WO2005021840A1 - Vorrichtung und verfahren zum abscheiden von metallen und/oder metalllegierungen aus metallorganischen elektrolyten - Google Patents
Vorrichtung und verfahren zum abscheiden von metallen und/oder metalllegierungen aus metallorganischen elektrolyten Download PDFInfo
- Publication number
- WO2005021840A1 WO2005021840A1 PCT/EP2004/009192 EP2004009192W WO2005021840A1 WO 2005021840 A1 WO2005021840 A1 WO 2005021840A1 EP 2004009192 W EP2004009192 W EP 2004009192W WO 2005021840 A1 WO2005021840 A1 WO 2005021840A1
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- WIPO (PCT)
- Prior art keywords
- solvent
- products
- section
- coating
- lock chamber
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 30
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 14
- 239000002184 metal Substances 0.000 title claims abstract description 14
- 150000002739 metals Chemical class 0.000 title claims abstract description 13
- 229910001092 metal group alloy Inorganic materials 0.000 title claims abstract description 11
- 239000005486 organic electrolyte Substances 0.000 title abstract description 3
- 239000002904 solvent Substances 0.000 claims abstract description 138
- 238000000576 coating method Methods 0.000 claims abstract description 114
- 239000011248 coating agent Substances 0.000 claims abstract description 110
- 239000007789 gas Substances 0.000 claims abstract description 68
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000001301 oxygen Substances 0.000 claims abstract description 51
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 51
- 239000011261 inert gas Substances 0.000 claims abstract description 43
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 238000000151 deposition Methods 0.000 claims abstract description 12
- 238000007789 sealing Methods 0.000 claims abstract description 7
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 239000003792 electrolyte Substances 0.000 claims description 53
- 238000004140 cleaning Methods 0.000 claims description 52
- 239000007788 liquid Substances 0.000 claims description 45
- 230000004913 activation Effects 0.000 claims description 34
- 238000011010 flushing procedure Methods 0.000 claims description 34
- 238000001816 cooling Methods 0.000 claims description 23
- 230000008569 process Effects 0.000 claims description 14
- 238000005086 pumping Methods 0.000 claims description 14
- 238000005192 partition Methods 0.000 claims description 13
- 230000008929 regeneration Effects 0.000 claims description 11
- 238000011069 regeneration method Methods 0.000 claims description 11
- 125000002524 organometallic group Chemical group 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 7
- 238000000746 purification Methods 0.000 claims description 7
- 230000008020 evaporation Effects 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000002318 adhesion promoter Substances 0.000 claims description 4
- 239000012442 inert solvent Substances 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 238000012806 monitoring device Methods 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000000047 product Substances 0.000 description 72
- 230000032258 transport Effects 0.000 description 20
- 239000003570 air Substances 0.000 description 9
- 238000011084 recovery Methods 0.000 description 7
- 239000007795 chemical reaction product Substances 0.000 description 6
- 230000035515 penetration Effects 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000011109 contamination Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000010926 purge Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000008151 electrolyte solution Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 125000003545 alkoxy group Chemical group 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
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- 230000000149 penetrating effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910001508 alkali metal halide Inorganic materials 0.000 description 1
- 150000008045 alkali metal halides Chemical class 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 239000013013 elastic material Substances 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000008570 general process Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
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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
- 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 a device and a method for depositing metals and / or metal alloys from organometallic electrolytes, in particular from organometallic complex salts in organic solvents, on products, with at least one coating section for coating the products, at least one further processing section and at least one lock chamber for one - and discharge of the products into and out of the device essentially without the penetration of oxygen and / or moisture.
- the metal alkyls used in the production of the individual electrolyte variants are known to react very violently with oxygen and water to form reaction products, such as, for example, alkoxy compounds or aluminum inoxanes. These reaction products are no longer able to form further complexes with the alkali metals or alkali metal halides used in electrolyte formulas. They remain in the electrolyte as soluble impurities and settle thereby reducing the electrical conductivity from it. The maximum applicable current density is also reduced with increasing concentration of these reaction products, as a result of which the coating process loses its economic viability and possibly its good quality.
- Various coating systems are known in the prior art, some of which also contain approaches to prevent oxygen and / or moisture from penetrating into parts of the coating system.
- Such a system in which an electrolytic coating of metallic or non-metallic continuous products with metals or alloys is provided in a continuous process from aprotic water and oxygen-free electrolytes, is described in DE 197 16 493 C2.
- rinsing and drying processes are connected to remove the residues from aqueous solutions.
- an exit of the coated continuous product from the system via a lock system is provided.
- the lock chamber has a middle chamber with a barrier liquid, which is a lock for represents the air contained in an outer chamber.
- a third chamber contains an inert gas.
