JP2002322598A - Method for controlling concentration of plating bath and device therefor - Google Patents
Method for controlling concentration of plating bath and device thereforInfo
- Publication number
- JP2002322598A JP2002322598A JP2001126485A JP2001126485A JP2002322598A JP 2002322598 A JP2002322598 A JP 2002322598A JP 2001126485 A JP2001126485 A JP 2001126485A JP 2001126485 A JP2001126485 A JP 2001126485A JP 2002322598 A JP2002322598 A JP 2002322598A
- Authority
- JP
- Japan
- Prior art keywords
- plating
- plating bath
- concentration
- electrode
- potentiostat
- 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.)
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、めっき浴中のめっ
き液を採取することなく、めっき浴中のめっき成分の濃
度を測定して管理するめっき液の濃度管理方法およびそ
の装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a plating solution concentration management method and apparatus for measuring and managing the concentration of plating components in a plating bath without collecting the plating solution in the plating bath.
【０００２】[0002]
【従来の技術】プリント基板への回路形成やバンプ形成
などを行うために、金属めっきが行われる。めっきを行
うためには、めっき浴に被めっき物を浸漬させるが、め
っき浴中のめっき成分濃度を適正な濃度に維持していな
いと、適正にめっきができない。そのため、めっき浴中
のめっき成分濃度を適時測定する必要がある。従来から
行われているめっき成分濃度の測定方法は、滴定、ＩＣ
Ｐ（誘導結合プラズマ）発光分析またはイオンクロマト
グラフフィなどの定量分析方法が挙げられる。2. Description of the Related Art Metal plating is performed to form a circuit or a bump on a printed circuit board. In order to perform plating, an object to be plated is immersed in a plating bath. However, unless the concentration of plating components in the plating bath is maintained at an appropriate concentration, plating cannot be performed properly. Therefore, it is necessary to measure the concentration of the plating component in the plating bath as appropriate. Conventional methods for measuring plating component concentrations include titration, IC
Examples include a quantitative analysis method such as P (inductively coupled plasma) emission analysis or ion chromatography.
【０００３】例えば、硫酸銅めっき浴中の硫酸銅濃度を
測定する場合、次のように行われる。始めに、めっき液
１ｍｌを水２００ｍｌで希釈し、これにフッ化アンモニ
ウム約１ｇを加え、さらにアンモニア水（１＋１）を深
青色になるまで加えて試料溶液とする。次いで、０．１
重量％ＰＡＮ指示薬を５〜６滴加え、０．０５ｍｏｌ／
ｌのエチレンジアミン四酢酸溶液で滴定を行う。赤紫色
の試料溶液が緑色になったときのエチレンジアミン四酢
酸溶液の消費量を読み取り、硫酸銅の濃度を算出する。For example, when measuring the concentration of copper sulfate in a copper sulfate plating bath, the measurement is performed as follows. First, 1 ml of the plating solution is diluted with 200 ml of water, about 1 g of ammonium fluoride is added thereto, and ammonia water (1 + 1) is further added until the solution becomes deep blue to obtain a sample solution. Then 0.1
5 to 6 drops of a weight% PAN indicator were added, and 0.05 mol /
The titration is carried out with 1 l of an ethylenediaminetetraacetic acid solution. The consumption of the ethylenediaminetetraacetic acid solution when the red-purple sample solution turns green is read, and the concentration of copper sulfate is calculated.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、このよ
うな滴定による定量分析では、測定用のめっき液をめっ
き浴から採取して、これを測定に供するため、結果が得
られるまで時間を要してしまう。測定が行われている際
にも、めっき成分は消費されており、変化し続けてい
る。したがって、測定結果が判明した時点で、この測定
結果を参考にめっき成分を追加添加して濃度を調整しよ
うとしても、測定結果とは既にずれが生じているため濃
度を規定値に保つのは難しい。ＩＣＰ発光分析、イオン
クロマトグラフィなどの定量方法も、めっき液を採取し
て測定することには変わりなく同様の問題があった。本
発明は、めっき浴からめっき液を採取することなく、そ
の場でめっき成分の濃度を測定し、濃度を規定値に保つ
ことが可能なめっき浴の濃度管理方法およびその装置を
提供することを目的とする。However, in such quantitative analysis by titration, a plating solution for measurement is sampled from a plating bath and used for measurement, so that it takes time until a result is obtained. I will. While the measurements are being made, the plating components are being consumed and are changing. Therefore, when the measurement result is found, even if an attempt is made to adjust the concentration by additionally adding a plating component with reference to the measurement result, it is difficult to keep the concentration at the specified value because the measurement result already deviates. . Quantitative methods such as ICP emission spectrometry and ion chromatography have the same problem as in the case of collecting and measuring a plating solution. The present invention provides a plating bath concentration management method and apparatus capable of measuring the concentration of plating components on the spot without collecting a plating solution from the plating bath and keeping the concentration at a specified value. Aim.
