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
  • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
  • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
  • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
  • C03C17/3618—Coatings of type glass/inorganic compound/other inorganic layers, at least one layer being metallic
• • 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
  • C23C14/46—Sputtering by ion beam produced by an external ion source
• • 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
  • C03C17/001—General methods for coating; Devices therefor
  • C03C17/002—General methods for coating; Devices therefor for flat glass, e.g. float glass
• • 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
  • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
  • C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
• • 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
  • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
  • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
• • 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
  • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
  • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
  • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
  • C03C17/3626—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer one layer at least containing a nitride, oxynitride, boronitride or carbonitride
• • 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
  • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
  • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
  • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
  • C03C17/3644—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the metal being silver
• • 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
  • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
  • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
  • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
  • C03C17/3652—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the coating stack containing at least one sacrificial layer to protect the metal from oxidation
• • 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
  • C23C14/0047—Activation or excitation of reactive gases outside the coating chamber
  • C23C14/0052—Bombardment of substrates by reactive ion beams
• • 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
  • C03C2217/70—Properties of coatings
  • C03C2217/73—Anti-reflective coatings with specific characteristics
  • C03C2217/734—Anti-reflective coatings with specific characteristics comprising an alternation of high and low refractive indexes

Definitions

• the present invention relates to a process for depositing thin layers on a substrate, in particular glass. It relates more particularly to deposition methods intended to be integrated within installation for the deposition of layers operating under vacuum, these installations having an industrial size (substrate whose dimension perpendicular to the direction of movement is greater than 1.5 m, even 2 m). It also targets substrates coated with a stack of layers of different functionalities (solar control, low-emissivity, electromagnetic shielding, heating, hydrophilic, hydrophobic, photocatalytic), layers modifying the level of reflection in the visible (antireflection or mirror layers in the visible domain or solar infrared) incorporating an active system (electrochromic, electroluminescent, photovoltaic, piezoelectric, diffusing, absorbing).
• the layers deposited by magnetron technique follow Thomton's law, namely that their microstructure is mainly columnar with a density and an average diameter of the columns varying according to the deposition pressure and other parameters such as the temperature of the substrate.
• This type of microstructure tends to lead to a fairly marked roughness of the deposited layers to the detriment of some of their properties.
• the grain boundaries predominantly perpendicular to the plane of the layer are also preferential pathways of chemical attack (for example air humidity)
• Certain macroscopic properties of thin layers are intimately linked to their microstructure, their state of crystallinity, their stoichiometry.
• the ionized gas atoms strike the target in a normal way, and the target is generally arranged in such a way that this normal is also perpendicular to the direction of the moving substrate, which implies that a large part kinetic energy of a atom atom is transmitted to the substrate, and is not used for the mobility of the formed atom.
• the off-axis spraying technique ie from the side
• magnetron sputtering can only be used on cathodes of length greater than 2 meters (for deposition on substrates of similar specific size) only if the sinusoidal or pulsed polarization for example is clocked at a frequency whose length of corresponding wave is large compared to the length of the cathode.
• it is notoriously difficult to deposit homogeneously using a 3 m cathode and radio frequency sputtering (of the order of 13.56 MHz).
• Patent US6214183 discloses a deposition method which combines a linear ion source, the beam of which is adapted to sputter the material of a target and a magnetron sputtering device.
• This process is designed to allow deposition on small surface substrates (a few tens of cm 2 at most) and in an enclosure operating in “batch”, that is to say in discontinuous regime.
• the present invention therefore aims to overcome the drawbacks of the magnetron spray deposition methods.
• the method of vacuum deposition of at least one thin layer on a substrate is characterized in that: - at least one species of spray is chosen which is chemically inactive or active with regard to a material to be sprayed , - a collimated beam of ions mainly comprising said spray type is generated, using at least one linear ion source positioned within an installation having an industrial size, - said beam is directed towards at least a target based on the material to be sprayed, - at least a portion of the surface of said substrate is positioned facing said target so that said material sprayed by ion bombardment of the target or a material resulting from the reaction of said sprayed material with at least one of the spray species is deposited on said surface portion.
