EP0122963B1 - Appareil pour régénérer une solution ammoniacale de décapage - Google Patents

Appareil pour régénérer une solution ammoniacale de décapage Download PDF

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Publication number
EP0122963B1
EP0122963B1 EP83111152A EP83111152A EP0122963B1 EP 0122963 B1 EP0122963 B1 EP 0122963B1 EP 83111152 A EP83111152 A EP 83111152A EP 83111152 A EP83111152 A EP 83111152A EP 0122963 B1 EP0122963 B1 EP 0122963B1
Authority
EP
European Patent Office
Prior art keywords
etching solution
oxygen
line
etching
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.)
Expired
Application number
EP83111152A
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German (de)
English (en)
Other versions
EP0122963A1 (fr
Inventor
Wolfgang Faul
Leander Fürst
Walter Holzer
Bertel Prof. Dr. Kastening
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.)
Forschungszentrum Juelich GmbH
Original Assignee
Forschungszentrum Juelich GmbH
Kernforschungsanlage Juelich 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 Forschungszentrum Juelich GmbH, Kernforschungsanlage Juelich GmbH filed Critical Forschungszentrum Juelich GmbH
Priority to AT83111152T priority Critical patent/ATE34781T1/de
Publication of EP0122963A1 publication Critical patent/EP0122963A1/fr
Application granted granted Critical
Publication of EP0122963B1 publication Critical patent/EP0122963B1/fr
Expired legal-status Critical Current

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    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/46—Regeneration of etching compositions

