EP1816237A1 - Verfahren und Vorrichtung zur Beschichtung von Substratoberflächen - Google Patents

Verfahren und Vorrichtung zur Beschichtung von Substratoberflächen Download PDF

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Publication number
EP1816237A1
EP1816237A1 EP06002099A EP06002099A EP1816237A1 EP 1816237 A1 EP1816237 A1 EP 1816237A1 EP 06002099 A EP06002099 A EP 06002099A EP 06002099 A EP06002099 A EP 06002099A EP 1816237 A1 EP1816237 A1 EP 1816237A1
Authority
EP
European Patent Office
Prior art keywords
electrolyte
density
coating
bath
density value
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Withdrawn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
EP06002099A
Other languages
German (de)
English (en)
French (fr)
Inventor
Helmut Horsthemke
Franz-Josef Stark
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 Inc
Original Assignee
Enthone Inc
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 Inc filed Critical Enthone Inc
Priority to EP06002099A priority Critical patent/EP1816237A1/de
Priority to JP2008552727A priority patent/JP5695295B2/ja
Priority to PCT/EP2007/000658 priority patent/WO2007088008A2/de
Priority to PL07703047T priority patent/PL1979511T3/pl
Priority to ES07703047T priority patent/ES2706874T3/es
Priority to US12/278,256 priority patent/US20090324804A1/en
Priority to EP07703047.6A priority patent/EP1979511B1/de
Priority to KR1020087021543A priority patent/KR101466995B1/ko
Priority to CN2007800119432A priority patent/CN101437986B/zh
Publication of EP1816237A1 publication Critical patent/EP1816237A1/de
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • C23C18/1633—Process of electroless plating
    • C23C18/1675—Process conditions
    • C23C18/1683—Control of electrolyte composition, e.g. measurement, adjustment
    • 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
    • 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
    • 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
    • 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
    • C23C18/31—Coating with metals
    • C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
    • C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
    • 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

