WO2021094919A1 - Machine pour le traitement de surface de produits au moyen d'un dépôt par plasma de couches minces de matériaux de revêtement, et procédé de traitement de produits par plasma - Google Patents

Machine pour le traitement de surface de produits au moyen d'un dépôt par plasma de couches minces de matériaux de revêtement, et procédé de traitement de produits par plasma Download PDF

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Publication number
WO2021094919A1
WO2021094919A1 PCT/IB2020/060573 IB2020060573W WO2021094919A1 WO 2021094919 A1 WO2021094919 A1 WO 2021094919A1 IB 2020060573 W IB2020060573 W IB 2020060573W WO 2021094919 A1 WO2021094919 A1 WO 2021094919A1
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WIPO (PCT)
Prior art keywords
products
processing
chamber
machine
carrier gas
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PCT/IB2020/060573
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English (en)
Inventor
Alessio NOE'
Stefano Ferrari
Original Assignee
Astro S.R.L.
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Publication date
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Priority to EP20817491.2A priority Critical patent/EP4058618A1/fr
Publication of WO2021094919A1 publication Critical patent/WO2021094919A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4505—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
    • C04B41/4529—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application applied from the gas phase
    • C04B41/4531—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application applied from the gas phase by C.V.D.
    • 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
    • C23C16/22—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 deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/401—Oxides containing silicon
    • 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
    • C23C16/22—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 deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/403—Oxides of aluminium, magnesium or beryllium
    • 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
    • C23C16/448—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 characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/4481—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 characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source 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
    • C23C16/448—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 characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/4486—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 characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by producing an aerosol and subsequent evaporation of the droplets or particles
    • 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
    • C23C16/458—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 characterised by the method used for supporting substrates in the reaction chamber
    • C23C16/4582—Rigid and flat substrates, e.g. plates or discs
    • C23C16/4583—Rigid and flat substrates, e.g. plates or discs the substrate being supported substantially horizontally
    • 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
    • C23C16/50—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 using electric discharges
    • C23C16/505—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 using electric discharges using radio frequency discharges
    • C23C16/509—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 using electric discharges using radio frequency discharges using internal electrodes
    • 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
    • C23C16/54—Apparatus specially adapted for continuous coating
    • C23C16/545—Apparatus specially adapted for continuous coating for coating elongated substrates
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32082—Radio frequency generated discharge
    • H01J37/321—Radio frequency generated discharge the radio frequency energy being inductively coupled to the plasma
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32431—Constructional details of the reactor
    • H01J37/3244—Gas supply means
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32733—Means for moving the material to be treated
    • H01J37/32752—Means for moving the material to be treated for moving the material across the discharge
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32798—Further details of plasma apparatus not provided for in groups H01J37/3244 - H01J37/32788; special provisions for cleaning or maintenance of the apparatus
    • H01J37/32899—Multiple chambers, e.g. cluster tools
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/21—Oxides
    • C03C2217/212—TiO2
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/21—Oxides
    • C03C2217/213—SiO2
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/21—Oxides
    • C03C2217/214—Al2O3
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/15—Deposition methods from the vapour phase
    • C03C2218/152—Deposition methods from the vapour phase by cvd
    • C03C2218/153—Deposition methods from the vapour phase by cvd by plasma-enhanced cvd

Definitions

  • the invention relates to the surface processing of products through plasma, in particular, although not exclusively, of slab-shaped products, such as resin-based processing, painting, protective coating etc. More in particular, the object of the invention is a machine for the surface processing of products through plasma deposition of coating materials, and a method for processing products through plasma.
  • the protective coating where the thickness is comprised between few nanometers and some microns, fall into the category of so-called thin films; where the thickness is greater than dozens microns, they fall into the category of thick films.
  • thin films Due to the their particular structure, thin films have been studied mainly for use in electronics and optics industry, but the use thereof is increasingly increasing in different sectors, for example mechanical processing, decorative applications, eyewear.
  • Ceramic-based thin films have been particularly studied for hardness and relative inertia with the aim to using them as protective materials against corrosion, oxidation and wear.
  • Plasma deposition is one of the known processes for depositing materials on products.
  • plasma deposition technologies is no perfectly adapted for producing large materials, for the difficult adequately to control thicknesses, and to make the process sufficiently fast for treating many products.
