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EP3658697A1 - Revêtement par un carbone similaire au diamant via un procédé pecvp-magnétron - Google Patents

Revêtement par un carbone similaire au diamant via un procédé pecvp-magnétron

Info

Publication number
EP3658697A1
EP3658697A1 EP18739878.9A EP18739878A EP3658697A1 EP 3658697 A1 EP3658697 A1 EP 3658697A1 EP 18739878 A EP18739878 A EP 18739878A EP 3658697 A1 EP3658697 A1 EP 3658697A1
Authority
EP
European Patent Office
Prior art keywords
target
substrate
magnetron
reactant
glass
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP18739878.9A
Other languages
German (de)
English (en)
Inventor
Jan Hagen
Norbert Huhn
Julian Lingner
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Saint Gobain Glass France SAS
Original Assignee
Saint Gobain Glass France SAS
Compagnie de Saint Gobain SA
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 Saint Gobain Glass France SAS, Compagnie de Saint Gobain SA filed Critical Saint Gobain Glass France SAS
Publication of EP3658697A1 publication Critical patent/EP3658697A1/fr
Pending legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C23C14/0057—Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C23C14/0063—Reactive sputtering characterised by means for introducing or removing gases
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0605—Carbon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0605—Carbon
    • C23C14/0611—Diamond
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/12—Organic 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • C23C16/26—Deposition of carbon only
    • 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
    • C23C16/513—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 plasma jets

