WO2016132175A1 - Coating or sealing internal surface of a workpiece - Google Patents

Coating or sealing internal surface of a workpiece Download PDF

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Publication number
WO2016132175A1
WO2016132175A1 PCT/IB2015/051275 IB2015051275W WO2016132175A1 WO 2016132175 A1 WO2016132175 A1 WO 2016132175A1 IB 2015051275 W IB2015051275 W IB 2015051275W WO 2016132175 A1 WO2016132175 A1 WO 2016132175A1
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WO
WIPO (PCT)
Prior art keywords
reactor
cavity
vapor deposition
workpiece
coating
Prior art date
Application number
PCT/IB2015/051275
Other languages
French (fr)
Inventor
Marsel ARIE LAOR
Dag-hartman INBAR
Macover ERAN
Avinoam TAMIR
Original Assignee
Pct Protective Coating Technologies Ltd.
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 Pct Protective Coating Technologies Ltd. filed Critical Pct Protective Coating Technologies Ltd.
Priority to PCT/IB2015/051275 priority Critical patent/WO2016132175A1/en
Publication of WO2016132175A1 publication Critical patent/WO2016132175A1/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/04Coating on selected surface areas, e.g. using masks
    • C23C14/046Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00Processes for applying liquids or other fluent materials
    • B05D1/60Deposition of organic layers from vapour phase
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/22Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to internal surfaces, e.g. of tubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/22Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to internal surfaces, e.g. of tubes
    • B05D7/222Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to internal surfaces, e.g. of tubes of pipes
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/12Organic material
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation

Definitions

  • the present invention relates to surface coatings, in particular using vapor deposition.
  • Vapor deposition processes such as physical vapor deposition (PVD) or chemical vapor deposition (CVD) and the like are used to improve characteristics such as hardness, wear resistance, oxidation and corrosion resistance; as well as other characteristics such as friction coefficient and adhesion of a workpiece's surface.
  • PVD physical vapor deposition
  • CVD chemical vapor deposition
  • a substrate is exposed to one or more volatile precursors that reacts, e.g. with other vapors or co-deposited species or decomposes on the substrate surface or polymerizes on the surface to produce desired deposit, for example an oxide, a nitride, a carbide or a carbonitride or a polymer.
  • Shadowing If the workpiece has not been designed or positioned properly in a coating chamber, lack of vapor exposure will cause improper coating or sealing.
  • Some solutions to those problems include using a rotating mechanism around one or more axes to reduce shadowing effects. Coating issues, such as shadowing, arise particularly when the workpiece or specimen has a cavity, and thus at least one aperture leading to that cavity. Specimen geometry, size and internal cavity structure may further increase shadowing effects and create un-reachable cavities that cannot be effectively coated. Particularly when CVD is used, maintaining the vapors and the co- deposited species chemically available for further reactions is a big challenge. Limited active vapor availability to such internal deposition targets inside a specimen cavity may sharply limit coating abilities.
  • the present invention relates to an apparatus and method for mitigating coating and/or surface sealing issues when coating a workpiece or specimen via CVD, PVD or the like (which may be referred to generically hereinafter in the specification and claims as "vapor deposition”, “vapor coating?', “vapor deposition coating”, or derivatives thereof).
  • an apparatus for providing a vapor deposition coating to a cavity surface of a workpiece the workpiece having a workpiece cavity defining a cavity surface, the cavity having at least one aperture.
  • the apparatus includes: at least one sealing element adapted to respectively seal the at least one aperture of the cavity and having at least one vacuum port configured for connection with a vacuum pump; and a vapor deposition reactor positionable within the cavity, the reactor having a vaporizer to provide a deposition vapor from a precursor, and the reactor having a vapor deposition outlet, whereby a vacuum can be achieved in the cavity and the vapor deposition reactor can be operated to produce a coating on the cavity surface.
  • the apparatus's vapor deposition reactor further includes a pyrolysis chamber. In some embodiments, the apparatus further includes a reactor transporting mechanism operably connected to the vapor deposition reactor and adapted to move the reactor within the workpiece cavity.
