JP2684413B2 - Method for preparing ultrafine gold particles - Google Patents
Method for preparing ultrafine gold particlesInfo
- Publication number
- JP2684413B2 JP2684413B2 JP9976889A JP9976889A JP2684413B2 JP 2684413 B2 JP2684413 B2 JP 2684413B2 JP 9976889 A JP9976889 A JP 9976889A JP 9976889 A JP9976889 A JP 9976889A JP 2684413 B2 JP2684413 B2 JP 2684413B2
- Authority
- JP
- Japan
- Prior art keywords
- gold
- particles
- solution
- water
- added
- 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
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Description
【発明の詳細な説明】 (産業上の利用分野) 本発明は触媒、各種ペースト、コロイド溶液等金の超
微粒子を調製する方法に関するものである。TECHNICAL FIELD The present invention relates to a method for preparing ultrafine particles of gold such as a catalyst, various pastes and colloidal solutions.
(従来技術とその問題点) 従来、金の微粒子としては200Å以上の大きさのもの
しか安定した微粒子として調製することが出来ていな
い。(Prior art and its problems) Conventionally, as fine particles of gold, only fine particles having a size of 200 Å or more can be prepared as stable fine particles.
その主な方法として、金の酸性溶液に保護コロイドと
してゼラチン等を加え、金を水素やヒドラジン等の還元
剤で還元する方法や、金を有機溶媒に抽出したのち、該
有機溶媒を微細な粒子として不活性ガス気流中に分散さ
せ加熱分解して、金に還元し微粒子とする方法等があ
る。As the main method, gelatin or the like is added to an acidic solution of gold as a protective colloid, and gold is reduced with a reducing agent such as hydrogen or hydrazine, or gold is extracted into an organic solvent, and then the organic solvent is divided into fine particles. For example, there is a method in which the particles are dispersed in an inert gas stream, decomposed by heating, and reduced to gold to form fine particles.
しかし、金の溶液の濃度や保護コロイドの量や、他の
高分子の界面活性剤等の種類や量を変えても安定した微
粒子として調製できるのは粒子径が200Å程度が限界で
あった。However, even if the concentration of the gold solution, the amount of protective colloid, and the type and amount of other polymeric surfactants and the like were changed, stable particles could be prepared with a particle size of about 200Å.
(発明の目的) 本発明は、上記の欠点を解決するために成されたもの
で、金の超微粒子として粒子系が30〜200Åで粒子系の
範囲がせまく安定したものを調製する方法を提供するこ
とを目的とする。(Object of the invention) The present invention has been made to solve the above-mentioned drawbacks, and provides a method for preparing ultrafine gold particles having a particle size of 30 to 200Å and a stable particle size. The purpose is to do.
(問題点を解決するための手段) 本発明は、金含有溶液と還元剤を含む溶液を反応させ
て、金の超微粒子を調製するに際し、金含有溶液に水溶
性キチンを加えてのちに還元剤を含む溶液を加えて反応
させることを特徴とする金超微粒子の調製方法であり、
水溶性キチンがキチンを脱アセチル変した構造のものを
含む還元剤を含む溶液が水酸化アルカリを含むホルムア
ルデヒド溶液である。(Means for Solving Problems) The present invention involves reacting a gold-containing solution with a solution containing a reducing agent to prepare ultrafine particles of gold, and then adding water-soluble chitin to the gold-containing solution and then performing reduction. A method for preparing ultrafine gold particles, which comprises reacting by adding a solution containing an agent,
A solution containing a reducing agent containing a structure in which water-soluble chitin is deacetylated from chitin is a formaldehyde solution containing alkali hydroxide.
以下、本発明の詳細について説明する。 Hereinafter, details of the present invention will be described.
本発明の金含有溶液は最も一般的である塩化金酸の水
溶液でよく、金濃度は0.01〜0.5g/であることが好ま
しい。The gold-containing solution of the present invention may be the most common aqueous solution of chloroauric acid, and the gold concentration is preferably 0.01 to 0.5 g /.
上記の理由は調製した金の超微粒子が凝集せずまた調
製する量が経済的な範囲であるからである。The reason described above is that the prepared gold ultrafine particles do not aggregate and the amount to be prepared is in an economical range.
水溶性キチンはキチン(N−アセチル−D−グルコサ
ミンが約850連なったもの)を脱アセチル化した構造の
ものを含むものであり、水溶性の高分子化合物として金
の超微粒子が安定させる効果を有するものと考えられ
る。Water-soluble chitin contains a structure in which deacetylated chitin (about 850 N-acetyl-D-glucosamine chains) is included, and gold ultrafine particles have the effect of stabilizing water-soluble polymer compounds. Considered to have.
上記水溶性キチンのの加える量は反応させる溶液中の
濃度を0.2〜3g/とすることにより、金の粒子径を30〜
200Åに調製することができ、粒子径と水溶性キチンと
の関係は水溶性キチンの濃度を高くするに従い粒子径が
小さくなり、粒子径の分布範囲は平均粒子径の±20%で
85%以上のものが得られる。The amount of the water-soluble chitin added is such that the concentration in the solution to be reacted is 0.2 to 3 g /, so that the particle size of gold is 30 to
The particle size can be adjusted to 200Å, and the relationship between the particle size and water-soluble chitin decreases as the concentration of water-soluble chitin increases, and the particle size distribution range is ± 20% of the average particle size.
More than 85% can be obtained.
還元剤を含む溶液は水酸化アルカリとして水酸化ナト
リウムまたは水酸化カリウムを加えてあるホルムアルデ
ヒド3%前後の水溶液で、水酸化アルカリを加えるのは
金をホルムアルデヒドで還元させやすい反応条件とする
ためである。The solution containing the reducing agent is an aqueous solution of about 3% formaldehyde to which sodium hydroxide or potassium hydroxide is added as an alkali hydroxide, and the alkali hydroxide is added to make the reaction condition easy to reduce gold with formaldehyde. .
