US3574650A - Vacuum vapor deposition with control of elevation of metal melt - Google Patents

Vacuum vapor deposition with control of elevation of metal melt Download PDF

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Publication number
US3574650A
US3574650A US806956A US3574650DA US3574650A US 3574650 A US3574650 A US 3574650A US 806956 A US806956 A US 806956A US 3574650D A US3574650D A US 3574650DA US 3574650 A US3574650 A US 3574650A
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Prior art keywords
pool
elevation
spot
molten
vapor deposition
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US806956A
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Randolph D House
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RTX Corp
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United Aircraft Corp
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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
    • C23C14/543—Controlling the film thickness or evaporation rate using measurement on the vapor source
    • 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
    • C23C14/24—Vacuum evaporation
    • C23C14/246—Replenishment of source material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
    • G01F23/00—Indicating or measuring liquid level or level of fluent solid material, e.g. indicating in terms of volume or indicating by means of an alarm
    • G01F23/22—Indicating or measuring liquid level or level of fluent solid material, e.g. indicating in terms of volume or indicating by means of an alarm by measuring physical variables, other than linear dimensions, pressure or weight, dependent on the level to be measured, e.g. by difference of heat transfer of steam or water
    • G01F23/28—Indicating or measuring liquid level or level of fluent solid material, e.g. indicating in terms of volume or indicating by means of an alarm by measuring physical variables, other than linear dimensions, pressure or weight, dependent on the level to be measured, e.g. by difference of heat transfer of steam or water by measuring the variations of parameters of electromagnetic or acoustic waves applied directly to the liquid or fluent solid material
    • G01F23/284—Electromagnetic waves
    • G01F23/292—Light, e.g. infrared or ultraviolet