【０００５】[0005]
【課題を解決するための手段】本発明のめっき浴の濃度
測定方法は、めっき浴に作用電極、対向電極および参照
電極を浸し、これらの電極とポテンショスタットとを接
続し、このポテンショスタットを用いて、めっき浴の分
極曲線を測定し、この分極曲線から作用電極と対向電極
との間の限界電流密度を求めて、さらにこの限界電流密
度からめっき成分の濃度を求める方法である。また、本
発明のめっき浴の濃度管理装置は、めっき浴中に浸され
る作用電極と対向電極と参照電極とが接続されたポテン
ショスタットを有し、このポテンショスタットによりめ
っき浴中のめっき成分の濃度を測定するようにしたもの
である。According to the method for measuring the concentration of a plating bath of the present invention, a working electrode, a counter electrode and a reference electrode are immersed in a plating bath, these electrodes are connected to a potentiostat, and the potentiostat is used. Then, the polarization curve of the plating bath is measured, the limit current density between the working electrode and the counter electrode is determined from the polarization curve, and the concentration of the plating component is further determined from the limit current density. Further, the concentration control device of the plating bath of the present invention has a potentiostat in which a working electrode, a counter electrode, and a reference electrode that are immersed in the plating bath are connected, and the potentiostat controls a plating component in the plating bath. This is to measure the concentration.
【０００６】[0006]
【発明の実施の形態】図１は本発明のめっき浴の濃度管
理装置の一例を示すものである。この濃度管理装置は、
負極であり、被めっき物でもある作用電極２と、作用電
極２との電位差を測定するための参照電極４と、正極で
ある対向電極３と、これら電極が接続されたポテンショ
スタット１とを有して構成されている。そして、前記の
３種の電極は、めっき浴５中に浸漬されている。また、
ポテンショスタット１には、濃度を算出する演算部６が
接続されている。本発明におけるポテンショスタット１
は、電源を内蔵しており、作用電極２と参照電極４との
電位差を一定にした定電位電解めっきを行うための装置
であり、それに加えて、本発明の特徴とするところの、
作用電極２と対向電極３との間の電流密度を測定するた
めの装置でもある。測定された電流密度はめっき浴中の
めっき成分濃度を求めるためのデータとして利用され
る。すなわち、電流密度は、ポテンショスタット１に接
続された演算部６で解析されて、限界電流密度が求めら
れ、さらに、限界電流密度からめっき成分濃度の算出が
行われる。また、演算部６でめっき成分の不足量を計算
し、そのデータを図示しない制御部に送り、めっき成分
を自動供給するようにしてもよい。FIG. 1 shows an example of a plating bath concentration control apparatus according to the present invention. This concentration control device
It has a working electrode 2 which is a negative electrode and a plating object, a reference electrode 4 for measuring a potential difference between the working electrode 2 and the counter electrode 3 which is a positive electrode, and a potentiostat 1 to which these electrodes are connected. It is configured. The three electrodes are immersed in the plating bath 5. Also,
The potentiostat 1 is connected to a calculation unit 6 for calculating the density. Potentiostat 1 in the present invention
Is a device for carrying out constant potential electroplating with a built-in power source and making the potential difference between the working electrode 2 and the reference electrode 4 constant. In addition to this, a feature of the present invention is that
It is also a device for measuring the current density between the working electrode 2 and the counter electrode 3. The measured current density is used as data for obtaining a plating component concentration in the plating bath. That is, the current density is analyzed by the calculation unit 6 connected to the potentiostat 1 to determine the limit current density, and further, the plating component concentration is calculated from the limit current density. Alternatively, the computing unit 6 may calculate the shortage of the plating component, send the data to a control unit (not shown), and automatically supply the plating component.