- regeneration circuits are provided in which all liquids used are processed, cleaned and recycled in a recycle process.
- DE 30 23 827 C2 discloses a tubular cell which is sealed off from the outside and through which the cathodically contacted material to be treated can be moved in the axial direction, in particular continuously, along anodes.
- a protective gas can be applied to the tubular cell in order to prevent both the undesired escape of the electrolyte from the tubular cell and the penetration of air atmosphere into it.
- a lock arrangement comprising a plurality of chambers is also provided, into which inert gas and / or an inert liquid can be introduced as a sealing medium for mutual sealing of the individual chambers.
- these parts are introduced into a container filled with electrolyte solution or into a rotating basket, which is continuously rotated during the treatment and thus repositioned the parts.
- the container is sealed gas-tight.
- the parts in the basket are handled without any reloading. Only the respective liquids or solutions are pumped into and out of the container. To dry, the container is centrifuged and the remnants of the electrolyte solution are thrown off by driving the basket. Due to its design, this system is not suitable for a separator made of organometallic electrolytes.
- a device for coating preferably relatively thinly dimensioned parts in which a coating by placing the parts in side by side Container is done.
- the containers or baths are in an inert gas atmosphere.
- a rinsing bath, an etching bath and a deposition bath are also provided.
- locks designed as partitions are provided, which can be penetrated by the parts to be treated.
- the penetrable partition wall is formed by a pair of rollers made of elastic material rotating against one another and sealingly sliding against the adjacent walls of the container.
- the present invention is therefore based on the object of providing a device and a method for depositing metals and / or metal alloys from organometallic electrolytes in which safety-related problems no longer occur, solvent emission from the device and in particular a reaction of the electrolyte systems used Oxygen and moisture from the ambient atmosphere of the device can be substantially completely avoided.
- the object is achieved for a device according to the preamble of claim 1 in that at least one siphon flushing device with a separating device for gas-related delimitation of the other sections of the device from or sealing these other sections with respect to the coating section and at least one essentially the coating section, the at least one Siphon flushing device, the at least one further processing section are provided which are essentially tightly enclosing a hood part which is floodable with an inert gas.
- the object is achieved in that an essentially solvent-free introduction of the products through at least one lock chamber into a device for separating metals and / or metal alloys is provided, the products essentially on at least one coating section are handed over under gas exclusion, the products are coated in at least one coating section, the coated products are transferred from the coating section via at least one sponge flushing device to at least one export section essentially with gas exclusion, and the finished products are discharged via at least one further lock chamber, all of them Sections of the device an inert gas atmosphere bell is held.
- the gas atmosphere in the essentially tightly closed hood part which encloses the individual sections of the device, can be optimally adjusted in each section of the device. This also makes it possible to prevent migration of solvents via the gas atmosphere into the electrolyte area. Since it frequently happens that the coating electrolyte is chemically incompatible with cleaning liquids or other solvents, this separation of the gas atmospheres of the individual sections of the device has proven to be particularly advantageous. This enables safe operation of the system.
- the provision of an essentially tightly enclosing hood part makes it possible, on the one hand, to encapsulate the entire atmosphere within the device and thus to separate it from the outside atmosphere which surrounds the device. This allows evaporating solvents to be collected before they exit the device and returned to the corresponding parts of the system.
- Contamination of the ambient air of the device can thus essentially be ruled out. It also makes it possible to maintain a constant and at the same time different pressure within the hood part than would correspond to the pressure in the surrounding atmosphere. Preferably, at least in a part of the individual sections of the hood part, a slight positive pressure is maintained and monitored over the atmosphere surrounding the device. Preferably, at least one pressure maintaining device is provided to maintain a constant pressure in the hood part and / or such a slight overpressure in the hood part with respect to the outside and / or ambient atmosphere. An involuntary penetration of the outside atmosphere into the device and thus contamination of the gas atmosphere inside the device can thus be substantially avoided.
- the device is preferably at least one gas buffer device provided and connectable or connected to this, in particular in the first and / or last section.
- gas buffer devices are thus preferably provided at the entrance and exit of the device, since pressure fluctuations can occur there due to the introduction and ejection of the products.
- the gas buffer devices are filled as soon as an overpressure outside the presettable tolerance occurs in the hood section, and are emptied when an underpressure outside of an adjustable tolerance occurs in the hood section, e.g. B. when gas atmosphere is removed from the respective hood section, such as for flooding a lock chamber with inert gas.
- At least one oxygen monitoring device is preferably provided in the at least one lock chamber and / or the sections of the hood part. At least one device for monitoring the solvent concentration in the lock chamber or chambers is also preferably provided. This makes it possible to continuously monitor the oxygen and / or solvent content of the gas atmosphere in the individual sections of the device. Since the lock chamber (s) serve to prevent air or oxygen from entering the device, after the introduction of products, the removal of the air introduced with the product and the purging of the chamber with e.g. B. inert gas regularly monitors the oxygen content of the lock chamber atmosphere. If the lock chamber is opened towards the hood part, the oxygen content within the chamber should be as zero as possible so that penetration of oxygen into the hood part and the other parts of the device can be avoided.
