US2842488A - Process for the production of metal electrodeposits - Google Patents
Process for the production of metal electrodeposits Download PDFInfo
- Publication number
- US2842488A US2842488A US458985A US45898554A US2842488A US 2842488 A US2842488 A US 2842488A US 458985 A US458985 A US 458985A US 45898554 A US45898554 A US 45898554A US 2842488 A US2842488 A US 2842488A
- Authority
- US
- United States
- Prior art keywords
- copper
- brightening
- electrodeposits
- electroplating baths
- baths
- 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
-
- A—HUMAN NECESSITIES
- A21—BAKING; EDIBLE DOUGHS
- A21D—TREATMENT, e.g. PRESERVATION, OF FLOUR OR DOUGH, e.g. BY ADDITION OF MATERIALS; BAKING; BAKERY PRODUCTS; PRESERVATION THEREOF
- A21D2/00—Treatment of flour or dough by adding materials thereto before or during baking
- A21D2/08—Treatment of flour or dough by adding materials thereto before or during baking by adding organic substances
- A21D2/30—Organic phosphorus compounds
- A21D2/32—Phosphatides
-
- 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
-
- 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
Definitions
- This invention relates to a process for producingbright metal electrodeposits, andmore particularly to electroplating solutions containing additives. which eliminate the adverse effects of impurities in such solutions upon the electrodeposits producedtherefrom. 7
- an object ofthe present invention to provide a method. of electroplating objects in electroplating baths containing brighteningagents whichmakes it possible to produce bright electrodeposits despite. the presence of interfering impurities in the electroplating bath.
- Another object of this invention is to. provide additives for electroplating baths containing brightening agents which will render impurities present in the bath impotent as interfering substances in the production ofzbrighb electrodeposits.
- United StatesPatent O 2,842,488 Patented July 8, 1958 ice ing electroplating baths containing brightening agents in accordance with our invention are the following:
- Tertiary amino compounds of this type may also be employed in the form of their salts of inorganic and organic acids, or in the form of the corresponding quaternary ammonium compounds.
- the additives in accordance with our invention are added to electroplating baths, modified with brightening agents, in amounts ranging from 0.01 gm./liter and 20 gm./liter of bath, preferably from 2 to 8 gm./1iter of bath.
- the particular amount required varies from one specific compound to the other and also depends upon the nature of the brightening agents employed as well as upon the type and amount of impurities present.
- objects are electroplated in a bath modified in accordance with our invention at a temperature ranging between 30 and C.
- Electroplating baths containing brightening agents and modified in the above manner in accordance with our invention will produce bright and lustrous electrodeposits over the entire effective range of current densities despite the presence of impurities of the above-described nature in the bath.
- the additives in accordance with our invention have the further advantage that they increase the ductility of the electrodeposit produced from electroplating baths modified with such additives.
- the additives of our invention are efiective in all those electroplating baths which contain magnesium and calcium ions due to the use of hard tap water, and ferric ions introduced by the use of technically pure metal salts in the preparation of the electroplating solution. How ever, it has beenfound that they do not act as watersoftening agents in the usual sense, and that they cannot be replaced by the typical water-softening agents such as sequestering agents or detergents. Nevertheless,
- these additives are capable of completely eliminating the adverse effect of the above-described impurities upon the brightness of electrodeposits produced from baths containing such impurities and brightening agents.
- the use of the additives in accordance with our invention does not require any changes in the conditions under which objects are usually electroplated in metal salt baths, particularly with respect to temperature and current densities.
- metal salt baths particularly with respect to temperature and current densities.
- amines they are soluble in acid metal salt solutions, particularly in electroplating baths made from copper, salts, and they are not decomposed by the action of heat or electric current during the plating process.
- the additives of our invention can be employed to modify all types of electroplating baths containing brightening agents and in which the qualities of electrodeposits produced therefrom are adversely aifected by the presence of impurities of the type described above.