【０００７】作用電極２には、被めっき物が電極として
用いられ、対向電極３にはイオン化傾向の小さい金属が
用いられており、作用電極２と対向電極３との間のポテ
ンショスタット内部には電源が設けられている。この電
源を印加することにより、めっきが行われる。参照電極
４は、めっきを行う際に作用電極２との電位差を測定す
るためのものである。ポテンショスタット１を用いた定
電位では作用電極２と参照電極４との電位差が一定にな
るように、作用電極２との電圧を変化させる。参照電極
４に使用される電極としては、標準水素電極、または標
準水素電極との電位差が一定である銀／塩化銀電極など
が用いられる。このような電極を用いることにより、作
用電極２と標準水素電極との電位差を求めることができ
る。An object to be plated is used for the working electrode 2, a metal having a low ionization tendency is used for the counter electrode 3, and a potentiostat between the working electrode 2 and the counter electrode 3 is provided inside the potentiostat. A power supply is provided. By applying this power, plating is performed. The reference electrode 4 is for measuring a potential difference from the working electrode 2 when performing plating. At a constant potential using the potentiostat 1, the voltage between the working electrode 2 and the reference electrode 4 is changed so that the potential difference between the working electrode 2 and the reference electrode 4 becomes constant. As the electrode used as the reference electrode 4, a standard hydrogen electrode, a silver / silver chloride electrode having a constant potential difference from the standard hydrogen electrode, or the like is used. By using such an electrode, the potential difference between the working electrode 2 and the standard hydrogen electrode can be obtained.
【０００８】ポテンショスタット１によりめっき成分の
濃度を測定するためには、あらかじめ、めっき成分濃度
と限界電流密度方法との検量線を作成しておく必要があ
る。検量線の作成は、めっき成分の濃度が既知であるめ
っき浴を複数用意する。その中の一つのめっき浴に電極
を浸し、作用電極２の電位を自然浸漬電位からカソード
方向に分極させる。そのときの作用電極２と対向電極３
との電流密度を測定して、図２に示すような分極曲線を
作成する。In order to measure the concentration of the plating component using the potentiostat 1, it is necessary to prepare a calibration curve between the plating component concentration and the limiting current density method in advance. In preparing the calibration curve, a plurality of plating baths having known concentrations of plating components are prepared. The electrode is immersed in one of the plating baths, and the potential of the working electrode 2 is polarized from the natural immersion potential toward the cathode. Working electrode 2 and counter electrode 3 at that time
Then, a polarization curve as shown in FIG. 2 is created.
