EP0013874B1 - Vorrichtung zur elektrolytischen Abscheidung von Aluminium - Google Patents

Vorrichtung zur elektrolytischen Abscheidung von Aluminium Download PDF

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Publication number
EP0013874B1
EP0013874B1 EP80100008A EP80100008A EP0013874B1 EP 0013874 B1 EP0013874 B1 EP 0013874B1 EP 80100008 A EP80100008 A EP 80100008A EP 80100008 A EP80100008 A EP 80100008A EP 0013874 B1 EP0013874 B1 EP 0013874B1
Authority
EP
European Patent Office
Prior art keywords
inert gas
liquid
aluminizing
lock
cell
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
EP80100008A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0013874A3 (en
EP0013874A2 (de
Inventor
Günther Dr. phil Herrnring
Klaus Perer Nüssen
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.)
Siemens AG
Original Assignee
Montblanc Simplo GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Montblanc Simplo GmbH filed Critical Montblanc Simplo GmbH
Priority to AT80100008T priority Critical patent/ATE6677T1/de
Publication of EP0013874A2 publication Critical patent/EP0013874A2/de
Publication of EP0013874A3 publication Critical patent/EP0013874A3/de
Application granted granted Critical
Publication of EP0013874B1 publication Critical patent/EP0013874B1/de
Expired legal-status Critical Current

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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
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/003—Electroplating using gases, e.g. pressure influence
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/004—Sealing devices

