EP1510600A1 - Verfahren und Vorrichtung zum Abscheiden von Metallen und Metalllegierungen aus Metallorganischen Elektrolyten - Google Patents

Verfahren und Vorrichtung zum Abscheiden von Metallen und Metalllegierungen aus Metallorganischen Elektrolyten Download PDF

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Publication number
EP1510600A1
EP1510600A1 EP03019235A EP03019235A EP1510600A1 EP 1510600 A1 EP1510600 A1 EP 1510600A1 EP 03019235 A EP03019235 A EP 03019235A EP 03019235 A EP03019235 A EP 03019235A EP 1510600 A1 EP1510600 A1 EP 1510600A1
Authority
EP
European Patent Office
Prior art keywords
solvent
products
section
coating
lock chamber
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.)
Withdrawn
Application number
EP03019235A
Other languages
German (de)
English (en)
French (fr)
Inventor
Jörg Dr. Heller
Hans De Vries
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.)
Aluminal Oberflachentechnik GmbH
Original Assignee
Aluminal Oberflachentechnik 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 Aluminal Oberflachentechnik GmbH filed Critical Aluminal Oberflachentechnik GmbH
Priority to EP03019235A priority Critical patent/EP1510600A1/de
Priority to PCT/EP2004/009192 priority patent/WO2005021840A1/de
Priority to DK04764184T priority patent/DK1658393T3/da
Priority to JP2006524288A priority patent/JP2007503527A/ja
Priority to EP04764184A priority patent/EP1658393B1/de
Priority to AT04764184T priority patent/ATE398195T1/de
Priority to DE502004007361T priority patent/DE502004007361D1/de
Priority to US10/569,658 priority patent/US20070114132A1/en
Publication of EP1510600A1 publication Critical patent/EP1510600A1/de
Withdrawn legal-status Critical Current

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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
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • 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
    • C25D17/02—Tanks; Installations therefor
    • 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
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/42—Electroplating: Baths therefor from solutions of light metals

