher, and the temperature during the reaction is 0.
If the temperature is below 100°C, the reaction will slow down, and if it exceeds 100°C, the silver particles will aggregate and the particle size distribution will become wider, so the range of 0 to 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１１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ｐ Ｈを８に調整する。(Example 1) After dissolving 50 g of silver nitrate crystals in water to make an aqueous solution of 11,
Add 28% ammonia water to prepare a silver ammonium complex solution and adjust its pH to 8.
また、Ｄ−エリソルビン酸３０ｇを水に溶解し、５００
ｍ ｌ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２
０℃にし、銀アンモニウム錯体溶液を攪拌しなからＤ−
エリソルビン酸溶液を添加し、２分間反応させる。In addition, 30 g of D-erythorbic acid was dissolved in water, and 500 g of D-erythorbic acid was dissolved in water.
After making an aqueous solution of 1 ml, 28% aqueous ammonia is added to adjust the pH to 1. Here, set the temperature of these two liquids to 2
While stirring the silver ammonium complex solution at 0°C,
Add erythorbic acid solution and allow to react 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 particles were filtered, washed, and subjected to particle size distribution measurement and electron microscopy observation.
その結果、この銀微粒子は球形で平均粒径が０．２μｍ
１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 silver particles were spherical and had an average particle size of 0.2 μm.
The particle size distribution was sharp with 70% falling 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１１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 make an aqueous solution of 11,
Add 28% ammonia water to prepare a silver ammonium complex solution and adjust its pH to 12.
また、Ｄ−エリソルビン酸３０ｇを水に溶解し、５００
ｍ ｌ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１
０℃にし、銀アンモニウム錯体溶液を攪拌しなからＤ−
エリソルビン酸溶液を添加し、４分間反応させる。In addition, 30 g of D-erythorbic acid was dissolved in water, and 500 g of D-erythorbic acid was dissolved in water.
After preparing an aqueous solution of 28% aqueous ammonia, the pH was adjusted to -10. Here, the temperature of these two liquids is 1
While stirring the silver ammonium complex solution at 0°C,
Add erythorbic acid solution and allow to react for 4 minutes.
得られた′ｉＢ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 'iB fine particles were filtered and washed, and subjected to particle size distribution measurement and electron microscope observation.
その結果、この銀微粒子は球形で平均粒径が０．５μｍ
１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, these fine silver particles were spherical and had an average particle size of 0.5 μm.
The particle size distribution was sharp with 70% falling in the range of 0.3 to 0.8 μm.
（実施例３）
硝酸銀結晶２５０ｇを水に溶解し１１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ｐ Ｈを１２に調整する。(Example 3) After dissolving 250 g of silver nitrate crystals in water to make an aqueous solution of 11, 28% aqueous ammonia was added to prepare a silver ammonium complex solution and its pH was adjusted to 12.
また、Ｄ−エリソルビン酸ナトリウム１３０ｇを水に溶
解し５００ｍ ｌの水溶液にする。Also, dissolve 130 g of sodium D-erythorbate in water to make 500 ml of an aqueous solution.
ここでこの２液を５０℃にし銀アンモニウム錯体を攪拌
しなから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, the two liquids were heated to 50°C, and the silver ammonium complex was stirred, and then sodium D-erythorbate was added and allowed to react 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 particles were filtered, washed, and subjected to particle size distribution measurement and electron microscopy observation.
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 silver particles were spherical and had an average particle size of 1.5 μm.
The particle size distribution was sharp with 70% falling within the range of 1.3 to 1.7 μm.
（従来例）
硝酸銀１５ｇを３０ｍ Ｉｔ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) Dissolve 15g of silver nitrate in 30ml of water and add 48g of silver nitrate to this water.
% sodium hydroxide solution was added to precipitate silver oxide particles, and the particles were reduced with formalin to produce 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 particles were filtered and washed, and the particle size distribution and electron microscope observation were performed.
その結果、この１１１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, these 111 particles were aggregates with an average particle size of 6.2 μm 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銀アン
モニウム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 clear from the above explanation, the production method of the present invention uses D-erythorbic acid or D-erythorbic acid salts as a reducing agent in the method of producing silver fine particles by reducing a silver ammonium complex solution. As a result, it is possible to manufacture fine silver particles with a narrow particle size distribution that is monodisperse, which cannot be obtained using conventional methods, by controlling the particle size, so it can be said to be a revolutionary product that can replace conventional manufacturing methods. .
Claims (1)
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。In the method of producing silver fine particles by reducing a silver ammonium complex solution, D-erythorbic acid or D
- A method for producing silver microparticles, which comprises obtaining monodispersed silver microparticles by using erythorbate salts.
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 true JPS63179010A (en) | 1988-07-23 |
| JPH07107172B2 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) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4863510A (en) * | 1988-07-27 | 1989-09-05 | Tanaka Kikinzoku Kogyo K.K. | Reduction process for preparing copper, silver, and admixed silver-palladium 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
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4863510A (en) * | 1988-07-27 | 1989-09-05 | Tanaka Kikinzoku Kogyo K.K. | Reduction process for preparing copper, silver, and admixed silver-palladium 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07107172B2 (en) | 1995-11-15 |
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