Definitions

  • the invention relates to a system for regenerating an ammoniacal etching solution.
  • Oxygen is fed to the etching solution for the re-oxidation of the etchant contained in the etching solution, optionally in the presence of a catalyst contained in the etching solution.
  • a catalyst contained in the etching solution In order to recover etched metal, at least part of the etching solution flows through an electrolysis cell, metal being deposited cathodically and oxygen being produced at the anode of the electrolysis cell.
  • Alkaline etchants are used for etching metallic objects, in particular for the production of printed circuit boards, which are also known under the name “printed circuits”, especially when the printed circuit boards to be etched are metal parts which are not resistant to acidic etching media, for example made of lead, tin or nickel, exhibit.
  • a reoxidation of the alkaline etching solution after etching off the metal is carried out with the addition of ammonia gas and / or ammonium chloride in the presence of oxygen or air.
  • the etching solution containing the catalyst particles is sprayed in air for reoxidation. This is done directly in the etching chamber by spraying the etching solution onto the workpieces to be processed.
  • the reoxidation with air is not an advantage in all cases. This is particularly not the case because ammonia is added to the etching solution to adjust the pH and odor nuisances and environmental problems caused by evaporating ammonia should be kept as low as possible.
  • the object of the invention is to mix the etching solution intensively in a simple manner with a gas having a high oxygen content in a system of the type mentioned.
  • the oxygen formed at the anode of the electrolytic cell is fed to the etching solution.
  • the gas fractions introduced into the etching solution which do not contribute to the reoxidation, such as the nitrogen fractions in air, are low.
  • oxygen is advantageously used which arises in the electrolysis cell when the etched metal is recovered.
  • a liquid jet pump serves for the entry, the working medium of which is the etching solution and the suction nozzle of which is connected to an oxygen line connected to the electrolysis cell. With the liquid jet pump, rapid reoxidation is achieved through intensive mixing and fine distribution of the gases containing oxygen.
  • the oxygen line connected to the gas space above the electrolyte of the electrolysis cell is guided over a condenser in which the gas mixture is cooled and Water vapor is excreted.
  • the condensed water is used as rinsing water for the etched workpieces and thus reduces the total amount of detergent required.
  • the condensate line leading away the condensate from the condenser expediently opens into the last rinsing chamber of the system. It is advantageous that the water separated in the condenser contains ammonia.
  • ammonia it is expedient to add ammonia to the etching solution at the same time as the oxygen (claim 2) in order to adjust the pH of the etching solution. As much ammonia must be added to the etching solution as is essentially lost through evaporation during the etching in the etching chamber and when the etching solution is regenerated.
  • the ammonia escaping into the gas space above the electrolyte during regeneration in the electrolysis cell can be returned to the etching solution with the extracted oxygen.
  • the ammonia is introduced into the etching solution with the oxygen and, like the oxygen, is mixed intensively with the etching solution.
  • a pressure relief line branches off from the return in front of the liquid jet pump and opens into a collecting container for etching solution, which is connected to the etching chamber for receiving the etching solution removed from the etching chamber.
  • the collecting container is connected to the etching chamber in such a way that the etching solution flows into the collecting container in a natural gradient.
  • the filter protecting the electrolytic cell from the ingress of catalyst particles is not required.
  • the amount of water vapor generated in the electrolysis cell depends on the temperature in the electrolysis cell. With increasing electrolyte temperature, the water vapor content in the gas space above the electrolyte increases, and more condensate can then be obtained in the condenser. By adjusting the temperature in the electrolysis cell, the amount of condensate to be generated can be regulated, claim 6.
  • the maximum temperature in the electrolysis cell is limited by the required pH in the electrolyte. The pH value drops with increasing temperature because the ammonia content in the electrolyte drops. The electrolyte must remain alkaline, especially to protect the electrodes.
  • a regeneration system connected to an etching chamber 1 with a rinsing chamber 2 is shown schematically in FIG.
  • the ammoniacal etching solution to be regenerated which contains ammonium sulfate in conjunction with copper tetrammine complex as an etchant and catalyst particles suspended in the etching solution, flows from the etching chamber 1 via an inlet 3 to a filter 4.
  • the catalyst particles contained in the etching solution serve to increase the etching speed and / or to accelerate the reoxidation of the etching solution.
  • activated carbon particles as described in DE-A 3 031 567 are suitable for catalysis.
  • the inlet 3 is connected to the etching chamber 1 in such a way that the etching solution can first of all flow out of the etching chamber into a collecting container 5. It is guided from the collecting container to the filter 4 by means of a pump 6 via a pressure line 7.
  • the supply of the etching solution to the filter thus includes the supply 3 itself, the collecting container 5, the suspension pump 6 and the pressure line 7.
  • the filter 4 is provided with a filter insert 8 which is impermeable to the catalyst particles suspended in the etching solution.
  • the filter 4 is arranged vertically and the etching solution flows through it with catalyst particles from top to bottom.
  • a return 9 from the filter 4 leads back to the etching chamber 1. In the reflux 9, an etching solution containing catalyst particles is passed.
  • a liquid jet pump 10 is inserted in the return 9, the suction port 11 of which is connected to an oxygen line 12.
  • the liquid jet pump uses the etching solution flowing out of the filter 4 and containing catalyst particles as the working medium.
  • the oxygen line 12 starts from an electrolysis cell 13. A portion of the etching solution flows through the electrolytic cell to deposit metal etched off in the etching chamber at cathode 14. Catalyst particle-free etching solution is to be fed to the electrolytic cell. A connecting line 16, 16 ′, 16 ′′ connected to the filter 4 and the electrolysis cell 13 is used for this purpose. Oxygen is produced at the anode 17 of the electrolysis cell.
  • the oxygen line 12 opens into the gas space above the electrolyte of the electrolysis cell and thus becomes operational when the liquid jet pump 10 is in operation In addition to oxygen, there is also ammonia and water vapor in the gas space, which evaporate from the electrolyte according to its vapor pressure.
  • An ammonia line 18 leads to the supply of ammonia in the oxygen line 12 and is connected to a storage container 20 for ammonia which can be closed by means of a shut-off device 19.
  • Fresh liquid ammonia can thus be introduced into the etching solution containing the catalyst particles from the liquid jet pump 10 with the oxygen drawn off from the electrolytic cell in order to regulate the pH of the etching solution.
