US20090308755A1 - Electrolyte for the galvanic deposition of aluminium from aprotic solvents in a plating barrel - Google Patents

Electrolyte for the galvanic deposition of aluminium from aprotic solvents in a plating barrel Download PDF

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Publication number
US20090308755A1
US20090308755A1 US12/517,006 US51700607A US2009308755A1 US 20090308755 A1 US20090308755 A1 US 20090308755A1 US 51700607 A US51700607 A US 51700607A US 2009308755 A1 US2009308755 A1 US 2009308755A1
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Prior art keywords
electrolyte
aluminium
coating
parts
coated
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Abandoned
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US12/517,006
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English (en)
Inventor
Hans DE Vries
Matthias Hartel
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Aluminal Oberflachentechnik GmbH
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Aluminal Oberflachentechnik GmbH
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Assigned to ALUMINAL OBERFLACHENTECHNIK GMBH & CO. KG reassignment ALUMINAL OBERFLACHENTECHNIK GMBH & CO. KG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HARTEL, MATTHIAS, DE VRIES, HANS
Publication of US20090308755A1 publication Critical patent/US20090308755A1/en
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
    • C07F5/06—Aluminium compounds
    • C07F5/061—Aluminium compounds with C-aluminium linkage
    • C07F5/062—Al linked exclusively to C

