EP0084816B2 - Elektrolyt zur galvanischen Abscheidung von Aluminium - Google Patents
Elektrolyt zur galvanischen Abscheidung von Aluminium Download PDFInfo
- Publication number
- EP0084816B2 EP0084816B2 EP83100245A EP83100245A EP0084816B2 EP 0084816 B2 EP0084816 B2 EP 0084816B2 EP 83100245 A EP83100245 A EP 83100245A EP 83100245 A EP83100245 A EP 83100245A EP 0084816 B2 EP0084816 B2 EP 0084816B2
- Authority
- EP
- European Patent Office
- Prior art keywords
- electrolyte
- aluminium
- aluminum
- organometallic
- electroplating
- 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
- C25D3/42—Electroplating: Baths therefor from solutions of light metals
- C25D3/44—Aluminium
Definitions
- the invention relates to an organometallic electrolyte for the electrodeposition of aluminum and the use of this electrolyte.
- Organometallic electrolytes ie organoaluminum complex compounds (DE-PS 1 047 450 and dissertation H.Letruckiche, TH Hachen, 1954) can be used for the galvanic deposition of aluminum.
- organoaluminum complex compounds DE-PS 1 047 450 and dissertation H.Letruckiche, TH Hachen, 1954
- a large number of compounds have been described which can be used for galvanic aluminizing, for example onium and alkali complex compounds.
- the complex salt NaF.2 Al (C 2 H 5 ) 3 described as optimal has been used ("Zeitschrift für inorganic und Rheine Chemie", vol. 283, 1956, pp. 414 to 424).
- Electroplating baths with NaF.2 Al (C 2 H 5 ) 3 as electrolyte salt have a decisive disadvantage for a technically broad and economical application: the spreadability is too low. It is comparable to that of aqueous chrome baths ("Galvanotechnik", vol. 73, 1982, pp. 2 to 8). Due to the low spreadability in galvanic aluminizing, strongly profiled parts can only be coated as rack goods where the geometry of the parts allows, using auxiliary anodes. However, this is a technically very complex and therefore expensive process. Due to the low spreadability, the drum aluminizing of small parts was also of no practical importance, since the aluminized parts have too great variations in layer thickness or are not coated at all at critical points.
- the object of the invention is to provide an organometallic electrolyte for the electrodeposition of aluminum, which has a high scatterability but also a high conductivity and good solubility and is easily accessible commercially.
- Me means metal
- Et stands for an ethyl radical, ie for C 2 H 5 ; otherwise, different metals can also be present side by side.
- the organoaluminum electrolyte according to the invention according to formula (1) proves to be extremely advanced in terms of electroplating technology, ie it fulfills the requirements placed on electrolytes for a technically widely applicable and economical aluminizing process to a far greater extent than was previously possible.
- the electrolyte according to the invention namely has a high scattering capacity and, at the same time, the electrical conductivity and solubility required for economical aluminizing, as well as good commercial accessibility. For the first time, it combines the electrotechnical properties relevant to electroplating. Another advantage is also that this electrolyte compared to NaF. 2 Al (C 2 H 5 ) 3 has a significantly lower sensitivity to oxygen and moisture.
- the electrolyte according to the invention is based on findings which have been obtained on the one hand with regard to the relationships between the composition of organoaluminum complex compounds and the electroplating requirements, such as scatterability, conductivity and solubility (in low-viscosity aromatic hydrocarbons which are liquid at room temperature and have low water absorption). These relationships were previously unknown.
- the electrolyte according to the invention is comparable to cadmium electrolytes in terms of scatterability in the field of electro-technical interest. For the first time there is the possibility to aluminize the same product range as for cadming. This creates the electro-technical prerequisite for replacing cadmium with aluminum as a corrosion protection coating.
- the electrolyte according to the invention is preferably used in the form of a solution.
