EP0084816B1 - Electrolyte pour dépôt électrolytique de l'aluminium - Google Patents

Electrolyte pour dépôt électrolytique de l'aluminium Download PDF

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Publication number
EP0084816B1
EP0084816B1 EP83100245A EP83100245A EP0084816B1 EP 0084816 B1 EP0084816 B1 EP 0084816B1 EP 83100245 A EP83100245 A EP 83100245A EP 83100245 A EP83100245 A EP 83100245A EP 0084816 B1 EP0084816 B1 EP 0084816B1
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EP
European Patent Office
Prior art keywords
electrolyte
aluminum
aluminium
electroplating
organometallic
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
Application number
EP83100245A
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German (de)
English (en)
Other versions
EP0084816B2 (fr
EP0084816A2 (fr
EP0084816A3 (en
Inventor
Siegfried Dr. Birkle
Klaus Stöger
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
AlumiPlate Inc
Original Assignee
Siemens AG
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Publication date
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Application filed by Siemens AG filed Critical Siemens AG
Priority to AT83100245T priority Critical patent/ATE20252T1/de
Publication of EP0084816A2 publication Critical patent/EP0084816A2/fr
Publication of EP0084816A3 publication Critical patent/EP0084816A3/de
Application granted granted Critical
Publication of EP0084816B1 publication Critical patent/EP0084816B1/fr
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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 organo-aluminum complex compounds (DE-PS 1 047 450), can be used for the galvanic deposition of aluminum.
  • organo-aluminum complex compounds DE-PS 1 047 450
  • 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 Reide Chemie", vol. 283, 1956, pp. 414 to 424).
  • Electroplating baths with NaF.2 Al (C 2 H 5 ) 3 as the 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 during galvanic aluminizing, strongly profiled parts can only be coated as frame 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 s ; 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 progressive in terms of electroplating technology, ie it fulfills the demands 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 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 has a significantly lower sensitivity to oxygen and moisture compared to NaF-2 Al (C 2 H 5 ) 3 .
  • 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 metal ion is decisive for the scatterability, whereas the conductivity is influenced both by the metal ion and by the halogen ion and by the length of the alkyl radicals.
  • the alkyl residues and the metal ion turn out to be particularly relevant for solubility.
  • the electrolyte according to the invention is - in gal Vanotechnically interesting work area - comparable with cadmium electrolytes in terms of scatterability. This is the first time that the same product range has been aluminized as for cadmeting. 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, advantageously in the following composition: 1 mol of electrolyte salt per 1 to 10 mol, preferably 1 to 5 mol, of solvent.
  • 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 table below shows the electrical conductivity (in 10- 2 S.cm- 1 ) at 100 ° C for several electrolytes of the general form KF. [(2-n) AlEt 3 ⁇ n AIR 3 ] ⁇ 3.4 mol toluene .
  • 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 sheet was attached to each end. Since the aluminum electrolytes are sensitive to air and moisture, the electroplating cell was provided with a special cover that has several openings: for a thermometer, for a conductivity cell, for a gas transfer tube (for flooding the cell with nitrogen), for two stirrers (diagonally opposite 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 using 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 provided with an approximately 1 ⁇ m thick nickel layer 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: each about 10 cm).
  • 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 In addition to the 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 examined the last three electrolytes were galvanized using direct current.
  • cyanidic cyanidic
  • zinc electrolyte weakly cyanidic
  • nickel electrolyte weakly acidic

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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)

Claims (4)

1. Electrolyte organométallique pour le dépôt électrolytique d'aluminium, caractérisé en ce qu'il présente la composition suivante:
Figure imgb0012
dans laquelle:
Me = K, Rb ou Cs;
R = H ou CxH2x+1 avec x = 1 et 3 à 8, au moins deux groupes R étant des radicaux alcoyle;
m = 1,3à2,4etn=0,1à1,1, m devant être plus grand que 2n.
2. Electrolyte organométallique suivant la revendication 1, caractérisé en ce que:
x = 1 ou 3 ou 4 et/ou
m = 1,8 à 2,2 et/ou
n = 0,2 à 0,5.
3. Electrolyte organométallique suivant la revendication 2, caractérisé par la composition suivante:
Figure imgb0013
dans laquelle:
m' = 1,8 à 2,2, de préférence 2,0;
n' = 0,2 à 0,5, de préférence 0,4, et
R' = CH3 ou C4H9.
4. Utilisation de l'électrolyte organométallique suivant l'une des revendications 1 à 3, pour le dépôt électrolytique d'aluminium, sous forme d'une solution dans 1 à 10 moles et, de préférence, dans 1 à 5 moles d'un hydrocarbure aromatique liquide à la température ambiante, notamment dans le toluène.
EP83100245A 1982-01-25 1983-01-13 Electrolyte pour dépôt électrolytique de l'aluminium Expired - Lifetime EP0084816B2 (fr)

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 (fr) 1983-08-03
EP0084816A3 EP0084816A3 (en) 1984-06-06
EP0084816B1 true EP0084816B1 (fr) 1986-06-04
EP0084816B2 EP0084816B2 (fr) 1991-10-30

Family

ID=6153853

Family Applications (1)

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EP83100245A Expired - Lifetime EP0084816B2 (fr) 1982-01-25 1983-01-13 Electrolyte pour dépôt électrolytique de l'aluminium

Country Status (8)