Definitions

  • the present invention relates in general to a method for sensing changes in the relative location of a material and more particularly relates to an electro-optical method for sensing and controlling the relative surface location of a light reflective material.
  • the invention is particularly useful in detecting and controlling the surface elevation of an incandescent metal melt as it is depleted by evaporation in a vacuum vapor deposition process.
  • aluminide coatings such as that described in the patent to Joseph 3,102,044, have in the past displayed satisfactory performance, it is well known that these coatings, because of their dependence upon the availability of substrate elements, often are characterized by a composition less than optimum.
  • CoCrAlY coating at a nominal composition of, by weight, percent chromium, 15 percent aluminum, O.5 percent yttrium, balance iron, as discussed in the copending application of Frank P. Talboom, r. et a]. entitled Iron Base Coating for the Superalloys, Ser. No. 731,650, filed May 23, 1968.
  • CoCrAlY composition at about, by weight, 21 percent chromium, 15 percent aluminum, 0.7 percent yttrium, balance cobalt.
  • a significant problem in existing vacuum vapor deposition processes has been a lack of effective means for sensing and maintaining the molten source pool at a constant height. It has been demonstrated that coating efiiciency, composition and uniformity are very susceptible to pool height changes. This is true not only with regard to relative changes in position and spacing between source and substrate, but more importantly, with regard to relative changes in elevation of the molten pool within the crucible. Recently, several techniques have been developed to improve the effectiveness of the basic process through the mechanism of monitoring the coating source material elevation. In one such method, a radioactive 1sotope is utilized as a source of radiation in a system wherein the amount of radiation passing over or through the molten pool indicates the elevational location thereof.
  • the present invention contemplates detection and control of a displaceable material having reflective properties by the utilization of a light beam of sufiicient intensity to be monitored in reflection.
  • a high intensity monochromatic light beam such as a laser beam is utilized in a vapor vacuum deposition process and is focused on the surface of the molten source metal pool at a predetermined angle of incidence.
  • the reflected beam is refocused onto a photodetector which is sensitive to movements of the beam caused by elevational displacement of the pool surface.
  • the photodetector in essence, monitors and maintains the evaporating molten metal at a constant elevation to ensure process uniformity and reproducibility.
  • a vacuum chamber 10 having an exit port 12 leading to a suitable high vacuum pump, preferably of the dilIusion type, for the rapid and continuous evacuation of the chamber.
  • a suitable high vacuum pump preferably of the dilIusion type
  • an electron gun 14 for generating a beam of charged particles to impinge upon and vaporize an ingot of source metal 16.
  • the electron beam is suitably directed by conventional magnetic deflection pole pieces 18.
  • the arrangement of the electron beam gun within the vacuum chamber is a function of design.
  • a 30 kilowatt electron beam unit has been used to melt and vaporize the upper end of ingot 16 to create a molten source pool having a reflecting surface 20. Satisfactory deposition rates have been achieved with a two inch diameter ingot of a FeCrAly coating material, the depth of the molten pool usually being /4 /2 inch.
  • the ingot 16 is slidably received at its upper end by a fixed annular water cooled copper crucible 22.
  • the ingot is movable vertically by an actuator or motor means 24 which in turn is electrically controlled by means herein- 3 after described.
  • the ingot 16 passes through a suitable heat resistant vacuum seal 26 in the chamber base.
  • a substrate 27, to be coated is disposed within the vacuum chamber vertically above the pool surface 20. Since the process is fundamentally line-of-sight, the part is typically mounted to effect rotation about its longitudinal axis, usually utilizing a vacuum sealed pass-through (not shown) through the vacuum chamber to an external drive system. Of course, more than one part may be coated at a time. In such a case, in order to minimize non-uniformity of coating between each of the plurality of parts, each part is normally mounted in a plane of vapor isodensity or roughly along an arc defining a zone of constant vapor concentration, the parts closest to the vertical passing through the center of the molten pool being located slight- 1y farther from the pool surface than those positioned at an angle with respect to the said vertical.
  • each substrate is further positioned as close as possible to the surface of the molten source pool without being subjected to nudesirable coating contamination by splash from the pool.
  • the substrate height varies with each system but for a two inch diameter pool and a deposition rate of about 0.3 mil per minute with a FeCrAlY coating material, a mean height of about inches has been found satisfactory.
  • a source of I high energy monochromatic light such as a laser 28.
  • a 1.0 milliwatt helium-neon gas laser has been found satisfactory.
  • the light beam designated by the numeral 30, is projected and focused to a small spot 31 on the reflecting surface of the molten body by appropriate source optics, such as by a microscope objective lens 32 and a lano-convex lens 34.