  • the general object of the invention is to overcome the problems of plasma deposition of thin layers of materials on large products.
  • an important object of the invention is to provide a machine for the surface processing of products through deposition of thin layers of coating materials, as well as a processing method, allowing to process large products.
  • a further important object of the invention is to provide a machine for the surface processing of products through deposition of thin layers of coating materials (as well as a processing method), allowing to have particularly hard thin layers.
  • a further object of the invention is to provide a machine for the surface processing of products through deposition of thin layers of coating materials (as well as a processing method), allowing high production rates.
  • a machine for the surface processing of products through plasma deposition of thin layers of coating materials comprising: a closed gastight space, provided with at least one opening, that can be closed, for inserting and removing the products to be processed, a device for reducing the pressure inside the closed space up to a value lower than the ambient pressure, a surface processing device comprising an inductive high radio frequency plasma source, operatively connected to a high radio frequency generator and provided in the closed space, the source comprising o an open dome facing the at least one closed space, o a vacuum closed electrode adapted to surround the center of the dome and to start the plasma generation discharge, and operatively connected to the inductive coil, o at least one inlet for a reactive gas entering the dome, o at least one inlet for a mixture of precursor gas and carrier gas, - a supply device for supplying said plasma source with said mixture of precursor gas and carrier gas, comprising o at least one first tank adapted to contain liquid for at
  • the plasma source comprises a primary circuit provided with inductive means, such as one or more inductive coils, operatively connected with the frequency generator, and a secondary circuit provided with induced means, such as one or more induced coils, operatively connected to the electrode for starting plasma discharged.
  • inductive means such as one or more inductive coils
  • secondary circuit provided with induced means, such as one or more induced coils, operatively connected to the electrode for starting plasma discharged.
  • the plasma source preferably comprises an impedance matching network, preferably automatic.
  • the machine comprises an operational area for arranging the product to be processed; the dome is arranged above, and directed towards, the operational area.
  • the at least one inlet for a mixture of precursor gas and carrier gas into the dome comprises a tube, which extends with an approximately ring shape and along whose surface calibrated holes are provided, forming the nozzles for the exit of the precursor gas-carrier gas mixture; the tube preferably surrounding the center of the dome.
  • the device for mixing and expanding the precursor liquid coming from the mass flow meter and the carrier gas coming from the at least one second tank comprises a mixing chamber, an inlet for atomizing the precursor liquid thus creating an aerosol, a second inlet for the carrier gas entering the mixing chamber, a valve for controlling the pressure inside the mixing chamber, an outlet for the mixture exiting from the said device, a heat exchanger provided between the mixing chamber and the outlet and adapted to increase the temperature of the mixture to make the liquid part completely evaporate.
  • the machine comprises at least one tank for at least one reactive gas; the tank preferably comprises oxygen (O2).
  • the at least one precursor liquid first tank is adapted to contain trimethylaluminum (TMA) or hexamethyldisiloxane (HDMSO), or titanium isopropoxide (TTIP), so that, in combination with the reactive gas oxygen (O2), preferably inside the dome, during plasma formation, a deposition material is produced comprised of aluminum oxide (AI2O3) or of silica oxide (SiOx), or of titanium dioxide (T1O2); two first tanks are preferably provided, one of them adapted to contained trimethylaluminum (TMA) and the other one adapted to contain hexamethyldisiloxane (HDMSO), or one of them adapted to contain trimethylaluminum (TMA) and the other one adapted to contain hexamethyldisiloxane (HDMSO) or titanium isopropoxide (TTIP), or one of them adapted to contain hexamethyldisiloxane (HDMSO) and the other one one
  • the at least one carrier gas second tank is adapted to contain inert gas, for example argon.
  • the closed space comprises at least one accumulation chamber, separate from the processing area, where products are accumulated; from an operational viewpoint, once all products to be processed have been inserted into the at least one chamber, the chamber is closed and the pressure inside is reduced up to an operational processing pressure, then the products are processed, and lastly the at least one chamber is opened and the products are taken therefrom.
