WO2024002484A1 - Apparatus for removing a protective film from and measuring optical properties of a coated flat glass product - Google Patents

Apparatus for removing a protective film from and measuring optical properties of a coated flat glass product Download PDF

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Publication number
WO2024002484A1
WO2024002484A1 PCT/EP2022/068097 EP2022068097W WO2024002484A1 WO 2024002484 A1 WO2024002484 A1 WO 2024002484A1 EP 2022068097 W EP2022068097 W EP 2022068097W WO 2024002484 A1 WO2024002484 A1 WO 2024002484A1
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WO
WIPO (PCT)
Prior art keywords
plasma
glass product
vacuum
plasma source
optical
Prior art date
Application number
PCT/EP2022/068097
Other languages
French (fr)
Inventor
Christian GROGG
Aneliia WÄCKERLIN
Matthias MUOTH
Original Assignee
Glas Trösch Ag
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 Glas Trösch Ag filed Critical Glas Trösch Ag
Priority to PCT/EP2022/068097 priority Critical patent/WO2024002484A1/en
Publication of WO2024002484A1 publication Critical patent/WO2024002484A1/en

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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
    • C03C17/34—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
    • C03C17/001—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
    • C03C17/36—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
    • C03C17/3657—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 multilayer coating having optical properties
    • C03C17/366—Low-emissivity or solar control coatings
    • 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
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0005—Other surface treatment of glass not in the form of fibres or filaments by irradiation
    • C03C23/006—Other surface treatment of glass not in the form of fibres or filaments by irradiation by plasma or corona discharge
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • 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
    • C03C2218/30—Aspects of methods for coating glass not covered above
    • C03C2218/32—After-treatment
    • C03C2218/328—Partly or completely removing a coating
    • 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
    • C03C2218/30—Aspects of methods for coating glass not covered above
    • C03C2218/32—After-treatment
    • C03C2218/328—Partly or completely removing a coating
    • C03C2218/33—Partly or completely removing a coating by etching
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N2021/1738—Optionally different kinds of measurements; Method being valid for different kinds of measurement
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/8422—Investigating thin films, e.g. matrix isolation method
    • G01N2021/8427—Coatings
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/8422—Investigating thin films, e.g. matrix isolation method
    • G01N2021/8438—Mutilayers