- Aromatic hydrocarbons which are liquid at room temperature, such as toluene, are advantageously used as solvents in the following composition: 1 mol of electrolyte salt per 1 to 10 mol, preferably 1 to 5 mol, of solvent.
- Approx. 1140 ml of toluene are placed in a Witt'schen stirring pot (capacity: 3 l), which is equipped with a mechanical stirrer, a dropping funnel, a thermometer and an inert gas transfer system and has a conductivity cell, and 183.5 g of potassium fluoride are slurried therein Slurry is gradually added with stirring, 577 g of aluminum triethyl and 250 g of aluminum triisobutyl.
- the electrolyte KF - [1.6 Al (C 2 H 5 ) 3 ⁇ 0.4Al (iC 4 H 9 ) 3 ] ⁇ 3.4 mol of toluene forms as clear, colorless, while increasing the specific conductivity and heating After the reaction liquid, this electrolyte composition - at 100 ° C - a specific conductivity of 2,25.10- 2 S ⁇ cm -1.
- the same method can also be used to produce electrolytes with a different composition.
- the solvent-free electrolytes can also be produced in this way. To do this, however, it is necessary to carry out the reaction above the melting temperature of the respective electrolyte.
- the good scatterability of the electrolyte according to the invention is to be demonstrated on the basis of electroplating tests.
- a galvanizing cell in the form of a rectangular glass vessel (20 cm x 8 cm x 20 cm) was used to carry out the electroplating tests, and an Al anode plate was attached to each end. Since the aluminum electrolytes to air and moisture sensitive, the plating was l elle with a special lid provided having a plurality of openings for a thermometer (diagonally opposite to a conductivity cell, for a gas transfer tube (for flooding the cell with nitrogen) for two stirrers in the corners of the cell in front of the anodes) and for charging the test specimens to be aluminized. Rectangular angle plates made of steel of a certain size were used as test specimens. To determine the scatterability, the thickness of the aluminum layer deposited on the angle plates was determined by means of a layer thickness measuring device
- test specimens were pretreated, as is customary in electroplating, ie pickled and degreased.
- the test specimen attached to a cathode rod was first degreased using an organic solvent and pickled by immersion in dilute hydrochloric acid.
- the test specimen was then degreased cathodically and an approximately 1 ⁇ m thick nickel layer was provided to improve the adhesive strength.
- the toluene-moist test specimen was introduced into the electroplating cell, ie into the electrolyte, and - as a cathode - arranged between the two anodes (cathode area: 2 dm 2 ; Distance between anode and cathode: approx. 10 cm each).
- the electroplating was carried out at an electrolyte temperature of 100 ° C by means of a so-called pulse current (deposition voltage: ⁇ 10 V).
- the test specimens were alternately poled cathodically and anodically, the cathodic deposition time in each case 80 ms and the anodic deposition time in each case 20 ms.
- electrolyte according to the invention the well-known electrolyte NaF.2 Al (C 2 H 5 ) 3 and, in each case in the commercially available form, a cadmium electrolyte (cyanidic), a zinc electrolyte (weakly cyanidic) and a nickel electrolyte (weakly acidic) were investigated, with the last three electrolytes were galvanized using direct current.