- the discharge of solvent from the device should also be reduced to zero if possible.
- devices for monitoring the solvent concentration are also provided there. If the oxygen and / or solvent content is one Predeterminable and / or adjustable or set threshold exceeds an adjustment of the pumping times for the introduction and discharge of gas into / from the lock chamber and / or an additional flushing phase with an inert gas during pump cycles to reduce the oxygen content in the at least one lock chamber to be triggered. A longer pump cycle is then provided, for example, for pumping out the contaminated gas atmosphere.
- the inert gas atmosphere bell of the device can also be monitored for its oxygen content, the oxygen content should be as zero as possible.
- At least one cleaning and / or activation section for cleaning and / or pretreating the surface of the products and / or at least one export section for discharging the products out of the device is preferably provided.
- the at least one cleaning and / or activation section preferably has one or more closable treatment basins with a cleaning liquid for cleaning the products to be coated and / or an activation liquid for activating their surface or for producing an adhesion promoter layer.
- cleaning of the raw products is advantageously possible, an oxide-free and bare surface being able to be produced on the products. This ensures optimal adhesive strength for the subsequent coating.
- an adhesion promoter layer can advantageously be applied to the surface of the product in this section of the device.
- the at least one cleaning and / or activation section preferably has at least one rinsing device downstream of the at least one treatment basin for rinsing the pretreated products and preventing chemical carryover from the cleaning and / or activation section.
- a siphon rinsing device is provided after the cleaning and / or activation section, i.e. before the coating section, it makes sense to provide such rinsing of the pretreated products in order to carry the chemicals from the cleaning and activation stage into the siphon rinsing device and thus subsequently to prevent in the coating electrolyte.
- a solvent preparation and / or regeneration device is preferably provided and connected to such a flushing device.
- the cleaned solvent is in particular returned to this rinsing device, whereas the cleaned cleaning liquid or activation or other liquid located in the upstream treatment tank can be returned to this treatment tank.
- a distillation is preferably provided, followed by provision of the purified solvent.
- the at least one solvent preparation and / or regeneration device is preferably provided for the cleaning and / or activation section in the bypass to the latter.
- the at least one lock chamber can also be connected or connected to a solvent separation and return device and / or a gas pendulum system.
- At least one lock chamber is preferably provided at the entrance of the cleaning and / or activation section and / or at least one lock chamber at the exit of the export section.
- the products are preferably introduced into the at least one lock chamber, the lock chamber being filled with the outside atmosphere, closed and then evacuated, that is to say the outside atmosphere is conveyed out of the chamber, and the latter is subsequently flooded with inert gas.
- the products are then introduced into a first treatment section of the device during the infiltration step.
- these products are introduced from the hood atmosphere into the lock chamber, the latter is closed and the hood atmosphere is pumped out of the lock chamber and returned to the hood section.
- the lock chamber can then be opened and the products removed.
- the lock chamber is then closed again, the penetrated outside atmosphere is removed and the chamber is flooded with inert gas.
- the pumped-out lock atmosphere is particularly preferably prepared, with dry inert gas and cleaned solvent being returned to the process, in particular dry inert gas into the inert gas atmosphere bell and cleaned solvent into a treatment basin.
- the gas pendulum system thus includes pumping dried inert gas into the hood atmosphere after pumping out the atmosphere of the lock chamber from the lock chamber.
- the product to be coated is thus introduced into the lock chamber preferably provided at the entrance of the device before coating, and since after the products have been coated they are brought back into the outside atmosphere by opening a lock chamber provided at the end of the device and penetration from outside atmosphere into the Lock chamber, it proves to be advantageous to provide a solvent separation and return device in the area of the lock chambers. It is precisely there that when the products are introduced and discharged, both oxygen and moisture can penetrate into the device and evaporated solvent can escape from the device. Using preferably provided cooling devices, the atmosphere pumped out and contaminated with solvent can be cooled from the lock chamber and the solvent can thus be separated, collected and returned. During the solvent separation process, the pumped gas is dried and can then be returned to the hood atmosphere.
- the products By separating the solvent in the discharge area, the products can be cleaned of the solvent residues adhering to them and leave the device essentially completely dry, so that essentially no more solvent emissions take place.
- the solvent residues discharged during the pumping process are also recondensed in the area where the products are discharged, collected and subsequently returned to the process, in particular to the last siphon rinsing device.