• a relative movement is carried out between the ion deposition source and the substrate, - the linear ion source generates a collimated beam of ions of energy between 0.2 and 10 keV, preferably between 1 and 5 keV, in particular close to 1.5 keV, - the installation is pressurized in a range between 10 '5 and 8.10 ' 3 torr, - the ion beam and the target form an angle ⁇ between 90 ° and 30 ° preferably between 60 ° and 45 °, - we deposit at l using at least said source of linear ionic deposit simultaneously or successively on two different surface portions of a substrate, - an additional species is introduced in addition to said spray species, said additional species being
• the latter also relates to a substrate, in particular glassmaking, at least a portion of the surface of which is coated with a stack of thin layers consisting of at least one first layer based on metal oxide chosen in particular from tin oxide or the oxide of titanium, the silicon nitride / oxynitride optionally doped Al, and / or Zr, optionally a layer of metallic oxide or semiconductor in particular based on zinc oxide or titanium oxide, deposited on the first layer, a layer functional metal chosen in particular from silver, platinum, gold, nickel chromium, a metallic layer chosen in particular from chromium nickel, titanium, niobium, zirconium, said co metal uche possibly being nitrided or oxide deposited on or under (or both) the silver layer and at least one upper layer comprising a metal or semiconductor oxide chosen in particular from tin oxide or titanium oxide, optionally silicon nitride doped deposited on this metallic layer, this upper layer possibly being of a protective layer known
• a substrate in particular glass, of which at least a portion of surface is coated with a stack of thin layers comprising an alternation of n functional layers A with reflection properties in infrared and / or in solar radiation, based in particular on silver, and (n + 1) coatings B with n> 1, said coatings B comprising one or a superposition of layers of dielectric material based in particular on nitride of silicon or of a mixture of silicon and aluminum, or of silicon oxynitride, or of zinc oxide, so that each functional layer A is disposed between two coatings B, the stack also comprising absorbent layers in visible C, in particular based on titanium, nickel chromium, zirconium, optionally nitrided or oxidized, situated above and / or below the functional layer characterized in that one at least ins of the layers of the coating B or C is deposited by the process which is the subject of the invention.
• this relates to a substrate, in particular glass, of which at least a portion of surface is coated with a stack of thin layers comprising an alternation of n functional layers A with infrared reflection properties. and / or in solar radiation, based in particular on silver, and (n + 1) coatings B with n> 1, said coatings B comprising a layer or a superposition of layers of dielectric material so that each layer A is arranged between two coatings B, characterized in that at least one of the layers of the coating A is deposited by the process which is the subject of the invention.
• this relates to a substrate with a glazing function, in particular glassmaking, comprising on at least one of its faces an anti-reflective or mirror coating in the visible range or solar infrared, made of a stack (A) of thin layers of dielectric materials with alternately strong and weak refractive indices, characterized in that at least one of the layers is deposited by the process mentioned above.
• this consists in inserting within a line, of industrial size (typically a line width of around 3.5 m), for the deposition of thin layers on a substrate, at least one source of linear ion deposition.
• the term industrial size is understood to mean a production line the size of which is adapted on the one hand, to operate continuously and on the other hand, to treat substrates of which one of the characteristic dimensions, for example, the width perpendicular to the direction of circulation of the substrate is at least 1.5 m.
• the term "ion deposition source” means a complete system integrating a linear ion source as well as a device integrating a target and a target holder. This source of linear ionic deposition is positioned within a treatment enclosure, the working pressure of which can easily be lowered below 0.1 mtorr (approximately 133 10 ⁇ 4 Pa), practically from 1.10 5 to 5.10 '3 torr.
• This working pressure can be globally between 2 to 50 times less than the lowest working pressure for a magnetron spraying line, but the linear ion deposition device can also operate at the deposition pressure of the conventional magnetron process.
• the fact of using a range of working pressure which is not too high makes it possible to obtain an improvement in a number of properties at the level of the deposited layers:
• the layers deposited by the process which is the subject of the invention have a very high defect density lower than that which would be obtained if a conventional magnetron line was used (with its specific working pressure range).
• the layers thus deposited make it possible to achieve increased chemical durability of the layered stacks because it is known that the resistance to chemical attacks improves when the number of defects in the final layers of the stacks decreases (the defects are initiated from the cavities / terminal layer holes).