Definitions

  • the object of the invention is an electrolyte for the electrodeposition of aluminium from aprotic solvents, preferably for the barrel coating of materials.
  • a further object of the invention is to provide a method for producing the electrolyte, the use of said electrolyte, a coating method and parts having been coated using said method.
  • electrodeposition of aluminium in non-aqueous systems is carried out by using an electrolyte that contains organic aluminium alkyl complex compounds dissolved in organic aprotic solvents.
  • the coating is carried out in a way that the materials to be coated are operated as a cathode in the electrolyte solution.
  • the electrolyte solution contains aluminium anodes to provide the necessary aluminium for the coating.
  • the aluminium from the aluminium anodes dissolves and is transported through the electrolyte solution towards the materials operated as the cathode and is deposited on them.
  • An electrolyte with the composition NaF.2 Al(C 2 H 5 ) 3 is described, for example, in DE 1 047 450 AS.
  • This electrolyte has been used in an aromatic hydrocarbon such as toluene. Deposits of aluminium using this electrolyte are of good quality. However, this electrolyte exhibits poor throwing power. Poor throwing power has the effect that particularly complex shapes with rough corners or edges are not or only insufficiently coated with aluminium. To achieve a uniform coating here, the use of auxiliary anodes is required. However, this method is technically very demanding and costly and cannot be carried out economically on an industrial scale. Therefore, for economically reasonable usage of the electrolyte it should exhibit a sufficient throwing power.
  • Electrocoating of small parts and bulk material is usually carried out in rotating, perforated barrels that are driven by an electric motor and installed in a plastic housing within a supporting frame.
  • the small parts to be coated are introduced into the barrel, followed by dipping the barrel into the electrolyte solution.
  • Trans-mission of current onto the goods to be coated inside the barrel is usually performed by means of copper wires positioned laterally on the barrel.
  • Plating barrels of this type described, for instance, in WO 03/012176 A1 and in WO 2005/021840 A1.
  • the small parts to be coated are coated in rotating, perforated barrels. In doing so, only the portion of the goods is coated which is in direct contact with the perforated wall and which has the shortest distance from the anode. The goods in the interior of the goods package in the barrel are not coated. Thus, the barrel must be rotated very often so that the goods are well mixed and all parts remain sufficiently long enough near the inner perimeter of the barrel in order to achieve a uniform coating.
  • the surface in the barrel effective for coating is called the enveloping surface.
  • This enveloping surface is very small compared to the total surface of the small parts in the barrel. In comparison to the interior of the barrel, a very high local current density is applied to this enveloping surface, which, depending on the barrel's filling level, is three to tenfold the average current density that is set with respect to the small parts in the barrel.
  • an electrolyte used for barrel coating has to exhibit a very high current density capacity since the current density distribution in the barrel is not uniform but considerably higher at the enveloping surface than in the interior of the barrel.
  • an accordingly suitable coating electrolyte has to exhibit a very high current density capacity in order to avoid unnecessarily long operating times when coating in the barrel. If the operating times are too long, the parts may suffer damage due to the barrel's rotation and mutual rubbing, and are furthermore subject to increased abrasion. This is particularly critical with threaded or precision parts.
  • the organometallic electrolyte systems that have hitherto been employed for aluminium deposition have only a relatively low maximum current density capacity.
  • the drawback here is that undesired side reactions occur and the quality of the coating is heavily affected as soon as a maximum threshold current density is exceeded.
  • the durability of the electrolyte is highly reduced by the high current density.
  • frequent changing of the electrolyte causes the coating method to become too expensive and uneconomical.
  • a further drawback is that sodium fluoride and potassium fluoride aluminium alkyl complexes, when loaded with high current densities, tend to produce a dendritic crystal growth.
  • irregular overgrowths (uncontrolled growth) of aluminium are deposited mostly on the edges of the parts to be coated or on protruding parts of the plating barrel. These dendrites are brittle and ground to loose particles in the barrel and are plated onto the goods to be coated and partially integrated into the coating. This renders the coated products unusable.
  • deposits in threads of small parts cause impeded joint ability or high friction losses when being screwed together, or the tolerances of the small parts are not adhered to.
  • a further drawback of the hitherto existing electrolyte systems based on potassium fluoride or sodium fluoride is that these complexes can only be employed at very low average current densities due to their low current density capacity. Thereby, long retention times inside the plating barrel are necessary in order to achieve the desired layer thicknesses. Hence, abrasion on the parts and also on the deposited layer is very high and the quality of the layer obtained too low.
  • the complexes containing sodium fluoride which are basically more suitable than potassium fluoride complexes due to their current density capacity, also have poor throwing power for the coating of bulk goods or small parts, such as screws or hollow rivets. Thus, said complexes are not suitable for electrocoating in barrels either.
  • onium complexes are known as electrolytes from older documents of the prior art dating from the years 1959-1967.
  • Onium complexes are complexes in which sodium or potassium fluoride is replaced by tetraalkylammonium halogenides. These electrolyte complexes were described in the 1960s, but never used on an industrial scale because the deposits caused a non-uniform pattern.