- the inert gas atmosphere bell is also preferably cleaned, in particular by condensing the inert gas atmosphere and returning the condensed solvent components to the respective circuits, in particular treatment tanks.
- At least one cooling device with a condensate separating device is preferably provided for the recovery of dragged and / or evaporated solvent residues, in particular in the hood part and / or coating section and / or connected to the at least one lock chamber.
- the one or more cooling devices in hood sections and / or in the hood part have solvent return devices for returning solvent to treatment and / or coating basins and / or the at least one siphon rinsing device. This makes it possible to remove solvent contaminants from the gas atmosphere in the Remove the hood part again.
- the solvent components condensed in the cooling devices can subsequently be returned to corresponding treatment tanks in the respective hood section.
- the respective cooling devices are preferably provided in the individual hood sections, since the evaporating liquids in these individual hood sections are mostly different in each case, so that the impurities in the gas atmosphere are also different. Therefore, a return is advantageously carried out within the respective hood section.
- the at least one coating section preferably has at least one coating basin which can be closed to prevent uncontrolled evaporation of solvent into the hood part.
- at least one cooling device for condensing evaporated solvent and at least one collecting device for collecting the condensed solvent in the gas space of the at least one coating basin are also provided.
- the at least one coating section can have at least one export rinsing device. After the coating process, the products are introduced into the rinsing bath provided in this export rinsing device in order to remove adhering electrolyte residues. In order to clean the rinsing bath, in particular a return of purified solvent from the solvent separation and / or regeneration device is provided.
- the siphon rinsing device is provided for separating the individual sections of the device, that is to say in particular the cleaning and / or activation section, the coating section and the export section, it proves to be advantageous to provide an essentially non-reacting solvent in these transition areas.
- the at least one siphon rinsing device is therefore preferably filled with an inert solvent. This can cause unwanted chemical reactions between mutually incompatible chemicals are essentially avoided from the individual sections of the device.
- the at least one siphon flushing device preferably comprises a closable double flushing device with an attached partition, which is oriented in such a way that hood sections located above are divided off.
- a gas-tight separation from different hood sections of the device can be created.
- at least one transport device is arranged within the double rinsing device for moving the products below the partition or can be arranged in this way, that when the double rinsing device is filled with a rinsing liquid, the transport device is positioned below the liquid level.
- At least one electrolyte-solvent separation device is preferably provided in the region of the coating section.
- the electrolyte-solvent separating device (s) comprise a distillation device for distilling off solvent from the electrolyte-solvent bath liquid discharged from the at least one coating basin.
- devices are preferably provided for returning the clean solvent obtained into the export sink and / or devices for returning the electrolyte into the electrolyte circuit.
- the electrolyte solution that is to say the coating solution, can thus be purified in the bypass of the coating section.
- This purification device is connected in particular to the coating baths, with clean solvent in particular being returned to the export sink downstream of the coating baths and in particular electrolyte to the coating baths.
- Electrolyte liquid and / or solvent are preferably conducted in essentially closed circuits. This substantially prevents contamination of the other baths in the device.
- the electrolyte liquid and / or solvent and / or a rinsing liquid is advantageously cleaned or prepared in order to avoid chemicals being carried over.
- rinsing is also preferably provided in the various rinsing devices. These flushing devices can be provided at different points in the device and in the coating process, in particular in the exit area of respective sections of the device.
- products of any shape can be coated with the devices according to the invention, including products with undercuts in which solvents can collect. This cannot be removed with devices from the stand, which is why a solvent discharge cannot be avoided with them.
- removal of solvent residues in any product forms is certainly possible.
- 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.
- it has a hood part 5 which essentially tightly encloses all three aforementioned sections.
- the hood part is divided into three sections 50, 51, 52.
- the three hood sections are delimited from one another by respective partition walls 53, 54.
- the cleaning and / or activation section 2 comprises a first lock chamber 20, a first treatment basin 21, a second treatment basin 22 and a sink 23.
- the cleaning and / or activation section comprises part of a first siphon rinsing device 60 Partition 53 divided into two parts so that it forms a double rinsing device which is accessible from section 2 and section 3, but otherwise forms a diffusion barrier. All basins or flushing devices can be closed with respective lids 24, 25, 26, 27, 62.
- the lock chamber 20 has a lock door 28, which enables products to be moved into the lock chamber. Such products are preferably moved into the lock chamber via a transport trolley, which is not shown in the figure.
- the lock chamber 20 is connected to a device 70 for the recovery of solvent and a gas pendulum system 80.
- the device for solvent recovery has a cooling trap 71, a valve 72, a condensate separator 73 and a line 74 between the valve 72 and the lock chamber 20, a line 75 between the cooling trap 71 and the condensate separator 73 and a Solvent return line 76 between the condensate separator 73 and the first treatment basin 21.