  • the optical components 32 and 34 are protected against vapor fouling by an inwardly projecting tubular encasement 36 having a transparent window 38 which seals the aforementioned optics from the chamber.
  • the window 38 is itself protected against fouling by suitable apparatus, such as a tube shield 40 provided with an inert gas swee introduced through a gas inlet 42.
  • the free end of the shield 40 is apertured at 44 with the opening just large enough to permit uninterrupted passage of the light beam.
  • the relative sizes of the optical and protective components can of course vary. However, best results have been obtained by providing a large focal distance between the lens 34 and the spot 31, and a relatively small aperture 44. For example, components giving a focal distance of 33 inches with a beam diameter of /2 inch at the lens 34 and a tube shield 15 inches long and apertured to closely circumscribe the beam at a location approximately 16 inches from the spot 31 were found desirable. As will subsequently be understood, such a relation is advantageous in that there is provided a large depth of field which reduces the effect of a changing spot size at the deflector face due to changes in the height of the molten pool.
  • a long focal distance ensures a greater separative distance from the molten pool to minimize vapor condensate contamination while a small aperture 44 corresponding to the small diameter beam reduces the gas load, on the vacuum system, imposed by the protective inert gas sweep.
  • the light beam reflected from spot 31 is intercepted and focused onto a spot 46 on the face of a light sensitive detector 48 by similar appropriate detector optics such as plane-convex lens 50 and microscope objective lens 52.
  • the detector optics are protected against vapor fouling in the same way as the source optics.
  • an encasement 54 having a window 56, the window being protected by an inert gas sweep in a tube shield 58 with a gas inlet 60 and aperture 62.
  • the detector 48 is preferably comprised of matching photo electric cells 64, disposed within the focal plane of the reflected beam and separated by a narrow horizontal gap 66, with each cell connected to appropriate electrical lead lines 68.
  • a photodetector comprised of a two element silicon Schottky barrier photodiode has been found satisfactory.
  • the detector 48 is preceded by a narrow bandpass filter 70 which has its bandpass centered on the laser wavelength, and which is preferably a narrow bandpass dielectric film optical interference filter. It can be seen that as the source material is depleted by evaporation, the pool surface 20 is lowered in elevation, thus altering the vertical and horizontal position of the spot 31 on the pool surface where reflection occurs.
  • the spot 46 is concomitantly displaced from a position of balance in relation to the gap 66 to a position of imbalance whereby the spot impinges more fully on one photo cell 64 than the other, thus causing electrically unbalanced signals to be generated in the lead lines 68.
  • the photo cells 64 may be employed as the active elements of a Wheatstone bridge circuit including in the signal processor whereby unbalancing of electrical signals can be utilized to cause the actuator to move the ingot 16 in the appropriate direction until balance is achieved.
  • the detector optics 50, 52 are positioned so that the reflecting spot 31 and the photoelectric detector 48 are at the conjugate foci thereof. In this way, even though the surface wave amplitudes may become large enough to cause the reflected beam to miss, at times, the detector optics entirely, the system still functions effectively because there results a periodic sweeping of the beam across the aforementioned detector optics.
  • the detectors At each sweep, the detectors produce output pulses the relative magnitudes of which are dependent upon the height of spot 31 during the brief interval that the reflected beam is intercepted by the detector optics.
  • the signal processor time averages the pulses and provides a control signal proportional to the diflerence between a desired control height and the time average height of the molten surface.
  • the incident beam 30 is preferably projected at a relatively large angle of incidence, 6. It will be appreciated that since the sensitivity to pool height is proportional to twice the sine of the angle 0, an angle of incidence in the range of 30 to is preferable, although the system is operable at angles as small as 10. An angle of incidence of approximately 70 however is found to give best results in the present system since 70 affords a satisfactory compromise between optimizing sensitivity while avoiding interference by the edges of the crucible with the incident and reflected beams.
  • a conventional beam splitter 74 and viewing screen with integral reticle 76 are illustrated as providing a means for effecting visual observation of the elevation of the pool surface.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Electromagnetism (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Fluid Mechanics (AREA)
  • General Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Physical Vapour Deposition (AREA)
  • Measurement Of Optical Distance (AREA)
  • Length Measuring Devices By Optical Means (AREA)
US806956A 1969-03-13 1969-03-13 Vacuum vapor deposition with control of elevation of metal melt Expired - Lifetime US3574650A (en)