- additives may be used in electroplating baths for elec-w trodepositing zinc, nickel, chromium, precious metals,
- Example 1 A copper-plating bath was prepared which contained distilled water, 200 gm./1iter crystalline chemically pure copper sulfate and 60 gm./liter chemically pure sulfuric acid. The bath was then modified with 0.75 gm./liter N,N-dipropyldithiocarbamic acid-n-butylester-w-sodium sulfonate as a brightening agent. Iron objects were then electroplated in the modified bath using a current density range of 0.5-8 amp./dm. The copper deposits produced thereby were bright and lustrous.
- a copper-plating bath having the same composition was prepared by using hard tap water instead of the distilled water, and technical grade copper sulfate rather than chemically pure copper sulfate. This bath was then modified with a brightening agent as above. Iron objects copper-plated in such a bath were provided with a copper deposit which was not as bright and lustrous as when distilled water and chemically pure copper sulfate were used to make up the copper-plating solution.
- Example 11 A copper-plating bath was prepared from hard tap water, 200 gm./liter technical grade copper sulfate and 60 gm./liter sulfuric acid. This bath was then modified by adding 0.75 gm./liter N,N-dipropyl-dithiocarbamic acid-n-butylester-w-sodium sulfonate. Thereafter, 2.5 gm./liter Z-diethylamino-ethylchloride-l were added. Iron objects were the electroplated in this bath within a current density range of 0.5-8 amp./dm. The copper deposits produced thereby were bright and lustrous, as well as being highly ductile.
- Example III To a copper electroplating bath, prepared as described in Example II, where added 0.5 gm./liter N,N-diethyldithiocarbamic n propylester w soditun sulfonate as brightening agent together with 4 gm./liter N-2-chloroethyl-piperidine. Iron objects were then electroplated in this bath within a current density range of 0.5-8 amp./dm. The copper deposits produced thereby were bright and lustrous, as well as being highly ductile.
- Example IV To a copper electroplating bath, prepared as described in Example II, were added 0.5 gm./1iter N,N-diethyldithiocarbamic n propylester w sodium sulfonate and thereafter 2 gm./liter of the quaternary compound, prepared by mixing together morpholine with epichloro- Iron objects were then electroplated in this bath within a current density range of 0.5-8 amp./dm. The copper deposits produced thereby were bright and lustrous, as well as being highly ductile.
- Example V were-then electroplated in this bath within a current density range of 0.5-8 amp./drn.
- the copper deposits produced thereby were bright and lustrous, as well as being highly ductile.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Food Science & Technology (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electrolytic Production Of Metals (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DED19045A DE1014404B (de) | 1954-11-05 | 1954-11-05 | Verfahren zur Herstellung galvanischer Metallueberzuege |
Publications (1)
Publication Number | Publication Date |
---|---|
US2842488A true US2842488A (en) | 1958-07-08 |
Family
ID=7036238
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US458985A Expired - Lifetime US2842488A (en) | 1954-11-05 | 1954-09-28 | Process for the production of metal electrodeposits |
US544586A Expired - Lifetime US2905602A (en) | 1954-11-05 | 1955-11-02 | Production of metal electrodeposits |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US544586A Expired - Lifetime US2905602A (en) | 1954-11-05 | 1955-11-02 | Production of metal electrodeposits |
Country Status (7)
Country | Link |
---|---|
US (2) | US2842488A (de) |
