US2849349A - Process for the electrolytic deposition of aluminium - Google Patents

Process for the electrolytic deposition of aluminium Download PDF

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Publication number
US2849349A
US2849349A US521424A US52142455A US2849349A US 2849349 A US2849349 A US 2849349A US 521424 A US521424 A US 521424A US 52142455 A US52142455 A US 52142455A US 2849349 A US2849349 A US 2849349A
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aluminium
compound
electrolyte
aluminum
electrolytes
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US521424A
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Ziegler Karl
Lehmkuhl Herbert
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ZIEGLER AG
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ZIEGLER AG
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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

Definitions

  • This invention relates to a process for the electrolytic deposition of aluminium.
  • aluminium on a technical scale exclusively makes use of melt electrolysis at SOD-900 C. in an electrolyte consisting mainly of molten cryolite.
  • the current consumption is about 24 kilowatt hours per kilogram of aluminium.
  • the same process is used in principle in the electrolytic refining treatment in the so-called three layer process.
  • the current consumption is somewhat lower, but nevertheless is still 20 kw.-h./ kg.
  • Aluminium trialkyls aluminium dialkyl hydrides AlR H, aluminium alkyl halides, such as AlR Cl, AlRCland similar substances are all non-conductors of electric current. However, they can be transformed into electrolytes by converting them into complex compounds, for example sodium ethyl with aluminium triethyl forms sodium-aluminium tetraethyl NaAl(C H In molten form, this substance has very good conductivity. This has already been shown by F.
  • Hein (Zeitschrift fiir anorganische Chemie, 141, 161-226 (1924)), who obtained an oily product from sodium ethyl and aluminium triethyl and investigated it concerning its conductivity; it is true that he designated this product as being a solution of sodium ethyl in aluminium triethyl, but, as is known for certain at the present time, this product was the complex compound just referred to. F. Hein did not indicate which element is deposited on the cathode in the electrolysis. If this is investigated, it is found that mainly sodium is formed on the cathode. In addition, some aluminium may also be deposited, and spongy mixtures of sodium and aluminium are frequently observed to form at the cathode.
  • Electrolytes which have proved to be particularly suitable are homogeneous melts of true organic aluminium compounds of the general formula AlR(R') in which R represents an alkyl radical and R represents an alkyl radical or a hydrogen or halogen atom, together with complex compounds thereof with alkali metal compounds of the general formula MeR, wherein Me represents an alkali metal, or quaternary ammonium compounds.
  • Alkali metal compounds which are particularly suitable for forming the complex are alkali metal alkyls, hydrides and halides, and also tetraethyl ammonium halides, triethyl-n-butyl-ammonium halides, ethyl-tri-nbutylammonium halides, dodecyl-tri-methyl-ammonium halides, such as the chloride, and also quaternary pyridinium, quinolinium and isoquinolinium salts, such as pyridinium methiodide.
  • the electrolytes can be homogeneously melting compounds of true organic compounds of the general formula AlR(R) in which R represents an alkyl radical and R represents an alkyl radical or a hydrogen or halogen atom, and their complex compounds with alkali metal compounds of the general formula MeR, wherein Me represents an alkali metal, or with quaternary ammonium compounds.
  • the basic complex compound is obtained very easily by adding sodium hydride to diisobutyl aluminium hydride.
  • Organic aluminium complex compounds containing fluorine have proved to be particularly suitable for com- Patented Aug. 26, 1958 bining'to give electrolytes of the type referred to.
  • the sodium-aluminium triethyl fluoride NaAl Cal-I5) F with-2 mols-'of aluminium triethyl forms a novel and welldefined :second complex compound with the composition NaF.2Al(C H this compound is described in a prior application of the applicants and melts at a ve'r-ylowtemperature.
  • the specific conductivity of the melt is as follows:
  • an electrolyte can be produced by dissolving sodium fluoride in a mixture of'aluminium trimethyl and aluminium triethyl. In this case, it is again a question of the formation of -a complex compound of 1 mol of sodium fluoride with -2 mols of aluminium trialkyls (which are here differentfrom one another).
  • An example of an excellent electrolyte is one which has exactly or substantially the following composition in themelt:
  • This electrolyte can be produced by melting together sodium fluoride, aluminium triethyl and aluminium diethyl "fluoride. Another excellent electrolyte of this group is formed if finely powdered dry cryolite is boiled with more than 6 mols of aluminium triethyl. The cryolite enters into solution. Two layers are formed, the upper layer consisting of aluminium triethyl, which can easily be separated while the lower layer has the composition:
  • KF ZAKCzHs NaH Al(-C
  • solvents which can be used are those which do not decompose the organic aluminium compounds, for example bydrocarbons, especially those of aromatic nature.
  • Ethers and tertiary amines such as tetrahydrofurane, dime'thyl aniline, dioxane and pyridine can also be used.
  • the heated melts of the electrolytes can be very easily protected against the action of air by covering them with a small amount of paraffin oil. They are not all miscible with paraflin oil. However, even while observing this precautionary measure, it is advisable to carry out the electrolysis processes in closed vessels and to fill the free space above the oil with an inert protective gas, such as nitrogen.
  • electrolytes can also be mixed with one another in suitable manner; for example, certain amounts of sodium aluminum tetraethyl can also be dissolved in the NaF.(Al(C H electrolyte without impairing the usefulness of the electrolyte. The excess of aluminum triethyl which even then is still present, is sufficient.