- the gas pendulum 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, a further 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 a further line 88 between the valve 83 and the hood part 50.
- the line 87 also leads to the valve 84 and from this a further line 89 to the outside into the outside atmosphere. This allows air to be blown out of the device.
- a solvent preparation and / or regeneration device 90 is also connected to the cleaning and / or activation section 2.
- Regeneration device comprises a distillation device 91 and one
- Condensate collection tank 92 Condensate collection tank 92.
- the desti11 ier noise is via a line
- a line 94 is also provided between the distillation device 91 and the condensate collection tank 92.
- the cleaning liquid purified in the desti11 ier Anlagen 91 is via a line 95, a
- Clean solvent distilled off by the desti11ing device can be pumped back from the condensate collecting tank 92 via a line 98, a pump 99 and a line 100 to the sink 23.
- 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 basins.
- the transport device has a carriage 56, which in this embodiment is provided with a hook 57 for attaching the products 7 to be coated.
- the hook 57 is attached to the carriage 56 so that it can be extended so that the products on this hook slowly enter the respective ones Baths let in and can be lifted out of these.
- the hood section 50 also has a cooling device 58. This is shown in the figure in the form of a cooling coil. About these
- Evaporated solvent can be condensed in the cooling coil and collected or collected in a collecting device 59 likewise provided in the hood section 50. In the figure it is
- Collecting device shown in the form of a gutter.
- the solvent condensate collected in the collecting trough or collecting device 59 can be returned to the first treatment basin 21 via a drain line 101. Solvent can thus be returned to both the first and the second treatment basin.
- further treatment pools can also be provided, the figure here merely shows a possible embodiment. It is also possible to provide several sinks; it would also be possible in principle to provide more than one lock chamber.
- Hood section located gas and cleaned despite recycling
- Gases is a gas buffer container 120 outside the hood part 5 intended.
- the gas buffer container 120 is connected to the interior of the hood section 50 via a line 121.
- a bilateral exchange of gas between the gas buffer container and the hood section 50 can take place via this line 121. This makes it possible to maintain a preset excess pressure, above all a constant pressure within the hood section.
- a first oxygen sensor 122 is provided in the area of the hood section 50, a second oxygen sensor 123 and a solvent concentration sensor 124 on the lock chamber 20. All sensors can be connected to a monitoring and control device (not shown in the figure) in order to monitor whether the set threshold values have been exceeded and, if necessary, to adapt pumping cycles of the lock chamber and a gas exchange in a targeted manner.
- the coating section 3 has the second part of the siphon flushing device 60, which, as mentioned above, is designed as a double flushing device.
- a transport device 66 is provided within the siphon rinsing device 60, which can in particular have a trolley, as shown in the figure.
- the products on the side of the coating section 3 can be removed again by means of a cover 63 of the siphon rinsing device 60 after being transported through the siphon rinsing device.
- the coating section 3 also has two coating basins 30, 31, and an export sink 32 and a first part of a further siphon flushing device 61.
- Each of these basins is provided with a lid 33, 34, 35 and the siphon flushing device with a lid 64 on the side of the coating section ,
- cooling coils 36, 37 and collecting channels 38, 39 are provided in order to condense solvent which evaporates from the electrolyte during coating and, in particular, to introduce it into the rinsing bath 32 after the coating basin.
- the coating section 3 is also provided with a purification device following the coating basin in order to purify the electrolyte in the bypass in an electrolyte-solvent separation device 110. This ensures that no significant amounts of electrolyte are carried over, which means that a largely closed material cycle can be generated.
- a purification device for the purification of the electrolyte, liquid is led from the two coating basins 30, 31 via lines 111 to a distillation device 112.
- a condensate collection tank 113 is provided, which is connected to the distillation device 112 via a line 114.
- the cleaned electrolyte is returned to the coating basin 30 via lines 115, 117 and a pump 116.
- the solvent distilled off from the electrolyte-solvent mixture is collected in the condensate collecting tank 113 and returned via a line 118, a pump 119 and a return line 102 to the rinsing bath in the export sink 32.
- the rinsing bath in the export sink 32 is always supplied with clean solvent. If the level in the export sink increases too high, an overflow line 103 is provided between the export sink and the second coating pool 31. The excess rinsing liquid, in particular solvent, runs back into the second coating basin.
- the coating section 3 also has a transport device 55 with a carriage 56 and a hook 57 in order to be able to transport the product 7 to be coated between the individual pools of the coating section.
- a cooling device 58 in the form of a cooling coil and a gutter are provided as a collecting device 59 for condensed solvent. The collected condensed solvent is returned to the first coating basin 30 via a drain line 104.