  • Said complexes have the disadvantage that in this form they are not suited for industrial application due to the high viscosity of the liquid compounds. Due to the high viscosity this can lead to a carry-over of the electrolyte and, therefore, because of the high inflammability of the electrolyte, to an increased safety risk. Moreover, the electrolyte in this form is also not suitable for electrolysis in a plating barrel because a relatively poor exchange of the electrolyte between anode and cathode occurs due to its high viscosity and there is a risk that the deposition will completely cease due to a depletion of the electrolyte in the barrel.
  • the technical goal of the invention was to provide an electrolyte systern ideally suitable for depositing aluminium on small parts in a plating barrel.
  • R 1 is a C 1 to C 4 alkyl group
  • X is F, Cl or Br
  • n is equal to 0.0 to 1.5, preferably 0.0 to 0.6
  • o is equal to 0.0 to 1.5, preferably 0.0 to 0.6
  • R 2 , R 3 is a C 1 or C 3 to C 6 alkyl group, wherein R 2 is unequal to R 3 , in an organic solvent.
  • the electrolytes of the invention have the advantage that they do not show any alkali metal co-deposition, especially at high current densities, and this thereby guarantees a uniform aluminium coating without losses in corrosion resistance.
  • these electrolytes have a high current density capacity and good conductivity.
  • a relatively high average current density becomes possible with regard to the total surface of the goods to be coated.
  • it is an advantage that the time required for coating in the barrel is considerably lower and, therefore, there is a lower risk that damages to and abrasions on the parts to be coated occur due to the barrel's rotation.
  • the electrolytes according to the invention also possess a very high throwing power, which in addition allows more complex shapes to be well coated.
  • the electrical conductivity of the electrolyte of the invention is greater than 25 mS/cm at 95° C., preferably between 28 and 35 mS/cm at 95° C.
  • the conductivity is measured using a commercially available conductivity probe (e.g. TetraCon 325 Pt by WTW Inc.) in a glass vessel with 25 ml of electrolyte in an atmosphere of argon, kept at 95° C. in an oil bath.
  • a commercially available conductivity probe e.g. TetraCon 325 Pt by WTW Inc.
  • a solvent is used as an organic solvent which is selected from the group containing toluene, xylene or benzene, or mixtures thereof.
  • the solvent is present in a concentration of 1 to 4 mol, preferably 2 mol, per mol of complex compound.
  • the compound of the General Formula I is as follows: N(C 2 H 5 ) 4 Cl.2Al(C 2 H 5 ) 3 2 toluene or N(C 2 H 5 ) 4 Cl.1.5Al(C 2 H 5 ) 3 .0.5 Al(CH 3 ) 3 .2 toluene or N(C 2 H 5 ) 4 Cl.1.5Al(C 2 H 5 ) 3 .0.5 Al(C 4 H 9 ) 3 2 toluene.
  • Another object of the invention is a method to produce the electrolyte.
  • the tetraalkylammonium halogen compound is dried in order to remove humidity.
  • the dried substance is suspended in an organic aprotic solvent, preferably toluene.
  • the aluminium trialkyl compounds or mixtures of aluminium trialkyl compounds are added dropwise during cooling until a clear solution of the end product is obtained.
  • the electrolyte is preferably used for the electrodeposition of aluminium on material parts. These material parts are selected from metals, alloys, ceramics, plastics, or composite materials made of one or more of said materials.
  • the material parts to be coated are placed into a coating barrel and coated with aluminium in said coating barrel.
  • the coating process is carried out in several steps. First, the parts to be coated, which have been pre-treated if necessary, are placed in the coating barrel. The coating barrel is dipped into the electrolyte of the present invention. Then, a cathodic current is applied to the coating barrel, and an anodic current is applied to the aluminium anodes, which have been placed into the electrolyte solution. This results in an aluminium layer being deposited onto the parts to be coated, and the aluminium anodes being dissolved. Afterwards, the parts are removed from the coating barrel and subsequently dried.
  • Examples for typical operating parameters under which the electrolytes of the invention are employed in plating barrels are: an operating temperature of the electrolyte solution of 90 to 100° C., a cell voltage of 10 to 40 V, and an average current density of 0.4 to 1.0 A/dm 2 , wherein the current density is 4 to 6 A/dm 2 at the enveloping surface of the plating barrel.
  • the speed of deposition on the materials to be coated is 10 to 12 ⁇ m per hour, with an average current density of 1 A/dm 2 .
  • a further object of the invention are parts coated with aluminium, produced using the method according to the invention.
  • the electrolyte of the invention exhibits considerable advantages regarding dendritic growth particularly in comparison to the electrolytes of the prior art, which contain sodium fluoride or potassium fluoride.
  • a series of experiments with an electrolyte having the composition NaF.2Al(C 2 H 5 ) 3 .2 toluene was carried out. When coating using said electrolyte a strong dendritic edge growth occurred on the gap plates that were used as test specimens.
  • an electrolyte of the invention e.g. N(C 2 H 5 ) 4 Cl.2Al(C 2 H 5 ) 3 .2 toluene, it was found that no dendritic growth occurred and a smooth surface layer was achieved on the edge. This too proves the superiority of the electrolyte of the invention as opposed to the hitherto used electrolytes containing sodium fluoride or potassium fluoride.
  • the maximum current density capacity of the electrolyte according to the invention is in the range of 5 to 6 A/dm 2 , whereas the current density capacity of the respective electrolyte containing potassium fluoride is in the range of 1 to 1.5 A/dm 2 , the electrolyte containing sodium fluoride is in the range of 3 to 4 A/dm 2 and the electrolyte containing ammonium benzyl is at 1.5 A/dm 2 . Due to the high current density capacity of the electrolyte of the invention a commercially viable deposition is possible in a plating barrel in a short time, without the parts being damaged. Thus, a high quality coating is achieved.