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US (1) US3574650A (enrdf_load_stackoverflow)
CA (1) CA959145A (enrdf_load_stackoverflow)
DE (1) DE2012075A1 (enrdf_load_stackoverflow)
FR (1) FR2037794A5 (enrdf_load_stackoverflow)
GB (1) GB1294234A (enrdf_load_stackoverflow)
SE (1) SE366832B (enrdf_load_stackoverflow)

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3740563A (en) * 1971-06-25 1973-06-19 Monsanto Co Electroptical system and method for sensing and controlling the diameter and melt level of pulled crystals
US3958129A (en) * 1974-08-05 1976-05-18 Motorola, Inc. Automatic crystal diameter control for growth of semiconductor crystals
US4046100A (en) * 1975-10-20 1977-09-06 Trw Inc. Apparatus for thermal deposition of metal
US4061800A (en) * 1975-02-06 1977-12-06 Applied Materials, Inc. Vapor desposition method
EP0024527A3 (de) * 1979-08-01 1981-10-28 Endress u. Hauser GmbH u.Co. Anordnung zur Messung des Badspiegels in einer Giessanlage, insbesondere in der Kokille einer Stranggiessanlage
US4396005A (en) * 1981-07-06 1983-08-02 Corning Glass Works Solar collector and control
US4508970A (en) * 1982-07-15 1985-04-02 Motorola, Inc. Melt level sensing system and method
US5617911A (en) * 1995-09-08 1997-04-08 Aeroquip Corporation Method and apparatus for creating a free-form three-dimensional article using a layer-by-layer deposition of a support material and a deposition material
US5718951A (en) * 1995-09-08 1998-02-17 Aeroquip Corporation Method and apparatus for creating a free-form three-dimensional article using a layer-by-layer deposition of a molten metal and deposition of a powdered metal as a support material
US5746844A (en) * 1995-09-08 1998-05-05 Aeroquip Corporation Method and apparatus for creating a free-form three-dimensional article using a layer-by-layer deposition of molten metal and using a stress-reducing annealing process on the deposited metal
US5787965A (en) * 1995-09-08 1998-08-04 Aeroquip Corporation Apparatus for creating a free-form metal three-dimensional article using a layer-by-layer deposition of a molten metal in an evacuation chamber with inert environment
US6342265B1 (en) * 1997-08-20 2002-01-29 Triumf Apparatus and method for in-situ thickness and stoichiometry measurement of thin films
US20080160171A1 (en) * 2006-12-29 2008-07-03 United Technologies Corporation Electron beam physical vapor deposition apparatus and processes for adjusting the feed rate of a target and manufacturing a multi-component condensate free of lamination
WO2017048523A1 (en) * 2015-09-15 2017-03-23 Retech Systems Llc Laser sensor for melt control of hearth furnaces and the like
US11213912B2 (en) * 2018-06-25 2022-01-04 Bwxt Nuclear Operations Group, Inc. Methods and systems for monitoring a temperature of a component during a welding operation
WO2022002371A1 (en) * 2020-06-30 2022-01-06 MAX-PLANCK-Gesellschaft zur Förderung der Wissenschaften e.V. Method for controlling an evaporation rate of source material, detector for measuring electromagnetic radiation reflected on a source surface and system for thermal evaporation with electromagnetic radiation
JP2023534894A (ja) * 2020-06-30 2023-08-15 マツクス－プランク－ゲゼルシヤフト ツール フエルデルング デル ヴイツセンシヤフテン エー フアウ 蒸発したソース材料のフラックス分布を制御するための方法、ソース表面で反射された電磁放射を測定するための検出器、及び、電磁放射を用いた熱蒸発のためのシステム

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2482290A1 (fr) * 1980-05-09 1981-11-13 Poncet Pierre Perfectionnements a la detection photoelectrique du niveau du bain dans les lingotieres de coulee continue
DE3336210C2 (de) * 1982-10-06 1986-04-10 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V., 8000 München Verfahren und Vorrichtung zur Füllstandsmessung
DE3740227C2 (de) * 1987-11-27 1994-03-24 Schenck Ag Carl Verfahren und Vorrichtung zur Messung von Verformungen an Proben oder Prüfkörpern in Prüfmaschinen
DE3720303C2 (de) * 1987-06-19 1993-09-30 Schenck Ag Carl Probeneinspannvorrichtung für Prüfmaschinen
DE3720248A1 (de) * 1987-06-19 1989-01-05 Schenck Ag Carl Verfahren und anordnung zur messung von verformungen an proben oder pruefkoerpern in pruefmaschinen
DE10040942A1 (de) * 2000-08-21 2002-03-07 Endress Hauser Gmbh Co Vorrichtung zur Bestimmung des Füllstands eines Füllguts in einem Behälter