Definitions

  • the invention relates to an apparatus and a method for depositing of metals and / or metal alloys of organometallic Electrolytes, in particular of organometallic complex salts in organic solvents, on products, with at least one Coating section for coating the products, at least one another processing section and at least one lock chamber for Injecting and discharging the products into and out of the device in the Essentially without the penetration of oxygen and / or moisture.
  • a galvanic deposition of aluminum, magnesium and their Alloys are due to the very low potential of these elements not, as usual in classical electroplating, from aqueous Systems possible.
  • aluminum, magnesium and their alloys deposited non-aqueous systems only the deposition could from aluminum or magnesium alkyl-containing complexes in the technical Enforce scale.
  • Metal alkyls are known to react very violently with oxygen and water to form reaction products, such as Alkoxy compounds or aluminoxanes. These reaction products are not more capable of further complexes with those in electrolyte formulas to form alkali metals or alkali metal halides used. she remain as soluble impurities in the electrolyte and put back while the electrical conductivity of this down. Also will the maximum applicable current density with increasing concentration of these Reaction products reduced, whereby the coating process its Profitability and possibly its good quality loses.
  • DE 41 18 416 A1 discloses a device for coating preferably known relatively thin-sized parts, in which a Coating by placing the parts in juxtaposed Container takes place.
  • the containers or baths are in one Inert gas atmosphere.
  • When arranging the different baths in one common containers are designed as partitions locks provided that are penetrated by the parts to be treated can. For this purpose is in a penetration area by a pair sealing against each other running around an axis of rotating rollers elastic material facing the adjacent walls of the Sealing container sealed, formed the penetrable partition.
  • the present invention is therefore based on the object, a Apparatus and method for depositing metals and / or To create metal alloys from organometallic electrolytes, at which no longer encounter any safety-related problems Solvent emission out of the device and in particular a Reaction of used electrolyte systems with oxygen and Moisture from the ambient atmosphere of the device substantially completely avoided.
  • the object is for a device according to the preamble of the claim 1 achieved in that at least one Siphon Why tastes with a Separating device for gas-related delimitation of the other sections of the Device of or sealing these other sections from the Coating section and at least one substantially the Coating section, the at least one Siphon Why tastes, the at least one further processing section substantially tight enclosing provided with an inert gas floodable hood part.
  • the object solved by a substantially solvent loss Introducing the products through at least one lock chamber into one Device for depositing metals and / or metal alloys is provided, the products to at least one coating section Essentially under gas seal, the products are delivered in the at least one coating section to be coated, the coated products from the coating section over at least a Siphonêtleaned at least one Ausbowabêt in Substantially be passed under gas seal, and the finished Products discharged via at least one other lock chamber be, with over all sections of the device a InertgasatmosphDCglocke is kept. Further developments of Invention are defined in the dependent claims.
  • a slight overpressure to the atmosphere, which the Device surrounds maintains and monitors this.
  • Prefers is at least one pressure-maintaining device for maintaining a constant pressure in the hood part and / or such a small Overpressure in the hood part opposite the outside and / or Ambient atmosphere provided. An involuntary intrusion of Outside atmosphere in the device and thus contamination of the Gas atmosphere within the device can thus essentially be avoided.
  • a in Maintaining substantially constant pressure, so in particular a slight overpressure relative to the outside atmosphere of Device is preferably at least one gas buffer device provided and with this / these, especially in the first and / or last section connectable or connected.
  • Gas buffer devices are thus preferred at the input and output of Device provided because there pressure fluctuations due to Infiltration and removal of the products may occur.
  • the Gas buffer devices are filled as soon as one outside one Presettable tolerance lying overpressure in hood section occurs and deflates when outside an adjustable tolerance lying negative pressure in the hood section occurs, for.
  • Gas atmosphere is taken from the respective hood section, as for example, for flooding a lock chamber with inert gas.
  • At least one oxygen monitoring device is in the at least one lock chamber and / or the sections of the hood part intended. Also preferred is at least one device for Monitoring the solvent concentration in the lock chamber (s) intended. This makes it possible to constantly oxygen and / or Solvent content of the gas atmosphere in the individual sections of the Monitor device. Because the lock chamber (s) for holding a Air or oxygen entry into the device, is after the Injecting products, removing the product with it introduced air and rinsing the chamber with z. B. inert gas of Oxygen content of the lock chamber atmosphere monitored regularly.
  • the should Oxygen content within the chamber should be zero, so that a Ingress of oxygen into the hood part as well as the remaining parts of the hood Device can be avoided.
  • the discharge of solvent from the Device should also be reduced as possible to zero.
  • To the Solvent content in the lock chambers, which is a compound of Represent device to the outside atmosphere to be able to monitor are There also facilities for monitoring the solvent concentration intended.
  • the oxygen and / or solvent content a predeterminable and / or adjustable or set threshold value may exceed, an adjustment of the pumping times for the entry and exit of gas in / out of the lock chamber and / or an additional Rinsing phase with an inert gas during pump cycles to reduce the Oxygen content triggered in the at least one lock chamber become. It is then for example a longer pumping cycle for Pumping out the contaminated gas atmosphere provided.