  • the electrolytes enumerated in detail and by way of example contain methyl, ethyl and l-butyl as organic radicals bonded to aluminium. It is obvious that a large number of similarly usable electrolytes can also be produced by using other alkyl radicals and'also by using those having a higher number of carbon atoms.
  • novel electrolytes can be used with advantage in all cases where it is important that a very pure aluminium should be deposited, i. e. they can be usedfor the production of aluminium coatings, possible on other metals such as copper, or also on a foundation material of less pure aluminium, or also for refining aluminium.
  • the electrolysis is preferably carried out using aluminium anodes.
  • the impurities of the aluminium remain undissolved in the form of a black sludge.
  • the sludge initially remains loosely clinging to the anode, but usually becomes detached during the electrolysis and falls to the bottom of the cell, but frequently also remains suspended in the electrolyte to some extent, with the possible result that particles of the anode sludge adhere to the cathode coatings and impair the deposition thereon.
  • the voltage during the electrolysis between terminals consisting of parallel plates of equal size can easily be maintained between 0.3 and 1 volt, when the spacing of the plates is about 3 cm. Under these circumstances, the energy consumption per kg. of deposited aluminium is between 0.9 and 3 kw.-h. at 150 C.
  • the aluminium coatings are initially dense and compact, but as the thickness of the deposited layer increases, they become gradually granular and blistered. However, the aluminium can be deposited up to a considerable thickness without the cells being damaged by bridge formation. Within the range of layer thicknesses which are used for surface treatment, the coating is completely dense and smooth and adheres firmly, provided that the surface of the foundation material has been thoroughly cleaned. A spectroscopic examination of the deposited aluminium shows that it is at least 99.999% pure, even when ordinary foundry aluminium has been used as anode.
  • the aluminium obtained according to the process of the present invention was compared with the best quality refined ultra-pure aluminium (99.99% It was not possible to detect a rise in temperature in either of the two cases, but the 99.99% aluminium had completely dissolved after 12 hours.
  • the aluminium obtained by a process of the invention merely showed a decrease in weight by about /3.
  • Copper plates or copper wires which have been provided by the process of the invention with an aluminium coating a few microns thick can be kept for hours in nitric acid without it being possible to detect any corrosion of the copper by the nitric acid.
  • the particularly high purity of the aluminium obtained is obviously the result of the fact that all electrolytes had been prepared from distillable and also distilled organic aluminium compounds. By this means it is clearly possible for the normal impurities of the aluminium to be separated with very great effectiveness in a very simple manner.
  • Example 1 42 g. of sodium fluoride and 260 g. of aluminium triethyl are brought together under a nitrogen atmosphere and heated while stirring to l00-120 C. The solid salt dissolves and two liquid layers are obtained. The upper layer consists of practically pure triethyl and the bottom layer is an excellent electrolyte for the electrolytic deposition of aluminium and has exactly the composition NaF.2Al(C H Example 2 melt electrolysis of this reaction product, a firmly adhering aluminium deposit is obtained on the cathode.
  • Example 3 58 g. of potassium fluoride are dissolved in 198 g. of aluminium triisobutyl H CH3 Al(CHr- ⁇ )2 at about 100 C. in a nitrogen atmosphere. 85 g. of aluminium trimethyl are added to this reaction mixture while stirring and heating to -90 C. Two liquid layers are formed. The upper layer is. practically non-conductive to electric current, andthe bottom layer has the composition KF;Al(i-C H .Al(CH and is quite suitable for the electrolytic deposition of aluminium.
  • Example 4 24 g, of sodium hydride, 142 g. of aluminium diisobutyl hydride H CH3 M r-C )2 and 114 g. of aluminium triethyl are combined in a nitrogen atmosphere and heated while stirring to 110-120".
  • the solid sodium hydride dissolves.
  • the liquid reaction mixture which is formed has the composition NaH.HAl i-C4H9) C2H5 3
  • Example 6 Pyridinium methiodide is brought together with aluminium triethyl, as described in Example 6. In this case also,
  • a yellowish to brownish liquid bottom layer is formedwhich is not miscible with aluminium triethyl, the said layer having the composition pyridinium methiodide.2 aluminium triethyl.
  • Example 8 Dodecyl-trimethyl-ammonium chloride is dissolved in liquid aluminium tri-n-butyl in such an amount that the molar ratio (mols) between the quaternary salt and the aluminum tri-n-butyl is greater than 1. Electrolytes of any desired composition are obtained (the quaternary salt being soluble in aluminium tri-n-butyl in all proportions) and these electrolytes deposit a good and firmly adhering precipitate on the cathode during the electrolysis.
  • a process for the electrolytic deposition of aluminum upon an electrically conductive surface which comprises passing an electric current between an anode and said electrically conductive surface as a cathode through an electrolyte which consists essentially of a homogeneous melt of a true organic compound of aluminum of the general formula AIR(R') in which R is an alkyl group and R is a substituent selected from the group consisting of alkyl, hydrogen and halogen, in combination with a complex compound of such aluminum compound AlR(R) with a compound of the formula MeR in which Me is selected from the group consisting of alkali metals and quaternary ammonium radicals and R has the same significance as above, said complex compound being of the formula MeRAlR(R) in which Me, R and R have the same significance as above, the quantity of said organic compound of aluminium of the formula AlR(R) in said homogeneous melt being in excess of that contained in said complex compound of the formula MeR'AlR(R') 2.

