JPS63293107A - Production of gold particle - Google Patents
Production of gold particleInfo
- Publication number
- JPS63293107A JPS63293107A JP12785087A JP12785087A JPS63293107A JP S63293107 A JPS63293107 A JP S63293107A JP 12785087 A JP12785087 A JP 12785087A JP 12785087 A JP12785087 A JP 12785087A JP S63293107 A JPS63293107 A JP S63293107A
- Authority
- JP
- Japan
- Prior art keywords
- gold
- gold particles
- particles
- particle size
- solution
- 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 63
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000010931 gold Substances 0.000 title claims abstract description 42
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- -1 gold iodide salt ion Chemical class 0.000 claims abstract description 9
- 229910001854 alkali hydroxide Inorganic materials 0.000 claims abstract description 5
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 19
- GCZKMPJFYKFENV-UHFFFAOYSA-K triiodogold Chemical class I[Au](I)I GCZKMPJFYKFENV-UHFFFAOYSA-K 0.000 claims description 5
- 229910001516 alkali metal iodide Inorganic materials 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- ZHHGTDYVCLDHHV-UHFFFAOYSA-J potassium;gold(3+);tetraiodide Chemical compound [K+].[I-].[I-].[I-].[I-].[Au+3] ZHHGTDYVCLDHHV-UHFFFAOYSA-J 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 11
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 150000004694 iodide salts Chemical class 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- LIAWOTKNAVAKCX-UHFFFAOYSA-N hydrazine;dihydrochloride Chemical compound Cl.Cl.NN LIAWOTKNAVAKCX-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000002497 iodine compounds Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 235000009518 sodium iodide Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は金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 gold particles.
（従来技術とその問題点）
従来金粒子の製造方法としては、塩化金酸溶液などにヒ
ドラジン等の還元剤を用いて還元する方法が用いられて
きた。(Prior art and its problems) As a conventional method for producing gold particles, a method has been used in which a chloroauric acid solution or the like is reduced using a reducing agent such as hydrazine.
ところが、この方法では、還元された粒子同士が引き寄
せ合うために、凝集してしまい粒度分布の幅の広い金粒
子しか得られないという欠点を有していた。However, this method has the disadvantage that the reduced particles attract each other and aggregate, resulting in gold particles having a wide particle size distribution.
また粒径の大きいものについても、整った結晶をもつも
のが得られず、得られても凝集したものである等の欠点
を有していた゛。In addition, those with large particle sizes also have the disadvantage that they cannot be obtained with well-ordered crystals, and even if they are obtained, they are agglomerated.
（発明の目的）
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、粒度分布の幅の狭い粒径コントロール可能な結晶
状の金粒子の製造方法を提供せんとするものである。(Objective of the Invention) The present invention has been made to solve the above-mentioned drawbacks, and aims to provide a method for producing crystalline gold particles with a narrow particle size distribution and controllable particle size. .
（問題点を解決するための手段）
発明者らは、ヨウ化合を溶かしたヨウ化カリウム溶液〔
（１）、（２）式〕に水酸化カリウム溶液を加えると、
分散した粒度分布幅の狭い金粒子が得られＡＣ（３）式
〕事に着目し、上記方法の改良の結果、本発明を成すに
至った。(Means for solving the problem) The inventors have developed a potassium iodide solution in which an iodine compound is dissolved [
When potassium hydroxide solution is added to equations (1) and (2),
Focusing on the fact that dispersed gold particles with a narrow particle size distribution width can be obtained (formula AC (3)), the present invention was accomplished as a result of improvements to the above method.
本発明は、核とする金粒子とヨウ化金酸イオンを含む水
溶液に水酸化アルカリ溶液を加え前記金粒子に金を析出
させ、より大きな金粒子を得ることを特徴とするもので
ある。The present invention is characterized in that an alkali hydroxide solution is added to an aqueous solution containing gold particles as cores and iodoaurate ions to precipitate gold onto the gold particles, thereby obtaining larger gold particles.