【０００９】この分極曲線は、横軸が作用電極２と標準
水素電極との電位Ｅであり、縦軸が作用電極２と対向電
極との間の電流密度Ｊである。図２中の点Ａはめっき浴
に電極が浸漬しただけの分極開始前の状態である。すな
わち、自然浸漬電位であり、電流密度は低い。この状態
からカソード方向に分極させると、電流密度は上昇し、
やがて点Ｂで一定となり、その状態が点Ｃまで継続す
る。この点Ｂから点Ｃの間の一定の電流密度は、めっき
成分である金属イオンの濃度に応じて電極間を流れるも
ので、一般的に限界電流密度と呼ばれている。なお、点
Ｃから点Ｄは金属イオンが関与する電流密度ではなく、
水素イオンが関与する電流密度である。このようにし
て、他のめっき浴についても限界電流密度を測定し、め
っき成分の濃度と限界電流密度との関係をプロットし、
検量線を作成する。上記のような分極曲線の作成および
検量線の作成は、ポテンショスタット１から演算部６に
電流密度のデータが送られ、演算部６で作成、記憶させ
ることができる。In the polarization curve, the horizontal axis represents the potential E between the working electrode 2 and the standard hydrogen electrode, and the vertical axis represents the current density J between the working electrode 2 and the counter electrode. Point A in FIG. 2 is a state before the start of polarization, in which the electrode is simply immersed in the plating bath. That is, it is a natural immersion potential and the current density is low. When polarized from this state to the cathode direction, the current density increases,
Eventually, it becomes constant at the point B, and the state continues up to the point C. The constant current density between the point B and the point C flows between the electrodes according to the concentration of the metal ion as the plating component, and is generally called a limiting current density. Note that points C to D are not current densities involving metal ions,
This is the current density involving hydrogen ions. In this way, the limiting current density was measured for other plating baths, and the relationship between the concentration of the plating component and the limiting current density was plotted.
Create a calibration curve. For the creation of the polarization curve and the calibration curve as described above, data of the current density is sent from the potentiostat 1 to the calculation unit 6, and the calculation unit 6 can create and store the data.
【００１０】次いで、ポテンショスタットに接続された
電極を、めっきを行うめっき浴に浸漬させ、めっきを行
う。被めっき物へのめっきを繰り返していくと、めっき
成分の濃度は低下していく。めっき作業の合間の適時
に、上記の方法で限界電流密度を測定し、作成した検量
線から濃度を求める。この測定では、めっき浴に浸漬し
た電極を用いて測定するので、めっき液を採取する必要
がなく、直ちに結果が判明する。したがって、この測定
結果に基づいてめっき成分を追加添加すれば、リアルタ
イムな濃度調整を行えるので、めっき浴中のめっき成分
の濃度を規定値に保つことができる。なお、本発明のめ
っき浴の測定方法で測定されるめっき成分は特に制限は
なく、いずれの金属塩、酸に対してもこの方法で行うこ
とができる。Next, the electrode connected to the potentiostat is immersed in a plating bath for plating, and plating is performed. As the plating of the object to be plated is repeated, the concentration of the plating component decreases. At an appropriate time between the plating operations, the limiting current density is measured by the above-described method, and the concentration is determined from the prepared calibration curve. In this measurement, since the measurement is performed using the electrode immersed in the plating bath, there is no need to collect a plating solution, and the result is immediately obtained. Therefore, if a plating component is additionally added based on the measurement result, the concentration can be adjusted in real time, so that the concentration of the plating component in the plating bath can be maintained at a specified value. The plating component measured by the plating bath measuring method of the present invention is not particularly limited, and any metal salt or acid can be measured by this method.
【００１１】[0011]
【実施例】作用電極に銅板１ｃｍ2 を用い、対向電極に
白金板を用い、参照電極に銀／塩化銀電極を用い、これ
らの電極をポテンショスタットに接続した。次いで、表
１に示す硫酸銅を含む溶液を調製した。この液に、ポテ
ンショスタットに接続された電極を浸漬させた。EXAMPLE A copper plate of 1 cm 2 was used as a working electrode, a platinum plate was used as a counter electrode, a silver / silver chloride electrode was used as a reference electrode, and these electrodes were connected to a potentiostat. Next, a solution containing copper sulfate shown in Table 1 was prepared. An electrode connected to a potentiostat was immersed in this liquid.
【００１２】[0012]
【表１】 [Table 1]
【００１３】次いで、分極速度−５ｍＶ／ｓで作用電極
をカソード方向に分極させて、参照電極との電位を広げ
た。作用電極と標準水素電極との電位差が−０．４〜−
０．５Ｖの時に電流密度がほぼ一定となり、これを限界
電流密度として読み取った。その結果を表２に示す。そ
して、この結果を用いて硫酸銅濃度と限界電流密度との
検量線を作成した。Next, the working electrode was polarized in the cathode direction at a polarization speed of -5 mV / s, and the potential with the reference electrode was widened. The potential difference between the working electrode and the standard hydrogen electrode is -0.4 to-
At 0.5 V, the current density became almost constant, and this was read as the limit current density. Table 2 shows the results. Then, a calibration curve of the copper sulfate concentration and the limiting current density was prepared using the results.