Definitions

  • the invention relates to an aluminizing cell, consisting of a galvanizing tank and this boiler upstream or downstream locks for introducing and removing the goods to be galvanized.
  • H 2 0 1 mole of H 2 0 should render 2-3 moles of electrolyte ineffective because the aluminum ethylates are no longer able to form complexes; therefore they do not show any electrical conductivity and their formation is therefore a loss of electrolyte.
  • the electrolyte can be regarded as a getter pump for O 2 and H 2 O.
  • This getter pump tries to maintain immeasurably small partial pressures of 0 2 and H 2 0 in its inert gas space and is used up in the process.
  • a technically usable apparatus for the electrolytic deposition of aluminum must therefore have leak rates as low as a high vacuum system if the service life of the electrolyte is to be sufficient from an economic point of view (about 1 year) and, for mechanical reasons, not too much degradation products of the electrolyte in the gas space on the walls and the controls are to be deposited.
  • the electrolyte compartment For the introduction and removal of the goods to be electroplated, the electrolyte compartment must have at least one opening which can be closed tightly and which must be designed as a lock in order to move the goods into and out of the electrolyte compartment without oxygen. Because of the large electroplating frames, which have to be used for economic reasons to attach the parts to be electroplated, suitable mechanical vacuum slides are very expensive, their tightness is difficult to test during operation, and a repair means that the aluminum cell is out of production.
  • Fig.1 Liquid locks based on the principle of a U-tube have already been used with great success for the technical solution of similar tasks.
  • Fig.1 Here is located next to the actual electroplating tank G, a lock S filled with liquid.
  • a connecting element between the electroplating tank G and the lock chamber S there is a U-shaped space I filled with inert gas.
  • the arrows shown indicate the manner in which the goods pass through the lock space S and the inert gas space I are conveyed into the electroplating tank G.
  • the return transport takes place in the opposite direction of the arrow.
  • a pressure relief valve V connected to the inert gas space I ensures that a slight excess pressure remains constantly in the inert gas space.
  • the conditions can be improved by known technical drying processes for toluene using silica gel columns which are regenerated using fresh, distilled, dry toluene.
  • toluene can be dried to about 5 to 10 ppm H 2 O compared to moisture values of 220 to 280 ppm of toluene, which is exposed to an atmosphere of 40 to 50% relative humidity.
  • This drying circuit for the toluene must be very efficient, since the toluene exposed to the atmosphere absorbs moisture very quickly.
  • the object of the present invention is to provide an improved aluminizing cell with which the difficulties outlined above can be remedied in a technically simple and economical manner and which also makes it possible to remain with a liquid lock instead of the complex mechanical lock.
  • liquid lock known per se with an inert gas atmosphere covering the electroplating tank and a lock chamber following in the direction of the lock entrance and filled with an aprotic solvent on the lock entry side is preceded by an additional pre-chamber provided with a loading opening, in which an aprotic solvent is covered Inert gas atmosphere.
  • a design of the aluminizing cell according to the invention is characterized in that the oxygen transport is reduced to the smallest values that can no longer be measured safely and that the water transport is reduced by a factor of about 10 2 to 10 3 , so that the durability of the electrolyte is at least one year to calculate.
  • a liquid-filled lock chamber 3 is also arranged parallel to the actual electroplating tank 1 in the aluminizing cell according to the invention. Electroplating tank 1 and lock chamber 3 are connected by a U-shaped inert gas space 2.
  • the main difference between the lock arrangement according to FIG. 1 and the arrangement according to the invention according to FIG. 2 is that the goods to be treated in the electroplating tank 1 are no longer introduced directly into the lock chamber, but first enter a closed antechamber 4, which is connected to a chamber essential gas-tight door is closed. Below the door 5, the pre-chamber 4 is provided with a calming space 14, which is in communication with the lock fluid in the lock chamber 3.
  • the inert gas space 2 contains an inert gas cushion which is as dry and oxygen-free as possible and which is kept under a small excess pressure by means of the pressure relief valve 13 arranged in the prechamber 4.
  • the pre-chamber 4 is also provided with a pressure relief valve 12, which ensures that the inert gas atmosphere present in the pre-chamber 4 also remains under a small overpressure, which is slightly less than the overpressure in the inert gas space 2.
  • the lock chamber 3 is filled with an aprotic solvent .
  • the partial pressure of 0 2 in the atmosphere is approximately 200 mbar. Since the aluminum triethyl in the electrolyte space consumes the oxygen to small values that are no longer measurable, as already mentioned, partial pressure ratios arise, as can be found in high vacuum systems.
  • Normal paraffin from n-C10 to n-C12 saturated hydrocarbons at a 02 partial pressure of 0.2 bar takes up about 10 ppm 0 2 . This value can be reduced to below 0.1 ppm by flushing with inert gas.
  • the movement of goods in the aluminizing cell according to the invention can be seen from the more detailed representation of FIGS. 3 to 6.
  • the individual goods racks W are introduced via the substantially gas-tight door 5, which, as shown in FIG. 4, is designed as a sliding door.
  • the goods racks W are then attached within the antechamber 4 to the conveyor, which contains two parallel chains or conveyor belts 20.
