EP3467157B1 - Composition de rechargement d'un matériau en métal - Google Patents

Composition de rechargement d'un matériau en métal Download PDF

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Publication number
EP3467157B1
EP3467157B1 EP17195558.6A EP17195558A EP3467157B1 EP 3467157 B1 EP3467157 B1 EP 3467157B1 EP 17195558 A EP17195558 A EP 17195558A EP 3467157 B1 EP3467157 B1 EP 3467157B1
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Prior art keywords
metal
composition
composition according
electrolytic bath
copper
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EP17195558.6A
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German (de)
English (en)
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EP3467157A1 (fr
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Ipt - International Plating Technologies GmbH
IPT International Plating Tech GmbH
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Ipt - International Plating Technologies GmbH
IPT International Plating Tech GmbH
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Priority to EP17195558.6A priority Critical patent/EP3467157B1/fr
Priority to DE102018124325.1A priority patent/DE102018124325A1/de
Publication of EP3467157A1 publication Critical patent/EP3467157A1/fr
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/12—Process control or regulation
    • C25D21/14—Controlled addition of electrolyte components
    • 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
    • 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
    • C25D3/04—Electroplating: Baths therefor from solutions of chromium
    • 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
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • 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
    • C25D3/20—Electroplating: Baths therefor from solutions of iron
    • 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
    • C25D3/22—Electroplating: Baths therefor from solutions of zinc
    • 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
    • C25D3/38—Electroplating: Baths therefor from solutions of copper

