US20050229847A1 - Method and device for in situ layer thickness determination - Google Patents

Method and device for in situ layer thickness determination Download PDF

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Publication number
US20050229847A1
US20050229847A1 US11/127,103 US12710305A US2005229847A1 US 20050229847 A1 US20050229847 A1 US 20050229847A1 US 12710305 A US12710305 A US 12710305A US 2005229847 A1 US2005229847 A1 US 2005229847A1
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Prior art keywords
layer thickness
sensor
coating process
coating
component
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US11/127,103
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Ulrich Bast
Roman Beyer
Ralph Reiche
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Individual
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Priority to US11/127,103 priority Critical patent/US20050229847A1/en
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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
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54—Controlling or regulating the coating process
    • C23C14/542—Controlling the film thickness or evaporation rate
    • C23C14/545—Controlling the film thickness or evaporation rate using measurement on deposited material
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/52—Controlling or regulating the coating process
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/14—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying for coating elongate material
    • C23C4/16—Wires; Tubes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
    • G01B7/02—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness
    • G01B7/06—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness for measuring thickness

Definitions

  • the invention generally relates to a method and/or device for layer thickness determination.
  • the layer thickness is determined by way of a metallographic examination.
  • a wire specimen is introduced into the coating process at a location which is representative of a component which is to be coated. After the coating process has ended, the wire specimen is removed and is then, expensively, cut open and examined. Each coating process is monitored and documented by the use of concomitant working specimens. These measuring and testing methods do not allow coating processes which are not to spec to be corrected as they are ongoing. Therefore, this is a very expensive form of quality assurance.
  • An object may be achieved by a method or device in which a sensor is exposed to the coating process in the same way as the component which is to be treated, and an electrical property of this sensor is measured. This property changes as a result of the coating process, so that in situ layer thickness determination during the coating process is possible.
  • the method is suitable in particular for alitizing processes in which aluminum is introduced into a component (refurbishment).
  • the electrical resistance is preferably used as a simple electrical measurement variable which is representative of the coating result.
  • the sensor is, for example, a sintered body, since a sintered body can take up the applied coating material in a representative way (accumulation and diffusion rate).
  • a sintered body can take up the applied coating material in a representative way (accumulation and diffusion rate).
  • it may be, for example, also porous or, for example, made from the material of the component which is to be coated or from MCrAlY.
  • the method and/or device is particularly suitable for coating processes in the interior of a component, since these are not readily accessible.
  • FIG. 1 shows a component with a sensor, which component is coated, with the method according to an embodiment of the invention being used for layer thickness determination, and
  • FIG. 2 shows a measuring arrangement having a sensor for the method according to an embodiment of the invention.
  • FIG. 1 shows a hollow component 1 which is to be coated, for example, on an inner surface 4 .
  • the method can also be used for the in situ layer thickness determination of external surfaces.
  • a layer 7 of the material M is applied to the inner surface 4 by means of known processes, such as for example CVD (chemical vapor deposition) processes, electrochemical processes or other known coating processes.
  • a sensor 10 is arranged in the cavity 19 of the component 1 and is therefore coated in the same way as the component 1 which is to be treated.
  • FIG. 2 shows an enlarged view of the sensor 10 .
  • the sensor 10 consists of a material which has an electrical property, such as for example its electrical resistance, impedance, capacitance or the like, which changes as a result of some form of interaction with the material M which forms the layer.
  • the sensor 10 may be of any desired shape, i.e. may, for example, be a piece of wire or in the shape of a small plate.
  • the sensor 10 is connected to an electrical measuring unit 16 via electrical lines 13 ; the measuring unit measures the electrical parameter which changes as a result of the sensor 10 being coated with the material M.
  • the way in which the layer thickness is dependent on the electrical variable is known from calibration curves determined in preliminary tests.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • General Physics & Mathematics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Measurement Of Length, Angles, Or The Like Using Electric Or Magnetic Means (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

A method and device for layer thickness determination allows for the layer thickness to be determined in situ during the coating process. This is achieved using a sensor which has an electrical property which, as a result of the coating process, changes in a manner which is representative of the layer thickness which has been reached. As such, this property can be measured.

