US2830014A - Electroplating process - Google Patents
Electroplating process Download PDFInfo
- Publication number
- US2830014A US2830014A US464638A US46463854A US2830014A US 2830014 A US2830014 A US 2830014A US 464638 A US464638 A US 464638A US 46463854 A US46463854 A US 46463854A US 2830014 A US2830014 A US 2830014A
- Authority
- US
- United States
- Prior art keywords
- liter
- nickel
- metal
- acid
- zinc
- 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 - Lifetime
Links
Classifications
-
- 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
Definitions
- Electroplating baths have heretofore been modified by the inclusion of organic sulfonic acids or organic sulfation products of various compounds. While the prior art brightening agents have usually elfected some improvement in the brightness characteristics and ductility of electrodeposits products from baths modified therewith, these brightening agents individually have not been sufficient to produce commercially desirable electrodeposits, and have to be used with another and sometimes with even two or more supplemental brightening agents to produce the desired result.
- an object of this invention to provide brightening agents for electroplating fbaths which may advantageously be used as a sole brightening agent or with other addition agents to produce bright and ductile electrodeposits.
- Another object of our invention is to provide electroplating compositions of improved character.
- Still another object of our invention is to provide electroplating baths which will produce bright, lustrous and ductile electrodeposits which in many instances may be used for their'intended purpose without further polishing or butting.
- the class of compounds having the above general structural formula consists essentially of well-known substances which may be produced very readily. For example, they can be obtained in a very simple manner and in a high degree of purity by reacting metal sulfides, metal hydro sulfides, or the salts of aliphatic, cycloaliphatic, aromatic-aliphatic, aromatic heterocyclic mercapto compounds, or metal compounds of dithiolic acids, thiol acids or thioamides with cyclic anhydrides or organic oxyalkanesulfonic acids (sultones), such as for example,
- Another method of producing the above sulfonic acid compounds is to react the sulfur-containing compounds referred to in the preceding paragraph with halogenalkanesulfonic acids or their salts rather than with sulitonesr In a few cases itis also possible to start with mercapto-alkane-sulfonic acid salts by reacting the same with corresponding halogen compounds.
- thioalkanesulfonic acids having the general structural formula referred to which can be prepared by any of the above methods and may then be added to electroplating baths as brightening agents and as agents which promote the increase of the ductility of metal electrodeposits produced from such baths in accordance with our invention are the following:
- the compounds or" our invention can beem- 'ployed in conjunction with other well-known brightening agents, conductivity-promotingsalts, wetting agents, porosity-preventing agents, smoothing agents, and the like.
- the amounts in which the thioalkanesulfonic acids, in accordance with our invention, are added to electroplating baths in order to produce bright and highly ductile metal electrodeposits range from 0.01 to 20 grams per liter of electroplating bath, depending upon the particular additive used and the type of metal which is intended to be electrodeposited.
- the temperature of electroplating baths modified in accordance with our invention should be about 60 C. during the electroplating operation and the current density range should be between 0.5 and 1 2 amp./dm.
- the current density which will produce the optimum brightening eifect depends upon the individual thioalkanesulfonic acid additive used to modify the electroplating bath in accordance with our invention.
- the surfaces of the objects to be electroplated in. electroplating baths modified in accordance with our .inven- 'tion may consist of any type of metal or alloy upon. which electroplates are usually deposited.
- the metal surface consists of steel, iron, zinc, and other non- 3 precious metals or their alloys, it is recommended that such surfaces be covered with a thin layer of copper in the customary cyanide-copper sulfate solution prior to plating such surface with the final metal electroplate.
- Electrodeposits produced from plating baths modified with the thioalkanesulfonic acids or their salts in accordance with our invention are extremely bright, adhere well to the base surface, have a high degree of ductility and are practically free from porosity. Their brightness is in most cases so high that subsequent polishing and buffing is not required.
- the thioalkanesulfonic acid additives of our invention are extremely stable in acid solutions, so that electro-- plating baths modified therewith remain capable of producing bright and duticle electrodeposits for extended periods of time even at high temperatures, and need to be rejuvenated only from time to time with small amounts of these additives.
- Example I nickel sulfate and 35 gm./liter boric acids Sheet steel which was pre-treated in a well-known manner in a copper sulfate-cyanide bath by dipping it therein in order to deposit a thin preliminary copper plate on the surface,
- the nickel plate thus produced was fine-bright, well-adhering and free from porosity, and required no further mechanical treatment such as buffing or polishing.