  • the machine preferably comprises in the at least one chamber, a moving device for moving the products from the bottom upwards and in reverse, so as to accumulate at least two products on levels put over one another, a plan moving device for moving the products from and towards the at least one opening when the products are arranged at the same level of the at least one opening, wherein, from an operational viewpoint, a plurality of products are inserted into the at least one chamber, and at least two products of the plurality of products are over one another for a span of processing, and wherein, once all the products to be processed have been inserted into the at least one chamber, the chamber is closed and the pressure inside is decreased up to an operational processing pressure, and then the at least one chamber is opened again and the products are removed therefrom.
  • the closed space comprises a processing room adjacent to the at least one accumulation chamber; the products are moved from the at least one accumulation chamber to the processing room in order to be processed.
  • the closed space preferably comprises at least two accumulation chambers connected to each other, each chamber being adapted to receive a plurality of products put over one another.
  • the surface processing device for processing a product is preferably arranged between the two accumulation chambers.
  • a processing room is provided, where the surface processing device is arranged, and where the operational area for arranging the product is provided, so that the products are adapted to move from a chamber to the following one passing through the room, where the processing is carried out.
  • the processing room has preferably dimensions adapted to receive the whole product to be processed; the product is preferably adapted to be moved from a first chamber to the room, where it is arranged stationary so as to carry out the deposition processing.
  • the plan moving device is adapted to allow the products to pass from a chamber to the following one under the processing device.
  • the plan moving device is adapted to allow the products to pass from a chamber to the following one under the processing device during the processing step; the room has preferably smaller dimensions than the dimensions of the products so that the deposition processing is carried out on the portion of the product inside the room while the product is moving.
  • the plan moving device is common to the chambers; preferably the plan moving device is a conveyor belt crossing the chambers from an entrance first opening of the machine up to an exit second opening of the machine, passing under the processing device.
  • the processing machine comprises a first opening for the products entering the closed space, defined in the first chamber, and a second opening for the products exiting the closed space, defined in the second chamber, respective sealing doors being provided associated with the openings.
  • a moving device for moving the products from the bottom upwards so as to accumulate at least two products over one another.
  • each bottom- upwards moving device defines N positions raised from the moving plane, and the maximal number of products that can be processed in the machine is N+l .
  • each product is borne by a respective support, so that the products enter and exit the closed space on these supports, and the bottom-upwards moving device and the plan moving device are adapted to move the products by directly moving the supports.
  • each product is in the form of a slab, preferably made of stone, glass, wood, ceramic or metal.
  • the invention relates to a method for thin layer plasma deposition, providing for a product, with a surface to be coated with a thin layer, arranged inside a vacuum processing room, with pressure preferably comprised between 6 x 10 3 mbar and 1.1 x 10 2 mbar, wherein in the processing room a surface processing device is provided, comprising a high radio frequency inductive plasma source arranged in the closed space, and wherein the source comprises
  • a vacuum closed electrode adapted to surround the center of the dome and to start the plasma generation discharge, and operatively connected to the inductive coil
  • the method providing the following steps for the product inside the vacuum processing room: a) supplying a mass flow meter with a precursor liquid, b) measuring the mass flow rate of the precursor liquid, c) supplying a mixing and expanding device with the desired mass flow rate of the precursor liquid, d) supplying the mixing and expanding device with a carrier gas, so that the precursor liquid and the carrier gas form a gaseous mixture, e) supplying the at least one inlet for a mixture of precursor gas and carrier gas with the gaseous mixture, f) supplying the at least one inlet for a reactive gas entering the dome with a reactive gas, g) generating, through the high frequency generator, an electromagnetic wave to obtain an inductive plasma of the mixture, h) waiting the time for the material formed from the inductive plasma to deposit.
  • the precursor liquid is atomized inside a pressure-controlled mixing chamber, to form an aerosol
  • the precursor/carrier gas mixture exits from the mixing chamber, - the mixture is heated so that the liquid part thereof completely evaporates,
  • the reactive gas preferably comprises oxygen (O2).
  • the precursor liquid is trimethylaluminum (TMA) or hexamethyldisiloxane (HDMSO), or titanium isopropoxide (TTIP), so that, in combination with the reactive gas oxygen (O2) inside the dome during plasma formation, a deposition material is produced comprised of aluminum oxide (AI2O3) or of silica oxide (SiOx), or of titanium dioxide (TiCh).
  • TMA trimethylaluminum
  • HDMSO hexamethyldisiloxane
  • TTIP titanium isopropoxide
  • a deposition material comprised of aluminum oxide (AI2O3) or of silica oxide (SiOx), or of titanium dioxide (TiCh).