Description

    DOMESTIC PRIORITY
  • This application is a divisional of allowed application Ser. No. 10/434,165, filed on May 9, 2003, the entire contents of which are hereby incorporated by reference and for which priority is claimed under 35 U.S.C. §120.
    • FOREIGN PRIORITY
  • The present application hereby claims priority under 35 U.S.C. §119 on European patent application number EP 02010628.2 filed May 10, 2002, the entire contents of which are hereby incorporated herein by reference.
    • FIELD OF THE INVENTION
  • The invention generally relates to a method and/or device for layer thickness determination.
    • BACKGROUND OF THE INVENTION
  • In coating processes, such as for example internal alitizing processes (aluminizing of internal surfaces), the layer thickness is determined by way of a metallographic examination. For this purpose, a wire specimen is introduced into the coating process at a location which is representative of a component which is to be coated. After the coating process has ended, the wire specimen is removed and is then, expensively, cut open and examined. Each coating process is monitored and documented by the use of concomitant working specimens. These measuring and testing methods do not allow coating processes which are not to spec to be corrected as they are ongoing. Therefore, this is a very expensive form of quality assurance.
    • SUMMARY OF THE INVENTION
  • It is an object of an embodiment of the invention to provide a method and device for layer thickness determination which solves at least one of the problems outlined above.
  • An object may be achieved by a method or device in which a sensor is exposed to the coating process in the same way as the component which is to be treated, and an electrical property of this sensor is measured. This property changes as a result of the coating process, so that in situ layer thickness determination during the coating process is possible.
  • The method is suitable in particular for alitizing processes in which aluminum is introduced into a component (refurbishment).
  • The electrical resistance is preferably used as a simple electrical measurement variable which is representative of the coating result.
  • The sensor is, for example, a sintered body, since a sintered body can take up the applied coating material in a representative way (accumulation and diffusion rate). Alternatively, it may be, for example, also porous or, for example, made from the material of the component which is to be coated or from MCrAlY.
  • The method and/or device is particularly suitable for coating processes in the interior of a component, since these are not readily accessible.
    • BRIEF DESCRIPTION OF THE DRAWINGS
  • An exemplary embodiment of the invention is illustrated in simplified form in the drawings, in which:
  • FIG. 1 shows a component with a sensor, which component is coated, with the method according to an embodiment of the invention being used for layer thickness determination, and
  • FIG. 2 shows a measuring arrangement having a sensor for the method according to an embodiment of the invention.
    • DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
  • FIG. 1 shows a hollow component 1 which is to be coated, for example, on an inner surface 4. However, the method can also be used for the in situ layer thickness determination of external surfaces.
  • A layer 7 of the material M is applied to the inner surface 4 by means of known processes, such as for example CVD (chemical vapor deposition) processes, electrochemical processes or other known coating processes. A sensor 10 is arranged in the cavity 19 of the component 1 and is therefore coated in the same way as the component 1 which is to be treated.
  • FIG. 2 shows an enlarged view of the sensor 10.
  • The sensor 10 consists of a material which has an electrical property, such as for example its electrical resistance, impedance, capacitance or the like, which changes as a result of some form of interaction with the material M which forms the layer. The sensor 10 may be of any desired shape, i.e. may, for example, be a piece of wire or in the shape of a small plate.
  • The sensor 10 is connected to an electrical measuring unit 16 via electrical lines 13; the measuring unit measures the electrical parameter which changes as a result of the sensor 10 being coated with the material M. The way in which the layer thickness is dependent on the electrical variable is known from calibration curves determined in preliminary tests.
  • The method is used in particular for internal alitizing processes in which aluminum is applied to an inner surface 4 of a component 1 (M=Al). In this case, the sensor consists, for example, of the material MCrAlY (M=Fe, Co, Ni) and changes with the aluminum applied during a CVD process in such a manner that the measured electrical characteristic variable changes in a manner which is representative of the coating result.
    • LIST OF REFERENCE SYMBOLS
    • 1 Component
    • 4 Inner surface
    • 7 Layer
    • 10 Sensor
    • 13 Electrical line
    • 16 Electrical evaluation/control
    • 19 Cavity
  • The invention being thus described, it will be obvious that the same may be varied in many ways. Such variations are not to be regarded as a departure from the spirit and scope of the invention, and all such modifications as would be obvious to one skilled in the art are intended to be included within the scope of the following claims.