- di-sodium salt of di-n-propylthioether-w-w-disulfonic acid can be used with equal success.
- Example 111 Example 1V 1 gm. of dithiobenzoic acid-n-propylester-w-sodium sultonate was added to each liter of a zinc galvanizing bath containing 60 gm./ liter zinc cyanide, 50 gm./liter sodium cyanide, l5 gm./liter sodium hydroxide and 1 gm./liter sodium sulfite. Metal objects were then zinc-plated in this modified bath at room temperature and a current density between 2 and 10 ampJdmF. The zinc plate produced thereby was fine-bright and adhered very well to the metal surface.
- Example V A small amount of S-benzyl-3-thiopropane 1-sodium sulfonate was added to an acid copper-plating bath which contained 220 gm./liter copper sulfate and 60 gm./liter sulfuric acid. Objects were then copper-plated in this modified bath at room temperature and a current density of 5 amp./dm. The copper depositsproduced thereby were bright, soft and had an extremely fine grain.
- An electroplating bath for producing electro-deposits of a metal selected from the group consisting of copper,
- An electroplating bath for producing electrodeposits of nickel comprising an acid solution of at least one inorganic salt of nickel and 0.01 to 20 -gm./liter of the disodium salt of di-n-propylithioether-w-w-disulfonic acid.
- An electroplating bath for producing electrodeposits ,of ,zinc comprising an acid. solution of at least one inorganic salt of zinc and 0.01 to 20 gm./liter of dithiobenzoic acid-n-propylester-w-sodium sulfonate.
- An electroplating bath for producing electrodeposits of zinc comprising an acid solution of at least one inorganic salt of zinc and 0.01 to'20 gm./liter of thiobenzamide-S-propane-w-sodium sulfonate.
- An electroplating bath for producing electrodeposits of copper comprising an acid solution of at least one inorganic salt of copper and 0.01 to 20 gm./liter of S- benzyl-3-thiopropane-l-sodiurn sulfonate.
- An electroplating bath for producing electrodeposits of nickel comprising an acid solution of at least one inorganic salt of nickel and 0.01 to 20 gm./liter of phenyl-thiopropane-w-sodiurn sulfonate.
- the process of producing bright and lustrous electrodeposits of a metal selected from the group consisting of copper, zinc and nickel which comprises electrodepositing said metal from a bath containing said metal principally in the form of an acid solution of an inorganic salt of the metal in the presence of from 0.01 to 20 gm./liter of a sulfonic acid brightening agent having a structural formula selected from the group consisting of and their alkali metal salts, wherein R is selected from the group consisting of hydrogen, acyclic hydrocarbon radicals and cyclic non-heterocyclic hydrocarbon radicals, R is a lower alkylene radical, and Y is selected from the group consisting of lower alkylene, -CSNH-, -CSNH-phenyl, -CO--, -CS- and SO 10.
- the process of producing bright and lustrous electrodeposits of a metal selected from the group consisting of copper, zinc and nickel which comprises electrodepositing said metal from a bath containing said metal principally in the form of an acid solution of an inorganic salt of the metal in the presence of from 0.01 to 20 gm./liter of a brightening agent selected from the group consisting of sulfonic acids having the structural formula and and their alkali metal salts, wherein R is an] acyclic I and their alkali metal salts, wherein R is a cyclic nonheterocyclic hydrocarbon radical, Y is selected from the group consisting of lower alkylene, CSNH-, CSNH- phenyl--, CO-, CS and SO,;, and R is a lower alkylene radical.
- the process of producing bright and lustrous nickel electrodeposits which comprises electrodepositing said nickel from a bath containing said nickel principally in the form of an acid solution of at least one inorganic salt of nickel, in the presence of 0.01 to 20 gm./liter of the disodium salt of di-n-propylthioether-w-w-disulfonic acid as a brightening agent.
- the process of producing bright and lustrous zinc electrodeposits which comprises electrodepositing said zinc from a bath containing said zinc principally in the form of an acid solution of at least one inorganic salt of zinc, in the presence of 0.01 to 20 gm./liter of dithiobenzoic acid-n-propylester-w-sodium sulfonate as a brightening agent.
- the process of producing bright and lustrous zinc electrodeposits which comprises electrodepositing said zinc from a bath containing said zinc principally in the form of an acid solution of at least one inorganic salt of zinc, in the presence of 0.01 to 20 gm./liter of thiobenzamide-S-propane-w-sodium sulfonate as a brightening agent.