- the export section 4 has the second part of the siphon flushing device 61. Like the siphon flushing device 60, this is provided with a transport device 67. The products introduced through the cover 64 into the siphon flushing device are transported to the section 65 on the other side of the partition 54 with the cover 65 of the siphon flushing device 61. As in the flushing device 60, the transport takes place below the surface of the flushing liquid located in the siphon flushing device. This enables an essentially complete gas seal during the transport of the products from the coating section into the export section.
- the export section also has a second lock chamber 40 for discharging the coated products from the device.
- the lock chamber is provided with a cover 41. It also has a lock door 42. Similar to the lock chamber 20, the lock chamber 40 is also provided with a device 130 for the recovery of solvent and a gas pendulum system 140.
- the device for recovering solvent is also equipped with a cold trap 131, a valve 132 between lock chamber 40 and cold trap 131, a condensate separator 133, a line 134 between valve 132 and lock chamber 40, a line 135 between condensate separator 133 and cold trap 131 and a solvent return line 136 between the condensate separator 133 and the siphon flushing device 61.
- the gas pendulum system 140 comprises a vacuum pump 141, three valves 142, 143, 144 and a plurality of lines located between them.
- a first one Line 145 leads from the lock chamber 40 to the first valve 142
- a second line 146 leads from the valve 142 to the pump 141.
- a line from the cold trap 131 also leads to this, as is also the case between the device 70 between the cold trap 71 and the vacuum pump 81 is the case.
- a line 147 leads from the pump 141 to the valve 143 and from this a return line 148 to the hood section 52. From the vacuum pump, the line 147 also leads to the valve 144, via which in particular air from the lock chamber 40 leads via a line 149 can be blown off into the environment.
- the hood section 52 likewise comprises a transport device 55 with a carriage 56 which has a hook 57 in order to be able to grip products 7 and lower them into the individual basins. Also provided are cooling coils 58 as a cooling device and a collecting trough 59 for condensed solvent, which can be returned from the collecting trough via a drain line 105 to the siphon rinsing device 61.
- the export section 4 is also provided with a gas buffer container 125 and a line 126 between the interior of the hood section 52 and the gas buffer container 125. This can ensure that a gas pressure that is as constant as possible is maintained within the export section, although, for. B. by returning dried inert gas via line 145, an overpressure could occur in the hood section of the export section, as could a negative pressure when flooding the lock chamber 40 with hood atmosphere from the export section after pumping out the outside atmosphere following a removal process of finished products from the lock chamber 40 ,
- first and second oxygen sensors 127, 128 and a Solvent concentration sensor 129 provided.
- the first oxygen sensor 127 is provided in the upper hood section 52, the second oxygen sensor 128 and the solvent concentration sensor 129 are provided on the lock chamber 40.
- the hood section 51 above the coating section 3 is also provided with such an oxygen sensor 150.
- a product to be coated is introduced into the first lock chamber 20 via the lock door 28. This is done in particular via a transport trolley, which is not shown in the figure.
- the lock chamber is inevitably filled with an outside atmosphere (air) and then closed. It is subsequently evacuated via the vacuum pump 81 and the lines 85 and 86.
- valve 82 is opened. Since there is then only unpolluted air in the lock chamber, it can be discharged directly to the outside via line 89 and open valve 84.
- the lock chamber is then flooded with inert gas from the hood section 50.
- the inner cover 24, which is arranged between the lock chamber and the hood section 50, can then be opened and the product can be introduced into the inert gas atmosphere within the hood section 50.
- the amount of oxygen that can penetrate into the first hood section 50 is very small, since the lock chamber to a final pressure of less than 1 to 2 mbar can be evacuated and it is also possible that intermediate purges with inert gas, in particular nitrogen or argon, are carried out.
- the atmosphere within the hood section can be monitored continuously by means of the oxygen sensors.
- the solvent concentration is monitored via the solvent concentration sensor 124. Checking the oxygen diffusion into the system is particularly useful with regard to the life of the electrolyte and the coating quality, but also with regard to the general process and operational safety of the entire system.
- the cover 24 can be closed again and the lock atmosphere can be pumped out, an inert gas solvent being present in the lock atmosphere and being pumped out. This takes place after opening the valve 72 via the line 74, the solvent / inert gas mixture being passed through the cold trap 71. After the condensation, the dried inert gas obtained is returned to the hood section 50 via the vacuum pump 81, the line 87 and the then opened valve 83 and the line 88. The inert gas can be made available to the atmosphere in the hood section 50 again as cleaned gas. The excess gas volume is collected by increasing the volume in the gas buffer container 120, as a result of which the pressure in the hood section 50 can be kept substantially constant.
- the resulting condensed solvent is introduced via line 75 into the condensate separating device 73 and can in particular be fed periodically to the first treatment basin 21 via the solvent return line 76.
