JPH04187800A - Method for controlling copper sulfate plating bath - Google Patents
Method for controlling copper sulfate plating bathInfo
- Publication number
- JPH04187800A JPH04187800A JP31535890A JP31535890A JPH04187800A JP H04187800 A JPH04187800 A JP H04187800A JP 31535890 A JP31535890 A JP 31535890A JP 31535890 A JP31535890 A JP 31535890A JP H04187800 A JPH04187800 A JP H04187800A
- Authority
- JP
- Japan
- Prior art keywords
- additive
- plating
- bath
- copper sulfate
- tank
- 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.)
- Granted
Links
- 238000007747 plating Methods 0.000 title claims abstract description 51
- 229910000365 copper sulfate Inorganic materials 0.000 title claims abstract description 21
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000000654 additive Substances 0.000 claims abstract description 58
- 230000000996 additive effect Effects 0.000 claims abstract description 51
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 239000006227 byproduct Substances 0.000 claims abstract description 6
- 230000001186 cumulative effect Effects 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 230000007812 deficiency Effects 0.000 abstract description 3
- 230000002950 deficient Effects 0.000 abstract 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 6
- 229910001431 copper ion Inorganic materials 0.000 description 6
- 230000000704 physical effect Effects 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910000367 silver sulfate Inorganic materials 0.000 description 2
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- -1 chlorine ions Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- BWFPGXWASODCHM-UHFFFAOYSA-N copper monosulfide Chemical compound [Cu]=S BWFPGXWASODCHM-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Landscapes
- Electroplating And Plating Baths Therefor (AREA)
Abstract
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。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for managing a copper sulfate plating bath, and particularly to a method for managing additives.
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。−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、−船釣
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。A copper sulfate plating bath basically consists of copper ions, sulfuric acid, chloride ions, additives, etc. Among these, sulfuric acid and chloride ions are factors whose concentration decreases with the plating reaction, and the concentration of copper ion increases with the plating reaction. Excess or deficiency of these factors will deteriorate plating uniformity and plating finish, so sulfuric acid is automatically analyzed using neutralization titration, chlorine ions and copper ions are analyzed using colorimetry, and increased copper ions are analyzed using weak electrolytic method. Excess copper ions were precipitated as metallic copper to keep the copper ion concentration constant. - On the other hand, the additive is
It is consumed by the plating reaction and produces its by-products. Insufficient additive concentration and increase in by-products have the strongest effect on plating finish, plating physical properties, etc., so controlling the concentration of additives is important. However, the content of additives in the copper sulfate plating bath was very small and quantitative analysis was very difficult. , replenishment was carried out depending on the finished state of the Hull cell test, etc.
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てきる
硫酸鋼めっき浴の管理方法を提供することにある。With conventional control methods, it is not possible to quantitatively analyze the additive concentration in the copper sulfate plating bath, making it difficult to maintain a constant plating finish and physical properties.If the additive concentration falls below the lower limit concentration, poor plating finish or physical properties may occur. The object of the present invention is to solve the conventional drawbacks and to maintain the additive concentration in a copper sulfate plating bath within a certain range, thereby maintaining the stability of the plating bath. An object of the present invention is to provide a method for managing a sulfuric acid steel plating bath that can prevent poor plating finish and maintain constant physical properties of copper sulfate plating.
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 method for managing a copper sulfate plating bath of the present invention includes a step of sampling a certain amount of plating solution from a copper sulfate plating bath, and quantifying the additive concentration in the sampled solution by a potential scanning stripping method using a rotating electrode. A process, a process of calculating the missing additive material from the additive concentration, a process of replenishing the missing additive, and a process of removing by-products in the plating solution by activated carbon filtration according to the cumulative replenishment amount of the additive. It is characterized by including a process.
本発明によれば硫Ｂ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て、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てきる。According to the present invention, the plating bath has a step of automatically measuring the additive concentration in the copper sulfur plating bath, replenishing the additive to the standard concentration, and performing activated carbon filtration according to the cumulative replenishment amount of the additive. The stability of the coating is maintained and defects in the plating finish can be prevented. In addition, certain physical properties of copper sulfate plating can be maintained.
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。Next, the present invention will be explained with reference to the drawings. FIG. 1 is a block diagram of an embodiment of the present invention.