Definitions

  • the invention relates to a composition for replenishing a metal in an electrolytic bath, in particular for replenishing a metal in an electrolytic bath used for electroplating, a method for replenishing a metal in an electrolytic bath, and the use of the composition according to the invention.
  • the concentration of the metal or metal combination used for the coating in the electrolytic bath decreases in the course of the coating process.
  • the metal must therefore be added to the electrolytic bath.
  • Different methods are known for the subsequent dosing, e.g. replenishment using a soluble anode.
  • the WO 2009/152915 A2 shows a process for the galvanic copper coating, in which copper is metered in via a subsequent metering of granular copper carbonate or a suspension of copper carbonate in deionized water into a lower trough or into an additional container, or via an additional container with saturated solution and supply of the saturated solution.
  • the KR 10-2012-0114648 A shows a composition with nickel sulfate, nickel hydroxide and a dispersant and the addition of sodium carbonate.
  • the composition is intended for galvanic coating.
  • the invention relates to a composition for replenishing at least one metal in an electrolytic bath.
  • the composition contains a solution of a sulfate or sulfamate of a first metal; a carbonate or oxide of the first metal dispersed in the solution; and a dispersant. It has been shown that high metal concentrations can be achieved with such a composition. It has also been shown that there is little or no crystal formation in the composition. For example, the composition is more stable than a pure nickel sulfate solution, in which clear crystal formation occurs.
  • the solution of a sulfate or sulfamate of a first metal is a saturated solution. Saturation can also occur through the addition of the metal carbonate or metal oxide. In one embodiment, the solution is an aqueous solution.
  • the first metal is nickel, copper, tin, zinc, iron or chromium. In a special embodiment, the first metal is copper. In another special embodiment, the first metal is nickel. In a further special embodiment, the first metal is chromium. In a further special embodiment, the first metal is zinc. In a further special embodiment, the first metal is iron.
  • the solution contains at least one other metal other than the first metal, which is selected from the group consisting of nickel, copper, tin, zinc, iron and chromium.
  • a carbonate of at least one other metal from the group consisting of nickel, copper, tin, zinc, iron and chromium is dispersed in the solution.
  • the first metal is zinc and the second metal is nickel. In another specific embodiment, the first metal is zinc and the second metal is iron.
  • a carbonate of the first metal is dispersed in the solution.
  • the metal carbonate is partially dissolved and partially dispersed in the solution.
  • the metal carbonate partially dissolves in the solution with the release of carbon dioxide. This also increases the pH of the composition.
  • the dispersion works in the same way with a corresponding metal oxide, for example nickel (II) oxide, copper (I) oxide, or copper (II) oxide.
  • the composition may preferably contain up to about 800 g / L metal carbonate in dispersed form. It is therefore possible to achieve significantly higher metal contents than, for example, in aqueous suspensions of metal carbonates. With copper, metal concentrations above 800 g / L could be achieved.
  • the concentration of the metal is preferably above 200 g / L and particularly preferably above 350 g / L. When specifying the concentration of the metal, the metal ions are also taken into account, since these also lead to an increase in the metal concentration in the galvanic bath.
  • the concentration can be determined depending on the needs of the customer and can be adapted, for example, to the consumption rate of the metal in the electroplating bath in order to enable a suitable replenishment.
  • the composition preferably contains at least one dispersant.
  • Dispersants are substances which facilitate the dispersing of solids, ie the metal carbonates or metal oxides contained in the composition, in a liquid, ie in the metal sulfate or metal sulfamate solution contained in the composition, by reducing the interfacial tension between the two components, so bring about wetting.
  • the dispersants support the formation of a stable suspension of the metal carbonates or metal oxides.
  • suitable dispersants include silica, polyethylene glycol, polyacrylamide, cellulose, methyl cellulose, hydroxyethyl cellulose and hydroxypropyl cellulose.
  • the dispersant is silica, preferably pyrogenic silica.
  • the amount of dispersant in the composition should be at least large enough to ensure stable dispersion of the metal carbonate or metal oxide. However, significantly higher amounts of dispersant can also be present in order to adjust the viscosity of the composition to a desired value. In one embodiment, the dispersant also functions as a thixotropic agent. The viscosity of the composition can be adjusted from thin to pasty as required.
  • the viscosity of the composition measured according to EN ISO 2555 at 25 ° C. with a type A viscometer, standard spindle 6, at 50 rpm, is from 10,000 to 30,000 mPa ⁇ s. In another embodiment of the invention, the viscosity of the composition, measured according to EN ISO 2555 at 25 ° C. with a type A viscometer, standard spindle 3, at 50 rpm, is from 500 to 5,000 mPa ⁇ s.
  • the viscosity of the compositions in the fully stirred state can be influenced, for example, by the amount of the dispersant or by other additives.
