EP1184487A1 - Verfahren zur Reinigung eines Elektrolyten - Google Patents

Verfahren zur Reinigung eines Elektrolyten Download PDF

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Publication number
EP1184487A1
EP1184487A1 EP00118640A EP00118640A EP1184487A1 EP 1184487 A1 EP1184487 A1 EP 1184487A1 EP 00118640 A EP00118640 A EP 00118640A EP 00118640 A EP00118640 A EP 00118640A EP 1184487 A1 EP1184487 A1 EP 1184487A1
Authority
EP
European Patent Office
Prior art keywords
electrolyte
cleaning liquid
cleaning
separation unit
impurities
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Withdrawn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
EP00118640A
Other languages
German (de)
English (en)
French (fr)
Inventor
Andreas Dr. Möbius
Axel Dr. König
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.)
MacDermid Enthone GmbH
Original Assignee
Enthone OMI Deutschland 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 Enthone OMI Deutschland GmbH filed Critical Enthone OMI Deutschland GmbH
Priority to EP00118640A priority Critical patent/EP1184487A1/de
Priority to JP2001254394A priority patent/JP2002105696A/ja
Priority to US09/939,502 priority patent/US6841074B2/en
Priority to CN01125266.9A priority patent/CN1342788A/zh
Publication of EP1184487A1 publication Critical patent/EP1184487A1/de
Withdrawn legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/16—Regeneration of process solutions
    • C25D21/18—Regeneration of process solutions of electrolytes
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1617—Purification and regeneration of coating baths