核とする金粒子は、どのような製法のものでも良いが、
粒径の大きなものを得る為には、なるべく大きな、好ま
しくは、数μから十数μのものが良い。これは、析出さ
せる際の金の量に限りがある事、直径を２倍にする為に
は８倍量の質量を要するからである。また得られる金粒
子の粒径を一定にするために、粒度分布幅の狭いものの
方が良い。The gold particles used as the core may be manufactured using any manufacturing method, but
In order to obtain particles with a large particle size, particles should be as large as possible, preferably from several microns to more than ten microns. This is because there is a limit to the amount of gold that can be deposited, and to double the diameter, eight times the mass is required. Further, in order to make the particle size of the obtained gold particles constant, it is better to have a narrow particle size distribution width.
ヨウ化金イオンを含む水溶液を得るためのヨウ化金塩と
してヨウ化合カリウム、ヨウ化合ナトリウム等のアルカ
リ金属塩の他、Ｃａ、Ｍｇ等のアルカリ土類金属塩、ア
ンモニウム塩等があげられる。またヨウ化アルカリ金属
塩として、カリウム塩、ナトリウム塩等のアルカリ金属
塩、カルシウム塩、マグネシウム塩等のアルカリ土類金
属塩、アンモニウム塩等があげられる。Examples of gold iodide salts for obtaining an aqueous solution containing gold iodide ions include alkali metal salts such as potassium iodide and sodium iodide, alkaline earth metal salts such as Ca and Mg, and ammonium salts. Examples of the alkali metal iodide salts include alkali metal salts such as potassium salts and sodium salts, alkaline earth metal salts such as calcium salts and magnesium salts, and ammonium salts.
濃度は、ヨウ化金塩として０．０１〜０．７５Ｍ／Ｊが
良い。０．０１Ｍ／ｆｆｉ未満では収量が少なく 、０
．’７５Ｍ／１を超えると溶解させることが難しいから
である。ヨウ化アルカリ金属塩については０．０１〜７
Ｍ／ｌが良い。ヨウ化金塩は水に溶けやすいが、ヨウ化
アルカリ金属がある場合はより良く溶解し、液も劣化し
にくい。しかし７Ｍ／１を超えると飽和濃度に近く結晶
が出やすくなる。The concentration is preferably 0.01 to 0.75 M/J as gold iodide salt. If it is less than 0.01M/ffi, the yield will be low and 0.
．． This is because if it exceeds 75M/1, it is difficult to dissolve it. 0.01-7 for alkali metal iodide salts
M/l is good. Gold iodide salts are easily soluble in water, but when alkali metal iodides are present, they dissolve better and the liquid is less likely to deteriorate. However, when the concentration exceeds 7M/1, crystals tend to form near the saturation concentration.
ｐＨは１３を超えると（３）式がおこるため不都合なの
で１３以下がよいが、操作上８〜１３がより好ましい。If the pH exceeds 13, formula (3) occurs, which is inconvenient, so a pH of 13 or less is preferable, but a pH of 8 to 13 is more preferable for operational reasons.
ｐ Ｈを調整するためには、通常使われる酸、アルカリ
の他にｐ Ｈの緩衝作用を有するものでも良い。In order to adjust the pH, in addition to the commonly used acids and alkalis, substances having a pH buffering effect may be used.
さらにその他の添加剤を入れて使用しても良く、Ｉ２や
Ｋ １０．等が入っていると系内が酸化性雰囲気となり
、液の保存時に金が析出しないなどの利点がある。Furthermore, other additives may be added and used, such as I2 and K10. etc., the system becomes an oxidizing atmosphere, which has the advantage that gold does not precipitate during storage of the liquid.
水酸化アルカリ溶液としては、ＫＯＨ，ＮａＯＨなどが
良い。濃度は０．１〜６．ＯＲ位の方が良く高濃度のも
のの使用は粒径が不ぞろいになり易く良くない。As the alkaline hydroxide solution, KOH, NaOH, etc. are preferable. The concentration is 0.1-6. It is better to have an OR level, but using a high concentration is not good because the particle size tends to be uneven.