【００１４】[0014]
【表２】 [Table 2]
【００１５】次に、ポテンショスタットに接続された電
極が浸漬した１５０ｇ／ｌの硫酸銅を含むめっき浴でめ
っきを行った。めっき作業を繰り返した後、ポテンショ
スタットにより限界電流密度を測定したところ、５．５
Ａ／ｄｍ2 であった。この時の硫酸銅の濃度は、上記で
作成した検量線から１００ｇ／ｌであることがわかっ
た。この結果に基づいて、再び硫酸銅濃度が１５０ｇ／
ｌになるように硫酸銅を追加添加した。上記のめっき浴
の濃度測定方法は直ちに結果を知ることができ、その結
果に基づいて硫酸銅を追加添加したので、めっき浴のめ
っき成分の濃度をほぼ１５０ｇ／ｌで一定にすることが
できた。Next, plating was performed in a plating bath containing 150 g / l copper sulfate in which the electrodes connected to the potentiostat were immersed. After the plating operation was repeated, the critical current density was measured using a potentiostat, and the result was 5.5.
A / dm 2 . At this time, the concentration of copper sulfate was found to be 100 g / l from the calibration curve prepared above. Based on this result, the concentration of copper sulfate was again 150 g /
Copper sulfate was further added so as to obtain 1. The above-mentioned method for measuring the concentration of the plating bath can immediately know the result, and based on the result, copper sulfate was added, so that the concentration of the plating component in the plating bath could be kept constant at approximately 150 g / l. .
【００１６】[0016]
【発明の効果】本発明のめっき浴の濃度管理方法によれ
ば、めっき浴に作用電極、対向電極および参照電極を浸
し、これらの電極とポテンショスタットとを接続し、こ
のポテンショスタットを用いて、めっき浴の分極曲線を
測定し、この分極曲線から作用電極と対向電極との間の
限界電流密度を求めて、さらにこの限界電流密度からめ
っき成分の濃度を求める方法であるので、めっき浴から
めっき液を採取することなく、濃度測定することができ
るため、直ちに測定結果を得ることができる。また、本
発明のめっき浴の濃度管理装置によれば、めっき浴中に
浸される作用電極と対向電極と参照電極とが接続された
ポテンショスタットを有し、このポテンショスタットに
よりめっき浴中のめっき成分の濃度を測定するようにし
たものであるので、めっき成分濃度を規定値に保つのが
容易である。According to the method for controlling the concentration of a plating bath of the present invention, a working electrode, a counter electrode and a reference electrode are immersed in a plating bath, these electrodes are connected to a potentiostat, and the potentiostat is used by using the potentiostat. This method measures the polarization curve of the plating bath, determines the limiting current density between the working electrode and the counter electrode from the polarization curve, and further determines the concentration of the plating component from the limiting current density. Since the concentration can be measured without collecting the liquid, the measurement result can be obtained immediately. Further, according to the concentration control apparatus for a plating bath of the present invention, there is provided a potentiostat in which a working electrode, a counter electrode, and a reference electrode that are immersed in the plating bath are connected. Since the concentration of the component is measured, it is easy to keep the plating component concentration at a specified value.
【図１】 本発明のめっき浴の濃度管理装置の一例を示
す模式図である。FIG. 1 is a schematic view showing an example of a plating bath concentration management device of the present invention.
【図２】 本発明におけるポテンショスタットにより測
定された分極曲線の一例を示すグラフである。FIG. 2 is a graph showing an example of a polarization curve measured by a potentiostat according to the present invention.