Definitions

  • the invention relates to a method for the production of layers
  • DLC diamond-like carbon
  • PECVD plasma enhanced chemical vapor deposition
  • magnetron magnetron
  • float glass inherently does not have high scratch resistance, but the application of a suitable thin film can significantly improve the scratch resistance of the glass surface.
  • DLC diamond-like carbon
  • CN 1 05441 871 A describes the preparation of superhard DLC layers by means of PVD and H I PI MS methods.
  • CN 1 04962914 A an industrial vapor deposition apparatus for depositing DLC layers is described.
  • Another device for producing DLC layers is described in CN 203834012 U.
  • J P 201 1068940 A relates to a method for
  • WO 2004/071981 A2 relates to an ion beam technology for depositing DLC layers on glass.
  • This technology provides good quality coatings, but is demanding in terms of process stability.
  • the deposition of material (DLC material) on the ion source can affect the operating stability of the ion source and z. B. because of problems with the electrical
  • Insulation, arcing, deposits, etc. lead to process interruptions.
  • Chemical vapor deposition is not suitable for large-scale coatings on glass because they require high deposition temperatures and off plant technical reasons are not easy insectsskalierbar on large areas.
  • the heating of large glass panes is very expensive in view of the energy consumption and risky because of the possible glass breakage.
  • the invention is based on the object to overcome the disadvantages described above in the prior art.
  • the object is in particular to provide a method for coating substrates with DLC layers that for the large-area coating of substrates such.
  • Glass sheets is suitable and provides DLC layers having mechanical properties, particularly scratch resistance, and optical properties comparable to those achieved by conventional ion beam techniques or CVD methods, but avoids the problems associated with these conventional techniques.
  • the process is intended to improve process stability and not require heating of the substrate.
  • the method should be realized with the existing common deposition devices.
  • this object is achieved by a coating method according to claim 1.
  • the invention also relates according to the further claim to a coated substrate obtainable by the coating method according to the invention.
  • Preferred embodiments of the invention are given in the dependent claims.
  • the invention thus relates to a method for coating a substrate with a diamond-like carbon (DLC) layer by a PECVD method with plasma generation via a magnetron (magnetron PECVD) in one
  • a vacuum chamber in which the targeted magnetron and the substrate are arranged comprising introducing at least one reactant gas into the plasma generated by the magnetron target in the
  • Vacuum chamber whereby fragments of the reactant gas are formed, which are deposited to form the DLC layer on the substrate.
  • the magnetron PECVD process used according to the invention has DLC coatings of
  • the magnetrontarget material is not noticeably incorporated into the formed DLC thin films and therefore does not alter the layer properties, in particular with regard to the optical properties, wherein, if desired, doping of the DLC layer via the target material may also be possible.
  • the magnetron PECVD method does not require heating of the substrate and is therefore suitable for large-scale deposition on glass or other temperature-sensitive substrates.
  • the inventive method can be realized with the usual deposition devices.
  • Fig. 1 is a schematic representation of the structure of a device for
  • Fig. 2 is a schematic representation of a planar magnetron
  • FIG. 3 shows a PECVD magnetron hysteresis curve for target voltage and pressure in FIG.
  • FIG. 4 shows a PECVD magnetron hysteresis curve for target voltage and pressure in FIG.
  • the method according to the invention for coating the substrate with a diamond-like carbon (DLC) layer is a PECVD method in which the plasma is generated by a magnetron or a magnetron target.
  • a magnetron or a magnetron target Such methods are known in principle and are described e.g. referred to as magnetron-supported PECVD, magnetron PECVD or PECVD magnetron method.
  • Plasma-assisted chemical vapor deposition is a well-known vapor deposition process, and PECVD (plasma-enhanced chemical vapor deposition) is used as an abbreviation.
  • PECVD plasma-enhanced chemical vapor deposition
  • CVD chemical vapor deposition
  • a solid component is deposited on a substrate due to chemical reactions in the gas phase.
  • the molecules of the reactant gas are decomposed or dissociated by means of heat or energy supply with the formation of fragments. It can be with these fragments are active species, such as excited atoms, radicals or ions, which form on the substrate to form the solid layer, here the DLC layer,
  • PVD physical vapor deposition
  • the plasma for the PECVD method is generated by a magnetron or a magnetron target.
  • Magnetrons include electrodes and a magnet assembly.
  • the cathode typically in the form of a cathode tube or a planar body, is also commonly referred to as a target or magnetron target, typically with an additional material attached to the cathode and serving as a target or magnetron target.
  • the magnet assembly is located behind the target, relative to the positioning to the substrate.
  • the target can be z.
  • Magnetrons with planar targets may include a magnet assembly fixed in a fixed position behind the target.
  • a target which is usually tubular, encloses a magnet assembly, the target being rotatably supported and driven, the magnet assembly being generally immobile, ie, not rotating.
  • the magnetron plasma source is generated by the magnetron target.