  • the reactor transporting mechanism includes a motor; in some embodiments the reactor transporting mechanism includes a flexible cable; in some embodiments, the reactor transporting mechanism includes a rigid shaft; in some embodiments, the reactor transporting mechanism includes a magnetic element.
  • the at least one sealing element further includes an electrical connection port.
  • the apparatus further includes a heating module associated with the reactor and having a temperature sensor and a controller therefor.
  • a method of coating a cavity surface of a workpiece cavity of a workpiece with a vapor deposition coating includes: disposing a vapor deposition reactor within the cavity of the workpiece, the reactor being configured to provide a vapor deposition coating and having a reactor transporting mechanism adapted to move the reactor within the cavity; sealing the workpiece cavity; providing a vacuum to the workpiece cavity; and operating the vapor deposition reactor to produce a vapor deposition within the cavity, whereby a coating can be formed on the cavity surface.
  • the method further includes moving the vapor deposition reactor within the cavity.
  • the at least one vacuum tight seal is configured to close (be seated on) at least one aperture of the cavity.
  • the at least one vacuum tight seal is configured to seal the workpiece's cavity so that fluid (vapor) flow through the aperture is blocked.
  • the at least one vacuum tight seal is configured to allow a connection from the sealed specimen's internal cavity to an external vacuum pump, to enable producing a suitable vacuum inside the specimen cavity. As will be described below, the at least one internal surface may then be vacuum coated or sealed.
  • the at least one vacuum tight seal has at least one feed through or connection port configured to be connected to an external vacuum pump.
  • the external vacuum pump should be designed to produce a sufficient vacuum level inside a specimen cavity, upon the proper placement of the vacuum tight seal, in order to allow vacuum coating or sealing of at least one internal surface of the specimen cavity.
  • the internal cavity of the specimen has more than one aperture, e.g. the specimen is a pipe-like workpiece having two (or more) apertures then, according to some embodiments of the invention, two (or more) vacuum tight seals may be used, with at least one or those vacuum tight seals having a feed through/connection port.
  • additional feed through vacuum ports may be connected to other vacuum tight seals or to same vacuum seal (e.g. sealing plate), for example if a stronger vacuum is required, or if the same vacuum level is to be achieved faster.
  • the at least one vacuum tight seal has an electrical port configured to electrically connect electrical devices, e.g. an electric motor located within the sealed cavity, to an external power supply.
  • the electrical port is designed to be vacuum sealable to help maintain the vacuum level produced by the vacuum pump.
  • at least some of the internal electrical elements located in the cavity are configured to work with induced energy converters without physical electrical wiring.
  • a reactor configured to be placed in the internal cavity of the specimen.
  • the reactor may have a heating module and may also have a driving module (e.g. a self-contained or associated reactor transporting mechanism).
  • the electrical port may connect the heating module or the driving module to a power supply.
  • the heating module may be an inductive heating module without any external wiring.
  • the driving module may be remotely controlled such as by magnetic elements or other driving means.
  • the driving module may include an electrical motor configured to drive/move the reactor along the cavity of the specimen with a cable or shaft.
  • the driving module is configured to move the reactor in a predefined path along the cavity of the specimen. The velocity of the reactor, among other parameters, may control the thickness of the coating or sealing layer achieved.
  • the driving module may be adapted to either (or both) concentrically or eccentrically move the reactor from one edge of the sealed pipe to the opposite edge thereof, typically at a predetermined speed.
  • the apparatus may be configured to hold the workpiece in a horizontal orientation and the driving module is adapted to move the reactor horizontally back and forth with a rigid shaft of the apparatus.
  • the apparatus may be configured to hold the workpiece in a vertical orientation and the driving module is adapted to move the reactor up and down along the internal cavity of the workpiece, for example using a flexible cable.
  • the specimen and its internal cavity may have any geometry and be regularly or irregularly shaped.
  • the reactor and driving module can be designed to allow the reactor to move within such a cavity to allow effective distribution of the coating or sealing material within the cavity and to maintain the vapor's chemical availability for an effective deposition of at least one surface of the cavity.