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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)
- Conductive Materials (AREA)
- Primary Cells (AREA)
- Sealing Battery Cases Or Jackets (AREA)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT83100245T ATE20252T1 (de) | 1982-01-25 | 1983-01-13 | Elektrolyt zur galvanischen abscheidung von aluminium. |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE3202265 | 1982-01-25 | ||
DE19823202265 DE3202265A1 (de) | 1982-01-25 | 1982-01-25 | Elektrolyt zur galvanischen abscheidung von aluminium |
Publications (4)
Publication Number | Publication Date |
---|---|
EP0084816A2 EP0084816A2 (de) | 1983-08-03 |
EP0084816A3 EP0084816A3 (en) | 1984-06-06 |
EP0084816B1 EP0084816B1 (de) | 1986-06-04 |
EP0084816B2 true EP0084816B2 (de) | 1991-10-30 |
Family
ID=6153853
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP83100245A Expired - Lifetime EP0084816B2 (de) | 1982-01-25 | 1983-01-13 | Elektrolyt zur galvanischen Abscheidung von Aluminium |
Country Status (8)
Country | Link |
---|---|
US (1) | US4417954A (da) |
EP (1) | EP0084816B2 (da) |
JP (1) | JPS58171591A (da) |
AT (1) | ATE20252T1 (da) |
CA (1) | CA1209157A (da) |
DE (2) | DE3202265A1 (da) |
DK (1) | DK154657C (da) |
ES (1) | ES519248A0 (da) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102007018489A1 (de) | 2007-04-19 | 2008-10-23 | Tec-Chem Gmbh | Aluminiumorganischer 4-Komponentenelektrolyt zur Abscheidung von Aluminium |
Families Citing this family (21)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4517253A (en) * | 1984-01-23 | 1985-05-14 | Rose Robert M | Cryoelectrodeposition |
NL8602856A (nl) * | 1986-11-11 | 1988-06-01 | Hga Galvano Aluminium B V | Werkwijze en inrichting voor het galvanisch afscheiden van metalen op een substraat. |
US4778575A (en) * | 1988-01-21 | 1988-10-18 | The United States Of America As Represented By The United States Department Of Energy | Electrodeposition of magnesium and magnesium/aluminum alloys |
DE3919068A1 (de) * | 1989-06-10 | 1990-12-13 | Studiengesellschaft Kohle Mbh | Aluminiumorganische elektrolyte zur elektrolytischen abscheidung von hochreinem aluminium |
DE3919069A1 (de) * | 1989-06-10 | 1990-12-13 | Studiengesellschaft Kohle Mbh | Aluminiumorganische elektrolyte und verfahren zur elektrolytischen abscheidung von aluminium |
EP0504705A1 (de) * | 1991-03-20 | 1992-09-23 | Siemens Aktiengesellschaft | Vorbehandlung von metallischen Werkstoffen für die galvanische Beschichtung mit Metall |
EP0504704A1 (de) * | 1991-03-20 | 1992-09-23 | Siemens Aktiengesellschaft | Vorbehandlung von metallischen Werkstoffen für die galvanische Beschichtung mit Metall |
EP0505886A1 (de) * | 1991-03-28 | 1992-09-30 | Siemens Aktiengesellschaft | Erzeugung dekorativer Aluminiumbeschichtungen |
DE19649000C1 (de) * | 1996-11-27 | 1998-08-13 | Alcotec Beschichtungsanlagen G | Elektrolyt zur galvanischen Abscheidung von Aluminium und dessen Verwendung |
DE19716495C1 (de) * | 1997-04-19 | 1998-05-20 | Aluminal Oberflaechentechnik | Elektrolyt für die elektrolytische Abscheidung von Aluminium und dessen Verwendung |
DE19716493C2 (de) * | 1997-04-19 | 2001-11-29 | Aluminal Oberflaechentechnik | Verfahren zum elektrolytischen Beschichten von metallischen oder nichtmetallischen Endlosprodukten und Vorrichtung zur Durchführung des Verfahrens |
WO2002088434A1 (en) * | 2001-04-30 | 2002-11-07 | Alumiplate Incorporated | Aluminium electroplating formulations |