また、還元剤としてのホルムアルデヒドの加える量は
金に対して70倍当量となるようにするのが好ましく、過
剰に加えると経済的でないばかりか金の超微粒子の粒子
径の分布が広くなってしまう等の問題が生ずる。Further, the amount of formaldehyde added as a reducing agent is preferably 70 times equivalent to that of gold. If added in excess, it is not economical and the particle size distribution of gold ultrafine particles becomes wide. Problems such as occur.
尚、反応させる溶液のそれぞれの液温は室温でよい。 The liquid temperature of each of the solutions to be reacted may be room temperature.
以下、本発明の実施例について記載するが、該実施例
は本発明を限定するものではない。Hereinafter, examples of the present invention will be described, but the examples do not limit the present invention.
(実施例1) 塩化金酸溶液(Au0.05g/)を50ml比色管に取り、水
溶性キチン(0.5gを水に溶解して50mlにメスアップした
もの)を1ml加えて十分に撹拌したのち、ホルムアルデ
ヒド溶液(1N−KOHを5ml+水を20ml+35%ホルムアルデ
ヒドを2.5ml)を1ml加えて撹拌して反応させたところ、
溶液は赤紫に変化して金の微粒子が生成した。(Example 1) A chloroauric acid solution (Au 0.05 g /) was placed in a 50 ml colorimetric tube, and 1 ml of water-soluble chitin (dissolved 0.5 g in water to 50 ml) was added and stirred sufficiently. After that, 1 ml of formaldehyde solution (5 ml of 1N-KOH + 20 ml of water + 2.5 ml of 35% formaldehyde) was added and stirred to react,
The solution turned red-purple and gold fine particles were formed.
この微粒子を拡大して観察したところ、平均粒子径は
200Åで±20%の範囲に85%が入るもので、30日間凝集
せずに安定していた。When the fine particles were enlarged and observed, the average particle size was
At 200Å, 85% was in the range of ± 20% and was stable for 30 days without agglomeration.
(実施例2) 水溶性キチンの加えた量が、2ml、5ml、15mlの3段階
にした以外は実施例1と同様の方法で行ったところ下記
の表−1の様な結果であった。Example 2 When the same procedure as in Example 1 was carried out except that the amount of water-soluble chitin added was changed to 3 stages of 2 ml, 5 ml and 15 ml, the results shown in Table 1 below were obtained.
(比較例) 水溶性キチンの加えた量が、0.1ml、0.2ml、0.5mlの
3段階にした以外は実施例1と同様の方法で行ったとこ
ろ下記の表−2の様な結果であった。 (Comparative Example) The same results as shown in Table 2 below were obtained by the same method as in Example 1 except that the amount of water-soluble chitin added was changed to three stages of 0.1 ml, 0.2 ml and 0.5 ml. It was
(発明の効果) 本発明は、以上の結果から明確なように、従来法では
得られなかった30〜200Åの金超微粒子の粒子径を調製
することができ、反応条件等も極めて簡便であり、金の
超微粒子を金の特性を利用した触媒、ペースト、あるい
は薄膜形成用材料の原料等広く利用することが期待され
るものである。 (Effect of the invention) As is clear from the above results, the present invention can prepare a particle size of ultrafine gold particles of 30 to 200 Å which cannot be obtained by the conventional method, and the reaction conditions and the like are extremely simple. It is expected that ultrafine gold particles will be widely used as catalysts, pastes, raw materials for thin film forming materials, and the like, which utilize the characteristics of gold.
Claims (3)
て、金の超微粒子を調製するに際し、金含有溶液に水溶
性キチンを加えたのちに還元剤を含む溶液を加えて反応
させることを特徴とする金超微粒子の調製方法。1. When gold ultrafine particles are prepared by reacting a gold-containing solution with a solution containing a reducing agent, water-soluble chitin is added to the gold-containing solution, and then a solution containing a reducing agent is added and reacted. A method for preparing ultrafine gold particles, comprising:
構造のものを含むことを特徴とする請求項1の金超微粒
子の調製方法。2. The method for preparing ultrafine gold particles according to claim 1, wherein the water-soluble chitin contains a structure in which chitin is deacetylated.
ホルムアルデヒド溶液であることを特徴とする請求項1
の金超微粒子の調製方法。3. The solution containing a reducing agent is a formaldehyde solution containing an alkali hydroxide.
Method for preparing ultrafine gold particles.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP9976889A JP2684413B2 (en) | 1989-04-19 | 1989-04-19 | Method for preparing ultrafine gold particles |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP9976889A JP2684413B2 (en) | 1989-04-19 | 1989-04-19 | Method for preparing ultrafine gold particles |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH02277705A JPH02277705A (en) | 1990-11-14 |
JP2684413B2 true JP2684413B2 (en) | 1997-12-03 |
Family
ID=14256150
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP9976889A Expired - Lifetime JP2684413B2 (en) | 1989-04-19 | 1989-04-19 | Method for preparing ultrafine gold particles |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP2684413B2 (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4640570B2 (en) * | 2003-06-23 | 2011-03-02 | 三菱マテリアル株式会社 | Metal fine particles and production method thereof |
JP4706835B2 (en) * | 2004-11-02 | 2011-06-22 | 三菱マテリアル株式会社 | Method for producing gold fine particles |
JP5282915B2 (en) * | 2004-11-02 | 2013-09-04 | 三菱マテリアル株式会社 | Gold nanoparticles |
-
1989
- 1989-04-19 JP JP9976889A patent/JP2684413B2/en not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
---|---|
JPH02277705A (en) | 1990-11-14 |
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