  • the apparatus includes a plurality of stationary reactors positioned inside the specimen cavity and designed to effectively spread the coating vapors to all targeted internal surfaces to be coated or sealed, which can be useful in large cavities.
  • a single stationary reactor may be positioned in a specimen cavity to allow the vacuum coating or sealing of at least one internal surface of a specimen cavity.
  • a method of coating or sealing a surface of at least one cavity of a specimen - each cavity having least one aperture includes sealing the at least one specimen aperture with at least one vacuum tight seal to allow creating a vacuum level, through a vacuum port, within the at least one cavity.
  • the method further includes positioning the vapor deposition reactor inside the at least one cavity and the placement of a volatile precursor inside the reactor.
  • the method may further include heating the reactor to create available active vapors to efficiently coat or seal a target deposition surface inside the cavity.
  • the method may further include operating a reactor transporting mechanism, through an electrical port or wirelessly, to move the reactor along the sealed cavity while keeping an appropriate vacuum level, to allow efficient distribution and availability of active vapors along the cavity to ensure functional coating or sealing.
  • an apparatus and method of coating a specimen's cavity which has undergone a micro arc oxidation process (known also as Plasma Electrolitic Oxidation, PEO).
  • the specimen thus has a porous oxidation film to be sealed in order to avoid corrosive agent penetration into the pores, and which may further result in corrosion of the substrate.
  • Such specimen may be sealed according to embodiments of the present invention by sealing the internal cavity with a vacuum tight seal, inserting a reactor into the cavity, inserting a volatile precursor into the reactor and heating the reactor to produce active vapors in the specimen cavity.
  • the method may further include creating a vacuum in the sealed cavity, heating the reactor and moving the reactor along the cavity of the specimen to achieve effective active vapor distribution along the internal target porous cavity surface to be sealed.
  • FIG. 1 is a side view of an embodiment of an apparatus for providing a vapor deposition coating to a cavity surface of a workpiece in accordance with the present invention.
  • Fig. 1 shows an embodiment of an apparatus for providing a vapor deposition coating to a cavity surface of a workpiece, in accordance with the present invention.
  • a non-limiting example of a specimen 2 in the form of a pipe is shown, and which may have a diameter of about 15 cm and a length of about 4 meters.
  • a sealing element 1 is configured to seal the pipe cavity at one end of the pipe/specimen 2.
  • a sealing element or seal 1 a is configured to seal the pipe cavity at the other end of specimen 2.
  • Sealing element 1 a is typically an essentially vacuum tight seal and has a vacuum port 9a connectable to a vacuum pump 9.
  • Seal 1 a has an electrical port 8a configured to allow connection of an external power supply (not shown) in order to power internal electrical components such as an electrical motor 8, which is some embodiments is a component of a vapor deposition reactor transporting mechanism 10, described below.
  • the apparatus further includes a vapor deposition reactor 20, also described below.
  • the electrical port 8a or vacuum port 9a is operably connected to wire sensors (not shown) such as position, speed, temperature, pressure, vapor density, impedance or optical sensors (e.g. a camera) located inside the cavity.
  • wire sensors such as position, speed, temperature, pressure, vapor density, impedance or optical sensors (e.g. a camera) located inside the cavity.
  • one or more of the sensors may be monitored by a microprocessor and controller (not shown), or by other means, to provide feedback and control in order to optimize the working parameters of the coating or sealing process.
  • the sublimation rate of the deposited coting vapor is monitored by the vapor pressure sensor so that a target predefined value of vapor pressure is maintained. At a known vapor pressure, the value of the deposition rate on the target deposited surface is known.
  • vapor deposition reactor transporting mechanism 10 includes motor 8 connected to a spool 6a, which is configured to roll a cable 6 and move the vapor deposition reactor 20, which in some embodiments includes a reactor vapor outlet 3, pyrolysis chamber 4 and vaporizer 5.
  • the vaporizer 5 is configured to hold a volatile precursor such as Parylene.
  • vaporizer 5 includes a heating element (not shown); while in some embodiments the vaporizer is configured to be connected to an external heating source (e.g. wired through the electrical port 8a). According to such embodiments, Parylene is heated to sublime at least part of the Parylene into dimmers.