- the process of producing bright and lustrous copper electrodeposits which comprises electrodepositing said copper from a bath containing said copper principally in the form of an acid solution of at least one inorganic salt of copper, the presence of 0.0lto 20 gm./liter of S-benyl-3-thiopropane-l-sodium sulfonate as a brightening agent.
- the process of producing bright and lustrous nickel electrodeposits which comprises electrodepositing said nickel from a bath containing said nickel principally in the form of an acid solution of at least one inorganic salt of nickel, in the presence of 0.01 to 20 gm./liter of .phenylthiopropane-w-sodium sulfonate as a brightening agent. 7
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Paints Or Removers (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Nitrogen And Oxygen As The Only Ring Hetero Atoms (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DED17379A DE1037801B (de) | 1954-03-22 | 1954-03-22 | Bad zur galvanischen Herstellung von Metallueberzuegen |
DED0028636 | 1958-07-29 |
Publications (1)
Publication Number | Publication Date |
---|---|
US2830014A true US2830014A (en) | 1958-04-08 |
Family
ID=25970687
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US464638A Expired - Lifetime US2830014A (en) | 1954-03-22 | 1954-10-25 | Electroplating process |
US829227A Expired - Lifetime US3023150A (en) | 1954-03-22 | 1959-07-24 | Bath for the production of metal electroplates |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US829227A Expired - Lifetime US3023150A (en) | 1954-03-22 | 1959-07-24 | Bath for the production of metal electroplates |
Country Status (6)
Country | Link |
---|---|
US (2) | US2830014A (fr) |
BE (1) | BE534701A (fr) |
CH (2) | CH336668A (fr) |
DE (1) | DE1075398B (fr) |
FR (1) | FR1119382A (fr) |
GB (2) | GB804833A (fr) |
Cited By (20)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3000799A (en) * | 1960-02-10 | 1961-09-19 | Harshaw Chem Corp | Nickel plating solutions |
US3023150A (en) * | 1954-03-22 | 1962-02-27 | Dehydag Gmbh | Bath for the production of metal electroplates |
US3075899A (en) * | 1958-04-26 | 1963-01-29 | Dehydag Gmbh | Baths for the production of metal electroplates |
US3267010A (en) * | 1962-04-16 | 1966-08-16 | Udylite Corp | Electrodeposition of copper from acidic baths |
US3276979A (en) * | 1961-08-31 | 1966-10-04 | Dehydag Gmbh | Baths and processes for the production of metal electroplates |
US4376685A (en) * | 1981-06-24 | 1983-03-15 | M&T Chemicals Inc. | Acid copper electroplating baths containing brightening and leveling additives |
EP0343559A1 (fr) * | 1988-05-25 | 1989-11-29 | Raschig AG | Utilisation de composés éthane sulfone substitués en position 2 comme agents auxiliaires galvaniques |
US20010013472A1 (en) * | 2000-02-01 | 2001-08-16 | Kenji Nakamura | Method of plating for filling via holes |
US6652731B2 (en) * | 2001-10-02 | 2003-11-25 | Shipley Company, L.L.C. | Plating bath and method for depositing a metal layer on a substrate |
US6709568B2 (en) | 2002-06-13 | 2004-03-23 | Advanced Technology Materials, Inc. | Method for determining concentrations of additives in acid copper electrochemical deposition baths |
US20050067304A1 (en) * | 2003-09-26 | 2005-03-31 | King Mackenzie E. | Electrode assembly for analysis of metal electroplating solution, comprising self-cleaning mechanism, plating optimization mechanism, and/or voltage limiting mechanism |
US20050109624A1 (en) * | 2003-11-25 | 2005-05-26 | Mackenzie King | On-wafer electrochemical deposition plating metrology process and apparatus |
US20050224370A1 (en) * | 2004-04-07 | 2005-10-13 | Jun Liu | Electrochemical deposition analysis system including high-stability electrode |
US20050247576A1 (en) * | 2004-05-04 | 2005-11-10 | Tom Glenn M | Electrochemical drive circuitry and method |