• the latter constitute in fact privileged entry points for corrosive / altering substances (water, acid, various corrosive agents), and are present locally in the form of "holes".
• the presence of defects or holes at the end layers of a stack is particularly harmful when said stack incorporates at least one layer of silver.
• the presence of holes may indeed cause the appearance of pitting, for example in the presence of water or a humid atmosphere. We therefore understand that by decreasing the density of holes, we increase the chemical resistance of this type of stack.
• the substrate comprises a coating of the “reinforced thermal insulation” or Low E (low emissive) type.
• This coating consists of at least one sequence of at least five successive layers, namely a first layer based on metal oxide chosen in particular from tin oxide or titanium oxide (according to a thickness between 10 and 30 nm), a layer of metallic or semiconductor oxide, in particular based on zinc oxide or titanium oxide, deposited on the first layer (at a thickness of between 5 and 15 nm), a layer of silver (depending on a thickness of between 5 and 15 nm), a metallic layer chosen in particular from nickel chromium, titanium, niobium, zirconium, said metallic layer being optionally nitrided or oxidized (according to a thickness of less than 5 nm) deposited on the silver layer and at least one upper layer (with a thickness between 5 and 45 nm) comprising a metal or semiconductor oxide chosen in particular from tin oxide or titanium oxide deposited on this metal layer, this upper layer (possibly consisting of a plurality of layers) optionally comprising a so-called “overcoat” protective
• a silver stack according to the prior art is deposited on a glass substrate 4 mm thick with a layer of sacrificial metal blocker in nickel-chromium and an upper dielectric layer in tin oxide.
• An E1 stack of the substrate / SnO 2 / ZnO / Ag / NiCr / SnO 2 type (41 nm) is obtained.
• This stack E1 is produced by magnetron sputtering by passing the substrate through an enclosure in front of metallic targets based on the materials in front. be deposited in an argon atmosphere to deposit a layer of metal and in an argon and oxygen atmosphere to deposit an oxide.
• E1 stack substrate / SnO 2 / ZnO / Ag / NiCr / SnO 2 (20 nm) "* 0 / SnO 2 (21 nm)
• IBS SnO 2 MAG is deposited by reactive sputtering of a planar tin target while SNO2IBS is deposited according to the process described above using a device installed in the same vacuum frame, therefore the stack is not subjected to atmospheric pressure between the two final layers of SnO 2 .
• MAG is equivalent to “deposited by magnetron” and IBS is equivalent to “deposited by the method according to the invention ie using a source of linear ionic deposit, in English IBS (Ion Beam Sputtering)”
• IBS Ion Beam Sputtering
• a substrate coated with a Low E stack the following is given: -substrate / SnO 2 / ZnO / Ag / NiCr / ZnO / Si 3 NA
• a silver stack according to the prior art is deposited on a glass substrate 4 mm thick with a layer of zinc oxide coated with a terminal layer of silicon nitride.
• An E3 stack of the substrate / SnO 2 / ZnO / Ag / NiCr / ZnO / Si 3 N 4 type is obtained (20 nf 0
• This stack E3 is produced by magnetron sputtering by passing the substrate through an enclosure in front of metal targets based on of materials to be deposited.
• E4 stack substrate / SnO 2 / ZnO / Ag / NiCr / ZnO / Si 3 N 4 (10 nm) w " J / Si 3 N 4 (10nm) IBS Comparative table of chemical durability
• the deposition method according to the invention generally makes it possible to improve the mechanical durability of the stack by controlling the level of compressive stress. More specifically, this improvement in mechanical durability results in increased resistance to "mechanical attack" of the scratch or abrasion type during the processing or life phases of the layered glazing.
• the vacuum deposition methods known from the prior art generally lead to the production of layers which have very high compressive stresses.
• a substrate is given below comprising a solar control coating, suitable for undergoing heat treatments (of the quenching type), and designed for applications specific to the automobile.