  • the InertgasatmosphDCglocke the device can in terms of their Oxygen content to be monitored, with the oxygen content as possible Should be zero. Through these measures can be optimally ensured be that the inert gas atmosphere of the device little or even not contaminated with oxygen, being optimal Coating results and a very high level of safety during the Treatment of the products can be achieved.
  • At least one cleaning and / or activation section is preferred for cleaning and / or pretreating the surface of the products and / or at least one export section for discharging the products from the Device provided.
  • the at least one Cleaning and / or activation section one or more Lockable treatment tank with a cleaning fluid for Cleaning the products to be coated and / or one Activation fluid for activating the surface thereof or for Generating a primer layer on.
  • a cleaning and / or Activation section is advantageous to a cleaning of Crude products possible, with an oxide-free and bright surface on the Products can be produced. This can be an optimal Adhesive strength can be ensured for the subsequent coating.
  • a primer layer on the Surface of the product are applied.
  • the at least one cleaning and / or activation section at least one at least one treatment tank downstream rinsing device for rinsing the pretreated products and preventing carryover of chemicals from the cleaning and / or Activation section on.
  • a Siphon flushing device following the cleaning and / or Activation section that is before the coating section, it is makes sense to provide such a rinse the pretreated products to a carryover of the chemicals from the cleaning and Activation stage in the siphon flushing device and thus in below to prevent the coating electrolyte.
  • one is Provided solvent treatment and / or regeneration device and connected to such a flushing device.
  • the purified Solvent is in particular again in this flushing device recycled, whereas the purified cleaning liquid or Aktivleitersoder located in the upstream treatment tank other liquid back into these treatment tanks can be returned.
  • For cleaning is preferably a Distillation and subsequent provision of the purified Solvent provided.
  • the at least one solvent treatment and / or Regeneration device for the cleaning and / or activation section provided in the bypass to this. This is during the Coating or already during the pre-cleaning and also the Aftertreatment step a permanent purification of the solvent and the electrolyte or other cleaning and bath liquids possible.
  • At least one lock chamber with a Solvent separation and return device and / or a vapor recovery system connectable or connected.
  • At least one is preferred Lock chamber at the entrance of the cleaning and / or activation section and / or at least one lock chamber at the exit of the Exhaust section provided.
  • Preference is given to the introduction step the products introduced into the at least one lock chamber, while the Lock chamber filled with external atmosphere, closed and then evacuated, so the outside atmosphere from the chamber and subsequently flooded with inert gas.
  • the Products are then in Einschleus Colour in a first Treatment section of the device introduced.
  • At the discharge step From the device, these products from the hood atmosphere in the lock chamber introduced, this closed and hood atmosphere pumped out of the lock chamber and into the hood section recycled.
  • the lock chamber can subsequently open and the Products are removed. Subsequently, the lock chamber is again closed, the penetrated outside atmosphere dissipated and the chamber flooded with inert gas.
  • inert gas particularly preferred is the pumped Schleusenatmosphot treated, with dry inert gas and purified solvent can be recycled to the process, in particular dry inert gas in the inert gas atmosphere bell and purified Solvent in a treatment tank. So the gas swing system includes the pumping of dried inert gas in the hood atmosphere after Pumping out the atmosphere of the lock chamber from the lock chamber.
  • the inert gas atmosphere bell is cleaned, in particular by condensing the inert gas atmosphere and recycling the condensed solvent components into the respective circuits, especially treatment tanks.
  • at least one Cooling device with Kondensatabscheide noticed for the recovery of entrained and / or evaporated solvent residues provided, in particular in the hood part and / or coating section and / or connected to the at least one lock chamber.
  • the respective cooling devices are in the individual Hood sections provided as the evaporating liquids in These individual hood sections are usually different in each case, so that the impurities in the gas atmosphere are also different are. Therefore, there is advantageously a return within the respective hood section.
  • the at least one coating section at least a for preventing uncontrolled evaporation of solvent in the hood part closable coating basin.
  • the at least one Coating section have at least one Ausbow Kunststoff Kunststoff.
  • the Siphon Press drove for separating the individual sections of Device, so in particular the cleaning and / or Activation section, the coating section and the export section is provided, it proves to be advantageous in the Substantially unreactive solvent in these transition areas provided.
  • the at least one siphon purging device is therefore preferred filled with an inert solvent. This can cause unwanted chemical reactions between incompatible chemicals essentially avoided from the individual sections of the device become.
  • the at least one siphon purging device comprises a closable Doppelteil adopted with an attached Divider wall oriented so that top hood sections be divided.
  • the in the rinsing bath of the siphon rinsing device dips can be a gas-tight Separation of various hood sections of the device be created.
  • the transport device below the liquid level is positioned. This is a complete immersion ensures the products in the rinse liquid, making this with the preferably rinsed and rinsed washing liquid can cause a carryover of chemicals and / or gas atmosphere a preliminary section in the subsequent section of the device avoid.