  • the carrier gas preferably comprises inert gas, preferably argon.
  • the method comprises the step of arranging a plurality of products to be subjected to plasma surface processing inside a closed space, making the closed space vacuum and moving the products, one by one, towards the processing room provided in the closed space to carry out, for one product at a time, the steps a)-h); once these steps have been carried out, the product is exited from the processing room and a subsequent product is inserted thereinto.
  • the products are preferably moved towards the processing room from a first chamber to make the plasma deposition; after the steps a)-h), each product being housed in a second chamber of the closed space, different than the first chamber.
  • - Fig. l is a schematic side view of a line of a surface processing plant using the processing machine of the invention
  • - Fig. 2 is a schematic side view, partially cut-away longitudinally, of a surface processing machine with a double sealed chamber
  • - Fig. 3 is a schematic front view, partially cut-away transversally, of the processing machine of Fig. 2
  • each of Figs. 4a to 4e is a schematic front view, partially cut-away transversally, of a portion of the processing machine of Fig. 2, relating to a specific step of loading the products in the sealed chambers of the machine;
  • - Fig. 5 is a schematic side view, partially cut-away longitudinally, of a machine similar to that of Fig. 2, wherein the processing room has larger dimensions than those of the slab;
  • FIG. 6 is a schematic side view, partially cut-away longitudinally, of a machine with only one chamber where only one slab is introduced to carry out the plasma deposition processing thereon;
  • Fig. 7 is a diagram of a plasma source arranged on the top of the processing room of a machine according to the previous figures, where some components are highlighted. Detailed description of embodiments
  • a machine for the surface processing of products through plasma deposition of thin layers of coating materials is indicated as a whole with the reference number 10. It is inserted in a processing line indicated with 100. More in particular, in this example the line is a line for the surface processing of slabs L made of stone, such as marble, granite and the like, or of glass, wood, ceramic, metal etc. The line is well known, with the exception of the part relating to the processing machine 10.
  • the line 1 comprises, in succession, a rotating storage space 101 for slabs L, an automatic loader 102 taking the slabs L from the storage space 101 and putting them on a comb-shaped loading conveyor belt 103 transferring the slabs L onto a first pantograph lifting device 104.
  • a second pantograph lifting device 105 is provided, bringing the slabs to the level of a comb-shaped unloading conveyor belt 106, after which an automatic unloader 107 and a further rotating storage space 108 for slabs L are provided.
  • a support LI for a slab L is provided, in the form of a mainly flat metal frame comprising poles and crossbars, onto which the slab is fastened in a flat fashion.
  • a corresponding support LI is provided for moving the slab inside the processing machine 10.
  • the set comprised of support LI and slab L arriving from the machine 10 onto the second pantograph lifting device 105 is separated, and the slab L is taken from the comb-shaped unloading conveyor belt 106 while the support LI returns to the comb-shaped loading conveyor belt 103 through a pair of movable belts 107 provided below the machine 10.
  • a number of supports L 1 is provided at least equal to the number of slabs to be processed in the processing machine 10, as it will be better explained below.
  • the surface processing machine 10 comprises a casing 11, internally defining two consecutive sealed chambers, respectively a first sealed chamber 12 and a second sealed chamber 13, separated through an intermediate room 14.
  • the two sealed chambers and the room define a gastight closed space.
  • the first sealed chamber 12 comprises an entrance first opening 15 for a support LI (bearing a first slab L; here below this set will be referred to as “support- slab L”) entering the machine 10.
  • the second sealed chamber 13 comprises an exit second opening 16 for a support-slab L.
  • Respective sealing doors 17, that can be opened and closed, are associated with these openings 15, 16.
  • the room 14, arranged between the two chambers 12 and 13, has two passages 18 for accessing the two chambers.
  • the intermediate room 14 is a room where the surface processing is carried out through plasma deposition of adequate material, and where a surface processing device 26 (preferably arranged on the top of the room 14) carries out the processing through plasma deposition.
  • the machine comprises a known apparatus 30 for reducing the pressure in the gastight closed space comprised of the two chambers 12 and 13 and the room 14 (for example up to a pressure comprised between 6 x 10 3 mbar e 1.1 x 10 2 mbar), the apparatus being part of an air suction system and being omitted in the figures for the sake of simplicity of drawing.
