JP2558388B2 - Management method of copper sulfate plating bath - Google Patents
Management method of copper sulfate plating bathInfo
- Publication number
- JP2558388B2 JP2558388B2 JP2315358A JP31535890A JP2558388B2 JP 2558388 B2 JP2558388 B2 JP 2558388B2 JP 2315358 A JP2315358 A JP 2315358A JP 31535890 A JP31535890 A JP 31535890A JP 2558388 B2 JP2558388 B2 JP 2558388B2
- Authority
- JP
- Japan
- Prior art keywords
- additive
- copper sulfate
- plating bath
- sulfate plating
- concentration
- 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 - Fee Related
Links
Landscapes
- Electroplating And Plating Baths Therefor (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は硫酸銅めっき浴の管理方法に関し、特に添加
剤の管理方法に関する。TECHNICAL FIELD The present invention relates to a method for controlling a copper sulfate plating bath, and more particularly to a method for controlling an additive.
硫酸銅めっき浴は、基本的に銅イオン、硫酸、塩素イ
オン、添加剤などで構成されている。この内、硫酸、塩
素イオンは、めっき反応によって濃度が低下する因子で
あり、銅イオンは、めっき反応と共に濃度が増加する。
これら因子の過不足は、めっき均一性やめっき仕上りを
悪化する為、硫酸は中和滴定法、塩素イオン,銅イオン
は比色法により自動分析管理をし、増加する銅イオンに
ついては弱電解法により過剰銅イオンを金属銅として析
出させ銅イオン濃度を一定にしていた。一方、添加剤
は、めっき反応により消耗されその副生成物を生じる。
添加剤濃度不足及び副生成物の増加は、めっき仕上りや
めっき物性等に最も強く影響する為、添加剤の濃度管理
は重要である。しかし、硫酸銅めっき浴中の添加剤の含
有量は、微量であり定量分析が大変困難であった為、一
般的には分析せずに硫酸銅めっきの積算印加電流値に基
づき補充するか、ハルセル試験等の仕上り状態により補
充を行っていた。The copper sulfate plating bath is basically composed of copper ions, sulfuric acid, chlorine ions, additives and the like. Of these, sulfuric acid and chlorine ions are factors that reduce the concentration by the plating reaction, and copper ions increase in concentration with the plating reaction.
Since the excess and deficiency of these factors deteriorates the plating uniformity and the finish of plating, sulfuric acid is automatically controlled by the neutralization titration method, and chlorine ion and copper ion are controlled by the colorimetric method. Excess copper ions were deposited as metallic copper to keep the copper ion concentration constant. On the other hand, the additive is consumed by the plating reaction and produces its by-product.
Insufficient additive concentration and increase of by-products have the strongest effect on the plating finish, plating physical properties, etc. Therefore, it is important to control the concentration of the additive. However, since the content of the additive in the copper sulfate plating bath was very small and quantitative analysis was very difficult, in general, do not analyze and supplement based on the cumulative applied current value of copper sulfate plating, It was replenished depending on the finished condition such as the Hull cell test.
従来の管理方法では、硫酸銅めっき浴中の添加剤濃度
を定量分析できず、めっき仕上りや物性を一定に保つこ
とが困難であり、添加剤濃度が下限濃度以下になるとめ
っき仕上り不良や、物性不良を引き起こすという問題が
あった、 本発明の目的は、かかる従来欠点を解決し、硫酸銅め
っき浴の添加剤濃度を一定範囲に維持することができ、
その結果めっき浴の安定性が保たれ、めっき仕上り不良
を防止でき、そして一定の硫酸銅めっき物性が維持でき
る硫酸銅めっき浴の管理方法を提供することにある。With the conventional control method, it is difficult to quantitatively analyze the additive concentration in the copper sulfate plating bath, and it is difficult to keep the plating finish and physical properties constant.If the additive concentration is below the lower limit concentration, poor plating finish and physical properties will occur. There was a problem of causing a defect, the object of the present invention is to solve such conventional drawbacks, it is possible to maintain the additive concentration of the copper sulfate plating bath in a certain range,
As a result, it is an object of the present invention to provide a method for controlling a copper sulfate plating bath, which can maintain the stability of the plating bath, prevent a plating finish defect, and maintain a certain copper sulfate plating physical property.