  • the gastric target is a target of silicon, carbon or a metal, which metal is preferably selected from titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum or tungsten.
  • the target is particularly preferably made of silicon or titanium.
  • the silicon target may be coated with aluminum and / or boron and / or zirconium and / or hafnium and / or titanium be doped. This may be advantageous to improve the target conductivity or the process stability of the deposition.
  • Magnetron and the substrate to be coated in a vacuum chamber arranged.
  • power is applied to the target to generate a plasma in the vacuum chamber through the magnetron or magnetron target.
  • the target and the substrate are positioned so that the plasma is between target and
  • Substrate is formed.
  • the substrate and / or magnetron may be slidably disposed to allow for various positioning as is common in such devices.
  • Usual vacuum coating systems eg. As commercial vacuum sputtering apparatus, can be used for the inventive method.
  • reactants which are passed as reactant gas in the vacuum chamber or in the plasma, z.
  • reactants liquids and gases; but solids are also conceivable if they can be converted into the gas phase.
  • reactants are suitable which contain or consist of the elements carbon and hydrogen or the elements silicon, carbon and hydrogen.
  • the at least one reactant is preferably selected from hydrocarbons, organosilicon compounds or mixtures thereof. Organosilicon compounds are preferred
  • Silicon compounds containing hydrocarbon radicals e.g. Alkyl groups.
  • the DLC layer formed can be doped with silicon.
  • the at least one reactant is selected from tetramethylsilane (TMS), C 1 -C 10 -alkanes, C 2 -C 10 -alkynes, benzene or
  • C 2 -C 10 -alkynes are ethyne, propyne, butyne, pentin, hexine, heptine, octyne, nonyne, decyne and their isomers.
  • Examples of C 1 -C 10 -alkanes are methane, ethane, propane, butane, pentane, hexane, heptane, octane, nonane, decane and their isomers.
  • the at least one reactant is particularly preferred selected from tetramethylsilane (TMS), methane (CH 4 ), ethyne (C2H2) or
  • Reactants may also be used which contain elements other than Si, C and H, e.g. Nitrogen, sulfur, fluorine or chlorine.
  • Reactants may be advantageous to modify the wetting properties or mechanical properties of the DLC layers. This may result from the doping of the DLC layers with elements other than carbon and hydrogen contained in such reactants.
  • the DLC layers produced by the process according to the invention may be doped with one or more such foreign atoms.
  • the term "foreign atoms" does not say anything about the bonding of these foreign atoms in the DLC layer in which they are incorporated.
  • the doping of the DLC layer with impurities can be used selectively to modify the properties of the DLC layer.
  • Reactants containing elements other than Si, C and H, if containing carbon and optionally hydrogen, may optionally be used alone. However, it is usually preferred to use these reactants in combination with at least one reactant derived from
  • Hydrocarbons and / or organosilicon compounds is selected, as described above, this being required for reactants that do not contain carbon and optionally hydrogen, of course.
  • a reactant containing elements other than Si, C and H is e.g. As nitrogen (N2 gas), optionally together with as an additional component
  • Reactants such as hydrocarbon or organosilicon compounds can be introduced as a reactant gas in the vacuum chamber.
  • reactants such as hydrocarbon or organosilicon compounds
  • N2 gas is usually not an inert gas here.
  • reactants containing fluorine are also examples. These may be advantageous because it may affect the hydrophobicity of the DLC layer.
  • Suitable optional fluorine-containing reactants are perfluorocarbons such.
  • Tetrafluoromethane (CF 4 ) or perfluorooctane.
  • fluorine-containing reactants are, if used, are usually used as additional reactants together with hydrocarbons and / or organosilicon compounds.
  • the inventive method comprises introducing one or more reactant gases into the vacuum chamber and thus into the plasma formed by the magnetron target.
  • reactant gases When using multiple reactant gases, they can be introduced separately or as a mixture.
  • the usual feed systems are used for the introduction of the reactant gases.
  • the reactant gases are subjected in the plasma to the above-described chemical reactions, whereby
  • Fragments of the reactant gas are formed, which are deposited to form the DLC layer on the substrate.
  • the method according to the invention further comprises introducing at least one inert gas into the vacuum chamber.
  • inert gases are neon, argon, krypton, xenon or a combination thereof.
  • the inert gas may, for. B. be useful to support the plasma generation.
  • Method is the ratio of the flow rates of reactant gas / I nertgas> 0.4, preferably> 0.5 and more preferably> 0.6.
  • the reactant gas is C2H2, CH4 or TMS and the inert gas Ar, ie. the ratio of the flow rates of C2H 2 Ar or CH 4 / Ar or TMS / Ar is> 0.4, preferably> 0.5 and more preferably> 0.6. With such ratios, particularly scratch-resistant coatings could be produced. It is understood that too
  • the magnetron PECVD method is operated so that during the deposition of the DLC layer on the substrate, the target is operated in the poisoned mode. This surprisingly leads to better mechanical
  • Process parameters such. As deposition rate, partial pressure of the reactant gas or target voltage can make noticeable. It is also said that the process is tilting from metallic to poisoned mode. This is also noticeable by the fact that process parameters show a hysteresis behavior.