- the evacuated lock chamber is then flooded again with fresh inert gas and the door to the outside atmosphere, namely the lock door 28, can be opened again to introduce new products into the device.
- the products can be introduced into the treatment tanks 21, 22, which in particular contain a cleaning liquid, and pre-cleaned there, and in particular a bare oxide-free surface can be produced thereon in order to ensure optimum adhesive strength during the subsequent coating.
- an adhesion promoter layer can be applied in this basin.
- the covers 25, 26 are provided, as are the covers 27 on the sink, which are preferably only opened when the goods or products are being brought in and out.
- the downstream sink 23 serves to prevent carryover of chemicals from the treatment tanks 21, 22 into the siphon flushing device 60, whereby the carryover into the coating electrolyte in the tanks in the coating section is also to be avoided.
- the liquid in the sink 23 is regularly processed via the solvent preparation and / or regeneration device 90, which is bypassed to the cleaning and / or activation section.
- the pretreated product After the pretreated product has been rinsed, it is introduced into the siphon rinsing device 60 via the cover 62. Due to the provision of the partition 53, the two hood sections 50 and 51 located at the top are separated from one another in a gas-tight manner, but are nevertheless connected to one another for the passage of products by the double sink of the siphon flushing device 60.
- the liquid in the siphon rinsing devices is preferably identical to the solvent used in the coating electrolyte. In order to avoid a reaction with cleaning liquid and / or coating electrolyte as far as possible, an inert solvent is preferably used.
- the provision of the siphon rinsing device between the activation section 2 and the coating section 3 results in the advantage that solvents which are poorly compatible with the coating electrolyte can also be used in the cleaning liquids of the cleaning and / or activation section, since the solvents migrate via the gas atmosphere in the electrolyte area is prevented. A carryover of solvent with the products to be coated is particularly largely prevented by the preparation of the liquid in the sink 23 via the distillation device 91.
- the products After the products have been lifted out through the cover 63 of the siphon rinsing device 60, they reach the coating section 3 and can be lifted into the coating basin 30, 31 therein.
- numerous more can be provided, as well as further export sinks 32, only one of which is shown in the figure.
- the covers 63, 33, 34, 35, 64 are closed in normal operation.
- the lids are preferably only opened for entering or removing products from the individual basins.
- the cooling coils 36, 37 and collecting channels 38, 39 are located in the two coating basins 30, 31.
- Solvent that has evaporated from the electrolyte during the coating is condensed here and the rinsing bath in the export rinsing basin 32 forwarded again. Larger amounts of electrolyte are regularly converted via the distillation device provided in the electrolyte circuit and pumped back to the basin 30 via the lines provided therein and the pump 116. The solvent distilled off from the electrolyte is collected in the collecting tank 113 and fed back via the lines and the pump 119 to the export sink 32 or the washing bath contained therein. Excess solvent is returned to the circuit or the basin 31 via the overflow line 103 in order to avoid overflow of the export rinsing basin 32. This ensures that no significant amounts of electrolyte are carried over into the downstream siphon flushing device 61, a largely closed material cycle also being able to be produced here.
- the siphon rinsing device 61 adjoining between the coating section and the export section is comparable in structure and mode of operation of the siphon rinsing device 60.
- the products completely immersed therein are removed again through the cover 65 on the side of the export section 4. Due to the previous rinsing in the export sink 32, which contains fresh solvent, the electrolyte residues previously adhering to the coating section 3 can be intercepted and cannot be carried over into the export section 4.
- the export sinks also serve to effectively use excess process heat generated during the coating process and to remove it from the system.
- the second lock chamber 40, into which the coated product is introduced, is also provided in the export section 4. This takes place via the cover 41.
- a pumping-off process is also initiated. This serves to recover any solvent residues still adhering to the coated product. This makes it possible for the completely coated product to leave the device dry and essentially no more solvent emissions take place. All the solvent evaporated during the pumping process and recondensed in the cold trap 131 and collected in the condensate separating device 133 is returned to the siphon rinsing device 61 via the line 136. Otherwise, the discharge process takes place in accordance with the injection process with regard to the pumping in and pumping out of the lock atmosphere and inert gas.
- the lock door 42 is opened to discharge.
- the individual hood sections 50, 51, 52 are flooded with inert gas and, at least in the present exemplary embodiment, are kept constantly at a slight excess pressure with respect to the ambient atmosphere by means of an automatic pressure maintaining system. This prevents air from entering the hood part.
- the oxygen sensors 122, 123, 127, 128, 150 continuously indicate the oxygen content in the respective gas atmosphere. If the preset threshold values are exceeded, the pumping time is adjusted with respect to the pumps 81, 141 or an additional flushing with inert gas is initiated in the lock chambers 20, 40 during the pumping cycle.