本発明の硫酸銅めっき浴の管理方法は、硫酸銅めっき
槽から一定量のめっき液をサンプリングする工程と、回
転電極を用いた電位走査ストリッピング法により前記サ
ンプリング液中の添加剤濃度を定量する工程と、その添
加剤濃度から不足する添加材料を演算する工程と、不足
する添加剤を補充する工程と、添加剤の積算補充量に応
じてめっき液中の副生成物を活性炭濾過で除去する工程
とを含むことを特徴として構成される。The management method of the copper sulfate plating bath of the present invention comprises a step of sampling a fixed amount of plating solution from a copper sulfate plating bath and a potential scanning stripping method using a rotating electrode to quantify the additive concentration in the sampling solution. Process, a process of calculating a deficient additive material from the additive concentration, a process of replenishing the deficient additive, and removal of by-products in the plating solution by activated carbon filtration according to the cumulative replenishment amount of the additive And a process.
本発明によれば硫酸銅めっき浴の添加剤濃度を自動的
に測定し、添加剤を基準濃度迄補充すると共に添加剤の
積算補充量に応じ活性炭濾過を行う工程を有するので、
めっき浴の安定性が保たれ、めっき仕上り不良を防止で
きる。また一定の硫酸銅めっき物性を維持できる。According to the present invention, there is a step of automatically measuring the additive concentration of the copper sulfate plating bath, supplementing the additive to the standard concentration, and performing activated carbon filtration according to the cumulative supplement amount of the additive.
The stability of the plating bath is maintained, and poor plating finish can be prevented. Further, it is possible to maintain constant copper sulfate plating physical properties.
次に、本発明について図面を参照して説明する。第1
図は本発明の一実施例の構成図である。硫酸銅めっき槽
1より、1時間毎に200mlを添加剤自動分析装置2にサ
ンプリングする。添加剤自動分析装置2にて分析した分
析値をコントローラー3にて演算し添加剤濃度を標準値
10ml/Lに合わせる為の補充量を定量ポンプ4に伝送す
る。又、コントローラー3により添加剤の積算補充量を
演算し補充量が200Lに達する毎に活性炭濾過循環ポンプ
6に伝送し、5時間活性炭濾過槽5にて濾過処理を行
う。Next, the present invention will be described with reference to the drawings. First
The figure is a block diagram of an embodiment of the present invention. From the copper sulfate plating tank 1, 200 ml is sampled in the additive automatic analyzer 2 every hour. The controller 3 calculates the analysis value analyzed by the additive automatic analyzer 2, and the additive concentration is the standard value.
The replenishment amount for adjusting to 10 ml / L is transmitted to the metering pump 4. Further, the controller 3 calculates an integrated replenishment amount of the additive, and every time the replenishment amount reaches 200 L, it is transmitted to the activated carbon filtration circulation pump 6, and the activated carbon filtration tank 5 performs the filtration treatment for 5 hours.
上述した方法により1時間毎の添加剤濃度の測定値に
基づく添加剤の補充及びその補充量200L毎の活性炭濾過
を繰り返しながら、硫酸銅めっき浴中の添加剤濃度の管
理を行う。The additive concentration in the copper sulfate plating bath is controlled by repeating the supplement of the additive based on the measured value of the additive concentration every hour and the filtration of the activated carbon for each 200 L of the supplement amount by the method described above.
第2図は本発明の実施例2の構成図である。硫酸銅め
っき槽7より、1時間毎に200mlを添加剤自動分析装置
8にサンプリングし分析した分析値をコントローラー9
にて演算し添加剤濃度を標準値10ml/Lに合わせる為の補
充量を定量ポンプ10に伝送する。又、コントローラー9
により添加剤の積算補充量を演算し補充量が200Lに達す
る毎に活性炭濾過循環ポンプ1に伝送し、5時間活性炭
濾過フィルター14にて濾過処理を行う。FIG. 2 is a configuration diagram of a second embodiment of the present invention. From the copper sulphate plating tank 7, 200 ml per hour is sampled by the additive automatic analyzer 8 and analyzed.
The calculated replenishment amount for adjusting the additive concentration to the standard value of 10 ml / L is transmitted to the metering pump 10. Also, the controller 9
The cumulative replenishment amount of the additive is calculated by the above, and is transmitted to the activated carbon filtration circulation pump 1 every time the replenishment amount reaches 200 L, and filtration is performed by the activated carbon filtration filter 14 for 5 hours.
上述した方法により1時間毎の添加剤濃度測定値の積
算印加電流値5000AHに基づく添加剤の補充及びその補充
量200L毎の活性炭濾過を繰り返しながら、硫酸銅めっき
浴中の添加剤濃度の管理を行う。この実施例では添加剤
補充を自動分析装置と積算電流値の併用により行う為、
硫酸銅めっき浴中添加剤濃度のバラツキを小さくするこ
とができ、また活性炭処理を濾過フィルターを用いて行
う為、フロアスペースを濾過槽を使用する場合よりも縮
小化できるという利点がある。The additive concentration in the copper sulfate plating bath is controlled by repeating the additive replenishment based on the accumulated applied current value 5000AH of the additive concentration measured value every hour and the activated carbon filtration for each 200L of the replenishment amount by the above-mentioned method. To do. In this example, since the additive replenishment is performed by using the automatic analyzer and the integrated current value in combination,
Variations in the additive concentration in the copper sulfate plating bath can be reduced, and since activated carbon treatment is performed using a filtration filter, there is an advantage that the floor space can be reduced as compared with the case where a filtration tank is used.
