JPS63179012A - Production of fine silver particles - Google Patents
Production of fine silver particlesInfo
- Publication number
- JPS63179012A JPS63179012A JP1197087A JP1197087A JPS63179012A JP S63179012 A JPS63179012 A JP S63179012A JP 1197087 A JP1197087 A JP 1197087A JP 1197087 A JP1197087 A JP 1197087A JP S63179012 A JPS63179012 A JP S63179012A
- Authority
- JP
- Japan
- Prior art keywords
- silver
- particle size
- soln
- particles
- ascorbic acid
- 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
- 239000002245 particle Substances 0.000 title claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000010946 fine silver Substances 0.000 title abstract description 8
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 30
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052709 silver Inorganic materials 0.000 claims abstract description 17
- 239000004332 silver Substances 0.000 claims abstract description 17
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 15
- NGBNXJUWQPLNGM-UHFFFAOYSA-N silver;azane Chemical compound N.[Ag+] NGBNXJUWQPLNGM-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002211 L-ascorbic acid Substances 0.000 claims abstract description 13
- 235000000069 L-ascorbic acid Nutrition 0.000 claims abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 15
- 239000011859 microparticle Substances 0.000 claims 2
- 125000003289 ascorbyl group Chemical class [H]O[C@@]([H])(C([H])([H])O*)[C@@]1([H])OC(=O)C(O*)=C1O* 0.000 claims 1
- 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 7
- 150000003863 ammonium salts Chemical class 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract 2
- 229910021529 ammonia Inorganic materials 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 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
- 239000010419 fine particle Substances 0.000 description 4
- 238000000034 method Methods 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
- 238000003756 stirring Methods 0.000 description 3
- 150000000994 L-ascorbates Chemical class 0.000 description 2
- 150000000996 L-ascorbic acids Chemical class 0.000 description 2
- 239000011668 ascorbic acid Substances 0.000 description 2
- 235000010323 ascorbic acid Nutrition 0.000 description 2
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 2
- 235000019187 sodium-L-ascorbate Nutrition 0.000 description 2
- 239000011755 sodium-L-ascorbate Substances 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
- 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L−アスコ
ルビン酸又はL−アスコルビン酸塩類を用いることによ
って単分散したiff1m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 L-ascorbic acid or L-ascorbate salts as a reducing agent. This method is characterized by obtaining dispersed if1m particles.
而して本発明の製造方法において、L−アスコルビン酸
及び、L−アスコ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 L-ascorbic acid and L-ascorbic 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, they are suitable for reducing aggregation of particles. This is because it works to prevent
また、本発明の請求範囲においてL−アスコルビン酸及
びL−アスコ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 addition, in the scope of the present invention, L-ascorbic acid and L-ascorbate 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(なり反応が遅くなるので
、8〜13の範囲がより好ましく、L−アスコルビン酸
のp H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、o>too℃の範囲がより好ましい。Furthermore, in the present invention, the pH of the silver ammonium complex solution
If the pH is lower than 8, silver oxide will be produced, and if it is higher than 13, ammonia gas will be generated (and the reaction will be slow), so a range of 8 to 13 is more preferable, and the pH of L-ascorbic acid is If it is lower than 0.1, the reaction will be extremely slow, so a temperature of 0.1 or more is more preferable, and if the reaction temperature is below 0°C, the reaction will be slow, and if it exceeds 100°C, the silver particles will aggregate. As the temperature increases, the width of the particle size distribution becomes wider, so a range of o>too°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IIlの水溶液としりt
t、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IOに調整する。(Example 1) Dissolve 50 g of silver nitrate crystals in water to make an aqueous solution of IIl.
t, add 28% aqueous ammonia to obtain a silver ammonium complex solution, and adjust its pH to IO.
また、L−アスコルビン酸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=2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がらL−
アスコルビン酸溶液を添加し、4分間反応させる。In addition, 30 g of L-ascorbic acid was dissolved in water and 500 g of L-ascorbic acid was dissolved in water.