Claims (7)

1. A device for in situ layer thickness determination during a coating process, comprising:
a sensor, adapted to be changed by the coating process in such a way that, as a result, an electrical property of the sensor which bears a correlation to the layer thickness is influenced; and
means for measuring the change in the electrical property to determine the layer thickness.
2. The device as claimed in claim 1, wherein the sensor consists of MCrAlY, where M is an element selected from the group consisting of iron, cobalt and nickel.
3. The device as claimed in claim 1, wherein the coating process is an alitizing process.
4. The device as claimed in claim 1, wherein the electrical property is the electrical resistance.
5. The device as claimed in claim 1, wherein the sensor is a sintered part.
6. The device as claimed in claim 1, wherein the coating process is a chemical vapor deposition process.
7. The device as claimed in claim 1, wherein the coating process is used for the internal coating of a component.
US11/127,103 2002-05-10 2005-05-12 Method and device for in situ layer thickness determination Abandoned US20050229847A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US11/127,103 US20050229847A1 (en) 2002-05-10 2005-05-12 Method and device for in situ layer thickness determination

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
EP02010628A EP1361292B1 (en) 2002-05-10 2002-05-10 Method for measuring coating thickness in-situ
EP02010628.2 2002-05-10
US10/434,165 US6936299B2 (en) 2002-05-10 2003-05-09 Method and device for in situ layer thickness determination
US11/127,103 US20050229847A1 (en) 2002-05-10 2005-05-12 Method and device for in situ layer thickness determination

Related Parent Applications (1)

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US10/434,165 Division US6936299B2 (en) 2002-05-10 2003-05-09 Method and device for in situ layer thickness determination

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US20050229847A1 true US20050229847A1 (en) 2005-10-20

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US11/127,103 Abandoned US20050229847A1 (en) 2002-05-10 2005-05-12 Method and device for in situ layer thickness determination

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US (2) US6936299B2 (en)
EP (1) EP1361292B1 (en)
JP (1) JP2003329406A (en)
CN (1) CN1456704A (en)
DE (1) DE50204021D1 (en)
ES (1) ES2247219T3 (en)

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ES2247219T3 (en) * 2002-05-10 2006-03-01 Siemens Aktiengesellschaft PROCEDURE FOR THE IN SITU DETERMINATION OF THE THICKNESS OF A LAYER.
FR2974174B1 (en) * 2011-04-18 2013-04-26 Peugeot Citroen Automobiles Sa METHOD FOR CONTROLLING THE ANTI-CORROSION PROTECTION LAYER DEPOSITED INSIDE THE HOLLOW BODIES OF THE BODY OF A MOTOR VEHICLE
TR202011047A2 (en) * 2020-07-13 2022-01-21 Tusaş Türk Havacilik Ve Uzay Sanayi̇i̇ Anoni̇m Şi̇rketi̇ A measurement system.
US20240091808A1 (en) * 2022-09-16 2024-03-21 Lawrence Livermore National Security, Llc High throughput materials screening
CN115652269A (en) * 2022-11-07 2023-01-31 东莞金坤新材料股份有限公司 Manufacturing method of magnetic sputtering vacuum coating permanent magnet