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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)
  • Electrolytic Production Of Metals (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
US521424A 1955-06-13 1955-07-11 Process for the electrolytic deposition of aluminium Expired - Lifetime US2849349A (en)

Applications Claiming Priority (2)

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DEZ4338A DE1047450B (de) 1955-06-13 1955-06-13 Elektrolyt zur elektrolytischen Abscheidung von Aluminium
DE130655X 1955-06-13

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FR (1) FR1134858A (en)van)
GB (1) GB813446A (en)van)

Cited By (28)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2952589A (en) * 1956-04-09 1960-09-13 Karl Ziegler Purification of aluminum
US3007857A (en) * 1957-07-31 1961-11-07 Nalco Chemical Co Preparation of organic lead compounds
US3028323A (en) * 1959-12-24 1962-04-03 Ethyl Corp Manufacture of organolead products
US3028322A (en) * 1962-04-03 Malmei
US3028318A (en) * 1960-02-01 1962-04-03 Ethyl Corp Manufacture of zinc organo compounds
US3028319A (en) * 1960-02-01 1962-04-03 Ethyl Corp Manufacture of magnesium organo compounds
US3028320A (en) * 1960-02-01 1962-04-03 Ethyl Corp Manufacture of tin alkyl compounds
US3069334A (en) * 1957-06-12 1962-12-18 Ziegler Karl Process for the production of tetraethyl lead
US3164538A (en) * 1960-06-07 1965-01-05 Ziegler Karl Electrolytic production of metal alkyls
US3206522A (en) * 1959-08-10 1965-09-14 Continental Oil Co Production of alpha-olefins
US3234114A (en) * 1961-06-30 1966-02-08 Ziegler Karl Process for the recovery of purified sodium
US3234115A (en) * 1963-07-31 1966-02-08 Ziegler Karl Process for the electrolytic precipitation of sodium
US3234113A (en) * 1961-05-09 1966-02-08 Ziegler Electrolytic separation of sodium
US3254008A (en) * 1961-05-23 1966-05-31 Ziegler Process for the electrolytic production of tetramethyl lead
US3254009A (en) * 1958-02-13 1966-05-31 Ziegler Production of metal alkyls
US3261773A (en) * 1959-01-12 1966-07-19 Siemens Ag Apparatus for doping and contacting semiconductor bodies
US3268421A (en) * 1961-12-04 1966-08-23 Nat Steel Corp Electrodeposition of metals from a fused bath of aluminum halohydride organic complex and composition therefor
US3306836A (en) * 1959-05-06 1967-02-28 Ziegler Process for the electrolytic production of magnesium dialkyls and aluminium trialkyls
US3325383A (en) * 1960-03-09 1967-06-13 Siemens Ag Method for producing gallium
US3379628A (en) * 1965-04-21 1968-04-23 Continental Oil Co Decorative etching of aluminum
US3409523A (en) * 1966-03-10 1968-11-05 Bell Telephone Labor Inc Electroetching an aluminum plated semiconductor in a tetraalkylammonium hydroxide electrolyte
US5007991A (en) * 1989-06-10 1991-04-16 Studiengesellschaft Kohle Mbh Organoaluminum electrolytes for the electrolytic deposition of high-purity aluminum