  • the apparatus 30 comprises the following elements (not shown in the figures for the sake of simplicity): an oil-less rotary pump with pumping speed of 650 m 3 /h and flow rate, up to 10 -3 mbar with the aid of roots pump, of 2000 m 3 /h, and an air-cooled turbomolecular pump with pumping speed of 22001/s and flow rate up to 10 8 mbar, with a gas pressurized dry air purge system, so ad to protect it against any corrosive gases resulting from the reaction.
  • an oil-less rotary pump with pumping speed of 650 m 3 /h and flow rate, up to 10 -3 mbar with the aid of roots pump, of 2000 m 3 /h
  • an air-cooled turbomolecular pump with pumping speed of 22001/s and flow rate up to 10 8 mbar, with a gas pressurized dry air purge system, so ad to protect it against any corrosive gases resulting from the reaction.
  • the apparatus 30 is adapted to manage the development of corrosive gases.
  • Automatic on/off valves may be provided on the pumping lines, allowing to evacuate the feeding chamber and the deposition chamber alternatively.
  • the pumping system flow rate may be controlled by means of an electronic unit acting on the rotation speed of the turbomolecular pump (throttle). In this way it is possible to adjust the pressure in the chamber and the gaseous flows in a (partially) independent way.
  • the surface processing device 26 comprises an inductive high radio frequency plasma source 200 provided in the top of the room 14, allowing processing through IPECVD-Inductive Plasma Enhanced Chemical Vapor Deposition.
  • Fig. 7 a diagram is shown of the plasma source 200.
  • the inductive plasma source 200 is, for example, a marketed source, such as the models RS-DPR COPRA RING Source manufactured by the German firm CCR GmbH.
  • the inductive plasma source is, for example, the same as that described in the patent application US20030091482 A1 of the inventors Manfred Weiler and Roland Dahl, to which reference should be made and which is intended as incorporated in the present description.
  • the source 200 provides, for example, for an induction primary circuit Cl, provided with an induction coil, operatively connected with a high radio frequency generator 203 (the generator being, for example, a 5000 W solid state generator, with radio frequency of 13.56 MHz, provided with an LCD indicating the supplied power and the transmitted and reflected power), and inductively coupled to an induced secondary circuit C2 provided with a respective induced coil 202.
  • the secondary circuit C2 has the starting electrode 204 for starting the plasma generation discharge.
  • the plasma source 200 comprises an automatic impedance matching network 203 A.
  • an automatic impedance matching network 203 A In combination with the circuits Cl and C2 it comprises, for example, two capacitors in series, so as to have variable electrical capacity. In this way, it is possible to control the generated input and output power, without the risk of damaging the radio-frequency generator due to reflected current surges.
  • This automatic impedance matching network 203A is, for example, as one of those described in the patent application US 20050001490 A1 of the inventors Weiler Manfred and Roland Dahl, to which reference should be made and which is intended as incorporated in the present description.
  • This automatic impedance matching network 203 A may operate manually or automatically.
  • the source 200 provides for an open dome 201 facing the room 14, on the flanks of which the induced coil 202 is provided.
  • the vacuum closed electrode 204 is adapted to surround the center of the dome 201 (for example the central axis, or a central area thereof), and to start the plasma generation discharge, being operatively connected to the induced coil.
  • the electrode 204 is, for example, the same as the electrode (or set of electrodes) disclosed in the above mentioned patent application US 20030091482 Al.
  • the electrode is shaped, for example, like an open ring.
  • the second inlet 206 for the mixture of precursor gas and carrier gas entering the dome comprises a tube 206A, which extends with an approximately ring shape and along whose surface calibrated holes 206B are provided, forming the nozzles for the exit of the precursor gas-carrier gas mixture; the tube 206A surrounds, for example, the center of the dome.
  • the tube may be, for example, a closed ring, where the beginning and the end of the tube match, or an open ring, where an end of the tube is closed.
  • the machine 10 further comprises a supply device 207 for supplying the plasma source with the mixture of precursor gas and carrier gas.
  • the supply device 207 includes an advantageous first tank 208 adapted to contain the precursor liquid, for example trimethylaluminum (TMA), and a second tank 209 adapted to contain the carrier gas, for example an inert gas such as argon.