  • target poisoning is detrimental to the process, since in particular the deposition rate decreases, which is why it is generally avoided to operate the process in such a way that the target is in the poisoned mode. It was thus more surprising that the operation of the method according to the invention with a target in the poisoned mode leads to significantly better results. The best DLC properties were obtained in the area of target poisoning.
  • Target voltage and / or the vacuum pressure depending on the flow rate of the reactant or are made.
  • the area in which target poisoning is present is in the diagram to the right of the hysteresis curve, ie in
  • the process control should therefore take place to the right of the hysteresis curve, ie outside the hysteresis range, in order to operate a target in the poisoned mode.
  • the appropriate for a target poisoning flow rate can be determined for each specific case.
  • Deposition of the DLC layer in the range of 20 ° C to 150 ° C.
  • the inventive method is in the vacuum chamber in a vacuum
  • the pressure is in the
  • Vacuum chamber in the range of 0, 1 ⁇ bar to 1 0 ⁇ bar.
  • Power output / target length can be z. B. in the range of 1 kW / m to 50 kW / m, preferably from 5 kW / m to 25 kW / m.
  • the deposition rate of DLC may be e.g. B. in the range of 1 nm * m / min to 200 nm * m / min, preferably from 1 0 nm * m / min to 1 00 nm * m / min, are.
  • the substrate may be a conductive substrate or a non-conductive substrate.
  • Preferred substrates are substrates of metal, plastic, paper, glass, glass ceramic or ceramic. In a particularly preferred
  • Embodiment is the substrate of glass, z. B. in the form of a glass.
  • a preferred glass substrate is float glass.
  • the thickness of the substrates, in particular of the glass substrates, can vary within wide ranges, wherein the thickness z. B. may be in the range of 0, 1 mm to 20 mm.
  • the substrate may be uncoated or precoated with at least one basecoat.
  • the DLC layer is applied to this precoat. I n a preferred
  • the substrate is an uncoated glass substrate or a precoated with a base layer glass substrate.
  • the precoat for the substrate, in particular a glass substrate, used as a base layer may contain or consist of a material selected from silicon carbide, silicon oxide, silicon nitride (S 13N4), silicon oxynitride, metal oxide, metal nitride, metal carbide or a combination thereof, where S 13N4 and / or doped S 13N4 is preferred and Zr, Ti, Hf and / or B doped S 13N4 is particularly preferred.
  • the metal may be e.g. Titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum or tungsten.
  • the base layer has, for example, a layer thickness of 1 nm to 1 00 nm, preferably from 5 nm to 50 nm.
  • the DLC layer has a layer thickness of 1 nm to 1 00 nm, preferably 1 nm to 50 nm, more preferably 1 nm to 20 nm, particularly preferably 2 nm to 10 nm, in particular 3 nm to 8 nm, up.
  • Diamond-like carbon is usually abbreviated to DLC (for "diamond-like carbon").
  • DLC layers hydrogen-free or hydrogen-containing amorphous carbon is the predominant component, which carbon may consist of a mixture of sp 3 and sp 2 -hybridized carbon;
  • DLC examples include those named ta-C and a: C-H.
  • the DLC layer used according to the invention can be doped or undoped.
  • the DLC layer formed may be doped with at least one impurity atom, wherein the impurity atom is preferably selected from silicon, oxygen, sulfur, nitrogen, chlorine, fluorine or a metal, wherein the metal is preferably selected from titanium, zirconium .
  • Hafnium, vanadium, niobium, tantalum, chromium, molybdenum or tungsten Hafnium, vanadium, niobium, tantalum, chromium, molybdenum or tungsten.
  • the foreign atoms can z.
  • the invention also relates to the coated substrate, in particular the
  • coated glass substrate obtainable by the method of the invention as described above.
  • the glass sheets according to the invention are suitable for. B. for buildings, vehicles, glass furniture, z. As shelves or tables, tactile applications and screens.
  • Fig. 1 shows a purely schematic representation of the structure of an apparatus for carrying out the magnetron PECVD method according to the invention.
  • a substrate 1 z.
  • a magnetron with a rotatable target 2 in the form of a cylinder.
  • the target may be a silicon target.
  • the substrate is displaceable. I m operation is by the
  • the reactant gas for. B. C2H2
  • inert gas 5 may, if necessary, inert gas, for. As argon, are introduced into the vacuum chamber.
  • the vacuum connection 7 serves to adjust the vacuum.
  • Fig. 2 shows a schematic representation of a planar magnetron 1 0, which has a mounted on the cathode target 9 and an underlying magnet assembly 1 1.
  • the resulting magnetic field 8 is sketched schematically.
  • magnetron hysteresis curves for different reactants in combination with a silicon target were tested.
  • Argon was used as the inert gas.
  • DLC layers were made on glass substrates by the magnetron PECVD method. The best DLC properties were obtained in the area of target poisoning.
  • FIG. 3 shows the obtained PECVD magnetron hysteresis curve for a silicon target and CH4 as a reactant, in which the process parameters target voltage and pressure were recorded as a function of the flow rate of the reactant.
  • FIG. 4 shows the PECVD magnetron hysteresis curve obtained for a silicon target and C2H2 as a reactant, in which the process parameters target voltage and pressure were recorded as a function of the flow rate of the reactant.
  • the process parameters selected for the deposition of the DLC thin films are shown in Table 1 below.
  • the equipment used is a conventional magnetron coating apparatus.
  • Table 1 Deposition parameters for DLC coatings using PECVD magnetron techniques
  • the layer quality obtained is very reproducible and the process stability is very good.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Physical Vapour Deposition (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