BE (2) | BE536575A (de) |
CH (2) | CH333941A (de) |
DE (2) | DE934508C (de) |
FR (2) | FR1120948A (de) |
GB (2) | GB806403A (de) |
NL (2) | NL92673C (de) |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3081240A (en) * | 1959-06-06 | 1963-03-12 | Debydag Deutsche Hydrierwerke | Acid copper electroplating baths |
US3318787A (en) * | 1964-02-07 | 1967-05-09 | Udylite Corp | Electrodeposition of zinc |
US3423297A (en) * | 1965-05-12 | 1969-01-21 | Surface Research Inc | Chromium electroplating bath including mist suppressors |
US4376685A (en) * | 1981-06-24 | 1983-03-15 | M&T Chemicals Inc. | Acid copper electroplating baths containing brightening and leveling additives |
US5972192A (en) * | 1997-07-23 | 1999-10-26 | Advanced Micro Devices, Inc. | Pulse electroplating copper or copper alloys |
US20040154926A1 (en) * | 2002-12-24 | 2004-08-12 | Zhi-Wen Sun | Multiple chemistry electrochemical plating method |
US6793796B2 (en) | 1998-10-26 | 2004-09-21 | Novellus Systems, Inc. | Electroplating process for avoiding defects in metal features of integrated circuit devices |
US20040206623A1 (en) * | 2003-04-18 | 2004-10-21 | Applied Materials, Inc. | Slim cell platform plumbing |
US20050109627A1 (en) * | 2003-10-10 | 2005-05-26 | Applied Materials, Inc. | Methods and chemistry for providing initial conformal electrochemical deposition of copper in sub-micron features |
US20060166032A1 (en) * | 2002-12-18 | 2006-07-27 | Masashi Kumagai | Copper electrolytic solution and electrolytic copper foil produced therewith |
EP3415664A1 (de) * | 2017-06-16 | 2018-12-19 | ATOTECH Deutschland GmbH | Wässriges saures kupfergalvanisierungsbad und verfahren zur elektrolytischen abscheidung einer kupferbeschichtung |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3006822A (en) * | 1957-05-08 | 1961-10-31 | Langbein Pfanhauser Werke Ag | Electro-deposition of nickel coatings |
NL238490A (de) * | 1958-04-26 | |||
US3120462A (en) * | 1960-09-16 | 1964-02-04 | Trifari Krussman And Fishel In | Apparatus for recovering electroplating salts by evaporative concentration |
SE302227B (de) * | 1963-05-28 | 1968-07-08 | Candor Kemiska Ab | |
US3255096A (en) * | 1963-11-01 | 1966-06-07 | Harshaw Chem Corp | Electrodeposition of nickel |
JPS5928588A (ja) * | 1982-08-09 | 1984-02-15 | Meidensha Electric Mfg Co Ltd | 亜鉛―臭素二次電池 |
GB8312104D0 (en) * | 1983-05-04 | 1983-06-08 | Shell Int Research | Preparation of 1-substituted azetidin-3-ol derivatives |
GB8412814D0 (en) * | 1984-05-18 | 1984-06-27 | Shell Int Research | 1-substituted azetidine-3-ol derivatives |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA461186A (en) * | 1949-11-22 | John Franklin Beaver, Jr. | Bright copper plating | |
DE888493C (de) * | 1951-11-03 | 1953-09-03 | Hydrierwerke A G Deutsche | Verfahren zur Herstellung festhaftender und glaenzender galvanischer Kupferueberzuege |
US2707166A (en) * | 1952-05-26 | 1955-04-26 | Udylite Corp | Electrodeposition of copper from an acid bath |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2541700A (en) * | 1946-02-28 | 1951-02-13 | Du Pont | Electroplating copper |
US2663684A (en) * | 1952-06-02 | 1953-12-22 | Houdaille Hershey Corp | Method of and composition for plating copper |
-
1954
- 1954-04-23 DE DED17614A patent/DE934508C/de not_active Expired
- 1954-09-28 US US458985A patent/US2842488A/en not_active Expired - Lifetime
- 1954-11-05 DE DED19045A patent/DE1014404B/de active Pending
-
1955
- 1955-03-08 CH CH333941D patent/CH333941A/de unknown
- 1955-03-17 BE BE536575D patent/BE536575A/xx unknown
- 1955-03-18 FR FR1120948D patent/FR1120948A/fr not_active Expired
- 1955-03-30 GB GB9226/55A patent/GB806403A/en not_active Expired