  • the conveyor chains 20 run via a pair of drive rollers 21 in the antechamber 4, a pair of rollers 22 in the lock chamber 3, two pairs of rollers 23 and 24 in the inert gas space 2, a pair of rollers 25 in the head part of the electroplating tank 1, two pairs of rollers 26 and 27 outside and above the pairs of rollers 23 and 24, a pair of rollers 28 above the pair of rollers 22 and two pairs of rollers 29 and 30 in the head part of the prechamber 4. Between the two pairs of rollers 29 and 30 there is a spring-loaded pair of tensioning rollers 31.
  • the goods racks W suspended in the antechamber 4 then go through the following path during the inward transfer: antechamber 4, calming space 14, below the liquid level 32, lock chamber 3 filled with aprotic solvent, above the liquid level 33 inert gas space 2 and below the electrolytic liquid level 34 electroplating tank 1.
  • the discharge takes place in reverse direction.
  • the actual electroplating tank is designed in the usual way apart from the seals to be described below. Electrodes 41, which are interchangeably suspended, are immersed in the actual container 40 of the electroplating tank provided with a heating jacket. At the top, the container 40 is covered with a dome 48, which is firmly connected to the actual inert gas space 2. In Fig. 3 with VII releasable seals allow to separate the container 40 from the dome. In the container 40 also dip pipes 42, which are used to circulate and filter the electrolyte and open with flanges 42 on the dome 48. Furthermore, of course, the electrodes 41 are provided with power connections, which are also led out in the dome 48 of the electroplating tank. The cathode current supply is carried out in isolation together with the chains 20 from the prechamber 4 to the isolated goods racks W.
  • the goods W introduced there are moved in a manner known per se within the electroplating tank.
  • the electric motor 44 is used, which moves the support rod 47 for the goods racks W back and forth via an eccentric disk 45 and the connecting rod 46.
  • This support rod 47 is mounted on opposite sides of the dome 48 in special seals, which are designated VIII in FIG. 6. These bushings for the support rod 47 are explained in more detail below.
  • a level meter 49 is also arranged in the electroplating tank, which is led out upwards via the dome 48 and the inert gas space 2.
  • FIG. 7 is the seal that is labeled VII in FIGS. 3 to 6.
  • a flange 53 on the upper edge of the electroplating tank container 40 which contains three annular grooves 51, 52, 54 extending over the circumference on its upper side.
  • the troughs 51 and 54 receive sealing rings made of Teflon, Viton or a similar material, while the circumferential trough 52 lying between them forms a liquid space.
  • the counter flange 55 of the dome 48 is ground on its contact surface and then comes to rest against the sealing rings in the grooves 51 and 54, so that the annular space 52 provided for a liquid filling is completely enclosed.
  • the two flanges 53 and 55 are pressed together with clamping jaws 57 and 58, which are clamped together with a screw bolt 59.
  • the annular space 52 is connected at opposite points of the annular flange 55 via pipes 56, through which an aprotic solvent, preferably paraffin oil, is passed. This passage takes place via a closed circle, which is indicated schematically in FIG. 3.
  • an aprotic solvent preferably paraffin oil
  • the paraffin oil is circulated by means of a pump 82 via the pipes 56 and 56 '.
  • the chamber 80 is covered with a further chamber 81, which is filled with an inert gas cushion. This inert gas, preferably N 2 , is also circulated.
  • the seal on the design of the level meter 49 is also formed on the top of the inert gas space 2.
  • the connecting flanges 83 are surrounded by a paraffin oil bath 84, which in turn is covered on its upper side with an inert gas cushion 85.
  • It can be the same Inert gas as in chamber 81, that is to say nitrogen, which is passed through the same circuit as the nitrogen in chamber 81 and the nitrogen still present in further seals for inert gas covers.
  • a separate circuit can also be provided if, as shown in FIG. 3, there is a further chamber 86 filled with aprotic solvent, preferably paraffin oil, which is covered with an inert gas cushion 87.
  • the aprotic solvent is circulated via a pump 88, with which the aprotic solvent is also introduced into the seals VII-VII, which are provided on an inspection and assembly cover 89, which closes the inert gas space 2.
  • the seals VII of the cover 89 are designed essentially as the seal described above with reference to FIG. 7.
  • the seal of goods movement rod 47 is shown in more detail in FIG. 8.
  • the goods movement rod 47 is mounted in a recirculating ball bushing with a needle bearing 90 attached.
  • This recirculating ball bushing 90 is surrounded by a tubular housing 91, which also forms the outer bearing.
  • the tubular housing 91 is connected at both ends to flanged glands 92 and 93, which are designed in a manner known per se and give the possibility of pressing the tubular packing together with a union nut and a pressure piece.
  • sealing rings 94 and 95 are provided, which can be made of Teflon $, Viton $ or the like.
  • pipes 96, 97 open into the tubular housing 91, via which an aprotic solvent can be introduced into the entire interior of the housing 91 and kept in circulation there. This also results in a series connection of a mechanical seal, a liquid seal and a further mechanical seal.
  • the pump and the filters are preferably installed in a boiler which is filled with paraffin oil and covered with inert gas. To change the filter, only the paraffin level needs to be lowered in this boiler.
  • the inert gas stream which is preferably conducted via a closed circuit, can be passed through a regenerator which reduces the water and oxygen content of the gas.