  • the shut-off device 19 is operatively connected to a pH value measuring device 21 inserted in the connecting line 16 with a measuring electrode. If the pH falls below a predetermined permissible limit value, the shut-off device 19 is opened and ammonia is introduced into the etching solution.
  • the pH value measuring device switches the shut-off device 19 with the aid of electrical control units.
  • a pressure relief line 22 opens into the return line 9 and is led to the drainage of etching solution in the collecting container 5.
  • An overflow 24 of etching solution depleted in metal ions leads from the outlet 23 of the electrolytic cell to the etching chamber.
  • the depleted ⁇ tzlö solution is mixed in the etching chamber as a fresh etching solution with the etching solution containing catalyst particles.
  • a drain container 25 Underneath the electrolysis cell 13 there is a drain container 25. It serves to empty the electrolysis cell and is connected to the bottom of the electrolysis cell 13 via an outlet 26 which can be shut off by means of a solenoid valve 27. Etching solution can also flow from the electrolysis cell 13 into the drain container 25 via a second overflow 28.
  • the quantity of etching solution to be conducted to the electrolytic cell 13 is measured by the flow meter 30.
  • the flow meter 30 is operatively connected to two controllable shut-off devices 31 and 32.
  • the flow meter 30 can effect the adjustment of the shut-off devices, for example mechanically, hydraulically, but also electrically. If the latter is desired, solenoid valves 31, 32 are used as shut-off devices.
  • the shut-off element 31 is inserted in the connecting line 16, the shut-off element 32 in a bypass 33 branching off from the connecting line 16 in front of the shut-off element 31.
  • the two shut-off elements are set in such a way that there is a constant in the connecting line part 16 'leading to the electrolysis cell Etching solution current sets.
  • the volume of etching solution to be introduced into the electrolysis cell per unit of time depends on the amount of metal that can be deposited in the electrolysis cell in the same unit of time.
  • the metal ion concentration in the etching solution measured by the device 29 determines the mode of operation of the electrolysis cell.
  • the device 29 is operatively connected to a three-way valve 34 inserted at the end of the connecting line part 16 ', to which on the one hand the end piece 16 "of the connecting line 16 leading to the electrolytic cell 13 is connected and on the other hand a bypass line 35 which opens into the bypass 33.
  • the three-way valve 34 opened toward the electrolysis cell 13. If the metal ion concentration of the etching solution falls below a predetermined value, the three-way valve 34 is switched over, and the etching solution then flows off via the bypass line 35. The electrolysis cell is switched off.
  • a solution pump 36 ensures circulation of the etching solution in the electrolysis cell 13.
  • the solution pump dips with its suction line 37 into the drain container 25, into which the etching solution flows via the overflow 28, and conveys the etching solution back in its pressure line 39 via a filter 38 to the electrolytic cell.
  • the etching solution enters the electrolysis cell between cathode 14 and anode 17.
  • the etching solution is emptied into the drain container 25 by opening the solenoid valve 27.
  • the etching solution is conveyed back from the drain container into the electrolysis cell by means of the solution pump 36.
  • an etching solution containing ammonium sulfate and copper tetrammine complex is used for etching copper.
  • the etching solution depleted of metal ions can serve as a rinsing solution for rinsing the workpieces etched in the etching chamber 1 after the end of the etching treatment.
  • the etched workpieces are to be cleaned in particular of catalyst particles still adhering.
  • the amount of etching solution required for this can be found in the overflow 24.
  • a rinsing line 40 which can be connected to the overflow 24 and which leads to the rinsing chamber 2 is shown in broken lines in FIG.
  • the rinsing chamber 2 and the etching chamber 1 are connected to one another in such a way that the etching solution can flow into the etching chamber after the rinsing process.
  • the system shown in FIG. 1 is to be supplemented by the condensation device shown in FIG.
  • the condensation device is the subject of both exemplary embodiments.
  • a condenser 42 is provided in the oxygen line 12 and a device 43 for regulating the electrolyte temperature is provided in the electrolysis cell 13.
  • a condensate line 44 leads from the condenser 42 to the rinsing chamber 2 of the etching system. The water separated in the condenser is used to rinse the etched workpieces.
  • the temperature in the electrolyte is regulated in the electrolytic cell by means of the device 43.
  • the amount of water vapor contained in the gas mixture increases with the electrolyte temperature.
  • the device 43 essentially serves to cool the electrolysis cell, which heats up during its operation as a result of the passage of current.
  • a high temperature constancy is achieved by designing the electrolysis cell with a cooling jacket through which cooling water flows, claim 14.
  • the amount of cooling water is regulated as a function of the temperature of the electrolyte.
  • FIG. 1 shows a regeneration system for an etching solution in which catalyst particles are suspended. If the oxygen input via the liquid jet pump and the intensive mixing of the oxygen with the etching solution and its fine distribution achieved is sufficient for rapid reoxidation, the catalyst particles are unnecessary and the system is simplified.
  • the filter 4 used in the pressure line 7 is omitted. Instead, as shown in the exemplary embodiment according to FIG. 2, a simple pipe connection 41 remains between the pressure line 7 and connecting line 16.
  • the regeneration system has individual parts which unchanged correspond to the design shown in FIG. 1, the same reference numerals as in FIG. 1 are entered in FIG.
  • an etching solution containing ammonium sulfate and copper tetrammine complex is also used in the system according to FIG. 2 for etching copper.
  • a temperature of 75 ° C. is set in the electrolysis cell by cooling the electrolyte when the etched copper is deposited.
  • About 5 m 3 / h of gas mixture are sucked out of the gas space above the electrolyte by the liquid jet pump from the electrolysis cell.
  • the electrolysis cell is closed, around 1.25 l / h of condensate can be generated from the gas mixture in the condenser as a rinsing agent under these conditions.
  • Approx. 500 l / h of oxygen are generated at the anode of the electrolysis cell at a current of 2400 A.
  • the etching solution containing copper ions introduced into the electrolytic cell was adjusted to a pH of 9.
  • curve A indicating the reoxidation of the etching solution when biospraying in the etching chamber
  • curve B representing the reoxidation by additionally introducing oxygen into the etching solution by means of the liquid jet pump.
  • the reoxidation in the etching solution is measured via the potential of the Cu ++ / Cu + - redox system against a calomel reference electrode (Hg / Hg 2 Cl 2 / saturated KCI).
  • Copper surfaces were etched with a copper tetrammine complex and ammonium sulfate containing etching solution with a copper content of 50 g / I and 150 g / I (NH 4 ) 2 S0 4 and with a pH value of 9 adjusted with ammonia at a temperature of 50 ° C.
  • the potential of the Cu ++ / Cu + redox system dropped from an initial value of 125 mV to approximately -60 mV within 3% minutes of the etching time. The reoxidation began after this etching time.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • ing And Chemical Polishing (AREA)
  • Manufacturing Of Printed Circuit Boards (AREA)
  • Weting (AREA)