US20060102475A1 (en) * | 2004-04-27 | 2006-05-18 | Jianwen Han | Methods and apparatus for determining organic component concentrations in an electrolytic solution |
US7153408B1 (en) * | 2006-04-13 | 2006-12-26 | Herdman Roderick D | Copper electroplating of printing cylinders |
US7435320B2 (en) | 2004-04-30 | 2008-10-14 | Advanced Technology Materials, Inc. | Methods and apparatuses for monitoring organic additives in electrochemical deposition solutions |
US20080283404A1 (en) * | 2007-05-14 | 2008-11-20 | Nec Electronics Corporation | Method of manufacturing semiconductor device to decrease defect number of plating film |
EP2551375A1 (fr) | 2011-07-26 | 2013-01-30 | Atotech Deutschland GmbH | Composition de bain pour placage autocatalytique de nickel |
CN104152877A (zh) * | 2014-07-17 | 2014-11-19 | 广东致卓精密金属科技有限公司 | 一种化学镀镍液 |
Families Citing this family (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR1418244A (fr) * | 1964-10-08 | 1965-11-19 | Pernix Enthone | Nouvelles sultones et leur application comme agents de nivellement des revêtements électrolytiques, notamment de nickel |
FR1519645A (fr) * | 1966-12-30 | 1968-04-05 | Pernix Enthone | Perfectionnements à l'étamage par voie électrolytique |
US3956079A (en) * | 1972-12-14 | 1976-05-11 | M & T Chemicals Inc. | Electrodeposition of copper |
US3956084A (en) * | 1972-12-14 | 1976-05-11 | M & T Chemicals Inc. | Electrodeposition of copper |
US3956120A (en) * | 1972-12-14 | 1976-05-11 | M & T Chemicals Inc. | Electrodeposition of copper |
US3966565A (en) * | 1972-12-14 | 1976-06-29 | M & T Chemicals Inc. | Electrodeposition of copper |
US3956078A (en) * | 1972-12-14 | 1976-05-11 | M & T Chemicals Inc. | Electrodeposition of copper |
US3940320A (en) * | 1972-12-14 | 1976-02-24 | M & T Chemicals Inc. | Electrodeposition of copper |
DE2355581C3 (de) * | 1973-11-07 | 1979-07-12 | Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler, 6000 Frankfurt | Galvanisches Glanzgoldbad mit hoher Abscheidungsgeschwindigkeit |
US4036710A (en) * | 1974-11-21 | 1977-07-19 | M & T Chemicals Inc. | Electrodeposition of copper |
US4014760A (en) * | 1974-11-21 | 1977-03-29 | M & T Chemicals Inc. | Electrodeposition of copper |
US4036711A (en) * | 1975-12-18 | 1977-07-19 | M & T Chemicals Inc. | Electrodeposition of copper |
DE2921241A1 (de) * | 1979-04-19 | 1980-10-23 | Alusuisse | Saurer zinn-ii-haltiger elektrolyt |
US5385661A (en) * | 1993-09-17 | 1995-01-31 | International Business Machines Corporation | Acid electrolyte solution and process for the electrodeposition of copper-rich alloys exploiting the phenomenon of underpotential deposition |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2647866A (en) * | 1950-07-17 | 1953-08-04 | Udylite Corp | Electroplating of nickel |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2489538A (en) * | 1941-05-24 | 1949-11-29 | Gen Motors Corp | Electrodeposition of copper |
US2663684A (en) * | 1952-06-02 | 1953-12-22 | Houdaille Hershey Corp | Method of and composition for plating copper |
NL109804C (fr) * | 1953-09-19 | |||
BE534701A (fr) * | 1954-03-22 | |||
NL217034A (fr) * | 1956-06-15 |
-
0
- BE BE534701D patent/BE534701A/xx unknown
- DE DENDAT1075398D patent/DE1075398B/de active Pending
-
1954
- 1954-10-25 US US464638A patent/US2830014A/en not_active Expired - Lifetime
-
1955
- 1955-01-12 CH CH336668D patent/CH336668A/de unknown
- 1955-02-16 FR FR1119382D patent/FR1119382A/fr not_active Expired
- 1955-03-21 GB GB8091/55A patent/GB804833A/en not_active Expired
-
1959
- 1959-04-28 CH CH7265059A patent/CH377611A/de unknown
- 1959-07-24 US US829227A patent/US3023150A/en not_active Expired - Lifetime
- 1959-07-28 GB GB25792/59A patent/GB868898A/en not_active Expired
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2647866A (en) * | 1950-07-17 | 1953-08-04 | Udylite Corp | Electroplating of nickel |