  • a further first tank 208A is provided, adapted t contain a second precursor liquid used in the machine, for example hexamethyldisiloxane (HDMSO).
  • a further first tank is provided (not shown in the figures), adapted to contain a third precursor liquid, for example titanium isopropoxide (TTIP).
  • TIP titanium isopropoxide
  • the supply device 207 comprises a mass flow meter 210 for measuring the mass flow rate of the precursor liquid exiting from the first tank 208 (or 208A).
  • the supply device 207 further comprises a device 211 for mixing and expanding the precursor liquid, coming from the mass flow meter 210, and the carrier gas, coming from the second tank 209.
  • the mixing and expanding device 211 comprises a mixing chamber 211 A, an inlet 21 IB for atomizing the liquid in the mixing chamber, thus creating an aerosol, a second inlet 211 C for the carrier gas entering the mixing chamber 211 A, a valve 21 ID for controlling the pressure inside the mixing chamber, an outlet 21 IE for the mixture exiting the mixing and expanding device 211.
  • a heat exchanger 21 IF is also provided, arranged between the mixing chamber 211 A and the outlet 21 IE of the device 211, allowing to increase the temperature of the mixture to make the liquid part thereof completely evaporate.
  • a supply duct 212 supplies the expanded mixture from the mixing and expanding device 211 to the second inlet 206 into the dome 201.
  • a third tank 213 is obviously provided, adapted to contain the reactive gas.
  • the third tank is adapted, for instance, to contain oxygen (O2), so that inside the dome, during plasma formation, in combination with the precursor trimethylaluminum (TMA) deposition material is produced formed by aluminum oxide (AI2O3), whilst in combination with the precursor hexamethyldisiloxane (HDMSO), deposition material is produced formed by silica oxide (SiOx), and, in combination with the precursor titanium isopropoxide (TTIP), deposition material is produced formed by titanium dioxide (TiCk).
  • a duct 214 connects the third tank 213 to the first inlet 205 into the dome 201
  • the dome 201 is provided on the top 14A of the intermediate room 14. Under the dome, on the bottom of the room 14, an operational area 220 is provided for arranging the support-slab L. The dome is directed towards the operational area, so that the plasma processing is directed towards the slab. When the support-slab L passes through the room 14, at least during processing, it is preferably grounded.
  • a plan moving device 19 i.e. a device for moving longitudinally, i.e. from the right to the left and in reverse, for example for moving horizontally (where movements according to a more or less inclined direction are even possible), is realized for example through a chain conveyor (defined by two lateral chains spaced from each other) arranged in the machine 10 and extends according to a rectilinear direction from the first opening 15 to the second opening 16 and vice versa, passing through the passages 18 of the intermediate room 14, i.e. crossing this room.
  • the plan moving device 19 practically defines a moving plane 19A for the support- slab L, aligned with, i.e. crossing, the openings 15 and 16 and the passages 18.
  • each chamber 12, 13 a respective moving device 20 is provided for moving, from the bottom upwards and in reverse, i.e. in this example in substantially vertical direction, the supports-slabs L entering the respective chamber, in order to accumulate the supports-slabs L on levels arranged over one another.
  • each vertical moving device 20 comprises a rack defining a plurality of resting levels arranged over one another, where the supports-slabs L can rest. Through one or more translation actuators 22 the rack translates vertically, lifting in succession the supports-slabs L following one another in the respective chamber, resting on the conveyor belt 19.
  • the rack comprises two side support flanks, each of which defines rests 23 for the supports-slabs L, that are vertically spaced. More in particular, each flank is formed by two horizontally spaced uprights 24, along which the rests 23 project.
  • the uprights 24 are outside the conveyor belt 19, so that the rests 23 do not interfere with the conveyor belt 19 (see Figs. 3 and 4). Furthermore, the supports-slabs L are wider than the conveyor belt 19, thus allowing the rests 23 abutting below the side edges of the same supports-slabs L.
  • the translation actuators 22 can be for example four worm actuators, the movable sliders of which are integral with the respective uprights 24.
  • the slabs L borne by the support LI, enter one by one the first sealed chamber 12 through the first opening 15, with the aid of the conveyor belt 19.
  • the first slab L’ enters the first chamber 12, it stops in correspondence of the rack of the vertical moving device 20.