  • the reactor 20 may further include a pyrolysis chamber 4.
  • the pyrolysis chamber 4 may include an integral heating module (not shown), or be configured as to be connected to an external heating source, in order to provide heat to crack Parylene dimmers into monomers to be deposited on the target surface/substrate.
  • the surface/substrate may be, for example, an oxidation porous layer in order to seal pores thereof.
  • the reactor outlet 3 is connected to pyrolysis chamber 4.
  • pyrolysis chamber 4 and the vaporizer 5 are connected by a connector.
  • the heating module may include one or more of a heater, isolation and temperature sensor; and a controller therefor.
  • the reactor 20 may be wrapped by the heating module or heating element thereof, or the reactor can include and integral heating module/element.
  • the reactor transporting mechanism 10 may be configured to move the vapor disposition reactor 20 along the pipe cavity 7 in such a way that monomer outlet 3 provides an effective amount of available active vapors for the target deposition surface.
  • outlet 3 may have a mechanism for facilitating a uniform coating distribution.
  • outlet 3 may have a non-uniform or directional orientation to serve specific deposition surface targets in the internal cavity of the specimen.
  • Parylene monomers have a spontaneous tendency to polymerize in the gas phase. Depositing polymerized Parylene provides poor sealing and coating results.
  • This apparatus is designed to enlarge the mean free path of the monomer, and overcome the problems encountered when costing cavities of various lengths and sizes. Maintaining a sufficient level of active vapors adjacent a deposition target surface, for example, when using Parylene, may be accomplished by keeping a sufficient level of monomers adjacent the target deposition surface to allow polymerization on the target surface with co-deposited monomers, or on-site polymerized surfaces.
  • the mean free path of Parylene monomers limits the distance at which one can get uniform deposition to a certain distance, based on the specific parameters of each case. Therefore, according to some embodiments the reactor 20 should travel along the internal cavity 7 of (pipe) specimen 2 so that any target deposition surface is within the aforementioned "certain distance" in order to achieve an effective coating along the whole cavity.
  • the temperature controller is adapted to facilitate temperature control along the cavity to improve coating thickness uniformity.
  • different volatile surface deposition precursors may require different temperature ranges to achieve sublimation of the deposition material (e.g. Parylene).
  • not all precursors require an extra separate step of pyrolysis.

Abstract

An apparatus for providing a vapor deposition coating to a cavity surface. The apparatus has a sealing element to seal the cavity and a vacuum port for connection with a vacuum pump. The apparatus also includes a vapor deposition reactor positionable within the cavity, the reactor having a vaporizer to provide a deposition vapor from a precursor. In some embodiments, the apparatus includes a reactor transporting mechanism to move the reactor within the workpiece cavity. In some embodiments the reactor includes a pyrolysis chamber. A method for coating the cavity surface is also disclosed.

Description

COATING OR SEALING AN INTERNAL SURFACE OF A WORKPIECE
FIELD OF THE INVENTION The present invention relates to surface coatings, in particular using vapor deposition.
BACKGROUND OF THE INVENTION
Vapor deposition processes such as physical vapor deposition (PVD) or chemical vapor deposition (CVD) and the like are used to improve characteristics such as hardness, wear resistance, oxidation and corrosion resistance; as well as other characteristics such as friction coefficient and adhesion of a workpiece's surface.
In the PVD process, a vacuum evaporation or mechanical sputtering of a precursor is followed by condensation of such vapors on a substrate surface to form thin film coating layers.
In a chemical vacuum deposition, a substrate is exposed to one or more volatile precursors that reacts, e.g. with other vapors or co-deposited species or decomposes on the substrate surface or polymerizes on the surface to produce desired deposit, for example an oxide, a nitride, a carbide or a carbonitride or a polymer.
One problem with the above processes is shadowing. If the workpiece has not been designed or positioned properly in a coating chamber, lack of vapor exposure will cause improper coating or sealing. Some solutions to those problems include using a rotating mechanism around one or more axes to reduce shadowing effects. Coating issues, such as shadowing, arise particularly when the workpiece or specimen has a cavity, and thus at least one aperture leading to that cavity. Specimen geometry, size and internal cavity structure may further increase shadowing effects and create un-reachable cavities that cannot be effectively coated. Particularly when CVD is used, maintaining the vapors and the co- deposited species chemically available for further reactions is a big challenge. Limited active vapor availability to such internal deposition targets inside a specimen cavity may sharply limit coating abilities.