  • the electrolyte-solvent separator (s) comprise / include a distiller for distilling off solvent from the discharged from the at least one coating tank Electrolytic solvent bath liquid.
  • they are preferable Means for recycling the recovered clean solvent into the export sink and / or facilities for returning the Electrolytes provided in the electrolyte circuit.
  • Electrolyte fluid and / or solvents are preferably used in the Mainly closed circuits. This will be a Contamination of the remaining baths of the device substantially avoided.
  • the purification or treatment of Electrolyte fluid and / or solvent and / or a rinsing fluid for avoiding carryover of chemicals.
  • electrolyte fluid and / or cleaning fluid and / or activating fluid also preferred rinses in the various rinsing devices intended.
  • These rinsing devices can be used in different places Device and the coating process are provided in particular in the exit region of respective sections of the device.
  • the figure shows a schematic diagram as an overall view of a device. 1 for depositing metals and / or metal alloys.
  • the device has a cleaning and / or activation section 2, a Coating section 3 and an export section 4 on. Furthermore it has a hood part 5, all three aforementioned sections in Essentially tightly encloses.
  • the hood part is divided into three sections 50, 51, 52 divided.
  • the three hood sections are by respective ones Partitions 53, 54 delimited against each other.
  • the cleaning and / or activation section 2 comprises a first Lock chamber 20, a first treatment tank 21, a second Treatment tank 22 and a sink 23. Also includes the Cleaning and / or activation section a part of a first Siphon purging 60.
  • the Siphon Vietnamese Republic 60 is through the Partition 53 divided into two parts, so that they have a Doppel Vietnamese styles formed by the section 2 and the section 3 is accessible, but otherwise forms a diffusion barrier. All Basins or flushing devices are with respective covers 24, 25, 26, 27, 62 closable.
  • the lock chamber 20 has a lock door 28 on, which allows a retraction of products in the lock chamber. Preferably, such products are transported by a trolley which is in the figure is not shown, retracted into the lock chamber.
  • the lock chamber 20 is provided with a means 70 for recovery of solvent and a vapor recovery system 80.
  • the device for the recovery of solvent a cold trap 71, a valve 72, a Kondensatabscheide responded 73 and a line 74 between the Valve 72 and the lock chamber 20, a line 75 between the Cold trap 71 and the Kondensatabscheide responded 73 and a Solvent return line 76 between the Kondensatabscheide responded 73 and the first treatment tank 21.
  • the gas swing system 80 comprises a vacuum pump 81, three valves 82, 83, 84 and a line 85 between the lock chamber 20 and the first Valve 82, another line 86 between the valve 82 and the Vacuum pump 81, a line 87 between the vacuum pump 81 and the Valve 83 in the return line to the hood part and another Line 88 between the valve 83 and the hood part 50.
  • the line 87 also leads to the valve 84 and from this another line 89 after outside into the outside atmosphere. Through this, air can escape from the device be blown out.
  • the solvent treatment and / or Regeneration device comprises a distillation device 91 and a Condensate collection tank 92.
  • the distiller is via a conduit 93, which comes from the sink 23, fed.
  • a line 94 is provided between the Distiller 91 and the condensate collection tank 92.
  • the in the distiller 91st purified cleaning liquid is via a line 95, a Pump 96 and another line 97 into the second treatment tank 22nd recycled. Clean distilled off by the distiller Solvent may be removed from the condensate collection tank 92 via a conduit 98, a pump 99 and a line 100 pumped back to the sink 23 become.
  • an overflow line 29 is provided, if necessary in excess returned to the solvent overflow the sink avoid. The excess solvent is then passed over the Overflow line 29 returned to the second treatment tank 22.
  • the hood section 50 of the cleaning and / or activation section 2 also comprises a transport device 55 for moving Products 7 between the individual treatment, rinsing and other Pool.
  • the transport device has a carriage 56, which is provided in this embodiment with a hook 57 to Attaching the products to be coated 7.
  • the hook 57 is included retractable attached to the carriage 56, so that the products on this Hook slowly into the respective baths let in and out of these can be lifted out.
  • the hood portion 50 also includes a cooling device 58. These is shown in the figure in the form of a cooling coil. About these Cooling coil can be condensed and condensed in evaporated solvent a collecting device 59 likewise provided in the hood section 50 collect or be caught in it. In the figure is the Tray shown in the form of a gutter. That in the Gutter or catcher 59 collected solvent condensate can via a drain line 101 to the first treatment tank 21st to be led back. Thus, solvent recycling can occur both in the first as well as in the second treatment tank done. It can In principle, even more treatment tanks are provided, the Figure is here only one possible embodiment again. Also is it is possible to provide several sinks; it would be the same in principle possible to provide more than one lock chamber.
  • a gas buffer container 120 outside of the hood part. 5 intended.
  • the gas buffer container 120 is connected via a line 121 with the Interior of the hood portion 50 connected.
  • This line 121 can a two-sided exchange of gas between the gas buffer tank and take the hood section 50. This makes it possible to have a preset overpressure, especially a constant pressure within of the hood section to maintain.
  • a first oxygen sensor 122 in FIG Area of the hood portion 50 a second oxygen sensor 123 and a solvent concentration sensor 124 at the lock chamber 20 intended. All sensors can be equipped with a monitoring and Control device (not shown in the figure) to be connected monitor exceeding of set thresholds and, if necessary, Discharge cycles of the lock chamber and a gas exchange targeted adapt.
  • the coating section 3 comprises the second part of Siphon Kirnd Road 60, which, as mentioned above, as Double flushing device is formed.