  • Tetraethylammonium chloride which can be purchased as monohydrate, is dried in a vacuum. 1 mol of the dried tetraethylammonium chloride is mixed with toluene so that a suspension is obtained. 2 mol of triethylaluminium, which is used either as a pure substance or dissolved in toluene, is added to this suspension dropwise during cooling. The reaction mixture is stirred. A clear solution of N(C 2 H 5 ) 4 Cl.2Al(C 2 H 5 ) 3 .2 toluene is obtained. 2 mol of toluene are used as a solvent with respect to the employed amount of tetraethylammonium chloride. The obtained product is used as an electrolyte.
  • a sufficient electrical conductivity of the electrolyte is a basic requirement for a sufficient coating, particularly of small parts in plating barrels.
  • the conductivity of the electrolyte of the invention is substantially higher than those of the prior art, which contain sodium fluoride or potassium fluoride.
  • a toluene-free electrolyte has a lower electrical conductivity than the electrolyte of the invention, which contains 2 mol of toluene.
  • the following table shows a comparison of the individual conductivities of the electrolytes of the invention and of the electrolytes of the prior art.
  • gap plates made of brass were used in coating experiments. These gap plates had the following dimensions: width 20 mm, stretched length 100 mm. Prior to coating, 25 mm of the lower region of the gap plate was bent 180°, resulting in a plate with a J-shaped longitudinal section, with a gap width of 1 mm between the two branches. After coating, the extent of the aluminium deposition in the gap between the two branches after bending the plate, and thus the throwing power of the electrolyte system, could be assessed and compared to further coating experiments with different coating parameters or electrolyte compositions.
  • Anodes with a width of 15 mm were used as aluminium anodes to particularly allow experiments concerning long time deposition.
  • electrolyte N(C 2 H 5 ) 4 Cl.2Al(C 2 H 5 ) 3 .2 toluene was used.
  • cathodic and anodic yields were calculated as a function of the load of the electrolyte with current (in Ah/L).
  • a gap plate was coated for 30 min at a current of 350 mA (corresponding to a current density of 2.5 A/dm 2 ) and a voltage of 2.4 V. Immediately after switching on the coating current the coating uniformly attached to the plate. The coating was white, smooth, uniform and matt. No dendrite forming occurred. Even under the microscope the edges were smooth. The inner surface was also completely coated. The electrolyte exhibited an excellent throwing power. The structure of the coating was microcrystalline and of high quality. No gas development was observed at the aluminium anodes.
  • Another coating of a gap plate was carried out within 30 min at a current of 450 mA (corresponding to a current density of 3.2 A/dm 2 ), at a voltage of 2.4 V.
  • the same electrolyte as in Example 1 was used. Again, white smooth satin-gloss layers were produced that did not exhibit any dendrite forming at the edges.
  • the inner surface of the gap plate was also completely coated. The structure was microcrystalline and no gas development was observed at the anodes.
  • a gap plate was coated for 30 minutes at a current of 600 mA (corresponding to a current density of 4.3 A/dm 2 ) and a voltage of 2.78 V.
  • the layer thickness achieved was about 25 ⁇ m.
  • the layer was silvery with slightly glittering areas and microcrystalline without dendrites at the edges and points. The plate was completely coated at the edges.
  • the microscopic exposures of the edges reveal significant differences when comparing the electrolyte of the prior art, containing sodium fluoride, to the electrolyte of the invention.
  • the coating created by the electrolyte of the prior art exhibited a clearly visible dendritic growth at the edges and no smooth structure (see FIG. 1 ).
  • the electrolyte of the invention did not exhibit any dendritic growth at the edges but had a clear smooth coating (see FIG. 2 ).
  • dendrites are extremely harmful for a coating. They are brittle and are ground to loose particles, particularly during electrocoating in barrels, and cement themselves during the coating process forming deposits on the goods to be coated. This deposit-forming and the partial integration into the aluminium layers renders the products unusable because, for example, deposits in screw threads of the goods cause an impeded joint ability of the thread or very high friction losses. Moreover, dimensional tolerances can no longer be adhered to.
  • the electrolyte according to the invention does not show any dendritic growth and can produce an aluminium layer which is smooth and of high quality and which does not exhibit the drawbacks described above.
  • the long-term stability of the electrolyte of the invention was also examined. A total of three anode sets were consumed. Coating times of up to 64 hours at a current density of 0.63 to 2.2 A/dm 2 were applied. The total load of the electrolyte after the first set of anodes was 417 Ah/L with eight coatings and 748 Ah/L with five further coatings after the second set of anodes.
  • the electrolyte of the invention therefore is a reasonable improvement on hitherto employed electrolytes based on sodium fluoride or potassium fluoride because it exhibits better properties and leads to aluminium deposits of higher quality.
  • a co-deposition of sodium or potassium is not possible with the electrolyte of the invention.
  • No dendrite forming can be observed.
  • the current density capacity and the throwing power of the electrolyte is very high, and the electrolyte of the invention furthermore also has a high long-term stability so that it can be used cost-effectively in large-scale industrial processes.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Electrolytic Production Of Metals (AREA)
US12/517,006 2006-11-29 2007-10-16 Electrolyte for the galvanic deposition of aluminium from aprotic solvents in a plating barrel Abandoned US20090308755A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EPEP06125040.3 2006-11-29
EP06125040A EP1927680A1 (de) 2006-11-29 2006-11-29 Elektrolyt zur galvanischen abscheidung von aluminium aus aprotischen lösungsmitteln in einer galvanisiertrommel
PCT/EP2007/061016 WO2008064954A2 (de) 2006-11-29 2007-10-16 Elektrolyt zur galvanischen abscheidung von aluminium aus aprotischen lösungsmitteln in einer galvanisiertrommel

