JPH0347972A - Method for preventing decomposition of electroless gold plating solution - Google Patents
Method for preventing decomposition of electroless gold plating solutionInfo
- Publication number
- JPH0347972A JPH0347972A JP18192089A JP18192089A JPH0347972A JP H0347972 A JPH0347972 A JP H0347972A JP 18192089 A JP18192089 A JP 18192089A JP 18192089 A JP18192089 A JP 18192089A JP H0347972 A JPH0347972 A JP H0347972A
- Authority
- JP
- Japan
- Prior art keywords
- plating
- plating solution
- soln
- gold plating
- electroless gold
- 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
- 238000007747 plating Methods 0.000 title claims abstract description 58
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000010931 gold Substances 0.000 title claims abstract description 34
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 34
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 27
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 9
- XTFKWYDMKGAZKK-UHFFFAOYSA-N potassium;gold(1+);dicyanide Chemical compound [K+].[Au+].N#[C-].N#[C-] XTFKWYDMKGAZKK-UHFFFAOYSA-N 0.000 claims abstract description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052796 boron Inorganic materials 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 31
- 229910052759 nickel Inorganic materials 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract 5
- 235000011118 potassium hydroxide Nutrition 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 10
- ZADPBFCGQRWHPN-UHFFFAOYSA-N boronic acid Chemical compound OBO ZADPBFCGQRWHPN-UHFFFAOYSA-N 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 230000008021 deposition Effects 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 2
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910000085 borane Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- NRTDAKURTMLAFN-UHFFFAOYSA-N potassium;gold(3+);tetracyanide Chemical compound [K+].[Au+3].N#[C-].N#[C-].N#[C-].N#[C-] NRTDAKURTMLAFN-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000003381 stabilizer 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、シアン化金カリ、シアン化カリ、水酸化カリ
、はう素系還元剤を含有する無電解金めっき液の分解を
防止する方法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention prevents the decomposition of an electroless gold plating solution containing potassium gold cyanide, potassium cyanide, potassium hydroxide, and a boronate reducing agent. Regarding the method.
〔従来の技術及び発明が解決しようとする課題〕従来よ
り、シアン化金カリ、シアン化カリ、水酸化カリ、はう
素系還元剤を含有するアルカリ性無電解金めっき液が電
子部品などの厚付は金めっきに用いられている。[Prior art and problems to be solved by the invention] Conventionally, an alkaline electroless gold plating solution containing potassium gold cyanide, potassium cyanide, potassium hydroxide, and a boronate reducing agent has been used to coat electronic parts, etc. It is used for gold plating.
しかしながら、この種の無電解金めっき液は、しばしば
液の分解が生じることがあり、その原因としては本発明
者の検討によるとニッケル等の不純物の混入によるもの
であった。従って、上記無電解金めっき液の分解を防止
するにはニッケル等の不純物の混入を防止すればよいが
、金めっきされる部品はその下地めっきとしてニッケル
めっきを施すことが多く、ニッケルめっき液から無電解
金めっき液中へのニッケル不純物の持ち込みは避けられ
ない。However, in this type of electroless gold plating solution, decomposition of the solution often occurs, and according to studies conducted by the present inventors, the cause of this is the contamination of impurities such as nickel. Therefore, in order to prevent the decomposition of the electroless gold plating solution mentioned above, it is sufficient to prevent impurities such as nickel from getting mixed in, but parts to be gold plated are often plated with nickel as a base plating, and from the nickel plating solution. The introduction of nickel impurities into the electroless gold plating solution is unavoidable.
このため、ニッケルが不純物として混入した場合にも上
記無電解金めっき液を安定化させ、その分解を防止する
ことが望まれる。Therefore, it is desirable to stabilize the electroless gold plating solution and prevent its decomposition even when nickel is mixed in as an impurity.
〔課題を解決するための手段及び作用〕本発明者は、上
記要望に応えるため鋭意検討を行なった結果、上述した
ようにシアン化金カリ。[Means and effects for solving the problem] As a result of intensive studies in order to meet the above-mentioned needs, the present inventors have developed potassium gold cyanide as described above.
シアン化カリ、水酸化カリ、ジメチルアミンボランや水
素化はう素カリ等のほう素系還元剤を含む無電解金めっ
き液はニッケルの混入、特に二ツケ−
−
ルが10ppm以上混入することによりめっき中におい
て液が不安定化し、析出速度が低下したり、析出が停止
し、更には液の分解が生じるものであるが、かかるめっ
き中にめっき液をポンプ循環させると、ニッケルが混入
していても析出速度の低下、停止、更には液の分解を防
止し得ることを知見した。この場合、ポンプによる液循
環の代りに液を空気撹拌したり、スタージー等で撹拌し
ても、後述する実験から明らかなように、液の分解を防
止したり析出停止を防止し得ないものであり、ポンプに
よる液循環を実施した場合にのみ特異的に液分解、析出
停止現象を防止し得るものである。Electroless gold plating solutions containing boron-based reducing agents such as potassium cyanide, potassium hydroxide, dimethylamine borane, and potassium borohydride may be contaminated with nickel, especially 10 ppm or more of nickel. During plating, the solution becomes unstable, the deposition rate decreases, precipitation stops, and the solution decomposes. However, if the plating solution is circulated with a pump during such plating, nickel may be mixed in. It has been found that the precipitation rate can be reduced or stopped, and furthermore, the decomposition of the liquid can be prevented. In this case, even if the liquid is agitated with air or stirred with a stirrer instead of circulating the liquid with a pump, it will not be possible to prevent the decomposition of the liquid or stop the precipitation, as is clear from the experiments described below. However, liquid decomposition and precipitation stoppage phenomena can be specifically prevented only when the liquid is circulated using a pump.