US5091063A (en) * 1989-06-10 1992-02-25 Studiengesellschaft Kohle Mbh Organoaluminum electrolytes and process for the electrolytic deposition of aluminum
WO2000032847A3 (de) * 1998-12-01 2000-11-16 Studiengesellschaft Kohle Mbh Aluminiumorganische elektrolyte und verfahren zur elektrolytischen beschichtung mit aluminium oder aluminium-magnesium-legierungen
US20040140220A1 (en) * 2002-04-30 2004-07-22 Fischer Juergen K S Aluminium electroplating formulations
US6960677B1 (en) 2003-10-28 2005-11-01 Albemarle Corporation Preparation of aluminates
EP2599896A3 (de) * 2011-12-01 2014-01-22 Volkmar Neubert Verfahren zur galvanischen Abscheidung wenigstens eines Metalls oder Halbleiters
EP2891730A4 (en) * 2012-08-31 2016-05-18 Hitachi Ltd NON-AQUEOUS ELECTROPLATING PROCESS AND DEVICE FOR NON-WATER ELECTROPLATING

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1162576B (de) * 1959-11-07 1964-02-06 Guenther Hans Dipl Chem Dr Elektrolyt und Verfahren zur Herstellung von Beryllium durch Schmelzflusselektrolyse von organischen Berylliumverbindungen
DE1170659B (de) * 1959-12-01 1964-05-21 Dr Cordes Verfahren zur elektrolytischen Abscheidung von Aluminium hoher Reinheit
DE1236208B (de) 1960-08-09 1967-03-09 Siemens Ag Verfahren zur Feinreinigung von metallischen Elementen der II. bis ó÷. Gruppe des Perioden-systems
GB956990A (en) 1960-10-29 1964-04-29 Sumitomo Chemical Co A method for manufacturing aluminum
DE1187380B (de) 1963-09-13 1965-02-18 Vaw Ver Aluminium Werke Ag Elektrolyt und Verfahren zur elektrolytischen Abscheidung von hochreinem Aluminium aus metallorganischen Komplexverbindungen
US3969195A (en) * 1971-05-07 1976-07-13 Siemens Aktiengesellschaft Methods of coating and surface finishing articles made of metals and their alloys
DE3202265A1 (de) * 1982-01-25 1983-07-28 Siemens AG, 1000 Berlin und 8000 München Elektrolyt zur galvanischen abscheidung von aluminium
DE3606325A1 (de) * 1986-02-27 1987-09-03 Talbot Waggonfab Laufwerkfederung fuer schienenfahrzeuge
EP1518946A1 (de) * 2003-09-27 2005-03-30 Aluminal Oberflächtentechnik GmbH & Co. KG Electrolyt zur galvanischen Abscheidung von Aluminium

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2321367A (en) * 1939-12-27 1943-06-08 Hanson Van Winkle Munning Co Anode bag
US2446349A (en) * 1944-02-29 1948-08-03 William Marsh Rice Inst For Th Electrodeposition of aluminum
US2728718A (en) * 1951-11-02 1955-12-27 Battelle Development Corp Aluminum coating

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2321367A (en) * 1939-12-27 1943-06-08 Hanson Van Winkle Munning Co Anode bag
US2446349A (en) * 1944-02-29 1948-08-03 William Marsh Rice Inst For Th Electrodeposition of aluminum
US2728718A (en) * 1951-11-02 1955-12-27 Battelle Development Corp Aluminum coating