  • the moving device 20 has the uprights 24 completely lowered, so that the first rests 23’ of the uprights 24, i.e. the ones arranged at the top, are at the same level as the support-slab moving plane 19A, i.e. below the supports-slabs L (Fig. 4a).
  • the vertical moving device 20 is actuated and the uprights 24 are lifted, to bring the second subsequent rests 23 ”, that are at a lower level relative to the first rests 23’, up to the support-slab moving plane 19A.
  • the first slab L’ is lifted with respect to this moving plane by a distance greater than the thickness of the set support- slab L (Fig. 4b).
  • a second slab L enters the first chamber 12 and stops in correspondence of the rack of the vertical moving device 20 (i.e. below the first slab L’, which is above the second slab).
  • the moving device 20 is actuated and the second slab L’ ’ (i.e. the set support-slab), supported by the subsequent second rests 23”, is translated upwards.
  • the first slab L’ is translated upwards.
  • Subsequent third rests 23” of the uprights 24 are at the same level as the support-slab moving plane, so as to receive a new support-slab (Fig. 4d).
  • N have been provided for the machine.
  • three levels are provided, arranged over one another, defined by three sets of rests 23.
  • the last slab L IV passes through the room 14. It should be noted that the length of the processing room 14, i.e. the dimension corresponding to the moving direction of the slabs in the machine, is lower than the dimensions of the single sealed chambers. [095] When the slab L IV passes in the room 14, the surface processing device 26 is actuated and the surface finishing material is thus deposited on the slab through plasma deposition. [096] The plasma deposition processing can provide for more coats, i.e. when the slab L IV arrives in the second chamber 13 the movement of the conveyor belt 19 is reversed and the slab is brought again in the first chamber for a further finishing. When the slab L IV has been processed again, the movement of the conveyor belt 19 is reversed again and the slab returns in the second chamber 13 (if necessary, a third finishing can be also applied). This forwards/backwards movement is performed based on the specific needs.
  • the closed spaced formed by the two chambers and the processing room is depressurized up to a pressure of preferably 6 x 10 3 mbar and 1.1 x 10 2 mbar.
  • the processing provides for the deposition of a thin layer of aluminum oxide (AI2O3) on a slab L, this latter is made pass through the processing room 14.
  • the dome is contemporaneously supplied with a reactive gas, for example oxygen (O2).
  • the high frequency generator generates an electromagnetic wave to realize an inductive plasma of the mixture, thus producing vapors of the deposition material, in this case aluminum oxide (AI2O3).
  • the plasma deposition process provides for supplying the mass flow meter with the precursor liquid, accurately measuring the mass flow rate of the precursor liquid, and supplying the mixing and expanding device with the desired measured mass flow rate of precursor liquid.
  • the mixing and expanding device is supplied with the carrier gas, so that the precursor liquid and the carrier gas form a gaseous mixture that, thanks to the mass flow meter, has the right amount of precursor (starting from a liquid) necessary for the reaction in the dome for forming the deposition material.
  • the precursor liquid is atomized inside a pressure-controlled mixing chamber, to form an aerosol: in the same chamber the carrier gas is inserted.
  • the precursor/carrier gas mixture exits from the mixing chamber and is heated through a heat exchanger, so that the liquid part thereof evaporates substantially completely. Then, the completely gaseous mixture is supplied to the inlet into the dome.
  • the reactive gas is supplied to the inlet into the dome, so that in the dome there are the reactive gas and the mixture with the precursor.
  • the plasma allows the mixture components to react so as to have vapors of the coating material that are deposited downwards, towards the operational area, where the slab is arranged.
  • the slab L IV is stopped in the second chamber 13 (the slab L IV is indicated by a broken line in Fig. 2), where the respective vertical moving device 20 lifts the slab L IV up to the next level.
  • the slab L’ is lowered by one level up to the moving plane. From here, the slab L’” moves and is processed in the same manner as the slab L IV up to the second chamber 13, where it is lifted by one level through the respective moving device.
  • the invention also provides for a machine where the length, i.e. the dimension corresponding to the moving direction of the slabs in the machine, of the processing room, indicated with the reference number 314 in the figure in question, is similar to that of the sealed chambers; anyway, it is equal to, or greater than, the dimensions of the single slabs under processing, i.e. of the single sets support-slab.