- 1955-04-21 NL NL196635A patent/NL92673C/xx active
- 1955-07-21 CH CH337380D patent/CH337380A/de unknown
- 1955-08-02 FR FR68634D patent/FR68634E/fr not_active Expired
- 1955-08-27 BE BE540855D patent/BE540855A/xx unknown
- 1955-10-05 NL NL200993A patent/NL95110C/xx active
- 1955-11-02 US US544586A patent/US2905602A/en not_active Expired - Lifetime
- 1955-11-04 GB GB31541/55A patent/GB815908A/en not_active Expired
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA461186A (en) * | 1949-11-22 | John Franklin Beaver, Jr. | Bright copper plating | |
DE888493C (de) * | 1951-11-03 | 1953-09-03 | Hydrierwerke A G Deutsche | Verfahren zur Herstellung festhaftender und glaenzender galvanischer Kupferueberzuege |
US2707166A (en) * | 1952-05-26 | 1955-04-26 | Udylite Corp | Electrodeposition of copper from an acid bath |
Cited By (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3081240A (en) * | 1959-06-06 | 1963-03-12 | Debydag Deutsche Hydrierwerke | Acid copper electroplating baths |
US3318787A (en) * | 1964-02-07 | 1967-05-09 | Udylite Corp | Electrodeposition of zinc |
US3423297A (en) * | 1965-05-12 | 1969-01-21 | Surface Research Inc | Chromium electroplating bath including mist suppressors |
US4376685A (en) * | 1981-06-24 | 1983-03-15 | M&T Chemicals Inc. | Acid copper electroplating baths containing brightening and leveling additives |
US5972192A (en) * | 1997-07-23 | 1999-10-26 | Advanced Micro Devices, Inc. | Pulse electroplating copper or copper alloys |
US6793796B2 (en) | 1998-10-26 | 2004-09-21 | Novellus Systems, Inc. | Electroplating process for avoiding defects in metal features of integrated circuit devices |
US7777078B2 (en) * | 2002-12-18 | 2010-08-17 | Nikko Materials Co., Ltd. | Copper electrolytic solution and electrolytic copper foil produced therewith |
US20060166032A1 (en) * | 2002-12-18 | 2006-07-27 | Masashi Kumagai | Copper electrolytic solution and electrolytic copper foil produced therewith |
US20040154926A1 (en) * | 2002-12-24 | 2004-08-12 | Zhi-Wen Sun | Multiple chemistry electrochemical plating method |
US20040206623A1 (en) * | 2003-04-18 | 2004-10-21 | Applied Materials, Inc. | Slim cell platform plumbing |
US7473339B2 (en) | 2003-04-18 | 2009-01-06 | Applied Materials, Inc. | Slim cell platform plumbing |
US20050109627A1 (en) * | 2003-10-10 | 2005-05-26 | Applied Materials, Inc. | Methods and chemistry for providing initial conformal electrochemical deposition of copper in sub-micron features |
EP3415664A1 (de) * | 2017-06-16 | 2018-12-19 | ATOTECH Deutschland GmbH | Wässriges saures kupfergalvanisierungsbad und verfahren zur elektrolytischen abscheidung einer kupferbeschichtung |
WO2018228821A1 (en) | 2017-06-16 | 2018-12-20 | Atotech Deutschland Gmbh | Aqueous acidic copper electroplating bath and method for electrolytically depositing of a copper coating |
CN110741109A (zh) * | 2017-06-16 | 2020-01-31 | 安美特德国有限公司 | 用于电解沉积铜涂层的水性酸性铜电镀浴及方法 |
US11174566B2 (en) * | 2017-06-16 | 2021-11-16 | Atotech Deutschland Gmbh | Aqueous acidic copper electroplating bath and method for electrolytically depositing of a copper coating |
CN110741109B (zh) * | 2017-06-16 | 2021-11-23 | 安美特德国有限公司 | 用于电解沉积铜涂层的水性酸性铜电镀浴及方法 |
Also Published As
Publication number | Publication date |
---|---|
NL95110C (de) | 1960-08-15 |
BE536575A (de) | 1959-01-30 |
NL92673C (de) | 1959-11-16 |
DE1014404B (de) | 1957-08-22 |
US2905602A (en) | 1959-09-22 |
FR1120948A (fr) | 1956-07-17 |
FR68634E (fr) | 1958-05-05 |
GB806403A (en) | 1958-12-23 |
CH333941A (de) | 1958-11-15 |
BE540855A (de) | 1959-08-14 |
DE934508C (de) | 1955-10-27 |
GB815908A (en) | 1959-07-01 |
CH337380A (de) | 1959-03-31 |
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