１・・・ポテンショスタット、２・・・作用電極、３・
・・対向電極、４・・・参照電極、５・・・めっき浴。DESCRIPTION OF SYMBOLS 1 ... potentiostat, 2 ... working electrode, 3 ...
..Counter electrode, 4 ... reference electrode, 5 ... plating bath.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 岩崎 庄治 東京都江東区木場一丁目５番１号 株式会 社フジクラ内 ──────────────────────────────────────────────────の Continuing on the front page (72) Inventor Shoji Iwasaki 1-5-1, Kiba, Koto-ku, Tokyo Inside Fujikura Co., Ltd.
Claims (2)
参照電極を浸し、これらの電極とポテンショスタットと
を接続し、 このポテンショスタットを用いて、めっき浴の分極曲線
を測定し、 この分極曲線から作用電極と対向電極との間の限界電流
密度を求めて、さらにこの限界電流密度からめっき浴中
のめっき成分の濃度を求めることを特徴とするめっき浴
の濃度管理方法。1. A working electrode, a counter electrode and a reference electrode are immersed in a plating bath, these electrodes are connected to a potentiostat, and a polarization curve of the plating bath is measured using the potentiostat. A method for controlling the concentration of a plating bath, comprising: determining a critical current density between a working electrode and a counter electrode from the working electrode; and determining a concentration of a plating component in the plating bath from the critical current density.
極と参照電極とが接続されたポテンショスタットを有
し、このポテンショスタットによりめっき浴中のめっき
成分の濃度を測定するようにしたことを特徴とするめっ
き浴の濃度管理装置。2. A potentiostat having a working electrode immersed in a plating bath, a counter electrode and a reference electrode connected thereto, and the concentration of a plating component in the plating bath is measured by the potentiostat. A concentration control device for a plating bath, characterized in that:
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| Application Number | Priority Date | Filing Date | Title |
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| JP2001126485A JP2002322598A (en) | 2001-04-24 | 2001-04-24 | Method for controlling concentration of plating bath and device therefor |
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| JP2001126485A JP2002322598A (en) | 2001-04-24 | 2001-04-24 | Method for controlling concentration of plating bath and device therefor |
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| JP2002322598A true JP2002322598A (en) | 2002-11-08 |
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| JP2001126485A Withdrawn JP2002322598A (en) | 2001-04-24 | 2001-04-24 | Method for controlling concentration of plating bath and device therefor |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007270320A (en) * | 2006-03-31 | 2007-10-18 | Ebara Corp | Polarization curve measurement method and electrolytic treatment apparatus |
| JP2013068359A (en) * | 2011-09-22 | 2013-04-18 | Hitachi Building Systems Co Ltd | Method and apparatus for grasping inhibitor concentration in absorbing liquid, and absorption chiller heater provided with the apparatus |
| KR20160131426A (en) | 2015-05-07 | 2016-11-16 | 가부시끼가이샤 제이씨유 | Management method of copper sulfate plating solution |
| JP2019127604A (en) * | 2018-01-22 | 2019-08-01 | トヨタ自動車株式会社 | Film deposition apparatus for metallic film |
-
2001
- 2001-04-24 JP JP2001126485A patent/JP2002322598A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007270320A (en) * | 2006-03-31 | 2007-10-18 | Ebara Corp | Polarization curve measurement method and electrolytic treatment apparatus |
| JP2013068359A (en) * | 2011-09-22 | 2013-04-18 | Hitachi Building Systems Co Ltd | Method and apparatus for grasping inhibitor concentration in absorbing liquid, and absorption chiller heater provided with the apparatus |
| KR20160131426A (en) | 2015-05-07 | 2016-11-16 | 가부시끼가이샤 제이씨유 | Management method of copper sulfate plating solution |
| JP2019127604A (en) * | 2018-01-22 | 2019-08-01 | トヨタ自動車株式会社 | Film deposition apparatus for metallic film |
| JP6996312B2 (en) | 2018-01-22 | 2022-02-04 | トヨタ自動車株式会社 | Metal film film forming equipment |
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