Cited By (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3740563A (en) * 1971-06-25 1973-06-19 Monsanto Co Electroptical system and method for sensing and controlling the diameter and melt level of pulled crystals
US3958129A (en) * 1974-08-05 1976-05-18 Motorola, Inc. Automatic crystal diameter control for growth of semiconductor crystals
US4061800A (en) * 1975-02-06 1977-12-06 Applied Materials, Inc. Vapor desposition method
US4046100A (en) * 1975-10-20 1977-09-06 Trw Inc. Apparatus for thermal deposition of metal
EP0024527A3 (de) * 1979-08-01 1981-10-28 Endress u. Hauser GmbH u.Co. Anordnung zur Messung des Badspiegels in einer Giessanlage, insbesondere in der Kokille einer Stranggiessanlage
US4420250A (en) * 1979-08-01 1983-12-13 Endress U. Hauser Gmbh U. Co. Arrangement for measuring the bath level in a continuous casting apparatus
US4396005A (en) * 1981-07-06 1983-08-02 Corning Glass Works Solar collector and control
US4508970A (en) * 1982-07-15 1985-04-02 Motorola, Inc. Melt level sensing system and method
US5960853A (en) * 1995-09-08 1999-10-05 Aeroquip Corporation Apparatus for creating a free-form three-dimensional article using a layer-by-layer deposition of a molten metal and deposition of a powdered metal as a support material
US5718951A (en) * 1995-09-08 1998-02-17 Aeroquip Corporation Method and apparatus for creating a free-form three-dimensional article using a layer-by-layer deposition of a molten metal and deposition of a powdered metal as a support material
US5746844A (en) * 1995-09-08 1998-05-05 Aeroquip Corporation Method and apparatus for creating a free-form three-dimensional article using a layer-by-layer deposition of molten metal and using a stress-reducing annealing process on the deposited metal
US5787965A (en) * 1995-09-08 1998-08-04 Aeroquip Corporation Apparatus for creating a free-form metal three-dimensional article using a layer-by-layer deposition of a molten metal in an evacuation chamber with inert environment
US5617911A (en) * 1995-09-08 1997-04-08 Aeroquip Corporation Method and apparatus for creating a free-form three-dimensional article using a layer-by-layer deposition of a support material and a deposition material
US6342265B1 (en) * 1997-08-20 2002-01-29 Triumf Apparatus and method for in-situ thickness and stoichiometry measurement of thin films
US6617574B2 (en) 1997-08-20 2003-09-09 Triumf Apparatus for in-situ thickness and stoichiometry measurement of thin films
EP1939924A3 (en) * 2006-12-29 2008-11-12 United Technologies Corporation Electron beam physical vapor deposition apparatus and processes
JP2008163464A (ja) * 2006-12-29 2008-07-17 United Technol Corp <Utc> 電子ビーム物理蒸着装置において送り速度を調整する方法、電子ビーム物理蒸着装置、およびこの装置を用いた層状化の発生していない多成分凝縮物の製造方法
US20080160171A1 (en) * 2006-12-29 2008-07-03 United Technologies Corporation Electron beam physical vapor deposition apparatus and processes for adjusting the feed rate of a target and manufacturing a multi-component condensate free of lamination
WO2017048523A1 (en) * 2015-09-15 2017-03-23 Retech Systems Llc Laser sensor for melt control of hearth furnaces and the like
US11213912B2 (en) * 2018-06-25 2022-01-04 Bwxt Nuclear Operations Group, Inc. Methods and systems for monitoring a temperature of a component during a welding operation
US12076812B2 (en) 2018-06-25 2024-09-03 Bwxt Nuclear Operations Group, Inc. Methods and systems for monitoring a temperature of a component during a welding operation
WO2022002371A1 (en) * 2020-06-30 2022-01-06 MAX-PLANCK-Gesellschaft zur Förderung der Wissenschaften e.V. Method for controlling an evaporation rate of source material, detector for measuring electromagnetic radiation reflected on a source surface and system for thermal evaporation with electromagnetic radiation
CN115917033A (zh) * 2020-06-30 2023-04-04 马克思-普朗克科学促进协会 控制源材料的蒸发速率的方法、测量在源表面上反射的电磁辐射的检测器及利用电磁辐射进行热蒸发的系统
JP2023534894A (ja) * 2020-06-30 2023-08-15 マツクス－プランク－ゲゼルシヤフト ツール フエルデルング デル ヴイツセンシヤフテン エー フアウ 蒸発したソース材料のフラックス分布を制御するための方法、ソース表面で反射された電磁放射を測定するための検出器、及び、電磁放射を用いた熱蒸発のためのシステム
US20230287556A1 (en) * 2020-06-30 2023-09-14 MAX-PLANCK-Gesellschaft zur Förderung der Wissenschaften e.V. Method for controlling a flux distribution of evaporated source material, detector for measuring electromagnetic radiation reflected on a source surface and system for thermal evaporation with electromagnetic radiation

Also Published As

Publication number Publication date
CA959145A (en) 1974-12-10
DE2012075A1 (enrdf_load_stackoverflow) 1970-09-10
SE366832B (enrdf_load_stackoverflow) 1974-05-06
GB1294234A (en) 1972-10-25
FR2037794A5 (enrdf_load_stackoverflow) 1970-12-31

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