  • a transport device 66 provided, in particular, may have a carriage, as shown in the figure is shown.
  • a lid 63 of Siphon purging 60 can after transport through the Siphon rinsing the products on the side of the Coating section 3 are removed again.
  • the Coating section 3 also has two coating tanks 30, 31 on, as well as an export sink 32 and a first part of another Siphon flushing device 61.
  • Each of these basins is provided with a cover 33, 34, 35 and the Siphon Why adopted with a lid 64 on the side the coating section provided.
  • a lid 64 on the side the coating section provided.
  • each cooling coils 36, 37 and gutters 38, 39 provided to solvent, which in the Coating evaporates from the electrolyte, condense and in particular after the coating tank in the rinse 32 to initiate.
  • the coating section 3 is provided with a purification device following the coating basin provided to the electrolyte in the Bypass in an electrolyte-solvent separator 110 purify. This ensures that no significant Quantities of electrolyte are trailed, creating a largely closed material cycle can be generated.
  • the electrolyte becomes liquid from the two coating tanks 30, 31 via lines 111 to a distiller 112 out.
  • a condensate collection tank 113 is provided, which has a Line 114 is connected to the distillation device 112. Of the Purified electrolyte is added via lines 115, 117 and a pump 116 the coating tank 30 returned.
  • the cleaning and / or activation section 2 also has the Coating section 3, a transport device 55 with a Trolley 56 and a hook 57 to the product to be coated. 7 between the individual basins of the coating section transport to be able to.
  • a cooling device 58 in the form of a cooling coil and a gutter as a catcher 59 for condensed solvent provided.
  • a drain line 104 is the collected condensed solvent to the first coating tank 30 returned.
  • the export section 4 comprises the second part of the siphon purging device 61 on. This is, as well as the Siphon réelle Road 60, with a Transport device 67 provided. Over this are the through the lid 64 introduced into the siphon rinsing products to those on the the other side of the partition wall 54 located portion with lid 65 of the Siphon purging 61 transported. The transport takes place, as well as in the rinsing device 60, below the surface of which is in the Siphon rinsing located flushing liquid. This will be an im Substantial complete gas closure during the transport of the products of allows the coating section in the export section.
  • the export section also includes a second lock chamber 40 Discharging the coated products from the device.
  • the Lock chamber is provided with a lid 41. Besides, she points a lock door 42. Similar to the lock chamber 20 is also the lock chamber 40 with a device 130 for the recovery of Solvent and a gas swing system 140 provided.
  • the device for Recovery of solvent is also provided with a cold trap 131, a valve 132 between lock chamber 40 and cold trap 131, a Kondensatabscheide observed 133, a line 134 between valve 132nd and lock chamber 40, a line 135 between Kondensatabscheide observed 133 and cold trap 131 and a Solvent return line 136 between Kondensatabscheide disturbed 133th and Siphon Congress adopted 61 provided.
  • the gas swing system 140 includes a vacuum pump 141, three valves 142, 143, 144 and several lines in between.
  • a first Line 145 leads from the lock chamber 40 to the first valve 142
  • a second conduit 146 leads from the valve 142 to the pump 141. Zu This also leads a line from the cold trap 131, as in the Case of the device 70 between the cold trap 71 and the vacuum pump 81 is the case.
  • a line 147 leads to the valve 143 and from this a return line 148 to the hood portion 52nd From the vacuum pump, the line 147 also leads to the valve 144, in particular air from the lock chamber 40 via a Line 149 can be blown outward into the environment.
  • the hood portion 52 also includes a transport 55 with a trolley 56 having a hook 57 to products 7th and be able to lower into the individual pelvis.
  • Cooling coils 58 as a cooling device and a gutter 59 for Condensed solvent provided by the gutter on a Drain line 105 are returned to the Siphon Jardin Marie adopted 61 can.
  • the Ausbowabites 4 is connected to a gas buffer tank 125 and a conduit 126 between the interior of the hood portion 52 and the Gas buffer container 125 provided. This can be ensured that within the export section, as constant a gas pressure as possible is maintained, although z. B. by returning dried Inert gas via the line 145 an overpressure in the hood section of the Exhaust section could occur, as well as a negative pressure in floods the lock chamber 40 with hood atmosphere from the export section after pumping out of external atmosphere following a Removal process finished products from the lock chamber 40th
  • first and second oxygen sensors 127, 128 and a solvent concentration sensor 129 are provided.
  • the first oxygen sensor 127 is in the upper hood section 52
  • the second Oxygen sensor 128 and solvent concentration sensor 129 are on the lock chamber 40 is provided.
  • the hood section 51 above the Coating section 3 is provided with such an oxygen sensor 150 Mistake.
  • a product to be coated is on the lock door 28 in the first Lock chamber 20 introduced. This is done in particular via a Dolly, which is not shown in the figure.
  • the lock chamber Outside atmosphere air
  • the valve 82 is opened. As in the lock chamber then Only not contaminated air, this can directly over the Line 89 and the open valve 84 are discharged to the outside.
  • the lock chamber with inert gas from the Hood section 50 flooded.
  • the inner lid 24, the is arranged between the lock chamber and the hood section 50, opened and the product in the inert gas atmosphere within the Hood portion 50 are introduced.
  • the amount of oxygen in the first hood section 50 can penetrate, is very low, since the Lock chamber up to a final pressure of less than 1 to 2 mbar It can be evacuated and it is also possible that Intermediate rinsing with inert gas, in particular nitrogen or argon, be made.
  • the amount of gas required for the flooding of the lock chamber, from the Gas atmosphere of the hood section 50 would be removed without Providing the gas buffer container is expected to decrease the Guide pressure in the hood section.