金を析出させるための条件としては、１０〜１００℃で
良いが、３０〜７０℃の方が粒径をコントロールし易い
。The conditions for depositing gold may be 10 to 100°C, but it is easier to control the particle size at 30 to 70°C.
（実施例１）
■β当りヨウ化カリウム３．ＯＭ、ヨウ化金塩０．２５
Ｍを含み０．０５Ｎの水酸化カリウム溶液でｐＨ１１，
０にした溶＊（以下Ａ液）を３０２と１．０Ｍ＃！の水
酸化カリウム溶液（以下Ｂ液）３０１を作り実験した。(Example 1) ■ Potassium iodide per β 3. OM, gold iodide salt 0.25
pH 11 with 0.05N potassium hydroxide solution containing M,
302 and 1.0M#! A potassium hydroxide solution (hereinafter referred to as B solution) 301 was prepared and an experiment was conducted.
（１１まずＡ液とＢ液を５０℃で各ｌｌを混合して金粒
子を含む溶液２１を得た（サンプルＡ）。金粒子を沈降
させた後上澄みを１．６１すて、残る０、４１を金粒子
を含む溶液（Ｃ液）とした。(11 First, each liter of solution A and solution B were mixed at 50°C to obtain a solution 21 containing gold particles (sample A). 41 was used as a solution containing gold particles (liquid C).
（２）Ｃ液にＡ液１１を加え１．４１とし５０℃にてＢ
液ＩＩ！と混合し金粒子を析出させ（計２．１）、上澄
みを２．ＯＲすて、残る０、４１の金粒子を含み溶液を
得る。(2) Add 11 of liquid A to liquid C to make it 1.41, and heat B at 50°C.
Liquid II! The gold particles were precipitated by mixing with (2.1 in total), and the supernatant was mixed with (2.1 in total). After discarding the OR, a solution containing remaining 0.41 gold particles is obtained.
この液を（２）でのＣ液とし結晶成長の為の核とし、こ
の操作を３０回繰り返し、１回目、２回目、５回目、１
０回目、２５回目にそれぞれサンプルＢ，Ｃ，Ｄ，Ｅと
し、粒度分布測定と電子顕微鏡観察を行った結果を表１
に示す。This liquid was used as the C solution in (2) and used as a nucleus for crystal growth, and this operation was repeated 30 times, 1st, 2nd, 5th, 1
Table 1 shows the results of particle size distribution measurement and electron microscope observation for samples B, C, D, and E at the 0th and 25th runs.
Shown below.
（従来例）
上述実施例１のＡ液のかわりに１β当り金０．２５Ｍを
含む塩化金酸塩酸酸性溶液とＢ液のかわりの２Ｍ／Ｉｌ
の二塩酸ヒドラジン溶液を用いて実施例１と同じ実験を
行いサンプルＡ゛〜Ｅ′を得たのでこれを実施例１と同
様の方法で評価をしたものを表１に示す。(Conventional example) A chloroauric acid acidic solution containing 0.25M gold per 1β instead of the A solution of Example 1 and 2M/Il instead of the B solution.
The same experiment as in Example 1 was carried out using the hydrazine dihydrochloride solution of 1. Samples A' to E' were obtained, and the samples A' to E' were evaluated in the same manner as in Example 1 and are shown in Table 1.
（以下余白）
表からもわかるように実施例１では金粒子に新たに金が
析出して粒径が徐々に大きくなることと粒度分布幅が狭
いことがわかるが従来例においては粒径は大きくならず
、粒度分布幅が凝集により広がってしまっていることが
わかる。(Margins below) As can be seen from the table, in Example 1, gold is newly precipitated on the gold particles and the particle size gradually increases, and the particle size distribution width is narrow, but in the conventional example, the particle size is large. It can be seen that the particle size distribution width is widened due to aggregation.
（実施例２） 実施例１のＡ液、Ｂ液を用いて実験した。(Example 2) An experiment was conducted using liquids A and B of Example 1.
Ａ液０．５１Ｂ液０．５！を加え金粒子を析出させたの
ち上澄み０，８１をすて、残る０、２１を核となる金粒
子を含む溶液とした。A liquid 0.51 B liquid 0.5! was added to precipitate gold particles, the supernatant 0.81 was discarded, and the remaining 0.21 was used as a solution containing gold particles serving as cores.