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US (1) US20090308755A1 (de)
EP (1) EP1927680A1 (de)
JP (1) JP2010511102A (de)
CN (1) CN101573476A (de)
CA (1) CA2670720A1 (de)
WO (1) WO2008064954A2 (de)

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JPWO2012043513A1 (ja) * 2010-10-01 2014-02-24 株式会社シンク・ラボラトリー シリンダ用メッキ装置

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3028319A (en) * 1960-02-01 1962-04-03 Ethyl Corp Manufacture of magnesium organo compounds
US3445127A (en) * 1967-05-26 1969-05-20 Hydrasearch Co Inc Universal flange connector
US4032413A (en) * 1974-11-13 1977-06-28 Siemens Aktiengesellschaft Electroplating bath and method for the electrodeposition of bright aluminum coatings
US5091063A (en) * 1989-06-10 1992-02-25 Studiengesellschaft Kohle Mbh Organoaluminum electrolytes and process for the electrolytic deposition of aluminum
EP0505886A1 (de) * 1991-03-28 1992-09-30 Siemens Aktiengesellschaft Erzeugung dekorativer Aluminiumbeschichtungen
US20040140220A1 (en) * 2002-04-30 2004-07-22 Fischer Juergen K S Aluminium electroplating formulations

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1200817B (de) * 1963-03-30 1965-09-16 Siemens Ag Verfahren zur Darstellung von Oniumsalz-Komplexverbindungen
DE3202265A1 (de) * 1982-01-25 1983-07-28 Siemens AG, 1000 Berlin und 8000 München Elektrolyt zur galvanischen abscheidung von aluminium
WO2002088434A1 (en) * 2001-04-30 2002-11-07 Alumiplate Incorporated Aluminium electroplating formulations

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3028319A (en) * 1960-02-01 1962-04-03 Ethyl Corp Manufacture of magnesium organo compounds
US3445127A (en) * 1967-05-26 1969-05-20 Hydrasearch Co Inc Universal flange connector
US4032413A (en) * 1974-11-13 1977-06-28 Siemens Aktiengesellschaft Electroplating bath and method for the electrodeposition of bright aluminum coatings
US5091063A (en) * 1989-06-10 1992-02-25 Studiengesellschaft Kohle Mbh Organoaluminum electrolytes and process for the electrolytic deposition of aluminum
EP0505886A1 (de) * 1991-03-28 1992-09-30 Siemens Aktiengesellschaft Erzeugung dekorativer Aluminiumbeschichtungen
US20070261966A1 (en) * 2001-04-30 2007-11-15 Alumiplate Incorporated Aluminum electroplating formulations
US20040140220A1 (en) * 2002-04-30 2004-07-22 Fischer Juergen K S Aluminium electroplating formulations

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Publication number Publication date
EP1927680A1 (de) 2008-06-04
CA2670720A1 (en) 2008-06-05
WO2008064954A2 (de) 2008-06-05
JP2010511102A (ja) 2010-04-08
WO2008064954A3 (de) 2009-06-04
WO2008064954A4 (de) 2009-07-16
CN101573476A (zh) 2009-11-04

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