  • a constant flow of inert gas, such as nitrogen, must be introduced into the hood section, in which then again oxygen and water traces can be, is the Gas buffer container 120 connected to the hood portion 50, the Pressure in the hood portion 50 due to the possible volume change essentially constant.
  • the Solvent concentration is via the solvent concentration sensor 124 supervised.
  • the control of oxygen diffusion into the plant is in particular with regard to the life of the electrolyte and the Coating quality useful, but also in terms of general procedural and operational safety of the entire system.
  • the lid 24 can be closed again and the Locked atmosphere can be pumped off, wherein an inert gas-solvent mixture is present in the lock atmosphere and pumped out becomes. This is done after opening the valve 72 via the line 74, wherein the solvent-inert gas mixture is passed through the cold trap 71. To the condensation, the obtained dried inert gas over the Vacuum pump 81, the line 87 and the then opened valve 83 and the conduit 88 is returned to the hood portion 50. The inert gas as a purified gas back to the atmosphere in the hood section 50th to provide. The excess gas volume is through Volume increase in the gas buffer container 120 collected, causing the Pressure in the hood portion 50 are kept substantially constant can.
  • the resulting condensed solvent is introduced via the line 75 in the Kondensatabscheide Rhein 73 introduced and can in particular recurring periodically the first treatment tank 21 via the Solvent return line 76 are supplied. Subsequently, the evacuated lock chamber again flooded with fresh inert gas and the Door to the outside atmosphere, namely the lock door 28, can again be opened to introduce new products into the device.
  • the products in the Treatment tank 21, 22, in particular a cleaning fluid contained, incorporated and pre-cleaned there and in particular a bare oxide-free surface can be generated on these to optimum To ensure adhesion during the subsequent coating.
  • a primer layer can be found in this basin be applied.
  • the lid 25, 26 are provided, as well as the lid 27 on Sinks, which are preferably opened only when goods or products are introduced and deployed.
  • the downstream Sink 23 serves a carryover of chemicals from the Treatment tank 21, 22 in the Siphonêt Road 60 to avoid wherein the carryover into the coating electrolyte in the Basin in the coating section should be avoided.
  • the liquid the sink 23 is regularly on the solvent processing and / or Regeneration device 90, which bypasses the cleaning and / or Activation section is switched, processed.
  • the partition 53 are the two top hood sections 50 and 51 gas-tight separated from each other, through the double sink of the Siphon purging device 60 but still together to pass through Connected products.
  • the liquid is in the Siphon Surprise Roaden identical to that in the coating electrolyte used solvents. To get a reaction with cleaning fluid and / or coating electrolyte as possible to avoid preferably an inert solvent is used.
  • the lid 63 of the Siphon purging device 60 After lifting the products through the lid 63 of the Siphon purging device 60 enter this in the coating section. 3 and can be elevated into the coating tanks 30, 31 therein. In addition to the two coating tanks shown in the figure many more are planned, as well as others Export sink 32, wherein in the figure, only one of them is shown. To prevent uncontrolled evaporation of solvents in to avoid the top hood portion 51 are in Normal operation, the lid 63, 33, 34, 35, 64 closed. Preferably The lids are only opened to retract or remove Products from the individual pools.
  • the second lock chamber 40th provided, in which the coated product is introduced. This via the lid 41.
  • the lock chamber with the finished coated product is also an Abpumpvorgang initiated. This is the recovery of possibly still the coated product adhering solvent residues. This is it possible that the completely coated product dry the Device leaves and essentially no solvent emissions occur. All evaporated during the pumping process and in the Cold trap 131 recondensed and in the Kondensatabscheide adopted 133 collected solvent is added via the line 136 in the Siphon purging 61 returned. Otherwise, the running Ausschleusvorgang according to the Einschleusevorgang in terms of Pumping in and out of sluice atmosphere and inert gas. To the Outward, while the lock door 42 is opened.
  • the individual hood sections 50, 51, 52 are flooded with inert gas and at least in the present embodiment via a automatic pressure maintenance system constantly at a low overpressure held against the ambient atmosphere. This will be a Ingress of air into the hood part avoided.
  • the oxygen sensors 122, 123, 127, 128, 150 continuously give the oxygen content in the respective gas atmosphere. In case of a detected exceeding of preset thresholds will be with respect to the pumps 81, 141 a Adjustment of the pumping time made or an additional flushing with Inert gas during the pumping cycle in the lock chambers 20, 40th initiated.
  • a barrier liquid in particular inert Solvent filled siphon flushing equipment provides another Increasing the barrier effect in this area, especially in combination with the covers 62, 63 and 64, 65, thereby further reducing the Diffusion of oxygen and moisture in the coating section 3 can be made into it.
  • the combination of lock chambers, a vacuum system, a vapor recovery system and the Siphon flushing devices ensures a very long service life organometallic coating electrolytes and a consistent Coating quality, since the formation of undesirable Reaction products such as alkoxy compounds or Aluminoxanes are effectively contained or substantially prevented can.
  • the cleaning and / or Activation section it is also possible the cleaning and / or Activation section to make smaller or possibly even complete to be dropped.
  • the devices have a closed hood atmosphere, which is a substantially dense Bell over the individual stations of the coating device forms, at the same time a constant purification of both the atmosphere and the treatment or coating baths and rinsing baths takes place. This can be done especially easily by guiding the cleaning sections in the Bypass to the respective processing or treatment sections respectively. Alternatively, more complex purification steps or cycles possible.