L'invention concerne un procédé pour le revêtement d'un substrat (1) présentant une couche de carbone similaire au diamant (diamond-like carbone) (DLC) par un procédé PECVD (dépôt chimique en phase vapeur assisté par plasma) avec génération d'un plasma via une cible de magnétron (PECVD-magnétron) dans une chambre à vide (3), dans laquelle le magnétron (10) pourvu de la cible (9) et le substrat (1) sont disposés, le procédé consistant à introduire au moins un gaz de réactif dans le plasma généré dans la chambre à vide par la cible de magnétron (9), des fragments du gaz de réactif étant ainsi formés, qui sont déposés tout en formant la couche de DLC sur le substrat (1). Le procédé selon l'invention convient pour le revêtement en grande surface de substrats (1), tels que par exemple des feuilles de verre, par des couches de DLC. Les couches de DLC obtenues présentent une qualité remarquable en ce qui concerne la résistance aux rayures et l'optique. Le procédé selon l'invention peut être réalisé à l'aide des dispositifs de dépôt usuels. Un chauffage du substrat n'est pas nécessaire.
EP18739878.9A 2017-07-26 2018-07-19 Revêtement par un carbone similaire au diamant via un procédé pecvp-magnétron Pending EP3658697A1 (fr)

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EP17183187 2017-07-26
PCT/EP2018/069609 WO2019020481A1 (fr) 2017-07-26 2018-07-19 Revêtement par un carbone similaire au diamant via un procédé pecvp-magnétron

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CN113913735B (zh) * 2021-09-07 2022-06-24 广州今泰科技股份有限公司 一种钒/钇共掺杂dlc涂层及其制备方法
WO2023161080A1 (fr) 2022-02-23 2023-08-31 Saint-Gobain Glass France Procédé pour la production d'un substrat traité thermiquement pourvu d'un revêtement de type diamant
WO2023198554A1 (fr) 2022-04-11 2023-10-19 Saint-Gobain Glass France Vitrage ayant une fenêtre de communication pour capteurs et systèmes de caméra
CN116949418A (zh) * 2022-04-15 2023-10-27 江苏菲沃泰纳米科技股份有限公司 一种dlc涂层、其制备方法及设备及复合涂层、涂覆制品
EP4289519A1 (fr) * 2022-06-10 2023-12-13 Basf Se Barrières créées par le plasma pour l'emballage
WO2024008565A1 (fr) 2022-07-04 2024-01-11 Saint-Gobain Glass France Vitre feuilletée pour système de projection
US20240392444A1 (en) * 2023-05-22 2024-11-28 IBC Materials & Technologies, LLC Coating compositions, methods to produce non-stick surfaces and non-stick surfaces made therefrom
DE202023103844U1 (de) 2023-07-11 2023-08-01 Saint-Gobain Glass France Beheizbare Verbundscheibe
WO2025082772A1 (fr) 2023-10-19 2025-04-24 Saint-Gobain Sekurit France Substrat à revêtement anti-rayures amélioré
CN120233472A (zh) * 2023-12-28 2025-07-01 江苏菲沃泰纳米科技股份有限公司 玻璃显示面板防护膜、其制备方法以及包括其的产品

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CN110914468A (zh) 2020-03-24
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KR20200034773A (ko) 2020-03-31
US20200208257A1 (en) 2020-07-02

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