  • the viscosity of the composition in the fully stirred state is preferably at least 50 mPas, more preferably at least 100 mPas, particularly preferably at least 300 mPas (measured in accordance with EN ISO 2555 at 25 ° C. with a type A viscometer , Standard spindle 1, at 10 rpm).
  • the composition contains at least one defoamer.
  • suitable defoamers include silicone oils with silica dispersed therein and dimethylpolysiloxanes.
  • silicon-free defoamers include diglycerides of fatty acids and phosphoric acid esters such as trin-butyl phosphate and triisopropyl phosphate. Experiments have shown that the use of a defoamer leads to a reduction in sedimentation in the dispersion.
  • the composition can be prepared using a solution of a sulfate or sulfamate of the first metal; a carbonate or oxide of the first metal; and a dispersant.
  • the solution of a sulfate or sulfamate of the first metal is preferably added in a first step, then the dispersant is added, and the carbonate of the first metal or the oxide of the first metal is then added.
  • the composition can be made with the addition of at least a portion of the carbonate or oxide of the first metal after the addition of dispersant. This addition of the dispersant or at least a part thereof before the addition of the metal carbonate or metal oxide prevents segregation or settling in the dispersion.
  • the dispersant can also be added after the addition of the metal carbonate or metal oxide.
  • a defoamer can then optionally be added.
  • the metal carbonate is not used as a dry powder, but rather as carbonate sludge, as is obtained as an intermediate in the technical production of the metal carbonates.
  • the composition can be used for replenishment for all types of electrolyte baths. In addition to acid baths, it can also be used in alkaline and cyanide baths.
  • the advantages of the composition include that it can maintain a sufficiently high metal content in the electrolytic bath so that a soluble anode can be dispensed with. It can therefore be used advantageously in systems with an insoluble anode, in which the anode is not used to replenish the metal.
  • the composition also offers advantages for occupational safety and environmental protection. For example, there is no dust when transferring and dosing, as happens with powders.
  • the composition is a paste, i.e. it has such a high solids content that it is spreadable. This offers additional advantages in handling, especially for occupational safety and environmental protection. In contrast to low-viscosity preparations, there is no risk of splashing or leaking. Due to the high metal concentration, lower transport volumes are incurred.
  • the pasty shape also offers the possibility of using a peristaltic pump or a squeeze cylinder for dosing. Certain delivery heights provide simple and precise dosing.
  • the filling container and dosing unit can be one unit, with the possibility of returning the container in the sense of recycling.
  • the invention also relates to a method for replenishing at least one metal into an electrolytic bath which contains this metal.
  • a composition containing the metal to be replenished is added to the electrolytic bath.
  • the metal to be replenished is nickel, copper, tin, zinc, iron or chromium.
  • the invention also relates to the use of the composition for adjusting the concentration of a metal in an electrolytic bath.
  • the metal is nickel, copper, tin, zinc, iron or chromium.
  • nickel sulfate solution 120 g / L Ni
  • pyrogenic silica was added as a dispersing agent while stirring.
  • 400 g of basic nickel carbonate nickel hydroxycarbonate, NiCO 3 .3Ni (OH) 2 .4H 2 O
  • ES 561 silicon-containing defoamer
  • the nickel sulfate solution contains residues of sulfuric acid. Part of the nickel carbonate is dissolved by the sulfuric acid and carbon dioxide is produced. In experiments, the addition of the metal carbonate has caused the pH to increase to above 6.0, for example 6.5.
  • the composition had thickened somewhat after a rest period of several days. However, the thickening could be removed again by stirring. In addition, a slight settling of the nickel carbonate occurred after several days. Due to the dispersant, the settling could also be reversed by stirring. Experiments without the dispersant have led to heavy settling and the formation of a compact nickel carbonate layer. Stirring with a commercially available mixer is hardly possible in this condition.
  • fumed silica was used as the dispersant stirred in until a concentration of 5 g / L was reached. This corresponds to an artificial aging of the nickel bath by replenishing a composition according to the invention. Coating was carried out in a beaker with low and high current densities in the range from 2.5 to 25.0 A / dm 2 on a standardized area of 0.25 dm 2 . Despite the relatively high concentration of the silica, there was no negative influence on the coating result.
  • composition proved to be largely stable over several days. A slight settling was evident in the beaker after several days, and a clear phase was visible at the top, which disappeared again by stirring. In a larger 25 l container, on the other hand, there was hardly any evidence of settling after three days.
  • the mass fraction can also be given.
  • 0.94% by weight of silica corresponds to a mass fraction of silica of 0.0094.
  • the composition proved to be largely stable over several days.
  • a composition was prepared as in Example 3, but microfibrillated cellulose was used instead of silica and no defoamer was added. 75-100 ml of a 2% aqueous solution of microfibrillated cellulose (Exilva® F01-L or Exilva F01 V; Borregaard, 1701 Sarpsborg, Norway) were used in 1 l of nickel sulfate solution with 120 g / L Ni.
