JPS63179011A - Production of fine silver particles - Google Patents
Production of fine silver particlesInfo
- Publication number
- JPS63179011A JPS63179011A JP1196987A JP1196987A JPS63179011A JP S63179011 A JPS63179011 A JP S63179011A JP 1196987 A JP1196987 A JP 1196987A JP 1196987 A JP1196987 A JP 1196987A JP S63179011 A JPS63179011 A JP S63179011A
- Authority
- JP
- Japan
- Prior art keywords
- particle size
- silver particles
- erythorbic acid
- silver
- fine silver
- 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
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000002245 particle Substances 0.000 title abstract description 44
- 239000010946 fine silver Substances 0.000 title abstract description 7
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 35
- 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 19
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 6
- 229910052709 silver Inorganic materials 0.000 claims description 18
- 239000004332 silver Substances 0.000 claims description 18
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 17
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 6
- 239000011859 microparticle Substances 0.000 claims 2
- 238000009826 distribution Methods 0.000 abstract description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 4
- 229910052708 sodium Inorganic materials 0.000 abstract description 3
- 150000003863 ammonium salts Chemical class 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract 2
- 150000002500 ions Chemical class 0.000 abstract 1
- 239000010944 silver (metal) Substances 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000000243 solution Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- 239000010419 fine particle Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000001493 electron microscopy Methods 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
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-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
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229940026231 erythorbate 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
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 230000009993 protective function Effects 0.000 description 1
- -1 silver ions Chemical class 0.000 description 1
- 159000000000 sodium salts Chemical class 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）
本発明は硝酸銀水溶液中の銀イオン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 the Problems) The present invention provides a method for producing silver fine particles by reducing silver ions in an aqueous silver nitrate solution, in which monodispersity is achieved by using D-erythorbic acid or D-erythorbic acid salts as a reducing agent. This method is characterized by obtaining fine 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
及び、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硝酸銀水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 and 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 nitrate aqueous solution, and at the same time, the aggregation of particles is prevented. This is because it has a protective function.
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間わない。Furthermore, 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、硝酸銀水溶液のｐＨは０．３
よりも低いと反応が遅くなり、７よりも高いと銀の酸化
物が生成するので、０．３〜７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 nitrate aqueous solution is 0.3.
If it is lower than 7, the reaction will be slow, and if it is higher than 7, silver oxide will be produced, so the range of 0.3 to 7 is more preferable.
If the pH of D-erythorbic acid is lower than 0.1, the reaction will be extremely slow, so a pH of 0.1 or higher is more preferable.
If the temperature exceeds 0.degree. C., the silver particles will aggregate and the particle size distribution will become wider, so a temperature range of 0 to 100.degree. 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、
希硝酸を加えてｐ Ｈ＝ ４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 dilute nitric acid to adjust pH=4.
また、Ｄ−エリソルビン酸３０ｇを水に溶解し、５００
ｍ Ａの水溶液とした後、２８％のアンモニア水を加え
て、ｐＨ＝９に調整する。ここで、この２液の温度を２
０℃にし、硝酸銀水溶液を攪拌しなからＤ−エリソルビ
ン酸溶液を添加し、１０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 mA, 28% aqueous ammonia is added to adjust the pH to 9. Here, set the temperature of these two liquids to 2
While stirring the silver nitrate aqueous solution, add the D-erythorbic acid solution and allow to react for 10 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、この銀微粒子は球状で平均粒径が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 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、
希硝酸をｐＨ＝６に調整する。(Example 2) After dissolving 40 g of silver nitrate crystals in water to make an aqueous solution of 11,
Adjust dilute nitric acid to pH=6.
また、Ｄ−エリソルビン酸３０ｇを水に溶解し、５００
１１１１の水溶液とした後、２８％のアンモニア水を加
えて、ｐＨ＝５に調整する。ここで、この２液の温度を
５０℃にし、硝酸銀水溶液を攪拌しなからＤ−エリソル
ビン酸溶液を添加し、７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 1111, 28% aqueous ammonia was added to adjust the pH to 5. Here, the temperature of these two liquids is set to 50°C, and while stirring the silver nitrate aqueous solution, the D-erythorbic acid solution is added, and the mixture is allowed to react for 7 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０．５μｍ
、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, 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 within 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１７！の水溶液とした
後、希硝酸を加えてｐＨ＝５に調整する。(Example 3) 250g of silver nitrate crystals were dissolved in water and 17! After making an aqueous solution, dilute nitric acid is added to adjust the pH to 5.
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７０℃にし硝酸銀水溶液を攪拌しなか
らＤ−エリソルビン酸ナトリウムを添加し２０分間反応
させる。Here, the two liquids were heated to 70°C, and the aqueous silver nitrate solution was stirred, and then sodium D-erythorbate was added and allowed to react for 20 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、この銀微粒子は球状で平均粒径が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３０ｍ１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, and a 48% aqueous sodium hydroxide solution was added thereto to precipitate silver oxide particles.
These particles were reduced with formalin to create 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 particles were aggregated 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硝酸銀
水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 is a method for producing silver fine particles by reducing an aqueous silver nitrate solution, by using D-erythorbic acid or D-erythorbic acid salts as a reducing agent. This method can be said to be an epoch-making method that can replace conventional manufacturing methods because it is possible to control the particle size and produce fine, monodisperse silver particles with a narrow particle size distribution that could not be obtained using conventional methods.
Claims (1)
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。A method for producing silver microparticles by reducing an aqueous silver nitrate solution, the method comprising obtaining monodispersed silver microparticles by using D-erythorbic acid or D-erythorbic acid salts as a reducing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1196987A JPS63179011A (en) | 1987-01-21 | 1987-01-21 | Production of fine silver particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1196987A JPS63179011A (en) | 1987-01-21 | 1987-01-21 | Production of fine silver particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63179011A true JPS63179011A (en) | 1988-07-23 |
Family
ID=11792444
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1196987A Pending JPS63179011A (en) | 1987-01-21 | 1987-01-21 | Production of fine silver particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63179011A (en) |
-
1987
- 1987-01-21 JP JP1196987A patent/JPS63179011A/en active Pending
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