SUMMARY OF THE INVENTION
The present invention relates to an apparatus and method for mitigating coating and/or surface sealing issues when coating a workpiece or specimen via CVD, PVD or the like (which may be referred to generically hereinafter in the specification and claims as "vapor deposition", "vapor coating?', "vapor deposition coating", or derivatives thereof).
The terms "workpiece" and "specimen" may be used interchangeably herein the specification and claims.
In accordance with embodiments of the present invention there is provided an apparatus for providing a vapor deposition coating to a cavity surface of a workpiece, the workpiece having a workpiece cavity defining a cavity surface, the cavity having at least one aperture. The apparatus includes: at least one sealing element adapted to respectively seal the at least one aperture of the cavity and having at least one vacuum port configured for connection with a vacuum pump; and a vapor deposition reactor positionable within the cavity, the reactor having a vaporizer to provide a deposition vapor from a precursor, and the reactor having a vapor deposition outlet, whereby a vacuum can be achieved in the cavity and the vapor deposition reactor can be operated to produce a coating on the cavity surface.
In some embodiments, the apparatus's vapor deposition reactor further includes a pyrolysis chamber. In some embodiments, the apparatus further includes a reactor transporting mechanism operably connected to the vapor deposition reactor and adapted to move the reactor within the workpiece cavity.
In some embodiments, the reactor transporting mechanism includes a motor; in some embodiments the reactor transporting mechanism includes a flexible cable; in some embodiments, the reactor transporting mechanism includes a rigid shaft; in some embodiments, the reactor transporting mechanism includes a magnetic element.
In some embodiments, the at least one sealing element further includes an electrical connection port. In some embodiments, the apparatus further includes a heating module associated with the reactor and having a temperature sensor and a controller therefor.
In accordance with embodiments of the present invention there is provided a method of coating a cavity surface of a workpiece cavity of a workpiece with a vapor deposition coating. The method includes: disposing a vapor deposition reactor within the cavity of the workpiece, the reactor being configured to provide a vapor deposition coating and having a reactor transporting mechanism adapted to move the reactor within the cavity; sealing the workpiece cavity; providing a vacuum to the workpiece cavity; and operating the vapor deposition reactor to produce a vapor deposition within the cavity, whereby a coating can be formed on the cavity surface.
In some embodiments, the method further includes moving the vapor deposition reactor within the cavity.
The at least one vacuum tight seal is configured to close (be seated on) at least one aperture of the cavity. The at least one vacuum tight seal is configured to seal the workpiece's cavity so that fluid (vapor) flow through the aperture is blocked. The at least one vacuum tight seal is configured to allow a connection from the sealed specimen's internal cavity to an external vacuum pump, to enable producing a suitable vacuum inside the specimen cavity. As will be described below, the at least one internal surface may then be vacuum coated or sealed.
The at least one vacuum tight seal has at least one feed through or connection port configured to be connected to an external vacuum pump. The external vacuum pump should be designed to produce a sufficient vacuum level inside a specimen cavity, upon the proper placement of the vacuum tight seal, in order to allow vacuum coating or sealing of at least one internal surface of the specimen cavity. In case the internal cavity of the specimen has more than one aperture, e.g. the specimen is a pipe-like workpiece having two (or more) apertures then, according to some embodiments of the invention, two (or more) vacuum tight seals may be used, with at least one or those vacuum tight seals having a feed through/connection port. According to some embodiments, additional feed through vacuum ports may be connected to other vacuum tight seals or to same vacuum seal (e.g. sealing plate), for example if a stronger vacuum is required, or if the same vacuum level is to be achieved faster.