US7250102B2 (en) * | 2002-04-30 | 2007-07-31 | Alumiplate Incorporated | Aluminium electroplating formulations |
DE10224089A1 (de) * | 2002-05-31 | 2003-12-11 | Studiengesellschaft Kohle Mbh | Verfahren zur Herstellung von aluminiumorganischen Komplexen und deren Verwendung zur Herstellung von Elektrolytlösungen zur elektrochemischen Abscheidung von Aluminium-Magnesium-Legierungen |
EP1927680A1 (de) * | 2006-11-29 | 2008-06-04 | Aluminal Oberflächentechnik GmbH & Co. KG | Elektrolyt zur galvanischen abscheidung von aluminium aus aprotischen lösungsmitteln in einer galvanisiertrommel |
EP2419551A2 (de) | 2009-03-18 | 2012-02-22 | Basf Se | Elektrolyt und oberflächenaktive additive für die galvanische abscheidung glatter, dichter aluminium-schichten aus ionischen flüssigkeiten |
US10190640B2 (en) | 2016-03-23 | 2019-01-29 | Schaeffler Technologies AG & Co. KG | Bearing with integrated shunt |
US10794427B2 (en) | 2016-04-05 | 2020-10-06 | Schaeffler Technologies AG & Co. KG | Bearing ring with insulating coating |
US10539178B2 (en) | 2017-05-18 | 2020-01-21 | Schaeffler Technologies AG & Co. KG | Vapor deposition bearing coating |
US11142841B2 (en) | 2019-09-17 | 2021-10-12 | Consolidated Nuclear Security, LLC | Methods for electropolishing and coating aluminum on air and/or moisture sensitive substrates |
US11661665B2 (en) | 2020-04-30 | 2023-05-30 | The Boeing Company | Aluminum and aluminum alloy electroplated coatings |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
BE540052A (da) * | 1955-06-13 | |||
US4101386A (en) * | 1971-05-07 | 1978-07-18 | Siemens Aktiengesellschaft | Methods of coating and surface finishing articles made of metals and their alloys |
US3929611A (en) * | 1974-07-19 | 1975-12-30 | Ametek Inc | Electrodepositing of aluminum |
NL8100569A (nl) * | 1981-02-06 | 1982-09-01 | Philips Nv | Elektrolytvloeistof voor het galvanisch neerslaan van aluminium. |
-
1982
- 1982-01-25 DE DE19823202265 patent/DE3202265A1/de not_active Withdrawn
-
1983
- 1983-01-13 AT AT83100245T patent/ATE20252T1/de not_active IP Right Cessation
- 1983-01-13 EP EP83100245A patent/EP0084816B2/de not_active Expired - Lifetime
- 1983-01-13 DE DE8383100245T patent/DE3363841D1/de not_active Expired
- 1983-01-18 JP JP58006551A patent/JPS58171591A/ja active Granted
- 1983-01-24 CA CA000420127A patent/CA1209157A/en not_active Expired
- 1983-01-24 DK DK025183A patent/DK154657C/da not_active IP Right Cessation
- 1983-01-25 US US06/460,817 patent/US4417954A/en not_active Expired - Lifetime
- 1983-01-25 ES ES519248A patent/ES519248A0/es active Granted
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102007018489A1 (de) | 2007-04-19 | 2008-10-23 | Tec-Chem Gmbh | Aluminiumorganischer 4-Komponentenelektrolyt zur Abscheidung von Aluminium |
Also Published As
Publication number | Publication date |
---|---|
ATE20252T1 (de) | 1986-06-15 |
CA1209157A (en) | 1986-08-05 |
EP0084816A2 (de) | 1983-08-03 |
JPS6122038B2 (da) | 1986-05-29 |
DK25183D0 (da) | 1983-01-24 |
DK154657C (da) | 1989-05-01 |
JPS58171591A (ja) | 1983-10-08 |
ES8403490A1 (es) | 1984-03-16 |
DK154657B (da) | 1988-12-05 |
EP0084816A3 (en) | 1984-06-06 |
EP0084816B1 (de) | 1986-06-04 |
US4417954A (en) | 1983-11-29 |
ES519248A0 (es) | 1984-03-16 |
DE3363841D1 (en) | 1986-07-10 |
DE3202265A1 (de) | 1983-07-28 |
DK25183A (da) | 1983-07-26 |
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