従って、本発明は、シアン化金カリ、シアン化カリ、水
酸化カリ及びほう素系還元剤を含む無電解金めっき液に
被処理物を浸漬して無電解金めっきを行なうに際し、上
記めっき液をポンプ循環させながらめっきを行なって、
該めっき液の分解を防止することを特徴とする無電解金
めっき液の分解防止方法を提供する。Therefore, the present invention provides a method for performing electroless gold plating by immersing a workpiece in an electroless gold plating solution containing potassium gold cyanide, potassium cyanide, potassium hydroxide, and a boron-based reducing agent. Plating is carried out while circulating with a pump,
Provided is a method for preventing decomposition of an electroless gold plating solution, which is characterized by preventing decomposition of the plating solution.
以下、本発明につき更に詳しく説明する。The present invention will be explained in more detail below.
本発明において、安定化の対象となる無電解金めっき液
は、上述した通りシアン化金カリ(通常0.005〜0
.1モル/fl) 、シアン化カリ(通常0.001〜
0.1モル/Q)、水酸化カリ(通常0.1〜2モル/
Il) 、はう素系還元剤(通常0.01〜0.2モル
/Q)を含むものであり、更に必要によりアルカノール
アミン、エチレンジアミン等のアミン類、鉛塩等の促進
安定剤などを含有していてもよく、そのpHは通常10
〜14とされる。なお、はう素系還元剤としてはジメチ
ルアミンボラン等のアミンボランや水素化はう素カリ等
の水素化はう素物が使用できる。In the present invention, the electroless gold plating solution to be stabilized is gold potassium cyanide (usually 0.005 to 0.0
.. 1 mol/fl), potassium cyanide (usually 0.001~
0.1 mol/Q), potassium hydroxide (usually 0.1-2 mol/Q)
Il) Contains a boronate reducing agent (usually 0.01 to 0.2 mol/Q), and further contains amines such as alkanolamines and ethylenediamine, accelerating stabilizers such as lead salts, etc. The pH is usually 10.
~14. As the boronate reducing agent, amine borane such as dimethylamine borane and hydrogenated boronates such as potassium borohydride can be used.
また、かかる無電解金めっき液を用いて金めっきする場
合、めっき温度としては通常50〜90℃が採用される
が、本発明においてはその金めつき方法としてこのめっ
き液をポンプ循環させながらめっきを行なうものである
。このポンプ循環の方法としては、図面に示したように
めっき槽1内に収容された無電解金めっき液2の一部を
ポンプ3の作動で連続的に抜き取り、これを再度めっき
3−
槽1に戻す方法であれば、いずれの方法を採用すること
もできる。なおこの場合、液循環量は2〜6回転/時と
することが好ましい。In addition, when gold plating is performed using such an electroless gold plating solution, the plating temperature is usually 50 to 90°C, but in the present invention, the gold plating method is to perform plating while circulating the plating solution with a pump. This is what we do. As shown in the drawing, a part of the electroless gold plating solution 2 contained in the plating tank 1 is continuously drawn out by the operation of the pump 3, and this is re-plated in the plating tank 1. Any method can be used as long as it returns to . In this case, the liquid circulation rate is preferably 2 to 6 revolutions/hour.
このポンプ循環方式の採用により、めっき速度を低下さ
せることなく、しかも液を分解させることなく、被めっ
き物に対し良好な金めつきを施すことができ、被めっき
物がその下地めっきとしてニッケルめっきが施され、金
めつき液に被めっき物が浸漬された際、該被めっき物に
付着している前工程のニッケルめっき液がこの金めつき
液にニッケルとして10ppm以上持ち込まれても支障
がないものである。By adopting this pump circulation method, it is possible to apply good gold plating to the object to be plated without reducing the plating speed or decomposing the liquid, and the object to be plated can be plated with nickel as its base plating. When the object to be plated is immersed in the gold plating solution, there will be no problem even if the nickel plating solution from the previous process adhering to the object is brought into the gold plating solution in an amount of 10 ppm or more as nickel. It's something that doesn't exist.
以下、実施例と比較例を示し、本発明を具体的に説明す
る。EXAMPLES Hereinafter, the present invention will be specifically explained by showing Examples and Comparative Examples.
下記組成の無電解金めっき液を調製した。 An electroless gold plating solution having the following composition was prepared.