• This coating consists of a stack of thin layers comprising an alternation of n functional layers A with reflection properties in the infrared and / or in the solar radiation, based in particular on silver (with a thickness of between 5 and 15 nm), and of (n + 1) coatings B with n> 1, said coatings B comprising one or a superposition of layers of dielectric material based in particular on silicon nitride (according to a thickness of between 5 and 80 nm), or of a mixture of silicon and aluminum, or of oxynitride of silicon, or of zinc oxide (according to a thickness of between 5 and 20 nm), so that each functional layer A is placed between two coatings B, the stack also comprising absorbent layers in the visible C, in particular based on titanium, nickel chromium, zirconium, optionally nitrided or oxidized, located above and / or below the functional layer.
• the E5 reference stack is as follows:
• the stack E6 is as follows: Si 3 N 4 ⁇ G / ZnO / Ti / Ag / ZnO / Si 3 N 4 IBS / ZnO / Ti / Ag / ZnO / Si 3 N, IBS
• the deposition method according to the invention generally makes it possible to improve the quality of the deposited layers, in particular in that this method reduces the roughness of the layers.
• obtaining an optimal (or even minimum) roughness is essential when the layer in question is a functional layer or an under-layer to be coated with a functional layer.
• the functional layer is silver-based, it is known that the optimal obtaining of an emissivity, an electrical conductivity, a reflectance in the infrared is dependent on the roughness of the silver layer. and that the latter depends on the roughness of the layer preceding it in the stack.
• E6 bis which illustrates this property at the level of the functional layer.
• Substrate / Si3N 4 / ZnO / Ti / Ag / ZnO / Si 3 N 4 At the level of this stacking structure, a 10 nm layer of silver is deposited by a traditional magnetron process and by the object process. the invention.
• the deposition process which is the subject of the invention reduces the roughness therefore, as previously mentioned, by reducing the resistance per square (decrease in resistivity and emissivity)
• the improvement in terms of roughness is illustrated on a layer of silica
• the roughness (determined by AFM on a quadrant 0.5 by 0.5 ⁇ m2) of the layer of SiO 2 deposited by the process object of the invention is less than the roughness of the SiO 2 layer deposited by magnetron of the same thickness.
• the reference E7 stack is as follows: substrate / ZnO ⁇ 0 (32nm) / Ag (10 nm) / NiCr (1 nm) / Sn0 2 (25 nm)
• E7 stack is compared to the E8 and E9 stack structures characterized by E8 stack: substrate / ZnO IBS (32 nm) / Ag (10 nm) / NiCr (1 nm) / Sn0 2 (25 nm) E9 substrate / Si stack 3 N 4 IBS (25 nm) / ZnO (10 nm) / Ag (10 nm) / NiCr (1 nm) / Sn0 2 (25 nm)
• the deposition method according to the invention generally makes it possible to improve the optical performance of stacks, and in particular anti-reflection stacks, or reflective stacks comprising only dielectric layers.
• the high index layers are generally made of Ti0 2 or Nb 2 Os which have actually a high index, of approximately 2.45 and 2.35 respectively and the low index layers are most often made of Si0 2 , of index approximately 1.45
• the stack retains its optical properties , mechanical (hardness, resistance to scratching, to abrasion), chemical resistance, during heat treatment (bending and / or quenching), it is known to use as a high index layer, a layer with base of Si 3 N 4 .
• its refractive index which is substantially close to 2.0 to 550 nm, limits the possibilities of optical optimization.
• the process which is the subject of the invention makes it possible to significantly improve the optical performance of the stacks mentioned above.
• This terminal layer can thus have hydrophobic properties (static contact angle greater than or equal to 80 °), or on the contrary have hydrophilic properties (static contact angle less than 20 °).
• a comparative table of refractive indices for high index materials is given below.
• the optical performances (resulting from optical simulations) of stacks of identical symmetrical structure E10 to E14 SiO 2 MAG / TiO 2 / SiO ⁇ 0 / M / substrate / M / SiO ⁇ 0 / TiO 2 / SiOa ⁇ 0 .
• the linear ionic source very schematically comprises an anode, a cathode, a magnetic device, a gas introduction source . Examples of this type of source are described in in particular in RU2030807, US6002208, or WO02 / 093987.
• the anode is brought to a positive potential by a continuous supply, the potential difference between the anode and the cathode, causes the ionization of a gas injected nearby.