Cited By (27)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3023150A (en) * | 1954-03-22 | 1962-02-27 | Dehydag Gmbh | Bath for the production of metal electroplates |
US3075899A (en) * | 1958-04-26 | 1963-01-29 | Dehydag Gmbh | Baths for the production of metal electroplates |
US3000799A (en) * | 1960-02-10 | 1961-09-19 | Harshaw Chem Corp | Nickel plating solutions |
US3276979A (en) * | 1961-08-31 | 1966-10-04 | Dehydag Gmbh | Baths and processes for the production of metal electroplates |
US3267010A (en) * | 1962-04-16 | 1966-08-16 | Udylite Corp | Electrodeposition of copper from acidic baths |
US4376685A (en) * | 1981-06-24 | 1983-03-15 | M&T Chemicals Inc. | Acid copper electroplating baths containing brightening and leveling additives |
EP0343559A1 (fr) * | 1988-05-25 | 1989-11-29 | Raschig AG | Utilisation de composés éthane sulfone substitués en position 2 comme agents auxiliaires galvaniques |
US20010013472A1 (en) * | 2000-02-01 | 2001-08-16 | Kenji Nakamura | Method of plating for filling via holes |
US6755957B2 (en) * | 2000-02-01 | 2004-06-29 | Shinko Electric Industries Co., Ltd. | Method of plating for filling via holes |
US6652731B2 (en) * | 2001-10-02 | 2003-11-25 | Shipley Company, L.L.C. | Plating bath and method for depositing a metal layer on a substrate |
US6709568B2 (en) | 2002-06-13 | 2004-03-23 | Advanced Technology Materials, Inc. | Method for determining concentrations of additives in acid copper electrochemical deposition baths |
US20050067304A1 (en) * | 2003-09-26 | 2005-03-31 | King Mackenzie E. | Electrode assembly for analysis of metal electroplating solution, comprising self-cleaning mechanism, plating optimization mechanism, and/or voltage limiting mechanism |
US20050109624A1 (en) * | 2003-11-25 | 2005-05-26 | Mackenzie King | On-wafer electrochemical deposition plating metrology process and apparatus |
US20050224370A1 (en) * | 2004-04-07 | 2005-10-13 | Jun Liu | Electrochemical deposition analysis system including high-stability electrode |
US20060102475A1 (en) * | 2004-04-27 | 2006-05-18 | Jianwen Han | Methods and apparatus for determining organic component concentrations in an electrolytic solution |
US7427344B2 (en) | 2004-04-27 | 2008-09-23 | Advanced Technology Materials, 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 |
US20050247576A1 (en) * | 2004-05-04 | 2005-11-10 | Tom Glenn M | Electrochemical drive circuitry and method |
US7427346B2 (en) | 2004-05-04 | 2008-09-23 | Advanced Technology Materials, Inc. | Electrochemical drive circuitry and method |
US7153408B1 (en) * | 2006-04-13 | 2006-12-26 | Herdman Roderick D | Copper electroplating of printing cylinders |
EP2004404A2 (fr) * | 2006-04-13 | 2008-12-24 | MacDermid, Incorporated | Cuivrage électrolytique de cylindres d'impression |
EP2004404A4 (fr) * | 2006-04-13 | 2012-06-27 | Macdermid Inc | Cuivrage électrolytique de cylindres d'impression |
US20080283404A1 (en) * | 2007-05-14 | 2008-11-20 | Nec Electronics Corporation | Method of manufacturing semiconductor device to decrease defect number of plating film |
EP2551375A1 (fr) | 2011-07-26 | 2013-01-30 | Atotech Deutschland GmbH | Composition de bain pour placage autocatalytique de nickel |
WO2013013941A1 (fr) | 2011-07-26 | 2013-01-31 | Atotech Deutschland Gmbh | Composition de bain de nickelage autocatalytique |
US20140150689A1 (en) * | 2011-07-26 | 2014-06-05 | Atotech Deutschland Gmbh | Electroless nickel plating bath composition |
CN104152877A (zh) * | 2014-07-17 | 2014-11-19 | 广东致卓精密金属科技有限公司 | 一种化学镀镍液 |
Also Published As
Publication number | Publication date |
---|---|
GB868898A (en) | 1961-05-25 |
US3023150A (en) | 1962-02-27 |
CH336668A (de) | 1959-02-28 |
CH377611A (de) | 1964-05-15 |
DE1075398B (de) | 1960-02-11 |
FR1119382A (fr) | 1956-06-19 |
BE534701A (fr) | |
GB804833A (en) | 1958-11-26 |
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