硫酸銅めっき槽１より、］時間毎に２００ｍ１を添加剤
自動分析装置２にサンプリンタする。添加剤自動分析装
置２にて分析した分析値をコントロ一ラー３にて演算し
添加剤濃度を標準値］○ｍ１／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２０ＯＬ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。From the copper sulfate plating tank 1, 200 ml is sampled every hour into the additive automatic analyzer 2. The analysis value analyzed by the automatic additive analyzer 2 is calculated by the controller 3, and the replenishment amount to adjust the additive concentration to the standard value]○ml/L is transmitted to the metering pump 4. Further, the controller 3 calculates the cumulative replenishment amount of the additive, and every time the replenishment amount reaches 20 OL, it is transmitted to the activated carbon filtration circulation pump 6, and filtration processing is performed in the activated carbon filtration tank 5 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。Using the method described above, the additive concentration in the copper sulfate plating bath is managed by repeating additive replenishment based on the additive concentration measurement value every hour and activated carbon filtration every 200 L of replenishment.
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２００ｍ１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１０ ｍ ｌ ／ Ｌ
に合わせる為の補充１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２０ＯＬ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 sulfate plating tank 7, 200 ml is sampled every hour into the automatic additive analyzer 8, and the analyzed value is calculated by the controller 9, and the additive concentration is set to the standard value of 10 ml/L.
Replenishment 1 is transmitted to the metering pump 10 to match the amount. In addition, the controller 9 calculates the cumulative replenishment amount of the additive, and every time the replenishment amount reaches 20OL, the activated carbon filtration circulation pump 1 is activated.
and filtered through an activated carbon 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２０ＯＬ毎の活性炭濾過を繰り返しながら、硫ｒ
１ｉ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
小さくすることかでき、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かある。Using the method described above, while repeating additive replenishment based on the cumulative applied current value of 5000 AH based on the additive concentration measurement value every hour and activated carbon filtration every 20 OL of the replenishment amount, sulfur r.
Control the concentration of additives in the 1i copper plating bath. In this example, since additive replenishment is performed using an automatic analyzer and integrated current value, it is possible to reduce the variation in additive concentration in the copper sulfate plating bath.Also, since the activated carbon treatment is performed using a filtration filter, This has the advantage that the floor space can be made smaller than when using a filtration tank.
前述した様に本発明は、硫酸銀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て補充すると共に
添加剤の積算補充量に応し活性炭濾過を行う工程を有す
るのて硫酸銀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 mentioned above, the present invention has a step of automatically measuring the additive concentration in the silver 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 in the silver sulfate 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) Stability of the plating bath is maintained and poor plating finish can be prevented.
（２）一定の硫酸銅めっき物性か維持てきる。(2) Constant physical properties of copper sulfate plating 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）・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、１
２ａ・・・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。
代理人 弁理士 内 原 習
ｊ≧Ｓ ノ’ａＸ ンＸＣａ
兜 １ 囚FIG. 1 is a block diagram showing the configuration of an embodiment of the present invention, and FIG. 2 is a block diagram showing the configuration of a second embodiment. 1... Copper sulfate plating tank, 2... Additive automatic analyzer,
3. Controller) roller, 4. Additive metering pump,
4a... Additive tank, 5... Activated carbon filtration tank, 6, Activated carbon filtration tank circulation pump, 7... Copper sulfate plating tank, 8...
Additive automatic analyzer, 9...controller, 10...
Additive metering pump, 10a...Additive tank, 11.
... Integral ammeter, 12 ... Additive regular replenishment pump, 1
2a... Additive regular replenishment tank, 13... Activated carbon filtration circulation pump, 14... Activated carbon filtration filter. Agent Patent Attorney Uchihara Xij≧S ノ'aX んXCa Kabuto 1 Prisoner
Claims (1)
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。A step of sampling a certain amount of plating solution from a copper sulfate plating tank, a step of quantifying the additive concentration in the sampled solution by a potential scanning stripping method using a rotating electrode, and determining the missing additive material from the additive concentration. Copper sulfate plating characterized by comprising a step of calculating, a step of replenishing missing additives, and a step of removing by-products in the plating bath by activated carbon filtration according to the cumulative replenishment amount of additives. How to manage your 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 true JPH04187800A (en) | 1992-07-06 |
| JP2558388B2 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) |
Cited By (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
Cited By (3)
| 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 |
| CN107532324A (en) * | 2015-04-27 | 2018-01-02 | 株式会社杰希优 | The management method of copper sulfate bath |
| JPWO2016174705A1 (en) * | 2015-04-27 | 2018-02-15 | 株式会社Ｊｃｕ | Management method of copper sulfate plating solution |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2558388B2 (en) | 1996-11-27 |
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