Definitions

  • the invention relates to a method for cleaning an electrolyte and further a device for performing the method.
  • electrolytic deposition of metals from their dissociated solutions Salts are well known from the prior art and are common in practice used.
  • the salts are in the metal solutions called electrolytes split form before as ion.
  • electrolytes can be aqueous or organometallic systems as well as salt melts, with the exception of aluminum deposition from organic electrolytes, in particular in electroplating aqueous electrolytes are preferably used.
  • Ions are electrically charged atoms or groups of atoms that, due to their electrical Charge can conduct electricity.
  • the substrates to be coated Before the actual electrolytic metal coating step, it is in the As a rule, the substrates to be coated have different pretreatment steps to undergo. This includes degreasing, for example Pickling, conditioning and, in the case of non-conductive substrates, application of conductive base layers. To carry out such preparatory In most cases, steps are provided for chemical strips into which the strips still to be coated are placed Substrates are immersed. Although each of these preparatory steps usually an appropriate rinsing process to clean the substrate downstream, a transmission of unwanted chemicals in the Finally, electrolytes cannot be prevented, so that an unwanted one Contamination of the electrolyte.
  • the quality of a metal layer produced by electrolytic metal deposition depends largely on the electrolyte composition. In this respect it is permanent Aim to contaminate the electrolyte and thereby change the Avoid electrolyte composition. But since a carry over from chemicals from upstream processing steps are not effective can be prevented, arises over the period of use of the electrolyte an ever increasing degree of pollution. With exceedance the electrolyte is then no longer at a certain impurity concentration usable and must be replaced.
  • Another disadvantage is that with increasing degree of contamination of the electrolyte at the same time, the probability increases that there are electrolytes Contamination unintentionally in the lattice structure of the separating Metal layer absorbed or incorporated with it and so it is faulty Metal layer training is coming. To avoid this, one is required dirty electrolytes early against a fresh one, none Exchange contaminated electrolytes. Especially before against the background of environmentally friendly disposal, this is usually very complex and last but not least cost-intensive.
  • the ion concentration increases in the Electrolyte the installation error rate, whereby in the course of the deposition of the nobler Metal also entrained ions of the less noble metal and in unwanted Way can be built into the metal grid structure.
  • galvanic baths as well as electroless baths, contain inorganic and organic additives. These substances are timely and depending on the effect (i.e. depending on the current density, the potential or the Temperature) changed or reduced. The amount of Components as well as their chemical composition. The mining or Conversion products interfere with galvanic or currentless deposition. This Fabrics must therefore be removed from the baths.
  • the invention is therefore based on the object , while avoiding the disadvantages mentioned above, of providing a method for cleaning an electrolyte which, in particular against the background of environmentally friendly use of resources, enables the electrolyte to be reused and which maintains a consistently good deposition quality by means of the electrolyte composition the duration of a metal deposition is essentially constant.
  • the invention is intended to provide a corresponding device for carrying out the method.
  • the invention proposes a method for cleaning an electrolyte, in which the electrolyte is brought into contact with an active surface of a separation unit which is permeable to impurities to be removed from the electrolyte, and in which a cleaning liquid is made available and with another active surface of the separation unit is brought into contact, the impurity concentration of the cleaning liquid for maintaining a driving force gradient between the electrolyte and cleaning liquid being maintained for the duration of the cleaning process for a transition of the impurities from the electrolyte into the cleaning liquid.
  • the core idea of the invention is therefore to use the contaminated electrolyte a corresponding cleaning liquid from impurities free and thus a reusable electrolyte in an environmentally friendly way provide.
  • the electrolyte can either be cleaned continuously, i.e. during the metal deposition process or in the sense of a Recycling carried out after a metal deposition process become. It is advantageous in both cases that the cleaning method according to the invention can be easily integrated into existing work processes and the contaminated electrolyte cleaned inexpensively and above all environmentally friendly becomes.
  • the method provides that the electrolyte has an active surface a separation unit is brought into contact.
  • This separation unit is for such impurities permeable, which must be removed from the electrolyte.
  • Derlei Contamination are, for example, from upstream process steps originating ions, such as foreign metal ions or ions from Halogens or molecules, such as polymer molecules or cleavage or Degradation products from organic or inorganic additives.
  • a cleaning liquid is also provided, which with another active surface of the same separation unit is brought into contact.
  • the electrolyte to be cleaned and the cleaning liquid are not directly fluidly connected with each other, but is the permeable Separation unit provided the possibility that contaminants from one Side of the partition can go to the other side of the partition.
  • the Contamination concentration of the cleaning liquid for maintenance a driving force gradient between electrolyte and cleaning liquid at least is kept less than those for the duration of the cleaning process of the electrolyte.
  • the gradient of the driving force gradient is understand chemical or electrochemical potential.
  • Electrolyte and cleaning fluid Due to the prevailing driving force or potential gradient between Electrolyte and cleaning fluid are in the electrolyte Contamination caused through the separation unit into the cleaning liquid to diffuse. There is a transition of the impurities from the electrolyte into the cleaning liquid only when the Driving force gradient equal to zero, i.e. the chemical potential in the electrolyte is the same that is in the cleaning liquid. So is the impurity concentration in the cleaning liquid compared to that in the electrolyte kept lower, so there is a concentration gradient from the electrolyte towards Cleaning liquid and there is a transition of contaminants from the Electrolytes are held in the cleaning fluid.
  • the method according to the invention opens up the in a simple and efficient manner Cleaning an electrolyte so that it can be reused in an advantageous manner can be supplied.