この液にＡ液を２１入れ３０℃とし強く攪拌しながら５
ｍ／分の速さでＢ液を２ｊ！加えた。これにより得られ
た金粒子を粒度分布測定と電子顕微鏡実験を行ったとこ
ろ平均粒径が３２μで２５〜３７μの間に全粒子数の７
０％が含まれるシャープなものが得られた。Add 21 parts of solution A to this solution and heat to 30°C while stirring vigorously.
2j of liquid B at the speed of m/min! added. The resulting gold particles were subjected to particle size distribution measurement and electron microscopy experiments, and found that the average particle size was 32 μm, and 7 of the total particles were between 25 and 37 μm.
A sharp product containing 0% was obtained.
（発明の効果）
以上の説明かられかるように本発明による金粒子の製造
方法は、従来法では得られなかった粒度分布の幅の狭い
金粒子を、粒径をコントロールして製造できるので、従
来の製造方法に比べ画期的なものといえる。(Effects of the Invention) As can be seen from the above explanation, the method for producing gold particles according to the present invention can produce gold particles with a narrow particle size distribution, which could not be obtained by conventional methods, by controlling the particle size. It can be said to be revolutionary compared to conventional manufacturing methods.
Claims (3)
に水酸化アルカリ溶液を加え、前記金粒子に金を析出さ
せ、より大きな粒径の金粒子を得ることを特徴とする金
粒子の製造方法。(1) Gold particles characterized by adding an alkali hydroxide solution to an aqueous solution containing gold particles as cores and gold iodide ions to precipitate gold on the gold particles to obtain gold particles with a larger particle size. manufacturing method.
属塩溶液に水酸化アルカリ溶液を加えて得られた金粒子
であることを特徴とする特許請求の範囲第１項記載の金
粒子の製造方法。(2) The gold according to claim 1, characterized in that the gold particles serving as the core are gold particles obtained by adding an alkali hydroxide solution to an alkali metal iodide salt solution of a gold iodide salt. Method of manufacturing particles.
れた金粒子であることを特徴とする特許請求の範囲第１
項記載の製造方法。(3) Claim 1, characterized in that the gold particles serving as the core are the gold particles obtained in Claim 1.
Manufacturing method described in section.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12785087A JPS63293107A (en) | 1987-05-25 | 1987-05-25 | Production of gold particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12785087A JPS63293107A (en) | 1987-05-25 | 1987-05-25 | Production of gold particle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63293107A true JPS63293107A (en) | 1988-11-30 |
Family
ID=14970210
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12785087A Pending JPS63293107A (en) | 1987-05-25 | 1987-05-25 | Production of gold particle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63293107A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004149903A (en) * | 2002-11-01 | 2004-05-27 | Kaken Tec Kk | Conductive powder, conductive composition, and production method for conductive powder |
| US7211135B2 (en) | 2004-03-16 | 2007-05-01 | Nanogate Coating Systems Gmbh | Writable and printable colloidal gold solution |
| JP2011105981A (en) * | 2009-11-16 | 2011-06-02 | Hiroshima Univ | Method for producing gold particle, gold particle, laser ablation apparatus, collecting member used therefor and method for producing particle |
-
1987
- 1987-05-25 JP JP12785087A patent/JPS63293107A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004149903A (en) * | 2002-11-01 | 2004-05-27 | Kaken Tec Kk | Conductive powder, conductive composition, and production method for conductive powder |
| US7211135B2 (en) | 2004-03-16 | 2007-05-01 | Nanogate Coating Systems Gmbh | Writable and printable colloidal gold solution |
| US7579074B2 (en) | 2004-03-16 | 2009-08-25 | Nanogate Ag | Writable and printable colloidal gold solution |
| JP2011105981A (en) * | 2009-11-16 | 2011-06-02 | Hiroshima Univ | Method for producing gold particle, gold particle, laser ablation apparatus, collecting member used therefor and method for producing particle |
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