Cited By (31)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3028322A (en) * 1962-04-03 Malmei
US2952589A (en) * 1956-04-09 1960-09-13 Karl Ziegler Purification of aluminum
US3069334A (en) * 1957-06-12 1962-12-18 Ziegler Karl Process for the production of tetraethyl lead
US3007857A (en) * 1957-07-31 1961-11-07 Nalco Chemical Co Preparation of organic lead compounds
US3254009A (en) * 1958-02-13 1966-05-31 Ziegler Production of metal alkyls
US3328272A (en) * 1959-01-12 1967-06-27 Siemens Ag Process using an oxygen free electrolyte for doping and contacting semiconductor bodies
US3261773A (en) * 1959-01-12 1966-07-19 Siemens Ag Apparatus for doping and contacting semiconductor bodies
US3306836A (en) * 1959-05-06 1967-02-28 Ziegler Process for the electrolytic production of magnesium dialkyls and aluminium trialkyls
US3206522A (en) * 1959-08-10 1965-09-14 Continental Oil Co Production of alpha-olefins
US3028323A (en) * 1959-12-24 1962-04-03 Ethyl Corp Manufacture of organolead products
US3028319A (en) * 1960-02-01 1962-04-03 Ethyl Corp Manufacture of magnesium organo compounds
US3028318A (en) * 1960-02-01 1962-04-03 Ethyl Corp Manufacture of zinc organo compounds
US3028320A (en) * 1960-02-01 1962-04-03 Ethyl Corp Manufacture of tin alkyl compounds
US3325383A (en) * 1960-03-09 1967-06-13 Siemens Ag Method for producing gallium
US3164538A (en) * 1960-06-07 1965-01-05 Ziegler Karl Electrolytic production of metal alkyls
US3234113A (en) * 1961-05-09 1966-02-08 Ziegler Electrolytic separation of sodium
US3254008A (en) * 1961-05-23 1966-05-31 Ziegler Process for the electrolytic production of tetramethyl lead
US3234114A (en) * 1961-06-30 1966-02-08 Ziegler Karl Process for the recovery of purified sodium
US3268421A (en) * 1961-12-04 1966-08-23 Nat Steel Corp Electrodeposition of metals from a fused bath of aluminum halohydride organic complex and composition therefor
US3234115A (en) * 1963-07-31 1966-02-08 Ziegler Karl Process for the electrolytic precipitation of sodium
US3379628A (en) * 1965-04-21 1968-04-23 Continental Oil Co Decorative etching of aluminum
US3409523A (en) * 1966-03-10 1968-11-05 Bell Telephone Labor Inc Electroetching an aluminum plated semiconductor in a tetraalkylammonium hydroxide electrolyte
US5007991A (en) * 1989-06-10 1991-04-16 Studiengesellschaft Kohle Mbh Organoaluminum electrolytes for the electrolytic deposition of high-purity aluminum
US5091063A (en) * 1989-06-10 1992-02-25 Studiengesellschaft Kohle Mbh Organoaluminum electrolytes and process for the electrolytic deposition of aluminum
WO2000032847A3 (de) * 1998-12-01 2000-11-16 Studiengesellschaft Kohle Mbh Aluminiumorganische elektrolyte und verfahren zur elektrolytischen beschichtung mit aluminium oder aluminium-magnesium-legierungen
US6652730B1 (en) * 1998-12-01 2003-11-25 Studiengesellschaft Kohle Mbh Aluminum organic electrolytes and method for electrolytic coating with aluminum or aluminum-magnesium-alloys
US20040140220A1 (en) * 2002-04-30 2004-07-22 Fischer Juergen K S Aluminium electroplating formulations
US7250102B2 (en) 2002-04-30 2007-07-31 Alumiplate Incorporated Aluminium electroplating formulations
US6960677B1 (en) 2003-10-28 2005-11-01 Albemarle Corporation Preparation of aluminates
EP2599896A3 (de) * 2011-12-01 2014-01-22 Volkmar Neubert Verfahren zur galvanischen Abscheidung wenigstens eines Metalls oder Halbleiters
EP2891730A4 (en) * 2012-08-31 2016-05-18 Hitachi Ltd NON-AQUEOUS ELECTROPLATING PROCESS AND DEVICE FOR NON-WATER ELECTROPLATING

Also Published As

Publication number Publication date
BE540052A (en)van)
GB813446A (en) 1959-05-13
DE1047450B (de) 1958-12-24
FR1134858A (fr) 1957-04-18
CH350112A (de) 1960-11-15

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