JP6603473B2 - 電気めっき浴分析 - Google Patents
電気めっき浴分析 Download PDFInfo
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- JP6603473B2 JP6603473B2 JP2015086711A JP2015086711A JP6603473B2 JP 6603473 B2 JP6603473 B2 JP 6603473B2 JP 2015086711 A JP2015086711 A JP 2015086711A JP 2015086711 A JP2015086711 A JP 2015086711A JP 6603473 B2 JP6603473 B2 JP 6603473B2
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/026—Dielectric impedance spectroscopy
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
- C25D21/14—Controlled addition of electrolyte components
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Molecular Biology (AREA)
Description
60g/LのCu2+(CuSO4から)、50g/Lの18N H2SO4、80mg/LのCl−(1NのHClから)を含む電解質、並びに8.0mL/Lの抑制剤を一緒にすることによりキャリブレーション溶液が調製された。それぞれが異なる量の促進剤を有する4種類のキャリブレーションサンプルが調製された。それぞれのキャリブレーション溶液は表1に示される促進剤の量および1.5mL/Lのレベラーの量で調製された。各キャリブレーション溶液についてのインピーダンス応答が測定された後で、追加の1mL/Lのレベラーが各キャリブレーション溶液に添加され(合計2.5mL/Lのレベラー)、そしてインピーダンスが再び測定された。このプロセスがさらに2回繰り返され、3.5および4.5mL/Lのレベラーを有するキャリブレーション溶液についてのインピーダンス測定を行った。各キャリブレーション溶液についての促進剤および合計のレベラー濃度が表1に示される。
Claims (9)
- a)回転可能な作用電極、対電極、参照電極、ポテンシオスタットおよび周波数応答分析器を有し、前記対電極が前記作用電極および前記参照電極に動作可能に連絡している装置を提供する工程、
b)未知の量の有機添加剤を含む金属電気めっき浴溶液を得る工程、
c)前記作用電極、参照電極および対電極のそれぞれを前記金属電気めっき溶液と接触させ、そして前記作用電極を第一の回転速度で回転させつつ陽電位を印加することによって前記作用電極表面を清浄化する工程、
d)開放回路電位で、前記工程c)において清浄化された前記作用電極を第二の回転速度で回転させることにより、前記電気めっき溶液中の対流を平衡化する工程、ここでかかる工程d)は、前記行程c)の後に、前記工程c)において用いられた前記金属電気めっき溶液中に前記作用電極を維持しながら開始され、及び前記第二の回転速度は、前記第一の回転速度とは異なる、
e)前記作用電極に金属アンダーポテンシャル析出ピークの50〜500mV卑である電位を印加し、かつ1〜100mVの交番電位変動をオーバーレイする工程、
f)10kHz〜1mHzの周波数範囲にわたる前記有機添加剤溶液のインピーダンス応答を測定する工程、
g)前記インピーダンス応答から周波数を選択する工程、並びに
h)前記選択された周波数において、前記インピーダンス応答をキャリブレーション曲線と比較することにより前記有機添加剤の濃度を決定する工程を含む、金属電気めっき浴中の1種以上の有機成分の濃度を決定する方法。 - 前記金属が銅である請求項1に記載の方法。
- 前記交番電位変動がサイン波および矩形波から選択される請求項1に記載の方法。
- 前記第一の回転速度が前記第二の回転速度よりも速い請求項1に記載の方法。
- 前記作用電極が白金ディスクである請求項1に記載の方法。
- 前記対電極が白金を含む請求項1に記載の方法。
- 前記有機添加剤が促進剤、抑制剤、レベラーおよびこれらの混合物から選択される請求項1に記載の方法。
- 前記インピーダンスが1Hzの周波数で選択される請求項1に記載の方法。
- 複数の周波数が工程g)において選択される請求項1に記載の方法。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US201461982726P | 2014-04-22 | 2014-04-22 | |
US61/982,726 | 2014-04-22 |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2015206794A JP2015206794A (ja) | 2015-11-19 |
JP6603473B2 true JP6603473B2 (ja) | 2019-11-06 |
Family
ID=52991577
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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JP2015086711A Expired - Fee Related JP6603473B2 (ja) | 2014-04-22 | 2015-04-21 | 電気めっき浴分析 |
Country Status (6)
Country | Link |
---|---|
US (1) | US9612217B2 (ja) |
EP (1) | EP2937686B1 (ja) |
JP (1) | JP6603473B2 (ja) |
KR (1) | KR20150122084A (ja) |
CN (1) | CN105154962B (ja) |
TW (1) | TWI571539B (ja) |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105891312B (zh) * | 2016-04-07 | 2018-10-30 | 广东天承科技有限公司 | 电镀铜药水的效果评价方法 |
TWI669419B (zh) * | 2018-06-08 | 2019-08-21 | 國立臺灣科技大學 | 電解裝置 |
US10590560B1 (en) | 2018-08-22 | 2020-03-17 | Eci Technology, Inc. | Control of additive turnover in an electrodeposition solution |
TWI704346B (zh) * | 2019-08-02 | 2020-09-11 | 財團法人工業技術研究院 | 智慧濃度測量系統、方法及智慧濃度分析模組 |
CN113046818A (zh) * | 2019-12-26 | 2021-06-29 | 鸿宇科技股份有限公司 | 电镀添加剂浓度监控装置 |
KR20220159469A (ko) * | 2020-03-30 | 2022-12-02 | 램 리써치 코포레이션 | 레벨링 화합물 제어 |