Claims (8)

1. Installation de régénération d'une solution ammoniacale de gravure, qui contient des particules de catalyseur pour la réoxydation avec apport d'oxygène, comprenant un conduit d'amenée de la solution de gravure prélevée d'une chambre de gravure à un filtre qui n'est pas perméable aux particules de catalyseur de la solution de gravure, et, raccordé au filtre, un conduit de retour de la solution de décapage contenant des particules de catalyseur à la chambre de gravure, ainsi qu'une cellule d'électrolyse dans laquelle débouche un conduit de liaison raccordé au filtre et destiné à la solution de gravure exempte de particules de catalyseur que l'on peut obtenir comme filtrat, et qui comporte une sortie pouvant être raccordée à la chambre de gravure et destinée à une solution de gravure appauvrie en ions métalliques, caractérisée en ce que, dans le conduit de retour (9), est monté un éjecteur à liquide (10), dont le fluide moteur est la solution de gravure et dont la tubulure d'aspiration (11) communique avec un conduit pour de l'oxygène (12) dans lequel passe de l'oxygène ou un mélange contenant de l'oxygène et qui peut être alimenté par l'oxygène formé à l'anode (17) de la cellule d'électrolyse, et en ce que le conduit pour l'oxygène (12) est raccordé à l'espace réservé au gaz au-dessus de l'électrolyte de la cellule d'électrolyse (13) et va à la tubulure d'aspiration (11), en passant par un condenseur (42) destiné à séparer la vapeur d'eau du mélange gazeux passant dans le conduit pour l'oxygène (12), et en ce qu'un conduit pour le produit condensé (44), évacuant le produit condensé obtenu dans le condenseur (42), débouche dans une chambre de rinçage (2) montée en aval de la chambre de gravue (1).
2. Installation suivant la revendication 1, caractérisée en ce qu'au conduit pour l'oxygène (12) est raccordé un conduit d'amenée d'ammoniac (18,19,20), qui peut être fermé.
3. Installation suivant la revendication 1 ou 2, caractérisée en ce que, dans le conduit de retour (9), un conduit de déchargement de la pression (22) débouche en amont, considéré dans le sens d'écoulement de la solution de gravure, de l'éjecteur à liquide (10).
4. Installation suivant la revendication 3, caractérisée en ce que le conduit de déchargement de la pression (22) débouche dans une cuve de réception (5) qui, en vue de recevoir la solution de gravure prélevée de la chambre de gravure (1), communique avec la chambre de gravure (1).
5. Installation suivant la revendication 4, caractérisée en ce que la cuve de réception (5), est raccordée à la chambre de gravue (1), de façon que la solution de gravure s'écoule naturellement par gravité dans la cuve de réception (5).
6. Installation suivant l'une des revendications 1 à 5, caractérisée en ce que, pour produire une quantité de produit condensé donnée à l'avance, la cellule d'électrolyse (13) est munie d'un dispositif (43) de réglage de la température de l'électrolyte.
7. Installation suivant la revendication 6, caractérisée en ce que la cellule d'électrolyse (13) est entourée d'une chemise de refroidissement parcourue par de l'eau de refroidissement.
8. Installation de régénération d'une solution ammoniacale de gravure avec apport d'oxygène, comprenant un conduit d'amenée de la solution de gravure prélevée d'une chambre de gravure et un conduit de retour de la solution de gravure à la chambre de gravure, ainsi qu'une cellule d'électrolyse, dans laquelle débouche un conduit de liaison raccordé au conduit d'amenée et destiné à une partie de la solution de gravure, et qui comporte une sortie pouvant être raccordée à la chambre de gravure et destinée à la solution de gravure appauvrie en ions métalliques, caractérisée en ce que, dans le conduit de retour (9), est monté un éjecteur à liquide (10), dont le fluide moteur est la solution de gravure et dont la tubulure d'aspiration (11) communique avec un conduit pour de l'oxygène (12) dans lequel passe de l'oxygène ou un mélange contenant de l'oxygène et qui peut être alimenté par l'oxygène formé à l'anode (17) de la cellule d'électrolyse, et en ce que le conduit pour l'oxygène (12) est raccordé à l'espace réservé au gaz au-dessus de l'électrolyte de la cellule d'électrolyse (13) et va à la tubulure d'aspiration (11), en passant par un condenseur (42) destiné à séparer la vapeur d'eau du mélange gazeux passant dans le conduit pour l'oxygène (12), et en ce qu'un conduit pour le produit condensé (44), évacuant le produit condensé obtenu dans le condenseur (42), débouche dans une chambre de rinçage (2) montée en aval de la chambre de gravure (1).
EP83111152A 1983-04-13 1983-11-08 Appareil pour régénérer une solution ammoniacale de décapage Expired EP0122963B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT83111152T ATE34781T1 (de) 1983-04-13 1983-11-08 Anlage zum regenerieren einer ammoniakalischen aetzloesung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3313293 1983-04-13
DE3313293 1983-04-13