  • the supports-slabs enter the processing room 314 from the first chamber 12, remain in the processing room for the time necessary for the plasma deposition processing, and move to the second chamber only when the plasma deposition processing has been carried out.
  • the slab is processed while remaining still in the processing room, instead of moving through the processing room.
  • the case is shown where only one chamber is provided, matching with the processing room.
  • the only chamber 412 comprises an entrance first opening 415 for a support-slab L, and an exit second opening 416 for a support- slab L.
  • the machine comprises a plan moving device 419, analogous to the moving device 19.
  • a pressure adjusting device 430 and the processing device 426 for surface processing through plasma deposition are also provided, as well as, in general, all the components necessary for plasma deposition, as described above for the processing room 14.
  • the supports-slabs enter the chamber 412 one by one, and therefore the cycle of door closing-opening, during which depressurization and processing are performed, is carried out for one slab at a time.

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Abstract

L'invention concerne une machine pour le traitement de surface de produits au moyen d'un dépôt par plasma de couches minces de matériaux de revêtement, comprenant une source plasma radiofréquence élevée inductive, un dôme, au moins une entrée pour un gaz réactif entrant dans ledit dôme, au moins une entrée pour un mélange de gaz précurseur et de gaz vecteur, un dispositif d'alimentation pour alimenter ladite source de plasma avec ledit mélange de gaz précurseur et de gaz vecteur, la machine comprenant - au moins un premier réservoir conçu pour contenir un liquide pour au moins un liquide précurseur, - un débitmètre massique pour mesurer le débit massique du liquide précurseur sortant dudit au moins un premier réservoir, - au moins un second réservoir pour un gaz vecteur, - un dispositif de mélange et d'expansion du liquide précurseur provenant dudit débitmètre massique et dudit gaz vecteur provenant dudit au moins un second réservoir, - un conduit d'alimentation pour amener ledit mélange expansé depuis ledit dispositif de mélange et d'expansion vers ladite au moins une entrée pour un mélange de gaz précurseur et de gaz vecteur dans ledit dôme.
PCT/IB2020/060573 2019-11-12 2020-11-10 Machine pour le traitement de surface de produits au moyen d'un dépôt par plasma de couches minces de matériaux de revêtement, et procédé de traitement de produits par plasma WO2021094919A1 (fr)

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EP20817491.2A EP4058618A1 (fr) 2019-11-12 2020-11-10 Machine pour le traitement de surface de produits au moyen d'un dépôt par plasma de couches minces de matériaux de revêtement, et procédé de traitement de produits par plasma

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040026371A1 (en) * 2002-08-06 2004-02-12 Tue Nguyen Two-compartment chamber for sequential processing method
WO2008125969A2 (fr) * 2007-04-17 2008-10-23 Lapidei Nantech S.R.L. Dalles en pierre, résistant à l'usure, à la corrosion provoquée par des acides, et à l'action colorante de substances huileuses
DE102008026314A1 (de) * 2008-05-31 2009-12-10 Roth & Rau Ag Vakuumanlage mit mindestens zwei Vakuumkammern und einer Schleusenkammer zwischen den Vakuumkammern
US20100183825A1 (en) * 2008-12-31 2010-07-22 Cambridge Nanotech Inc. Plasma atomic layer deposition system and method
WO2011026936A2 (fr) * 2009-09-03 2011-03-10 Luciano Babbini Pierres naturelles recouvertes d'une couche de protection, leur procédé de production et d'utilisation

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040026371A1 (en) * 2002-08-06 2004-02-12 Tue Nguyen Two-compartment chamber for sequential processing method
WO2008125969A2 (fr) * 2007-04-17 2008-10-23 Lapidei Nantech S.R.L. Dalles en pierre, résistant à l'usure, à la corrosion provoquée par des acides, et à l'action colorante de substances huileuses
DE102008026314A1 (de) * 2008-05-31 2009-12-10 Roth & Rau Ag Vakuumanlage mit mindestens zwei Vakuumkammern und einer Schleusenkammer zwischen den Vakuumkammern
US20100183825A1 (en) * 2008-12-31 2010-07-22 Cambridge Nanotech Inc. Plasma atomic layer deposition system and method
WO2011026936A2 (fr) * 2009-09-03 2011-03-10 Luciano Babbini Pierres naturelles recouvertes d'une couche de protection, leur procédé de production et d'utilisation

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