• the gas injected can be a mixture of gases based on oxygen, argon, nitrogen, helium, a noble gas, such as for example neon, or a mixture of these gases.
• the gas plasma is then subjected to a magnetic field (generated by permanent or non-permanent magnets), which makes it possible to accelerate and focus the ion beam.
• the ions are therefore collimated and accelerated towards the outside of the source towards at least one target, possibly polarized, of which the material is to be pulverized, and their intensity is in particular a function of the geometry of the source, the gas flow rate, their nature, and the voltage applied to the anode.
• the operating parameters of the ion deposition source are adapted so that the energy and the acceleration transmitted to the collimated ions are sufficient to atomize, due to their mass, their effective atomization section, material aggregates of the material forming the target.
• the respective orientation of the ion source (or ion sources) and of the target is such that the ion beam (the ion beams) ejected from the source comes to spray the target at one or more angles. means determined in advance (between 90 ° and 30 °, preferably between 60 and 45 °).
• the vapor of atomized atoms must be able to reach a moving substrate whose width is at least 1 meter (1 m being a critical size from which an installation can be qualified as industrial).
• the target can be integrated within a magnetron sputtering device.
• a magnetron sputtering device In the vicinity of the substrate, it is possible to inject, optionally, by means of a gas injection device, a second species in the form of gas or a plasma, chemically active with respect to the sprayed or bombarded material originating of the target.
• a gas injection device In the vicinity of the substrate, it is possible to inject, optionally, by means of a gas injection device, a second species in the form of gas or a plasma, chemically active with respect to the sprayed or bombarded material originating of the target.
• an ion neutralizing device electrostatic source
• This device can consist of a magnetron cathode operating nearby.
• the substrates on the surface of which it is intended to deposit the previously mentioned thin layers are preferably transparent, flat or curved, made of glass or plastic (PA ⁇ MA, PC ).
• PA ⁇ MA, PC glass or plastic
• the method according to the invention makes it possible to develop in a chamber of industrial size, a substrate, in particular glassmaking, comprising on at least one of its faces a stack of thin layers comprising at least one layer deposited by said process and whose roughness / stress / density of defects / state of crystallinity / optical dispersion law has (have) been modified (es) relative to a stack comprising only layers deposited by magnetron sputtering.
• the linear ion source directed towards a target with another linear ion source oriented towards the layer covering the substrate resulting from the spraying of said target.
• an ion source directed towards the target in an enclosure or in the immediate vicinity of an enclosure incorporating conventional cathodes these cathodes being able to be planar or rotary with one or two tubes.
• the target used within the ion deposition device can be one or a plurality of plates or tubes, fixed or else set in motion during the process.
• glazing intended for applications relating to the automotive industry, in particular a car roof, a side glazing, a windshield, a rear window, a rear-view mirror, or a single or double glazing intended for the building industry.
• a display store counter that can be curved, of a protective glass of an object of the table type, of a computer anti-glare screen, d '' glass furniture, a sill, an anti-fouling system.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• Materials Engineering (AREA)
• Organic Chemistry (AREA)
• Life Sciences & Earth Sciences (AREA)
• General Chemical & Material Sciences (AREA)
• Geochemistry & Mineralogy (AREA)
• Mechanical Engineering (AREA)
• Metallurgy (AREA)
• Physical Vapour Deposition (AREA)
• Surface Treatment Of Glass (AREA)

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  • 2004-04-21 FR FR0404204A patent/FR2869324B1/fr not_active Expired - Fee Related
• 2005
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  • 2005-04-15 RU RU2006141003/02A patent/RU2006141003A/ru not_active Application Discontinuation
  • 2005-04-15 CN CNA2005800125256A patent/CN1950540A/zh active Pending
  • 2005-04-15 KR KR1020067021550A patent/KR20070004042A/ko not_active Application Discontinuation
  • 2005-04-15 US US11/578,938 patent/US20090226735A1/en not_active Abandoned
  • 2005-04-15 WO PCT/FR2005/050250 patent/WO2005106070A2/fr active Application Filing
  • 2005-04-15 JP JP2007508949A patent/JP2007533856A/ja active Pending
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