  • it enables the invention Process the electrolyte composition over a period of one To keep the metal deposition process essentially constant, with which a reproducibly good metal deposition quality is achieved.
  • the impurity concentration of the Cleaning liquid kept below a predetermined target concentration. This ensures a consistently good metal deposition result. moreover becomes a with the specification of a target concentration not to be exceeded Measurement specification provided, which can be checked by measurement. So can for example, it can be provided that when a predefinable limit is exceeded Target concentration an alarm signal is triggered, which indicates that the Pollution concentration of the cleaning liquid is too high for a effective cleaning of the electrolyte can still be guaranteed. Consequently it is ensured that the cleaning fluid is replaced early can be made and the metal deposition result in the electrolyte is not affected by a worsened cleaning effect.
  • the cleaning liquid diluted over the duration of the cleaning process or is regenerated is regenerated.
  • This simple measure will lower the Impurity concentration in the cleaning liquid achieved, the Relationship between dilution and concentration reduction proportional is.
  • the cleaning can be carried out continuously or discontinuously and in Cycle operated.
  • the impurities be removed from the cleaning liquid.
  • the cleaning liquid is distilled off or in other form is recovered purely. This advantageously results in a reduction in the concentration of impurities in the cleaning liquid achieved with the same volume of cleaning fluid, on the other enables the contaminants to be removed for recycling. This is particularly useful when using an electrolyte for electroless Metal deposition, in which the impurities by the in Electrolyte dissolved metal ions of the base metal are formed.
  • the impurities removed from the cleaning liquid in that the contaminants chemically bound and precipitated from the cleaning liquid. So can corresponding to the cleaning liquid depending on the contamination to be precipitated Ions are added, the ones to be removed from the cleaning liquid Chemically bind impurities and thus the possibility of easy removal, for example by failures. Can also be provided be to remove the impurities from the cleaning liquid by means of filters, or to recover the cleaning liquid itself. This can for example by distillation, membrane distillation or freezing.
  • the electrolyte and / or the Cleaning liquid relative to their respective active surface Separation unit moves.
  • the cleaning effect is advantageous elevated. This is due to the fact that from the electrolyte into the cleaning liquid diffused impurities immediately after a transition from the Active surface of the separation unit are moved away, so that the highest possible Driving force or potential gradient in the immediate vicinity of the separation unit is maintained.
  • the fluidically independent systems of the electrolyte and the cleaning fluid in system circuits that are each other have opposite flow directions. Also through this measure will maintain the highest possible driving force gradient in favored in the immediate vicinity of the separation unit.
  • the intensive condition variables include in particular the pressure as well the temperature.
  • the object is proposed to solve a device, characterized by two by means of a permeable from the electrolyte to remove impurities separation unit fluidically separated from each other arranged volume regions, wherein the one volume region of the receptacle to be cleaned electrolyte and the other volume range of the Absorption of the cleaning liquid is used.
  • the one proposed here Device essentially characterized by two volume ranges, the fluidically separated from each other by interposing a separation unit are.
  • the separation unit is permeable to those Impurities that need to be removed from the electrolyte.
  • the one The volume area serves to hold the electrolyte, whereas the other volume range is used to hold the cleaning liquid.
  • the volume ranges are therefore fluidic with the interposition of the separation unit juxtaposed, so that a mixture of electrolyte and cleaning liquid not taking place.
  • the separation unit of the device is according to a first proposal of the invention designed porous or liquid-tight.
  • the structure of the separation unit is included such that it is only the impurities due to the Driving force gradient is possible out of the electrolyte through the Diffusion unit to diffuse into the cleaning liquid.
  • Example of a Porous separation unit is a sponge-like hardened Graphite foam. Materials such as PP, PE, ceramics, metals can also be used or other suitable materials are used. Furthermore, for the Formation of a dense separation unit combinations of porous and not porous materials or other structures be used.
  • the separation unit is a Membrane module, e.g. in the form of a hollow fiber, capillary or flat membrane. This is formed from a large number of subordinate separating elements and allows in Dependence of the active surface of the membrane and / or the membrane thickness Permeability of impurities. In other words: about the design of the Separating elements of the membrane modules, the permitting mass flow is adjustable.
  • the Volume area of the electrolyte surrounding walls from a Inert material are formed. This advantageously ensures that all of the impurities to be removed from the electrolyte pass into the cleaning liquid and not become unwanted Way to the walls surrounding the volume area of the electrolyte adhere. It also ensures that not the electrolyte itself with the Wall material reacts with the formation of undesirable impurities.
  • the volume areas are receptacles.
  • the one receptacle serves the receptacle of the electrolyte and the other receptacle of the receptacle the cleaning liquid.
  • the volume range can also be done in a different way be trained, it is only crucial that the two Volume areas form a separate system and the electrolyte as well the cleaning fluid are fluidically independent of each other.
  • a volume area is connected to a circulating device.
  • a circulation device For example, a stir bar can be provided. This mixes the liquid in the volume range and thus ensures that a Consistent concentration of impurities over the entire volume range prevails.
  • a liquid pump can also be used as the circulating device be provided. Unlike a stir bar, one provides Liquid pump for a uniform and directional flow movement. In the event that both volume areas are each connected to a separate one Liquid feed pump can be connected, it can be provided that Electrolyte and cleaning fluid either in opposite directions or in the same direction on the Flow past the active surface of the separation unit.
  • a circulation device in the form of a pump is that due to the flow movement the impurities which have not diffused into the cleaning liquid immediately after transition into the cleaning liquid from the immediate vicinity of the Active surface of the separation unit are transported away. That way an optimized driving force gradient can be maintained.