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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 Methods And Accessories (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Secondary Cells (AREA)
EP80100008A 1979-01-17 1980-01-03 Vorrichtung zur elektrolytischen Abscheidung von Aluminium Expired EP0013874B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT80100008T ATE6677T1 (de) 1979-01-17 1980-01-03 Vorrichtung zur elektrolytischen abscheidung von aluminium.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE2901586 1979-01-17
DE19792901586 DE2901586A1 (de) 1979-01-17 1979-01-17 Aluminierzelle

Publications (3)

Publication Number Publication Date
EP0013874A2 EP0013874A2 (de) 1980-08-06
EP0013874A3 EP0013874A3 (en) 1981-01-07
EP0013874B1 true EP0013874B1 (de) 1984-03-14

Family

ID=6060706

Family Applications (1)

Application Number Title Priority Date Filing Date
EP80100008A Expired EP0013874B1 (de) 1979-01-17 1980-01-03 Vorrichtung zur elektrolytischen Abscheidung von Aluminium

Country Status (5)

Country Link
US (1) US4265726A (enrdf_load_stackoverflow)
EP (1) EP0013874B1 (enrdf_load_stackoverflow)
JP (1) JPS55115994A (enrdf_load_stackoverflow)
AT (1) ATE6677T1 (enrdf_load_stackoverflow)
DE (1) DE2901586A1 (enrdf_load_stackoverflow)

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3044975C2 (de) * 1980-11-28 1985-10-31 Siemens AG, 1000 Berlin und 8000 München Vorrichtung zum galvanischen Abscheiden von Aluminium
DE3102021C2 (de) * 1981-01-22 1984-02-23 Siemens AG, 1000 Berlin und 8000 München Vorrichtung zum galvanischen Abscheiden von Aluminium
DE3111786A1 (de) * 1981-03-25 1982-10-07 Siemens AG, 1000 Berlin und 8000 München Elektrisch isolierende schutzeinrichtung
DE3133232A1 (de) 1981-08-21 1983-03-10 Siemens AG, 1000 Berlin und 8000 München Vorrichtung zum galvanischen abscheiden von aluminium
DE3133162C2 (de) 1981-08-21 1984-08-02 Siemens AG, 1000 Berlin und 8000 München Vorrichtung zum galvanischen Abscheiden von Aluminium
DE3231855A1 (de) 1982-08-26 1984-03-01 Siemens AG, 1000 Berlin und 8000 München Vorrichtung zum galvanischen abscheiden von aluminium
US4668367A (en) * 1985-07-09 1987-05-26 Siemens Aktiengesellschaft Lock for loading and unloading goods into a treatment apparatus having a protective atmosphere
US4759831A (en) * 1986-07-04 1988-07-26 Siemens Aktiengesellschaft Electroplating apparatus particularly for electro-deposition of aluminum
SE9302995L (sv) * 1993-09-15 1994-09-26 Aba Sweden Ab Anordning vid slangklämmor
JP5704026B2 (ja) * 2011-09-12 2015-04-22 住友電気工業株式会社 アルミニウム構造体の製造方法
DE102011055911B3 (de) * 2011-12-01 2012-11-29 Volkmar, Prof. Dr. Neubert Verfahren zur galvanischen Abscheidung wenigstens eines Metalls oder Halbleiters
JP6050888B2 (ja) * 2013-03-07 2016-12-21 株式会社日立製作所 基材上へのアルミナイド皮膜の形成方法
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

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1838666A (en) * 1925-08-12 1931-12-29 Colin G Fink Electroplating apparatus
US2897129A (en) * 1957-03-04 1959-07-28 Titanium Metals Corp Electrode handling and storing apparatus
US3136709A (en) * 1959-07-14 1964-06-09 Nat Steel Corp Method of electroplating an aluminum containing coating
DE2537256C3 (de) * 1975-08-21 1979-05-17 Siemens Ag, 1000 Berlin Und 8000 Muenchen Vorrichtung zum galvanischen Abscheiden von Aluminium
DE2716805C3 (de) * 1977-04-15 1979-10-31 Siemens Ag, 1000 Berlin Und 8000 Muenchen Vorrichtung zum galvanischen Abscheiden von Aluminium
DE2719641A1 (de) * 1977-05-03 1978-11-09 Montblanc Simplo Gmbh Galvanisierbad zum abscheiden von metallen, z.b. aluminium in aprotischen loesungsmitteln und inerter atmosphaere
DE2719680A1 (de) * 1977-05-03 1978-11-09 Montblanc Simplo Gmbh Anlage zum aluminieren

Also Published As

Publication number Publication date
DE2901586A1 (de) 1980-07-31
JPS6332880B2 (enrdf_load_stackoverflow) 1988-07-01
ATE6677T1 (de) 1984-03-15
EP0013874A3 (en) 1981-01-07
US4265726A (en) 1981-05-05
JPS55115994A (en) 1980-09-06
EP0013874A2 (de) 1980-08-06

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