  • the composition proved to be largely stable over several days.
  • the solution gradually thickened during storage, but could be liquefied again by shaking.
  • the electrolyte baths with 110 g / l nickel content were operated for three months, the metal content being supplemented if necessary with a composition according to the invention prepared according to Example 3.
  • a total amount of nickel was added that corresponds to 1.5 times the total metal content of the baths.
  • Viscosity measurements were carried out on compositions according to the invention using a RVDV3TX viscometer from Brookfield Engineering.
  • Viscosity measurements were carried out on compositions according to the invention using a RVDV3TX viscometer from Brookfield Engineering.
  • Viscosity measurements were carried out on compositions according to the invention using a RVDV3TX viscometer from Brookfield Engineering.
  • Viscosity measurements were carried out on compositions according to the invention using a RVDV3TX viscometer from Brookfield Engineering.
  • Viscosity measurements were carried out on compositions according to the invention using a RVDV3TX viscometer from Brookfield Engineering.
  • viscosities of 17,500 mPa ⁇ s were measured in the unstirred state (25 ° C., standard spindle 3, 1 rpm).
  • the viscosity was in the order of 770 mPa ⁇ s (25 ° C, standard spindle 3, 10 rpm).
  • Fig. 1 shows a galvanizing system 10 in which the composition according to the invention can be used for metal replenishment.
  • the electroplating system 10 has an upper trough (container) 12 and a lower trough (container) 14.
  • an electrolytic bath 32 In the lower tub 14 there is an electrolytic bath 32, a heater 16, a cooling 18, a circulating device 20, e.g. in the form of a pump and / or an agitator, and a controllable depletion device 22 for reducing the copper concentration if necessary.
  • an electrolytic bath 30 In the upper tub 12 there is an electrolytic bath 30, an insoluble, dimensionally stable anode 40, a circulating device 54 and a shaft 42 which is supported by two rotary bearings 44, 46 and which can be driven by a motor 48 and raised and lowered by a height adjustment device.
  • a direct current device (e.g. rectifier with current control) 52 is usually contacted with its minus connection on the shaft 42 and its plus connection on the anode 40.
  • a fluid connection 24 with a controllable pump 26 enables the electrolytic bath 32 to be pumped from the lower tub 14 into the upper tub 12, and a fluid connection 28 with a controllable valve 29 enables the electrolytic bath 30 to be drained into the lower tub 14.
  • a replenishment container (Scdazzling) 76A is filled with a composition 79A according to the invention containing copper and is connected to the upper tub 12 via a controllable valve 78A.
  • a replenishment container (chute) 76B is filled with a composition 79B according to the invention containing copper and is connected to the lower trough 12 via a controllable valve 78B.
  • An energy measuring device 84 is provided on the direct current device 52, a copper concentration measuring device 81 in the upper trough 12, and a copper concentration measuring device 82 in the lower trough 14.
  • the signals of the energy measuring device 84 and the copper concentration measuring devices 81, 82 are fed to a control device 80 via lines, and the control device 80 is used to control or output control signals via control lines with the controllable (metering) valves 29, 78A and 78B , connected to the controllable (metering) pump 66 and to the controllable depletion device 22.
  • the galvanic coating of the printing cylinder 50 with copper this is e.g. 20% to 100%, preferably about 50%, lowered into the electrolytic bath 30 and rotated continuously via the motor 48.
  • the current flowing between the anode 40 and the pressure cylinder (cathode) 50 causes copper to be deposited on the pressure cylinder 50 depending on the current density.
  • the temperature of the electrolytic bath is e.g. between 18 ° C and 60 ° C.
  • the electrolytic bath can either be finished (e.g. "ROTOCOPPER Make-Up” from IPT International Plating Technologies GmbH) or e.g. from the components of copper sulfate solution, deionized water, concentrated sulfuric acid and a hardness additive (e.g. ROTOCOPPER HS from IPT International Plating Technologies GmbH).
  • the electrolytic bath is initially filled into the lower trough 14 and brought to the predetermined temperature there via the heating 16 or cooling 18.
  • the electrolytic bath 32 is then pumped into the upper tub 12 via the pump 26.
  • the electrolytic baths 30 and 32 have similar properties, and by increasing the copper concentration in the lower one Trough 14, for example, the copper concentration in the upper trough 12 can also be increased, and conversely, by increasing the copper concentration in the upper trough 12, the copper concentration in the lower trough 14 can also be increased.
  • the copper concentration measuring device 81 in the upper trough 12 and the copper concentration measuring device 82 in the lower trough 14 monitor the copper concentration and control the controllable (metering) valves 78A and 78B via the control device 80 to supply the composition 79A according to the invention to the electrolytic bath 34 or 79B.
  • the copper carbonate dispersed in the composition 79A or 79B according to the invention dissolves in the sulfuric acid electrolytic bath 34. This increases or maintains the concentration of copper. When released, carbon dioxide is generated, which escapes or is extracted as a gas.
  • composition 79A may be zinc as the first metal-containing composition and composition 79B may be iron or nickel as the first metal-containing composition.