Definitions

  • the present invention relates to a method and a device for coating substrate surfaces with a metallic or oxidic layer in a coating bath.
  • a substrate surface is to be provided with a metallic coating
  • the substrate to be coated is brought into contact with a treatment solution which contains the metal to be deposited in the form of its cations.
  • the cations in solution can be deposited as a metallic layer on the substrate surface.
  • the reduction can take place with the aid of a voltage applied between the substrate and a counterelectrode or else by means of reducing agents present in the solution. Accordingly, they are galvanic (electrochemical) or autocatalytic (electroless) coating processes.
  • the treatment solutions which are generally referred to as electrolytes, comprise further additives which, in particular, have the properties of the deposited layers, such as, for example, B. influence the compressive residual stress or hardness.
  • the said method has in common that the electrolytes used change their composition during the treatment process.
  • the electrolyte is depleted by the ions of the metal to be deposited.
  • corresponding metal ion releasing components must be added to the electrolyte.
  • a measure of the performance of an electrolyte is the number of so-called metal turn-overs (MTO).
  • MTO metal turn-overs
  • This object is achieved with regard to the method by a method for coating substrate surfaces with a metallic or oxidic layer in a coating bath, wherein the bath has at least one component whose concentration changes in the course of the coating process and which as a result complements or maintains the bath quality must be removed, characterized in that the addition and / or removal of the electrolyte component takes place in dependence on the density of the bath composition.
  • this is achieved by determining the density of the electrolyte, comparing the determined density value with a stored nominal density value for an optimum electrolyte composition, ie an electrolyte composition in the equilibrium state, and at least one component of the electrolyte as a function of the deviation of the determined density value from the nominal density value removed and / or supplemented.
  • this can be done by continuously withdrawing from the coating bath a tunable amount of the electrolyte composition from the electrolyte, thereby artificially depriving electrolyte.
  • the method according to the invention deposits layers while the electrolyte composition remains the same, resulting in consistent coating results and layer properties, such as consistently high compressive residual stress, over the entire period of use of the electrolyte.
  • the determination of the density of the electrolyte composition may be continuous or discontinuous during the coating process.
  • the determined density value of the coating bath is compared according to the invention with a setpoint density value and the supplementation and / or removal takes place as a function of the deviation of the determined density value from the setpoint density value.
  • the setpoint density value can be stored in a data storage unit.
  • the setpoint density value can then be compared by means of a computer unit with the determined density value of the coating bath.
  • the computer unit determines the deviation of the current density value of the coating bath from the setpoint density value and determines the one to be taken and / or to be supplemented amount of electrolyte composition or at least one component thereof.
  • the computer unit controls an electronically controllable removal and / or supplemental device for removing or supplementing the electrolyte composition or at least one component of the electrolyte composition, with the proviso to adjust the density of the coating bath to the stored nominal density value.
  • the withdrawn amount of electrolyte or electrolyte component can be collected and fed to a central reprocessing.
  • electrolytes can be used in the equilibrium state, which can be held in this by means of the method according to the invention.
  • the user immediately has an electrolyte available, which immediately, ie without start-up phase, delivers consistent coating results.
  • the inventive method can be used both for the galvanic and for the autocatalytic deposition of metal or metal alloy layers on surfaces of a substrate.
  • the method according to the invention can also be used in treatment solutions for forming an oxide layer on the surface of a metallic substrate.
  • These treatment solutions can also be optimized by controlling the density of the treatment solution. For example, the anodizing of aluminum surfaces is mentioned here.
  • an apparatus for the continuous extraction and / or addition of at least one electrolyte component of an electrolyte for coating substrate surfaces with a metal or oxide layer which is a device for removing and / or adding at least one electrolyte component, means for Determining the density of the electrolyte and a computer unit, wherein the means for removing and / or adding the at least one electrolyte component is controlled by the computer unit, wherein the Computer unit compares the determined by the device for determining the density of the electrolyte density value with a stored target density value, with the proviso that the density of the electrolyte is adjusted to the predetermined and stored in the data storage device setpoint density by adding and / or removing at least one component of the electrolyte.
  • the means for adding and / or removing may advantageously be a pump or a valve.
  • the device for determining the density may be a pycnometer, a spindle, a density balance, a bending vibrator or any other suitable device for density determination.
  • the density can be determined indirectly via the calculation index by means of a refractometer.
  • the device according to the invention can comprise further devices for determining bathing properties such as temperature, conductivity, pH, specific extinction or absorption, turbidity, wherein the values determined by means of this device can also be fed to the computer unit and compared with desired values stored in the storage device can be, with the computer unit can further control the determined bathing properties influencing facilities such as heating and cooling systems, filter systems or regeneration systems, with the proviso to adjust the bathing properties to the stored setpoints.
  • bathing properties such as temperature, conductivity, pH, specific extinction or absorption, turbidity
  • the device according to the invention can be integrated into existing coating systems.
  • the amount of electrolyte removed by the device, or at least one component of the electrolyte, may be collected in suitable equipment and sent for central reprocessing.
  • suitable devices may be, for example, reusable containers, tank systems and the like.
  • the method according to the invention and the device according to the invention can be combined with further methods or devices for improving the duration of use of electrolyte compositions.
  • the inventive method can be with that of the European patent application EP 1 413 646 A2 combine known methods for electroless deposition of metals, in which metal base salts are used, the anions are volatile.
  • the increase in density occurring during the lifetime of an electrolyte is reduced by the escape of the anions from the electrolyte composition, which can be further optimized in combination with the method according to the invention and the device according to the invention.
  • FIG. 1 shows the profile of the density of different electrolyte compositions as a function of the operating time of the electrolyte and the amount of electrolyte withdrawn.
  • Curve No. 1 shows the density profile of an electrolyte known from the prior art for the deposition of nickel layers.
  • Curve No. 2 shows the density profile of an electrolyte known from the prior art for depositing a nickel layer at a set removal quantity of electrolyte of 3.3%.
  • Curve No. 3 shows the density profile of an electrolyte, as it is known from the European patent application EP 1 413 646 is known and in which metal salts are used as the metal base salt of the electrolyte composition, the anions are volatile.
  • Curve No. 4 shows the electrolyte described in Curve No. 3 at a 3.3% electrolyte removal set.
  • Curve No. 5 shows the electrolyte described for Curve No. 3 at a set removal amount of electrolyte of 10%.
  • the designated in Fig. 2 with no. 6 area represents the optimum working range for electrolytes. It can be seen that at a set continuous withdrawal of 3.3% for one of the EP 1 413 646 A2 known electrolyte composition without leaving the optimum working range already 10 MTO's can be achieved. At a set continuous removal of 10%, the upper limit of the density of the optimum working range for one of the EP 1 413 646 A2 known electrolyte is no longer achieved and the electrolyte composition has a theoretically unlimited life.
  • Fig. 3 shows the relative loss of material in the electrolyte per MTO compared to the electrolyte age in the equilibrium state.
  • the left boundary represents a conventional electrolyte system.
  • the right boundary corresponds to an electrolyte system according to the EP 1 413 646 A2 ,
  • FIG. 4 shows a process diagram of a device according to the invention.
  • the individual components required for the production of the electrolyte are transferred into the electrolyte bath 2 by means of suitable conveying media, such as pumps.
  • the electrolyte composition in the electrolyte bath 2 is either directly in the electrolyte bath or in an external one supplied with a partial flow from the electrolyte bath Control Module 3 analyzed for its chemical-physical properties such as density, pH, temperature, conductivity or metal content. If a partial flow of the electrolyte is removed from the electrolyte bath 2, this can optionally be supplied to a heat recovery 5.
  • Both the component containers 1A to 1F and the electrolyte bath and the receptacle for removed electrolyte advantageously have fill level sensors which register an exceeding or falling below filling limits and output appropriate messages and / or initiate appropriate process steps to maintain the trouble-free coating operation.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Automation & Control Theory (AREA)
  • Chemically Coating (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
EP06002099A 2006-02-02 2006-02-02 Verfahren und Vorrichtung zur Beschichtung von Substratoberflächen Withdrawn EP1816237A1 (de)