After preparing an aqueous solution of 28% aqueous ammonia, the pH was adjusted to 2. Here, set the temperature of these two liquids to 2
At 0°C, add L- while stirring the silver ammonium complex solution.
Add ascorbic acid solution and allow to react 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 particles were filtered, washed, and subjected to particle size distribution measurement and electron microscopy observation.
その結果、このtlfi!粒子は球形で平均粒径が0.
1μm、粒度分布は0.07〜0.13μmに70%が
入るシャープなものであった。As a result, this tlfi! The particles are spherical and have an average diameter of 0.
1 μm, and the particle size distribution was sharp with 70% falling between 0.07 and 0.13 μm.
(実施例2)
硝酸銀結晶40gを水に溶解し1Nの水溶液としり後、
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 2) After dissolving 40 g of silver nitrate crystals in water to make a 1N aqueous solution,
Add 28% ammonia water to prepare a silver ammonium complex solution, and adjust its pH to 8.
また、L−アスコルビン酸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=12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攪拌しながらL
−アスコルビン酸溶液を添加し、2分間反応させる。In addition, 30 g of L-ascorbic acid was dissolved in water and 500 g of L-ascorbic acid was dissolved in water.
After making an aqueous solution of 1 ml, 28% aqueous ammonia was added to adjust the pH to 12. Here, the temperature of these two liquids was set to 10°C, and while stirring the silver ammonium complex solution, L
- Add ascorbic 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0.5μm
、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 3) After dissolving 250 g of silver nitrate crystals in water to make an aqueous solution of 11, 28% aqueous ammonia is added to prepare a silver ammonium complex solution and its pH is adjusted to 12.
また、L−アスコルビン酸ナトリウム130gt−水に
溶解し500m lの水溶液にする。Also, dissolve 130g of sodium L-ascorbate in water to make a 500ml aqueous solution.
ここでこの2液を50°Cにし銀アンモニウム錯体を攪
拌しながらL−アスコ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 are heated to 50°C, and sodium L-ascorbate is added while stirring the silver ammonium complex, and the mixture is 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1.0μm
、粒度分布は0.8〜1.3μm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 1.0 μm.
The particle size distribution was sharp with 70% falling in the range of 0.8 to 1.3 μm.
(従来例)
硝酸銀15gを3On+ 1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 3On+1 water and add 48g of silver nitrate to this solution.
% 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L−アスコルビン酸又はL−アス
コ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 L-ascorbic acid or L-ascorbic 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L−アスコルビン酸又はL
−アスコ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 a method for producing silver particles by reducing a silver ammonium complex solution, L-ascorbic acid or L-ascorbic acid is used as a reducing agent.
- A method for producing silver microparticles, which comprises obtaining monodisperse silver microparticles by using ascorbate salts.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP1197087A JPS63179012A (en) | 1987-01-21 | 1987-01-21 | Production of fine silver particles |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP1197087A JPS63179012A (en) | 1987-01-21 | 1987-01-21 | Production of fine silver particles |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS63179012A true JPS63179012A (en) | 1988-07-23 |
Family
ID=11792474
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP1197087A Pending JPS63179012A (en) | 1987-01-21 | 1987-01-21 | Production of fine silver particles |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS63179012A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH06172822A (en) * | 1992-12-07 | 1994-06-21 | Sumitomo Metal Mining Co Ltd | Production of fine silver powder |
KR100713660B1 (en) | 2005-10-07 | 2007-05-02 | 한국지질자원연구원 | Refining Method of High Purity Silver from Silver Scrap |
-
1987
- 1987-01-21 JP JP1197087A patent/JPS63179012A/en active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH06172822A (en) * | 1992-12-07 | 1994-06-21 | Sumitomo Metal Mining Co Ltd | Production of fine silver powder |
KR100713660B1 (en) | 2005-10-07 | 2007-05-02 | 한국지질자원연구원 | Refining Method of High Purity Silver from Silver Scrap |
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