Claims (13)

  1. Composition de rechargement d'au moins un métal dans un bain électrolytique, ladite composition contenant :
    une solution d'un sulfate ou d'un sulfamate d'un premier métal ;
    un carbonate ou un oxyde du premier métal dispersé dans la solution ; et
    un agent dispersant,
    caractérisée en ce que la composition présente une concentration en métal supérieure à 120 g/L.
  2. Composition selon la revendication 1, dans laquelle la solution d'un sulfate ou d'un sulfamate d'un premier métal est une solution saturée.
  3. Composition selon la revendication 1 ou 2, dans laquelle le premier métal est le nickel, le cuivre, l'étain, le zinc, le fer ou le chrome.
  4. Composition selon l'une des revendications précédentes, dans laquelle l'agent dispersant contient de l'acide silicique, du polyéthylèneglycol, du polyacrylamide, de la cellulose, de la méthylcellulose, de l'hydroxyéthylcellulose ou de l'hydroxypropylcellulose.
  5. Composition selon l'une des revendications précédentes, contenant un agent antimoussant qui est notamment une huile de silicone, contenant de l'acide silicique dispersé, ou un diméthylpolysiloxane.
  6. Composition selon l'une des revendications précédentes, dans laquelle le carbonate de métal ou l'oxyde métallique est présent en partie à l'état dissous et en partie à l'état dispersé.
  7. Composition selon l'une des revendications précédentes, dans laquelle la solution contient au moins un autre métal différent du premier, choisi dans le groupe constitué du nickel, du cuivre, de l'étain, du zinc, du fer et du chrome.
  8. Composition selon l'une des revendications précédentes, présentant une concentration en métal entre 200 g/L et 800 g/L et de préférence entre 350 g/L et 800 g/L.
  9. Composition selon l'une des revendications précédentes, présentant une viscosité à l'état parfaitement remué d'au moins 50 mPa·s, mesurée selon EN ISO 2555 à 25°C à l'aide d'un viscosimètre de type A, en utilisant une broche standard 1, à 10 rpm.
  10. Procédé de rechargement d'au moins un matériau dans un bain électrolytique contenant ce métal, dans lequel une solution contenant ce métal selon l'une des revendications précédentes est introduite dans le bain électrolytique.
  11. Procédé selon la revendication 10, dans lequel au moins deux compositions selon l'une des revendications 1 à 9 sont introduites dans le bain électrolytique, chacune des compositions contenant un métal différent.
  12. Utilisation d'une composition selon l'une des revendications 1 à 9 pour ajuster la concentration d'un métal dans un bain électrolytique.
  13. Utilisation selon la revendication 12 avec une anode insoluble.
EP17195558.6A 2017-10-09 2017-10-09 Composition de rechargement d'un matériau en métal Active EP3467157B1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP17195558.6A EP3467157B1 (fr) 2017-10-09 2017-10-09 Composition de rechargement d'un matériau en métal
DE102018124325.1A DE102018124325A1 (de) 2017-10-09 2018-10-02 Zusammensetzung zur Nachdosierung eines Metalls

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP17195558.6A EP3467157B1 (fr) 2017-10-09 2017-10-09 Composition de rechargement d'un matériau en métal

Publications (2)

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EP3467157A1 EP3467157A1 (fr) 2019-04-10
EP3467157B1 true EP3467157B1 (fr) 2020-04-15

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DE (1) DE102018124325A1 (fr)

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1957158A1 (de) * 1969-11-13 1971-05-19 Dr Dettner Heinz W Nickelbadzusatz-Tabletten und Verfahren zu ihrer Herstellung
DE102009023124A1 (de) 2008-05-28 2009-12-03 Ipt International Plating Technologies Gmbh Verfahren zur galvanischen Kupferbeschichtung und Vorrichtung zur Durchführung eines solchen Verfahrens
KR101173879B1 (ko) * 2011-03-22 2012-08-14 남동화학(주) 니켈플래시 도금용 다기능성 과포화 슬러리 도금용액
KR101264089B1 (ko) * 2011-04-07 2013-05-14 주식회사 유니테크 수산화니켈 슬러리 도금 조성물
JP6384369B2 (ja) * 2015-03-16 2018-09-05 三菱マテリアル株式会社 Ｓｎ合金めっき用Ｓｎ補給剤

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

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