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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)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Cleaning By Liquid Or Steam (AREA)
  • Chemical Vapour Deposition (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
EP03019235A 2003-08-26 2003-08-26 Verfahren und Vorrichtung zum Abscheiden von Metallen und Metalllegierungen aus Metallorganischen Elektrolyten Withdrawn EP1510600A1 (de)

Priority Applications (8)

Application Number Priority Date Filing Date Title
EP03019235A EP1510600A1 (de) 2003-08-26 2003-08-26 Verfahren und Vorrichtung zum Abscheiden von Metallen und Metalllegierungen aus Metallorganischen Elektrolyten
PCT/EP2004/009192 WO2005021840A1 (de) 2003-08-26 2004-08-17 Vorrichtung und verfahren zum abscheiden von metallen und/oder metalllegierungen aus metallorganischen elektrolyten
DK04764184T DK1658393T3 (da) 2003-08-26 2004-08-17 Anordning og fremgangsmåde til at adskille metaller og/eller metallegeringer fra metalorganiske elektrolytter
JP2006524288A JP2007503527A (ja) 2003-08-26 2004-08-17 金属有機電解液から金属及び／又は金属合金を沈積する装置及び／又は方法
EP04764184A EP1658393B1 (de) 2003-08-26 2004-08-17 Vorrichtung und verfahren zum abscheiden von metallen und/oder metalllegierungen aus metallorganischen elektrolyten
AT04764184T ATE398195T1 (de) 2003-08-26 2004-08-17 Vorrichtung und verfahren zum abscheiden von metallen und/oder metalllegierungen aus metallorganischen elektrolyten
DE502004007361T DE502004007361D1 (de) 2003-08-26 2004-08-17 Vorrichtung und verfahren zum abscheiden von metallen und/oder metalllegierungen aus metallorganischen elektrolyten
US10/569,658 US20070114132A1 (en) 2003-08-26 2004-08-17 Device and method for separating metals and/or metal alloys from metallo-organic electrolytes