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US4331702A (en) * 1980-02-05 1982-05-25 Siemens Aktiengesellschaft Method for reproducible manufacture of metallic layers
US4543576A (en) * 1981-06-12 1985-09-24 Siemens Aktiengesellschaft System for measuring electrical resistance and temperature during manufacture of thin, conductive films deposited on substrates by means of evaporation or sputter deposition
US4823073A (en) * 1987-03-31 1989-04-18 Siemens Aktiengesellschaft Sensor for measuring the current or voltage of electrically conductive layers present on a reference substrate
US4851300A (en) * 1988-05-09 1989-07-25 United Technologies Corporation Precoat for improving platinum thin film adhesion
US4898746A (en) * 1988-06-28 1990-02-06 Rca Licensing Corporation Material deposition process analysis system
US5057781A (en) * 1989-07-31 1991-10-15 At&T Bell Laboratories Measuring and controlling the thickness of a conductive coating on an optical fiber
US5142228A (en) * 1989-04-24 1992-08-25 Corning Incorporated Method for statically or dynamically monitoring the thickness of electrically-conductive coatings on optical fibers
US5466638A (en) * 1990-06-26 1995-11-14 Mitsubishi Denki Kabushiki Kaisha Method of manufacturing a metal interconnect with high resistance to electromigration
US6436246B1 (en) * 1997-01-27 2002-08-20 Micron Technology, Inc. Collimated sputter deposition monitor using sheet resistance
US6936299B2 (en) * 2002-05-10 2005-08-30 Siemens Aktiengesellschaft Method and device for in situ layer thickness determination

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Publication number Priority date Publication date Assignee Title
DE3613112A1 (en) * 1986-04-18 1987-10-22 Grundig Emv Device for measuring the magnetic properties of layers, which are applied by sputtering or vapour-deposition, during the machining process
JP2660467B2 (en) * 1992-02-03 1997-10-08 井前工業株式会社 Heat-resistant insulator for induction heating coil

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4331702A (en) * 1980-02-05 1982-05-25 Siemens Aktiengesellschaft Method for reproducible manufacture of metallic layers
US4543576A (en) * 1981-06-12 1985-09-24 Siemens Aktiengesellschaft System for measuring electrical resistance and temperature during manufacture of thin, conductive films deposited on substrates by means of evaporation or sputter deposition
US4823073A (en) * 1987-03-31 1989-04-18 Siemens Aktiengesellschaft Sensor for measuring the current or voltage of electrically conductive layers present on a reference substrate
US4851300A (en) * 1988-05-09 1989-07-25 United Technologies Corporation Precoat for improving platinum thin film adhesion
US4898746A (en) * 1988-06-28 1990-02-06 Rca Licensing Corporation Material deposition process analysis system
US5142228A (en) * 1989-04-24 1992-08-25 Corning Incorporated Method for statically or dynamically monitoring the thickness of electrically-conductive coatings on optical fibers
US5057781A (en) * 1989-07-31 1991-10-15 At&T Bell Laboratories Measuring and controlling the thickness of a conductive coating on an optical fiber
US5466638A (en) * 1990-06-26 1995-11-14 Mitsubishi Denki Kabushiki Kaisha Method of manufacturing a metal interconnect with high resistance to electromigration
US6436246B1 (en) * 1997-01-27 2002-08-20 Micron Technology, Inc. Collimated sputter deposition monitor using sheet resistance
US6936299B2 (en) * 2002-05-10 2005-08-30 Siemens Aktiengesellschaft Method and device for in situ layer thickness determination

Also Published As

Publication number Publication date
DE50204021D1 (en) 2005-09-29
EP1361292B1 (en) 2005-08-24
US6936299B2 (en) 2005-08-30
JP2003329406A (en) 2003-11-19
US20030230138A1 (en) 2003-12-18
ES2247219T3 (en) 2006-03-01
EP1361292A1 (en) 2003-11-12
CN1456704A (en) 2003-11-19

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