  • the flow velocities are adjustable in the volume ranges. hereby can both an optimized concentration distribution, as well as an optimized Partial pressure can be set.
  • the cleaning performance of the inventive method by adjusting the intensive State variables of the electrolyte and / or the cleaning liquid can be set is.
  • the figure shows an electrolyte volume system 10 and a cleaning fluid volume system 20. These two volume systems 10 are separate and 20 by a common separation unit 3.
  • the electrolyte volume system 10 comprises a container 11, a liquid line 12 and a circulating device in the form of a pump 13, the The direction of conveyance is adjustable. The content of the container 11 is too cleaning electrolyte 1.
  • the cleaning liquid volume system 20 comprises a container 21, one Liquid line 22 and a circulating device in the form of a pump 23.
  • the delivery direction of the pump 23 is preferably freely selectable.
  • Content of the Container 21 is a cleaning liquid 2.
  • the electrolyte 1 and the cleaning liquid 2 are fluidically different from one another independently.
  • the separation unit 3 is permeable to the from the Electrolytes to remove impurities and can, for example, as Hollow fiber membrane can be designed. About the pumps 13 and 23 to one of the electrolyte 1 and the other the cleaning liquid 2 in motion held, being in the opposite or the same direction on the Separation unit 3 are passed.
  • the impurities in the electrolyte 1 are indicated by dots in the figure shown. As can be clearly seen from the figure, are in the shown situation only impurities in the electrolyte, but not in the cleaning liquid.
  • the impurity concentration gradient between Electrolyte and cleaning fluid thus take up in the situation shown here a maximum of. Because of this driving force gradient, those in the electrolyte 1 contaminants strives through the permeable separation unit 3rd diffuse into the cleaning liquid 2. Conversely, it means this means that the driving force or potential gradient is zero when the Impurity concentration in the electrolyte 1 is identical to that in the Cleaning liquid 2. In such a case, the cleaning of the Do not advance electrolytes.
  • Contamination concentration of the cleaning liquid 2 is kept lower than that of the electrolyte 1, i.e. the driving force gradient is always greater than zero. Keeping the impurity concentration low Cleaning liquid 2 permanently and continuously, i.e. during a electrolytic metal deposition, or alternatively in the Connection to a metal deposition in the sense of reprocessing of the electrolyte.
  • the material separation device 4 The function of the material separation device 4 is to the contaminants present in dissolved form, for example ions, that from the electrolyte 1 have passed into the cleaning liquid 2 and the cleaning liquid volume system 20 or the Separate cleaning liquid itself, for example by distillation. This has two advantages. For one thing, the same Cleaning liquid volume a reduction in the cleaning liquid 2 contaminants are reached, on the other hand, the precipitated so Contaminants can be reused. This is useful, for example when the electrolyte 1 is used for demetallization and the possibility recovery of valuable metals.
  • This first alternative of Cleaning is therefore based on either the cleaning liquid from the To remove electrolyte ingested impurities, for example what can be achieved by filtering, or the cleaning liquid itself through suitable measures, for example by distilling off, recover. Regardless of which process alternative is chosen, it is crucial that the cleaning is carried out continuously or discontinuously and can be operated in a circuit, so that for a perfect condition Cleaning liquid care can be taken.
  • the second alternative to Reduction of the concentration of impurities in the cleaning liquid 2 consists in the dilution.
  • a reservoir 7 is provided Dilution liquid, for example water, is provided. This is about one Line 8 connected to the liquid line 22.
  • valve 5 can Line 8 are shut off, wherein if necessary by opening valve 5 Dilution liquid is transferred from the reservoir 7 into the liquid line 22 can be.
  • a pump 6 is used to transfer the dilution liquid intended. This alternative way of reducing concentration is on easily realized. The degree of dilution is proportional to Concentration reduction.
  • the two can be done beforehand mentioned alternative possibilities can also be combined with each other.
  • These amounts of contaminated cleaning fluid can then according to the first alternative are preferably cleaned in the form that in Bottom line cleaned and reusable cleaning fluid for Available. This can then be returned to the cycle, whereby contaminated in the same amount as the purified liquid is added Liquid can be removed and cleaned.
  • the combination of both alternative recovery options offers the advantage that the from the Cleaning liquid separated from the circuit outside the circuit of Impurities can be freed, but at the same time the amount of in Circulating cleaning liquid can be kept constant.
  • the Cleaning liquid 2 and / or the separation unit 3 by the addition appropriate substances are selectively formed, i.e. either only certain Impurities can be removed from the electrolyte or certain impurities also against the potential gradient from the Electrolytes can be transported out into the cleaning liquid.
  • This measure ensures that very specific Impurities can be removed from the electrolyte, whereby a Pull out the impurities from the electrolyte a driving force or potential gradient is possible.
  • the selective Mass transfer can be achieved by various measures. So it can Selectivity of the cleaning liquid itself can be set. This can can be achieved, for example, by complex or cluster formers. Can also the cleaning liquid is geared towards certain impurities Solvents or mixtures of suitable solvents are added. In addition, the intense process conditions can be varied and require selective mass transport.
  • the core element of the invention is that the electrolyte has an active surface a separation unit is brought into contact, which is permeable to the from the Electrolytes to remove contaminants.
  • a separation unit is brought into contact, which is permeable to the from the Electrolytes to remove contaminants.
  • the active surface of the separation unit 3 is brought into contact, there is a transition in the direction of arrow 9 of the impurities from the electrolyte 1 in the Cleaning liquid 2. It is provided that for the duration of the cleaning process the contamination concentration of the cleaning liquid 2 is lower is held as that of the electrolyte 1.
  • a concentration meter 26 to provide the concentration of the electrolyte 1 Measures impurities. Such a concentration measurement can can of course also be carried out in the cleaning liquid circuit. The concentration measurement allows the exact setting of the Process parameters with regard to existing actual conditions. So can for example to achieve an optimized cleaning result intensive State variables changed depending on the measured concentration and for Achieve an optimized cleaning result continuously to the Process flow can be adapted.