Publications (2)

Publication Number Publication Date
EP0122963A1 EP0122963A1 (fr) 1984-10-31
EP0122963B1 true EP0122963B1 (fr) 1988-06-01

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EP83111152A Expired EP0122963B1 (fr) 1983-04-13 1983-11-08 Appareil pour régénérer une solution ammoniacale de décapage

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EP (1) EP0122963B1 (fr)
JP (1) JPS6013083A (fr)
AT (1) ATE34781T1 (fr)
DE (1) DE3376853D1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2449164A1 (fr) * 1979-02-14 1980-09-12 Sogreah Bloc artificiel pour structures maritimes et fluviales
DE3345050A1 (de) * 1983-12-13 1985-06-20 Walter 7758 Meersburg Holzer Verfahren zum umweltfreundlichen aetzen von leiterplatten und vorrichtung zur ausuebung des arbeitsverfahrens
EP0393270A1 (fr) * 1989-04-21 1990-10-24 Ming-Hsing Lee Procédé de décapage de cuivre à l'aide d'une solution de gravure ammoniacale et reconditionnement de la solution usée
US5085730A (en) * 1990-11-16 1992-02-04 Macdermid, Incorporated Process for regenerating ammoniacal chloride etchants
US5248398A (en) * 1990-11-16 1993-09-28 Macdermid, Incorporated Process for direct electrolytic regeneration of chloride-based ammoniacal copper etchant bath
JP5711856B2 (ja) * 2011-10-08 2015-05-07 ヘルクレ、クリストフHERKLE, Christoph 銅の電解エッチングを行うエッチング装置

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2008766B2 (de) * 1970-02-23 1971-07-29 Licentia Patent Verwaltungs GmbH, 6000 Frankfurt Verfahren zum regenerieren einer kupferhaltigen aetzloesung insbesondere fuer die herstellung von gedruckten schaltungen
US3705061A (en) * 1971-03-19 1972-12-05 Southern California Chem Co In Continuous redox process for dissolving copper
DE2216269A1 (de) * 1972-04-05 1973-10-18 Hoellmueller Maschbau H Verfahren zum aetzen von kupfer und kupferlegierungen
US3785950A (en) * 1972-05-19 1974-01-15 E Newton Regeneration of spent etchant
DE2641905C2 (de) * 1976-09-17 1986-03-20 Geb. Bakulina Galina Aleksandrovna Batova Verfahren zur Regenerierung verbrauchter Ätzlösungen
DE3031567A1 (de) * 1980-08-21 1982-04-29 Elochem Ätztechnik GmbH, 7758 Meersburg Verfahren zum regenerieren einer ammoniakalischen aetzloesung

Also Published As

Publication number Publication date
DE3376853D1 (en) 1988-07-07
ATE34781T1 (de) 1988-06-15
EP0122963A1 (fr) 1984-10-31
JPS6013083A (ja) 1985-01-23
JPH0429745B2 (fr) 1992-05-19

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