- Providing a solvent preparation for the cleaning and / or activation section 2 can effectively prevent contamination of the coating electrolytes by oxygen and moisture as well as carryover of other chemicals, in particular also the carryover of solvents used in the cleaning liquids, which may contain a certain amount Coating electrolyte are incompatible.
- By providing the solvent preparation and / or regeneration device 90 direct return of the cleaning liquid and solvent into the corresponding circuits can thus be made possible. This also allows impurities in the sink 23 to be kept at a very low level.
- hood atmosphere in the hood sections 50, 51, 52 By condensing the hood atmosphere in the hood sections 50, 51, 52, it can be kept as dry and clean as possible. A condensation of solvent residues on the goods, which evaporate during the transport time, especially when the products are still warm, can be condensed in a controlled manner and returned to the individual material cycles via the drain lines.
- numerous further ones can be formed, in each of which it is possible to keep solvent emissions from the device as low as possible and to reduce the carry-over of oxygen and moisture and other impurities as much as possible Reaching coating electrolyte into it and thus significantly extending the life of coating electrolytes while avoiding the formation of unwanted reaction products.
- the devices have a closed hood atmosphere, which forms an essentially tight bell over the individual stations of the coating device, with a simultaneous cleaning of both the atmosphere and the treatment or coating baths and rinsing baths. This can be done particularly easily by guiding the cleaning sections in the bypass to the respective processing or treatment sections. Alternatively, more complex purification steps or cycles are also possible. LIST OF REFERENCE NUMBERS
Landscapes
- 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)
- Chemical Vapour Deposition (AREA)
- Cleaning By Liquid Or Steam (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
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 |
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 |
DK04764184T DK1658393T3 (da) | 2003-08-26 | 2004-08-17 | Anordning og fremgangsmåde til at adskille metaller og/eller metallegeringer fra metalorganiske elektrolytter |
DE502004007361T DE502004007361D1 (de) | 2003-08-26 | 2004-08-17 | Vorrichtung und verfahren zum abscheiden von metallen und/oder metalllegierungen aus metallorganischen elektrolyten |
EP04764184A EP1658393B1 (de) | 2003-08-26 | 2004-08-17 | Vorrichtung und verfahren zum abscheiden von metallen und/oder metalllegierungen aus metallorganischen elektrolyten |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP03019235.5 | 2003-08-26 | ||
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 |
---|---|
WO2005021840A1 true WO2005021840A1 (de) | 2005-03-10 |
Family
ID=34089604
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2004/009192 WO2005021840A1 (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 (de) |
EP (2) | EP1510600A1 (de) |
JP (1) | JP2007503527A (de) |
AT (1) | ATE398195T1 (de) |
DE (1) | DE502004007361D1 (de) |
DK (1) | DK1658393T3 (de) |
WO (1) | WO2005021840A1 (de) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102004032659B4 (de) | 2004-07-01 | 2008-10-30 | Atotech Deutschland Gmbh | Vorrichtung und Verfahren zum chemischen oder elektrolytischen Behandeln von Behandlungsgut sowie die Verwendung der Vorrichtung |
CN103938239A (zh) * | 2014-05-11 | 2014-07-23 | 山东建筑大学 | 一种钢带连续镀铜ⅰ |
CN103938238B (zh) * | 2014-05-11 | 2016-08-03 | 山东建筑大学 | 一种钢带连续镀铜方法 |
Citations (4)
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)
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 |
-
2003
- 2003-08-26 EP EP03019235A patent/EP1510600A1/de not_active Withdrawn
-
2004
- 2004-08-17 WO PCT/EP2004/009192 patent/WO2005021840A1/de active IP Right Grant
- 2004-08-17 DE DE502004007361T patent/DE502004007361D1/de not_active Expired - Lifetime
- 2004-08-17 DK DK04764184T patent/DK1658393T3/da active
- 2004-08-17 JP JP2006524288A patent/JP2007503527A/ja active Pending
- 2004-08-17 US US10/569,658 patent/US20070114132A1/en not_active Abandoned
- 2004-08-17 EP EP04764184A patent/EP1658393B1/de not_active Expired - Lifetime
- 2004-08-17 AT AT04764184T patent/ATE398195T1/de not_active IP Right Cessation
Patent Citations (4)
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 |
Also Published As
Publication number | Publication date |
---|---|
EP1658393B1 (de) | 2008-06-11 |
DK1658393T3 (da) | 2008-10-20 |
EP1510600A1 (de) | 2005-03-02 |
EP1658393A1 (de) | 2006-05-24 |
ATE398195T1 (de) | 2008-07-15 |
US20070114132A1 (en) | 2007-05-24 |
DE502004007361D1 (de) | 2008-07-24 |
JP2007503527A (ja) | 2007-02-22 |
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