CN113252749B (zh) * | 2021-05-13 | 2023-03-21 | 天津理工大学 | 检测冰晶电流及阻抗的电化学测试方法 |
CN113913913A (zh) * | 2021-10-29 | 2022-01-11 | 矽磐微电子(重庆)有限公司 | 电镀锡液中整平剂浓度的测试方法及电镀空白溶液 |
Family Cites Families (15)
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US4812210A (en) * | 1987-10-16 | 1989-03-14 | The United States Department Of Energy | Measuring surfactant concentration in plating solutions |
US5370776A (en) | 1993-10-20 | 1994-12-06 | Chevron Research And Technology Company | Electrochemical impedance spectroscopy method for evaluating corrosion inhibitor performance |
US5755954A (en) | 1996-01-17 | 1998-05-26 | Technic, Inc. | Method of monitoring constituents in electroless plating baths |
US6508924B1 (en) | 2000-05-31 | 2003-01-21 | Shipley Company L.L.C. | Control of breakdown products in electroplating baths |
DE60113214T2 (de) | 2000-11-02 | 2006-06-08 | Shipley Co., L.L.C., Marlborough | Plattierungsbadanalyse |
US6572753B2 (en) * | 2001-10-01 | 2003-06-03 | Eci Technology, Inc. | Method for analysis of three organic additives in an acid copper plating bath |
US7022212B2 (en) * | 2001-10-26 | 2006-04-04 | American Air Liquide, Inc. | Micro structured electrode and method for monitoring wafer electroplating baths |
AU2003261193A1 (en) | 2002-07-19 | 2004-02-09 | Aleksander Jaworski | Method and apparatus for real time monitoring of electroplating bath performance and early fault detection |
JP2004323971A (ja) * | 2003-04-25 | 2004-11-18 | Rohm & Haas Electronic Materials Llc | 改良された浴分析 |
JP2004325441A (ja) * | 2003-04-25 | 2004-11-18 | Rohm & Haas Electronic Materials Llc | 分析方法 |
US6984299B2 (en) | 2004-04-27 | 2006-01-10 | Advanced Technology Material, Inc. | Methods for determining organic component concentrations in an electrolytic solution |
US7435320B2 (en) | 2004-04-30 | 2008-10-14 | Advanced Technology Materials, Inc. | Methods and apparatuses for monitoring organic additives in electrochemical deposition solutions |
US7186326B2 (en) | 2004-05-27 | 2007-03-06 | Eci Technology, Inc. | Efficient analysis of organic additives in an acid copper plating bath |
JP5365296B2 (ja) * | 2009-03-26 | 2013-12-11 | 富士電機株式会社 | 湿式めっき方法及び湿式めっき装置 |
KR20110110462A (ko) | 2010-04-01 | 2011-10-07 | 삼성전기주식회사 | 도금액의 활성도 측정 장치 및 방법 |
-
2015
- 2015-04-20 EP EP15164281.6A patent/EP2937686B1/en not_active Not-in-force
- 2015-04-21 KR KR1020150055797A patent/KR20150122084A/ko unknown
- 2015-04-21 JP JP2015086711A patent/JP6603473B2/ja not_active Expired - Fee Related
- 2015-04-22 TW TW104112835A patent/TWI571539B/zh not_active IP Right Cessation
- 2015-04-22 CN CN201510341903.0A patent/CN105154962B/zh not_active Expired - Fee Related
- 2015-04-22 US US14/693,818 patent/US9612217B2/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
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KR20150122084A (ko) | 2015-10-30 |
US9612217B2 (en) | 2017-04-04 |
US20150300970A1 (en) | 2015-10-22 |
JP2015206794A (ja) | 2015-11-19 |
TW201610239A (zh) | 2016-03-16 |
CN105154962A (zh) | 2015-12-16 |
CN105154962B (zh) | 2017-08-08 |
EP2937686A1 (en) | 2015-10-28 |
TWI571539B (zh) | 2017-02-21 |
EP2937686B1 (en) | 2017-03-08 |
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