Country Link
US (1) US4417954A (fr)
EP (1) EP0084816B2 (fr)
JP (1) JPS58171591A (fr)
AT (1) ATE20252T1 (fr)
CA (1) CA1209157A (fr)
DE (2) DE3202265A1 (fr)
DK (1) DK154657C (fr)
ES (1) ES8403490A1 (fr)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0267534A1 (fr) * 1986-11-11 1988-05-18 INTERATOM Gesellschaft mit beschränkter Haftung Procédé et dispositif pour le dépôt galvanique de métaux sur un substrat
EP0402760A1 (fr) * 1989-06-10 1990-12-19 Studiengesellschaft Kohle mbH Electrolytes organoaluminique pour le dépôt électrolytique de l'aluminium de haute pureté
EP0402761A1 (fr) * 1989-06-10 1990-12-19 Studiengesellschaft Kohle mbH Electrolytes organoaluminiques et procédés de dépôt électrolytique de l'aluminium
EP0504705A1 (fr) * 1991-03-20 1992-09-23 Siemens Aktiengesellschaft Prétraitement pour matériaux métalliques pour la déposition de métaux par électrolyse
EP0504704A1 (fr) * 1991-03-20 1992-09-23 Siemens Aktiengesellschaft Prétraitement pour matériaux métalliques pour la déposition de métaux par électrolyse
EP0505886A1 (fr) * 1991-03-28 1992-09-30 Siemens Aktiengesellschaft Formation de revêtements décoratifs d'aluminium
DE19716495C1 (de) * 1997-04-19 1998-05-20 Aluminal Oberflaechentechnik Elektrolyt für die elektrolytische Abscheidung von Aluminium und dessen Verwendung
DE19716493A1 (de) * 1997-04-19 1998-10-22 Aluminal Oberflaechentechnik Verfahren zum elektrolytischen Beschichten von metallischen oder nichtmetallischen Endlosprodukten und Vorrichtung zur Durchführung des Verfahrens

Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4517253A (en) * 1984-01-23 1985-05-14 Rose Robert M Cryoelectrodeposition
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
DE19649000C1 (de) * 1996-11-27 1998-08-13 Alcotec Beschichtungsanlagen G Elektrolyt zur galvanischen Abscheidung von Aluminium und dessen Verwendung
US7250102B2 (en) * 2002-04-30 2007-07-31 Alumiplate Incorporated Aluminium electroplating formulations
WO2002088434A1 (fr) * 2001-04-30 2002-11-07 Alumiplate Incorporated Formulations d'electrodeposition d'aluminium
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 (fr) * 2006-11-29 2008-06-04 Aluminal Oberflächentechnik GmbH & Co. KG Electrolyte destiné à la déposition galvanique d'aluminium à partir de solvants aprotiques dans un tambour à galvanisation
DE102007018489A1 (de) 2007-04-19 2008-10-23 Tec-Chem Gmbh Aluminiumorganischer 4-Komponentenelektrolyt zur Abscheidung von Aluminium
US20120006688A1 (en) 2009-03-18 2012-01-12 Basf Se Electrolyte and surface-active additives for the electrochemical deposition of smooth, dense aluminum layers from ionic liquids
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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE540052A (fr) * 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.

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0267534A1 (fr) * 1986-11-11 1988-05-18 INTERATOM Gesellschaft mit beschränkter Haftung Procédé et dispositif pour le dépôt galvanique de métaux sur un substrat
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.
EP0402760A1 (fr) * 1989-06-10 1990-12-19 Studiengesellschaft Kohle mbH Electrolytes organoaluminique pour le dépôt électrolytique de l'aluminium de haute pureté
EP0402761A1 (fr) * 1989-06-10 1990-12-19 Studiengesellschaft Kohle mbH Electrolytes organoaluminiques et procédés de dépôt électrolytique de l'aluminium
EP0504705A1 (fr) * 1991-03-20 1992-09-23 Siemens Aktiengesellschaft Prétraitement pour matériaux métalliques pour la déposition de métaux par électrolyse
EP0504704A1 (fr) * 1991-03-20 1992-09-23 Siemens Aktiengesellschaft Prétraitement pour matériaux métalliques pour la déposition de métaux par électrolyse
EP0505886A1 (fr) * 1991-03-28 1992-09-30 Siemens Aktiengesellschaft Formation de revêtements décoratifs d'aluminium
DE19716495C1 (de) * 1997-04-19 1998-05-20 Aluminal Oberflaechentechnik Elektrolyt für die elektrolytische Abscheidung von Aluminium und dessen Verwendung
DE19716493A1 (de) * 1997-04-19 1998-10-22 Aluminal Oberflaechentechnik Verfahren zum elektrolytischen Beschichten von metallischen oder nichtmetallischen Endlosprodukten und Vorrichtung zur Durchführung des Verfahrens
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

Also Published As

Publication number Publication date
ES519248A0 (es) 1984-03-16
ATE20252T1 (de) 1986-06-15
EP0084816B2 (fr) 1991-10-30
DK154657C (da) 1989-05-01
US4417954A (en) 1983-11-29
DK25183A (da) 1983-07-26
DE3363841D1 (en) 1986-07-10
JPS58171591A (ja) 1983-10-08
JPS6122038B2 (fr) 1986-05-29
EP0084816A2 (fr) 1983-08-03
DE3202265A1 (de) 1983-07-28
ES8403490A1 (es) 1984-03-16
DK25183D0 (da) 1983-01-24
DK154657B (da) 1988-12-05
EP0084816A3 (en) 1984-06-06
CA1209157A (fr) 1986-08-05

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PLAB Opposition data, opponent's data or that of the opponent's representative modified

Free format text: ORIGINAL CODE: 0009299OPPO

R26 Opposition filed (corrected)

Opponent name: STUDIENGESELLSCHAFT KOHLE MBH

Effective date: 19870224