第一シアン化金カリ 0.02モル/Ωシアン化カ
リ 0.1
水酸化カリ 0.2
水素化はう素カリ 0.2 〃塩化鉛
3.5xlQ−6n次に、上記めっき液に硫酸
ニッケルを金属ニッケルとして20ppm添加し、温度
75℃において第1表に示す撹拌態様でめっきを行ない
、その時の析出速度、めっき液の分解の有無を調べた。Potassium gold cyanide 0.02 mol/Ω Potassium cyanide 0.1 Potassium hydroxide 0.2 Potassium borohydride 0.2 Lead chloride
3.5xlQ-6n Next, 20 ppm of nickel sulfate as metallic nickel was added to the above plating solution, and plating was performed at a temperature of 75°C in the stirring mode shown in Table 1, and the precipitation rate at that time and the presence or absence of decomposition of the plating solution were evaluated. Examined.
結果を第1表に示す。The results are shown in Table 1.
第 1 表
なお、上記めっき液に硫酸ニッケルを添加しない通常の
状態における析出速度は2.0戸/hrであった。Table 1 Note that the deposition rate in the normal state in which nickel sulfate was not added to the above plating solution was 2.0 units/hr.
第1表の結果からも明らかなように、空気や窒素撹拌、
スターラー撹拌ではニッケルが混入して無電解金めっき
液の析出を停止させ或いはめっき液を分解させてしまう
ものであるが、ポンプによる液循環を採用した場合にの
み特異的に液分解を防止し、しかも析出速度を低下させ
ないことがわかる。As is clear from the results in Table 1, air and nitrogen agitation,
When stirring with a stirrer, nickel gets mixed in and stops the deposition of the electroless gold plating solution or causes it to decompose, but only when liquid circulation using a pump is used can this specifically prevent liquid decomposition. Moreover, it can be seen that the precipitation rate is not reduced.
以上説明したように、本発明によれば、ニッケル不純物
が混入したシアン化金カリ、シアン化力り、水酸化カリ
、はう素系還元剤を含む無電解金めっき液の分解を確実
に防止し、その析出速度を低下させることなく良好な金
めつきの析出を可能とするものである。As explained above, according to the present invention, decomposition of an electroless gold plating solution containing potassium cyanide, potassium cyanide, potassium hydroxide, and a boronate reducing agent mixed with nickel impurities is reliably prevented. However, it is possible to deposit good gold plating without reducing the deposition rate.
図面は本発明の実施に用いる装置の一例を示す概略断面
図である。
1・・・めっき槽、 2・・・無電解金めっき液、3
・ポンプ。
−The drawing is a schematic sectional view showing an example of an apparatus used to implement the present invention. 1... Plating tank, 2... Electroless gold plating solution, 3
·pump. −
Claims (1)
う素系還元剤を含む無電解金めっき液に被処理物を浸漬
して無電解金めっきを行なうに際し、上記めっき液をポ
ンプ循環させながらめっきを行なって、該めっき液の分
解を防止することを特徴とする無電解金めっき液の分解
防止方法。1. When performing electroless gold plating by immersing the workpiece in an electroless gold plating solution containing potassium gold cyanide, potassium cyanide, potassium hydroxide, and a boron-based reducing agent, the plating solution is circulated with a pump while plating. 1. A method for preventing decomposition of an electroless gold plating solution, the method comprising: preventing decomposition of the plating solution.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP18192089A JPH0347972A (en) | 1989-07-14 | 1989-07-14 | Method for preventing decomposition of electroless gold plating solution |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP18192089A JPH0347972A (en) | 1989-07-14 | 1989-07-14 | Method for preventing decomposition of electroless gold plating solution |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH0347972A true JPH0347972A (en) | 1991-02-28 |
Family
ID=16109221
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP18192089A Pending JPH0347972A (en) | 1989-07-14 | 1989-07-14 | Method for preventing decomposition of electroless gold plating solution |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH0347972A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5753881A (en) * | 1995-03-10 | 1998-05-19 | Okamoto Machine Tool Works, Ltd. | Method and apparatus for rotating a machining portion of an electrodischarge machine |
US6211480B1 (en) | 1997-02-04 | 2001-04-03 | Mitsubishi Denki Kabushiki Kaisha | EDM machine for fine hole and EDM method using such machine |
CN109280908A (en) * | 2017-07-19 | 2019-01-29 | 凯基有限公司 | The continuous purification system of plating by chemical displacement gold solution and Impurity Nickel and impurity copper |
-
1989
- 1989-07-14 JP JP18192089A patent/JPH0347972A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5753881A (en) * | 1995-03-10 | 1998-05-19 | Okamoto Machine Tool Works, Ltd. | Method and apparatus for rotating a machining portion of an electrodischarge machine |
US6211480B1 (en) | 1997-02-04 | 2001-04-03 | Mitsubishi Denki Kabushiki Kaisha | EDM machine for fine hole and EDM method using such machine |
CN109280908A (en) * | 2017-07-19 | 2019-01-29 | 凯基有限公司 | The continuous purification system of plating by chemical displacement gold solution and Impurity Nickel and impurity copper |
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