According to some embodiments the at least one vacuum tight seal has an electrical port configured to electrically connect electrical devices, e.g. an electric motor located within the sealed cavity, to an external power supply. Typically, the electrical port is designed to be vacuum sealable to help maintain the vacuum level produced by the vacuum pump. According to some embodiments, at least some of the internal electrical elements located in the cavity are configured to work with induced energy converters without physical electrical wiring. According to embodiments of another aspect of the present invention there is provided a reactor configured to be placed in the internal cavity of the specimen. The reactor may have a heating module and may also have a driving module (e.g. a self-contained or associated reactor transporting mechanism). The electrical port may connect the heating module or the driving module to a power supply. In some embodiments, the heating module may be an inductive heating module without any external wiring. In some embodiments, the driving module may be remotely controlled such as by magnetic elements or other driving means. In some embodiments, the driving module may include an electrical motor configured to drive/move the reactor along the cavity of the specimen with a cable or shaft. In some embodiments, the driving module is configured to move the reactor in a predefined path along the cavity of the specimen. The velocity of the reactor, among other parameters, may control the thickness of the coating or sealing layer achieved.
In one non-limiting example, if the specimen is a pipe and the cavity to be coated is the internal surface of the pipe. With such a specimen configuration, the driving module may be adapted to either (or both) concentrically or eccentrically move the reactor from one edge of the sealed pipe to the opposite edge thereof, typically at a predetermined speed.
According to some embodiments, the apparatus may be configured to hold the workpiece in a horizontal orientation and the driving module is adapted to move the reactor horizontally back and forth with a rigid shaft of the apparatus. According to some embodiments, the apparatus may be configured to hold the workpiece in a vertical orientation and the driving module is adapted to move the reactor up and down along the internal cavity of the workpiece, for example using a flexible cable.
The specimen and its internal cavity may have any geometry and be regularly or irregularly shaped. For such geometries, the reactor and driving module can be designed to allow the reactor to move within such a cavity to allow effective distribution of the coating or sealing material within the cavity and to maintain the vapor's chemical availability for an effective deposition of at least one surface of the cavity.
In some embodiments, the apparatus includes a plurality of stationary reactors positioned inside the specimen cavity and designed to effectively spread the coating vapors to all targeted internal surfaces to be coated or sealed, which can be useful in large cavities. Alternatively, a single stationary reactor may be positioned in a specimen cavity to allow the vacuum coating or sealing of at least one internal surface of a specimen cavity.
According to another aspect of the present invention there is provided a method of coating or sealing a surface of at least one cavity of a specimen - each cavity having least one aperture. The method includes sealing the at least one specimen aperture with at least one vacuum tight seal to allow creating a vacuum level, through a vacuum port, within the at least one cavity. The method further includes positioning the vapor deposition reactor inside the at least one cavity and the placement of a volatile precursor inside the reactor. In some embodiments, the method may further include heating the reactor to create available active vapors to efficiently coat or seal a target deposition surface inside the cavity. In some embodiments, the method may further include operating a reactor transporting mechanism, through an electrical port or wirelessly, to move the reactor along the sealed cavity while keeping an appropriate vacuum level, to allow efficient distribution and availability of active vapors along the cavity to ensure functional coating or sealing.
According to some embodiments there is provided an apparatus and method of coating a specimen's cavity, which has undergone a micro arc oxidation process (known also as Plasma Electrolitic Oxidation, PEO). The specimen thus has a porous oxidation film to be sealed in order to avoid corrosive agent penetration into the pores, and which may further result in corrosion of the substrate. Such specimen may be sealed according to embodiments of the present invention by sealing the internal cavity with a vacuum tight seal, inserting a reactor into the cavity, inserting a volatile precursor into the reactor and heating the reactor to produce active vapors in the specimen cavity. The method may further include creating a vacuum in the sealed cavity, heating the reactor and moving the reactor along the cavity of the specimen to achieve effective active vapor distribution along the internal target porous cavity surface to be sealed. BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be understood and appreciated more fully from the following detailed description taken in conjunction with the appended drawings in which: Fig. 1 is a side view of an embodiment of an apparatus for providing a vapor deposition coating to a cavity surface of a workpiece in accordance with the present invention.
The following detailed description of embodiments of the invention refers to the accompanying drawing referred to above. Dimensions of components and features shown in the figures are chosen for convenience or clarity of presentation and are not necessarily shown to scale.