前述した様に本発明は、硫酸銅めっき浴の添加剤濃度
を自動的に測定し、添加剤を基準濃度まで補充すると共
に添加剤の積算補充量に応じ活性炭濾過を行う工程を有
するので硫酸銅めっき浴の添加剤濃度を一定範囲に維持
することができ、下記の効果が得られる。As described above, the present invention has a step of automatically measuring the additive concentration of the copper sulfate plating bath, replenishing the additive to the standard concentration, and performing activated carbon filtration according to the cumulative replenishment amount of the additive. The additive concentration of the plating bath can be maintained within a certain range, and the following effects can be obtained.
(1)めっき浴の安定性が保たれ、めっき仕上り不良を
防止できる。(1) The stability of the plating bath is maintained and defective plating finish can be prevented.
(2)一定の硫酸銅めっき物性が維持できる。(2) Constant copper sulfate plating properties can be maintained.
第1図は本発明の一実施例を構成を示すブロック図、第
2図は実施例2の構成を示すブロック図である。 1……硫酸銅めっき槽、2……添加剤自動分析装置、3
……コントローラー、4……添加剤定量ポンプ、4a……
添加剤タンク、5……活性炭濾過槽、6……活性炭濾過
槽循環ポンプ、7……硫酸銅めっき槽、8……添加剤自
動分析装置、9……コントローラー、10……添加剤定量
ポンプ、10a……添加剤タンク、11……積算電流計、12
……添加剤定期補充ポンプ、12a……添加剤定期補充タ
ンク、13……活性炭濾過循環ポンプ、14……活性炭濾過
フィルター。FIG. 1 is a block diagram showing the structure of an embodiment of the present invention, and FIG. 2 is a block diagram showing the structure of the second embodiment. 1 ... Copper sulfate plating tank, 2 ... Automatic additive analyzer, 3
...... Controller, 4 …… Additive metering pump, 4a ……
Additive tank, 5 ... Activated carbon filter tank, 6 ... Activated carbon filter tank circulation pump, 7 ... Copper sulfate plating tank, 8 ... Additive automatic analyzer, 9 ... Controller, 10 ... Additive metering pump, 10a ... Additive tank, 11 ... Integrating ammeter, 12
...... Additive regular replenishment pump, 12a …… Additive regular replenishment tank, 13 …… Activated carbon filtration circulation pump, 14 …… Activated carbon filtration filter.
Claims (1)
ンプリングする工程と、回転電極を用いた電位走査スト
リッピング法により前記サンプリング液中の添加剤濃度
を定量する工程と、その添加剤濃度から不足する添加材
料を演算する工程と、不足する添加剤を補充する工程
と、添加剤の積算補充量に応じてめっき浴中の副生成物
を活性炭濾過で除去する工程とを有することを特徴とす
る硫酸銅めっき浴の管理方法。1. A step of sampling a fixed amount of a plating solution from a copper sulfate plating bath, a step of quantifying the additive concentration in the sampling solution by a potential scanning stripping method using a rotating electrode, and the additive concentration. Is characterized by having a step of calculating an additional material lacking from the above, a step of replenishing the insufficient additive, and a step of removing a by-product in the plating bath by activated carbon filtration according to the integrated supplemental amount of the additive Control method of copper sulfate plating bath.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2315358A JP2558388B2 (en) | 1990-11-20 | 1990-11-20 | Management method of copper sulfate plating bath |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2315358A JP2558388B2 (en) | 1990-11-20 | 1990-11-20 | Management method of copper sulfate plating bath |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH04187800A JPH04187800A (en) | 1992-07-06 |
JP2558388B2 true JP2558388B2 (en) | 1996-11-27 |
Family
ID=18064456
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2315358A Expired - Fee Related JP2558388B2 (en) | 1990-11-20 | 1990-11-20 | Management method of copper sulfate plating bath |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP2558388B2 (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2016174705A1 (en) * | 2015-04-27 | 2016-11-03 | 株式会社Jcu | Method for managing copper sulfate plating solution |
-
1990
- 1990-11-20 JP JP2315358A patent/JP2558388B2/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
JPH04187800A (en) | 1992-07-06 |
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