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP03019235A EP1510600A1 (de) 2003-08-26 2003-08-26 Verfahren und Vorrichtung zum Abscheiden von Metallen und Metalllegierungen aus Metallorganischen Elektrolyten

Publications (1)

Publication Number Publication Date
EP1510600A1 true EP1510600A1 (de) 2005-03-02

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EP03019235A Withdrawn EP1510600A1 (de) 2003-08-26 2003-08-26 Verfahren und Vorrichtung zum Abscheiden von Metallen und Metalllegierungen aus Metallorganischen Elektrolyten
EP04764184A Expired - Lifetime EP1658393B1 (de) 2003-08-26 2004-08-17 Vorrichtung und verfahren zum abscheiden von metallen und/oder metalllegierungen aus metallorganischen elektrolyten

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EP04764184A Expired - Lifetime EP1658393B1 (de) 2003-08-26 2004-08-17 Vorrichtung und verfahren zum abscheiden von metallen und/oder metalllegierungen aus metallorganischen elektrolyten

Country Status (7)

Country Link
US (1) US20070114132A1 (ko)
EP (2) EP1510600A1 (ko)
JP (1) JP2007503527A (ko)
AT (1) ATE398195T1 (ko)
DE (1) DE502004007361D1 (ko)
DK (1) DK1658393T3 (ko)
WO (1) WO2005021840A1 (ko)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006002969A3 (en) * 2004-07-01 2007-03-22 Atotech Deutschland Gmbh Device and method for chemically and electrolytically treating work pieces
CN103938238A (zh) * 2014-05-11 2014-07-23 山东建筑大学 一种钢带连续镀铜ⅲ
CN103938239A (zh) * 2014-05-11 2014-07-23 山东建筑大学 一种钢带连续镀铜ⅰ

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4363712A (en) * 1980-11-28 1982-12-14 Siemens Aktiengesellschaft Device for galvanic precipitation of aluminum
US4425211A (en) * 1981-08-21 1984-01-10 Siemens Aktiengesellschaft Device for electrodeposition of aluminum
US4435265A (en) * 1982-08-26 1984-03-06 Siemens Aktiengesellschaft Device for electro-deposition of aluminum
US4759831A (en) * 1986-07-04 1988-07-26 Siemens Aktiengesellschaft Electroplating apparatus particularly for electro-deposition of aluminum

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3133232A1 (de) * 1981-08-21 1983-03-10 Siemens AG, 1000 Berlin und 8000 München Vorrichtung zum galvanischen abscheiden von aluminium

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4363712A (en) * 1980-11-28 1982-12-14 Siemens Aktiengesellschaft Device for galvanic precipitation of aluminum
US4425211A (en) * 1981-08-21 1984-01-10 Siemens Aktiengesellschaft Device for electrodeposition of aluminum
US4435265A (en) * 1982-08-26 1984-03-06 Siemens Aktiengesellschaft Device for electro-deposition of aluminum
US4759831A (en) * 1986-07-04 1988-07-26 Siemens Aktiengesellschaft Electroplating apparatus particularly for electro-deposition of aluminum

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006002969A3 (en) * 2004-07-01 2007-03-22 Atotech Deutschland Gmbh Device and method for chemically and electrolytically treating work pieces
US8656858B2 (en) 2004-07-01 2014-02-25 Atotech Deutschland Gmbh Device and method for chemically and electrolytically treating work pieces using a conveyor system to transport work pieces between treatment tanks
CN103938238A (zh) * 2014-05-11 2014-07-23 山东建筑大学 一种钢带连续镀铜ⅲ
CN103938239A (zh) * 2014-05-11 2014-07-23 山东建筑大学 一种钢带连续镀铜ⅰ

Also Published As

Publication number Publication date
DE502004007361D1 (de) 2008-07-24
DK1658393T3 (da) 2008-10-20
WO2005021840A1 (de) 2005-03-10
ATE398195T1 (de) 2008-07-15
EP1658393A1 (de) 2006-05-24
JP2007503527A (ja) 2007-02-22
US20070114132A1 (en) 2007-05-24
EP1658393B1 (de) 2008-06-11

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