DESCRIPTION OF EMBODIMENTS OF THE INVENTION
Illustrative embodiments of the invention are described below. In the interest of clarity, not all features/components of an actual implementation are necessarily described.
Fig. 1 shows an embodiment of an apparatus for providing a vapor deposition coating to a cavity surface of a workpiece, in accordance with the present invention. A non-limiting example of a specimen 2 in the form of a pipe is shown, and which may have a diameter of about 15 cm and a length of about 4 meters. A sealing element 1 is configured to seal the pipe cavity at one end of the pipe/specimen 2. A sealing element or seal 1 a is configured to seal the pipe cavity at the other end of specimen 2. Sealing element 1 a is typically an essentially vacuum tight seal and has a vacuum port 9a connectable to a vacuum pump 9. Seal 1 a has an electrical port 8a configured to allow connection of an external power supply (not shown) in order to power internal electrical components such as an electrical motor 8, which is some embodiments is a component of a vapor deposition reactor transporting mechanism 10, described below. The apparatus further includes a vapor deposition reactor 20, also described below.
According to some embodiments, the electrical port 8a or vacuum port 9a is operably connected to wire sensors (not shown) such as position, speed, temperature, pressure, vapor density, impedance or optical sensors (e.g. a camera) located inside the cavity. In some embodiments, one or more of the sensors may be monitored by a microprocessor and controller (not shown), or by other means, to provide feedback and control in order to optimize the working parameters of the coating or sealing process. According to some embodiments, the sublimation rate of the deposited coting vapor is monitored by the vapor pressure sensor so that a target predefined value of vapor pressure is maintained. At a known vapor pressure, the value of the deposition rate on the target deposited surface is known. By controlling the reactor temperature, the sublimation rate can be controlled and hence the vapor pressure is controlled. At any controlled vapor pressure, a controlled deposition rate may be achieved. It should be noted that, in large cavities in which the optionally moving vapor deposition reactor transporting mechanism 10 is located, the velocity of the reactor 20 may also be controlled, among other parameters, by the diffusion rate at a certain working condition. In some embodiments, vapor deposition reactor transporting mechanism 10 includes motor 8 connected to a spool 6a, which is configured to roll a cable 6 and move the vapor deposition reactor 20, which in some embodiments includes a reactor vapor outlet 3, pyrolysis chamber 4 and vaporizer 5. In some embodiments, the vaporizer 5 is configured to hold a volatile precursor such as Parylene. In some embodiments, vaporizer 5 includes a heating element (not shown); while in some embodiments the vaporizer is configured to be connected to an external heating source (e.g. wired through the electrical port 8a). According to such embodiments, Parylene is heated to sublime at least part of the Parylene into dimmers. According to some embodiments, the reactor 20 may further include a pyrolysis chamber 4. In some embodiments, the pyrolysis chamber 4 may include an integral heating module (not shown), or be configured as to be connected to an external heating source, in order to provide heat to crack Parylene dimmers into monomers to be deposited on the target surface/substrate. The surface/substrate may be, for example, an oxidation porous layer in order to seal pores thereof.
According to some embodiments, the reactor outlet 3 is connected to pyrolysis chamber 4. In some embodiments, pyrolysis chamber 4 and the vaporizer 5 are connected by a connector.
The heating module may include one or more of a heater, isolation and temperature sensor; and a controller therefor. The reactor 20 may be wrapped by the heating module or heating element thereof, or the reactor can include and integral heating module/element.
In various embodiments, the reactor transporting mechanism 10 may be configured to move the vapor disposition reactor 20 along the pipe cavity 7 in such a way that monomer outlet 3 provides an effective amount of available active vapors for the target deposition surface. Optionally, outlet 3 may have a mechanism for facilitating a uniform coating distribution. In some embodiments, there might be an internal dispersion device (not shown) inside the pyrolysis chamber 4 that improves the uniformity of the coating distribution. In some embodiments, outlet 3 may have a non-uniform or directional orientation to serve specific deposition surface targets in the internal cavity of the specimen.