Priority Applications (9)

Application Number Priority Date Filing Date Title
EP06002099A EP1816237A1 (de) 2006-02-02 2006-02-02 Verfahren und Vorrichtung zur Beschichtung von Substratoberflächen
JP2008552727A JP5695295B2 (ja) 2006-02-02 2007-01-26 基板表面をコーティングする方法および装置
PCT/EP2007/000658 WO2007088008A2 (de) 2006-02-02 2007-01-26 Verfahren und vorrichtung zur beschichtung von substratoberflächen
PL07703047T PL1979511T3 (pl) 2006-02-02 2007-01-26 Sposób powlekania powierzchni substratu
ES07703047T ES2706874T3 (es) 2006-02-02 2007-01-26 Procedimiento para el revestimiento de superficies de sustrato
US12/278,256 US20090324804A1 (en) 2006-02-02 2007-01-26 Method and device for coating substrate surfaces
EP07703047.6A EP1979511B1 (de) 2006-02-02 2007-01-26 Verfahren zur beschichtung von substratoberflächen
KR1020087021543A KR101466995B1 (ko) 2006-02-02 2007-01-26 기재 표면을 코팅하는 방법 및 장치
CN2007800119432A CN101437986B (zh) 2006-02-02 2007-01-26 坯件表面镀层的方法与装置

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP06002099A EP1816237A1 (de) 2006-02-02 2006-02-02 Verfahren und Vorrichtung zur Beschichtung von Substratoberflächen

Publications (1)

Publication Number Publication Date
EP1816237A1 true EP1816237A1 (de) 2007-08-08

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Family Applications (2)

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EP06002099A Withdrawn EP1816237A1 (de) 2006-02-02 2006-02-02 Verfahren und Vorrichtung zur Beschichtung von Substratoberflächen
EP07703047.6A Active EP1979511B1 (de) 2006-02-02 2007-01-26 Verfahren zur beschichtung von substratoberflächen

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Application Number Title Priority Date Filing Date
EP07703047.6A Active EP1979511B1 (de) 2006-02-02 2007-01-26 Verfahren zur beschichtung von substratoberflächen

Country Status (8)

Country Link
US (1) US20090324804A1 (ja)
EP (2) EP1816237A1 (ja)
JP (1) JP5695295B2 (ja)
KR (1) KR101466995B1 (ja)
CN (1) CN101437986B (ja)
ES (1) ES2706874T3 (ja)
PL (1) PL1979511T3 (ja)
WO (1) WO2007088008A2 (ja)

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KR101635661B1 (ko) * 2009-07-03 2016-07-01 엔쏜 인코포레이티드 베타-아미노산 함유 전해질 및 금속 층 침착 방법
US20130087463A1 (en) * 2011-10-05 2013-04-11 Globalfoundries Inc. Method and System for Metal Deposition in Semiconductor Processing
KR101502795B1 (ko) * 2012-03-15 2015-03-13 김종호 포물선의 전체 또는 일부의 굴절경로를 갖는 진주광택 안료 입자 및 이의 제조방법
US9708693B2 (en) * 2014-06-03 2017-07-18 Macdermid Acumen, Inc. High phosphorus electroless nickel
DE102018008312A1 (de) 2018-10-22 2020-04-23 RIAG Oberflächentechnik AG Verfahren zur Beschichtung von Substratoberflächen, Vorrichtung mit Beschichtungsbad, Dichtemesseinrichtung, Entnahmeeinrichtung, Zugabeeinrichtungen und Steuerung
CN113755937B (zh) * 2021-09-09 2022-12-09 中国航发南方工业有限公司 电镀铂槽液的维护方法
CN114351231B (zh) * 2022-01-04 2022-11-25 深圳技术大学 电解液中金属离子浓度的测量和监控的设备和方法

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Also Published As

Publication number Publication date
JP2009525404A (ja) 2009-07-09
EP1979511A2 (de) 2008-10-15
CN101437986A (zh) 2009-05-20
ES2706874T3 (es) 2019-04-01
CN101437986B (zh) 2013-12-11
PL1979511T3 (pl) 2019-05-31
WO2007088008A2 (de) 2007-08-09
JP5695295B2 (ja) 2015-04-01
KR101466995B1 (ko) 2014-12-01
KR20080093451A (ko) 2008-10-21
US20090324804A1 (en) 2009-12-31
WO2007088008A3 (de) 2008-04-17
EP1979511B1 (de) 2018-10-31

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