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  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Cleaning By Liquid Or Steam (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)
EP00118640A 2000-08-29 2000-08-29 Verfahren zur Reinigung eines Elektrolyten Withdrawn EP1184487A1 (de)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP00118640A EP1184487A1 (de) 2000-08-29 2000-08-29 Verfahren zur Reinigung eines Elektrolyten
JP2001254394A JP2002105696A (ja) 2000-08-29 2001-08-24 電解液の清浄方法
US09/939,502 US6841074B2 (en) 2000-08-29 2001-08-24 Method and apparatus of purifying an electrolyte
CN01125266.9A CN1342788A (zh) 2000-08-29 2001-08-29 电解质净化方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP00118640A EP1184487A1 (de) 2000-08-29 2000-08-29 Verfahren zur Reinigung eines Elektrolyten

Publications (1)

Publication Number Publication Date
EP1184487A1 true EP1184487A1 (de) 2002-03-06

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ID=8169679

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Application Number Title Priority Date Filing Date
EP00118640A Withdrawn EP1184487A1 (de) 2000-08-29 2000-08-29 Verfahren zur Reinigung eines Elektrolyten

Country Status (4)

Country Link
US (1) US6841074B2 (zh)
EP (1) EP1184487A1 (zh)
JP (1) JP2002105696A (zh)
CN (1) CN1342788A (zh)

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TWI737554B (zh) * 2020-12-22 2021-08-21 鈦工房有限公司 金屬離子回收裝置

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US7168429B2 (en) * 2001-10-12 2007-01-30 Ric Investments, Llc Auto-titration pressure support system and method of using same
JP2004131766A (ja) * 2002-10-09 2004-04-30 Fujitsu Ltd Ｎｉめっき膜の製造方法
JP4510369B2 (ja) 2002-11-28 2010-07-21 日本リーロナール有限会社 電解銅めっき方法
DE102004002778C5 (de) * 2004-01-20 2017-04-20 Enthone Inc. Verfahren zur Regenerierung von Metallisierungsbädern
CA2469769A1 (en) * 2004-06-04 2005-12-04 Aker Kvaerner Canada Inc. Apparatus and method for spent alkali metal halide solution concentration using osmotic membrane distillation
EP1726683B1 (de) * 2005-05-25 2008-04-09 Enthone Inc. Verfahren und Vorrichtung zur Einstellung der Ionenkonzentration in Elektrolyten
ES2698205T3 (es) 2005-11-25 2019-02-01 Macdermid Enthone Inc Procedimiento y dispositivo para la purificación de soluciones de proceso
US20090301894A1 (en) * 2008-06-09 2009-12-10 Carsten Ehlers Method of fabricating an integrated circuit
GB0822362D0 (en) * 2008-12-08 2009-01-14 Surrey Aquatechnology Ltd Improved solvent removal
CN105274556B (zh) * 2015-11-09 2017-12-08 武汉科技大学 一种定向流电解工艺
US10345254B2 (en) * 2017-06-22 2019-07-09 Taiwan Semiconductor Manufacturing Co., Ltd. Detection method for electroplating process

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Publication number Priority date Publication date Assignee Title
TWI737554B (zh) * 2020-12-22 2021-08-21 鈦工房有限公司 金屬離子回收裝置

Also Published As

Publication number Publication date
US6841074B2 (en) 2005-01-11
US20020029974A1 (en) 2002-03-14
JP2002105696A (ja) 2002-04-10
CN1342788A (zh) 2002-04-03

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