Parylene monomers have a spontaneous tendency to polymerize in the gas phase. Depositing polymerized Parylene provides poor sealing and coating results. This apparatus, among other things, is designed to enlarge the mean free path of the monomer, and overcome the problems encountered when costing cavities of various lengths and sizes. Maintaining a sufficient level of active vapors adjacent a deposition target surface, for example, when using Parylene, may be accomplished by keeping a sufficient level of monomers adjacent the target deposition surface to allow polymerization on the target surface with co-deposited monomers, or on-site polymerized surfaces. The mean free path of Parylene monomers limits the distance at which one can get uniform deposition to a certain distance, based on the specific parameters of each case. Therefore, according to some embodiments the reactor 20 should travel along the internal cavity 7 of (pipe) specimen 2 so that any target deposition surface is within the aforementioned "certain distance" in order to achieve an effective coating along the whole cavity.
In some embodiments, the temperature controller is adapted to facilitate temperature control along the cavity to improve coating thickness uniformity. It should be noted that different volatile surface deposition precursors may require different temperature ranges to achieve sublimation of the deposition material (e.g. Parylene). Moreover, not all precursors require an extra separate step of pyrolysis. Some polymer coatings and metallic coatings, such as titanium oxide, nitride, chrome, cadmium, gold or silver, can be evaporated and become available active vapors in a single step. It should be understood that the above description is merely exemplary and that there are various embodiments of the present invention that may be devised, mutatis mutandis, and that the features described in the above- described embodiments, and those not described herein, may be used separately or in any suitable combination; and the invention can be devised in accordance with embodiments not necessarily described above.

Claims

1. An apparatus for providing a vapor deposition coating to a cavity surface of a workpiece, the workpiece having a workpiece cavity defining a cavity surface, the cavity having at least one aperture, the apparatus comprising: at least one sealing element adapted to respectively seal the at least one aperture of the cavity and having at least one vacuum port configured for connection with a vacuum pump; and a vapor deposition reactor positionable within the cavity, the reactor comprising a vaporizer to provide a deposition vapor from a precursor, and the reactor having a vapor deposition outlet, whereby a vacuum can be achieved in the cavity and the vapor deposition reactor can be operated to produce a coating on the cavity surface.
2. The apparatus of claim 1 , wherein the vapor deposition reactor further comprises a pyrolysis chamber.
3. The apparatus of claim 1 , further comprising a reactor transporting mechanism operably connected to the vapor deposition reactor and adapted to move the reactor within the workpiece cavity.
4. The apparatus of claim 3, wherein the reactor transporting mechanism comprises a motor.
5. The apparatus of claim 3, wherein the reactor transporting mechanism comprises a flexible cable.
6. The apparatus of claim 3, wherein the reactor transporting mechanism comprises a rigid shaft.
7. The apparatus of claim 3, wherein the reactor transporting mechanism comprises a magnetic element.
8. The apparatus of claim 1 , wherein the at least one sealing element further comprises an electrical connection port.
9. The apparatus of claim 1 , further comprising a heating module associated with the reactor and having a temperature sensor and a controller therefor.
10. A method of coating a cavity surface of a workpiece cavity of a workpiece with a vapor deposition coating, the method comprising: disposing a vapor deposition reactor within the cavity of the workpiece, the reactor being configured to provide a vapor deposition coating and having a reactor transporting mechanism adapted to move the reactor within the cavity; sealing the workpiece cavity; providing a vacuum to the workpiece cavity; and operating the vapor deposition reactor to produce a vapor deposition within the cavity, whereby a coating can be formed on the cavity surface.
11. The method of claim 10, further comprising moving the vapor deposition reactor within the cavity.
PCT/IB2015/051275 2015-02-19 2015-02-19 Coating or sealing internal surface of a workpiece WO2016132175A1 (en)

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GB2517436A (en) * 2013-08-19 2015-02-25 Pct Protective Coating Technologies Ltd Coating or sealing an internal surface of a workpiece

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JP2009206008A (en) * 2008-02-29 2009-09-10 Fujitec International Inc Method of manufacturing light-emitting device and manufacturing device used for the same
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