Definitions

  • the present invention relates to an apparatus for removing a protective film from a coated flat glass product and subsequently measuring optical properties of the glass product and to a flat glass in-line coating system comprising such an apparatus.
  • the invention further pertains to a method for measuring optical properties of a flat glass product provided with an optical coating system which is protected by a final protective, e.g., scratch-resistant film.
  • optical coatings like antireflective, solar control, low-emissivity, decorative (e.g., colour) or functional coatings.
  • optical measurements transmission, reflection, colour, etc.
  • DLC film is used in the sense of any DLC (diamond like carbon) coating known from the state of the art. This may comprise hydrogen rich (DLCH) or hydrogen poor DLC films, as well as pure carbon films, or films comprising other elements such as a-C:H- or MeC:H films and the like.
  • an apparatus for removing a protective film from a coated flat glass product extending in a longitudinal direction x and a lateral direction y and for measuring optical properties of the glass product (and/or a remaining optical coating after plasma treatment) comprises: a glass support, such as a roller table, defining a basic plane B at which the glass product is supported; - at least one plasma source, in particular a plasma-jet source, movable relative to the glass product, in particular in the lateral direction y and optionally also in the longitudinal direction x and/or a vertical direction z, in particular movable parallel to the basic plane B, the at least one plasma(-jet) source having a plasma outlet aperture adjustable in a first distance di above a surface plane S, the surface plane S being substantially parallel and at a thickness distance t of the glass product above the basic plane B in which the glass product is supported;
  • the glass product may be a float glass with a thickness in a range from 3 to 19 mm, or could even be a thin or ultra-thin glass product with a thickness in a range from 0.2 to 3 mm or from 0.01 to 0.2 mm, respectively.
  • flat "glass-like" products for instance based on a transparent plastic substrate, also fall within the scope of the present invention.
  • the thickness distance t hereby equals substantially the thickness of the coated glass product and surfaces of the flat glass product will in many cases be parallel to each other.
  • certain flat glass products may comprise steps, areas of diminished or increased thickness t or comprise areas of decreasing/increasing thickness, for instance from the coordinates yi to y2, which may be coordinates y a to y z defining the glass product's boundaries (sides) in the lateral y direction.
  • Flat glass products according to the present invention will in this sense also encompass glass products with respectively varying thickness and/or bow and/or warpage.
  • the plasma source(s) and the glass product can be moved relative to each another. This is also true for the optical spectrometer(s) and the glass product. Movements of the plasma source(s) and optical spectrometer(s) relative to the glass product may for instance be achieved by either moving the plasma source(s) and optical spectrometer(s), e.g., be means for an appropriate transport mechanism onto which the plasma source(s) and optical spectrometer(s) are mounted, and/or by moving the glass product, e.g., by means of one or more roller tables, which for instance can themselves be moved in order to change the direction in which the glass product is moved.
  • moving the plasma source(s) and optical spectrometer(s) e.g., be means for an appropriate transport mechanism onto which the plasma source(s) and optical spectrometer(s) are mounted
  • moving the glass product e.g., by means of one or more roller tables, which for instance can themselves be moved in order to change the direction in which the glass product is moved.
  • the plasma source(s) and together with them the optical spectrometer(s) may be moved along and/or across, e.g., diagonally over, the glass product in any desired manner. Accordingly, it is for instance possible to mount the plasma source(s) and optical spectrometer(s) at (a) fixed location(s) and move the glass product about this/these location(s) in order to treat by the plasma a certain desired area of the glass product and subsequently measure the optical properties of the glass product in this treated area.
  • both the glass product as well as the plasma source(s) and optical spectrometer(s) may be moved in order to treat by the plasma a certain desired area of the glass product and subsequently measure the optical properties of the glass product in this treated area.
  • all these various options are collectively referred to (especially in the claims) by the expression that the at least one plasma source / optical spectrometer (or optical fibre connected to the optical spectrometer) is movable relative to the glass product.
  • the working direction is a direction during which the plasma source(s) are turned on and moved in a working distance di over the surface plane, e.g., when the plasma source(s) and spectrometer(s) are moved from a start position, e.g., near or at y a , to an end position, e.g., near or at y z .
  • the plasma source(s) and spectrometer(s) are moved back from an end to a start position, the plasma source(s) can be turned off and/or lifted away from the surface plane S in a greater vertical distance.
  • the working distance d2 above the surface plane of the spectrometer(s) can be equal to or different from the working distance di above the surface plane of the plasma source(s).
  • the optical spectrometer(s) can be a single or multichannel spectrometer comprising one or several gauge/measurement heads.
  • the optical spectrometer(s) cover the wavelength range of interest, in particular the visible and near-infrared (NIR) range, e.g., from 330 to 2100 nm.
  • the measurement can include one or multiple measurement points at the glass plane.
  • one or more measurement heads can be fixedly arranged above the glass panel which is then moved, or the one or more measurement heads are moved across the glass panel to the desired measurement positions.
  • the optical spectrometer(s) can be fixedly mounted and measurements can be conducted via optical fibre(s) connected to the optical spectrometer(s), whereby the optical fibre(s) are moved across the glass panel to the desired measurement position(s) or measurements are collected from a plurality of fixed fibre positions by means of multiplexing.
  • optical spectrometer(s) or in addition thereto, single wavelength or broadband photodiodes/detectors may be employed.
  • optical spectroscopy measurements can for instance be performed: transmission (T), reflection from the coated side (Rc), reflection from the glass side (Rg), or in case of a double-sided coating (i.e., on both sides of the glass panel), transmission (T), reflection from the first/front coated side (Rci), reflection from the second/rear coated side (RC2).
  • T transmission
  • T reflection from the coated side
  • Rg glass side
  • RC2 reflection from the second/rear coated side
  • Each of the optical measurements can be performed under multiple angles and/or polarizations. It is advantageous to perform multiple optical measurements at various angles and/or polarizations, i.e., at two or more angles and/or polarizations.
  • Additional measurement heads for measurement of glass thickness and/or electrical sheet resistance of the coating can be used.
  • the distance from the measurement head to the glass panel during measurement may be in a range from 1 to 30 mm.
  • the optical spectroscopy measurement should not take longer than one minute per measurement position, preferably not longer than 30 seconds per measurement position. It is of advantage for the quality control of architectural glass coatings to perform measurement at multiple measurement points (i.e., at several different x, y coordinates) across the glass panel.
  • the location of the measurement points is chosen such as to characterize a coating distribution 1) across the width of the glass in one line, i.e., x held constant, y variable, or 2) across the length of the glass in one line, i.e., x variable, y held constant, or 3) in a mixed way, both x and y variable, e.g., diagonally along and across the glass panel.
  • the optical measurement can be performed simultaneously with the plasma treatment downstream thereof (i.e., position shifted) or after plasma treatment (i.e., time-shifted/delayed).
  • the optical spectrometer(s) can also be used to determine the effectiveness of removing by means of the plasma(-jet) source(s) the protective (scratch-resistant DLC) film on top of the glass product by measuring the properties of the remaining top protective coating.
  • the apparatus according to the invention may comprise two or more plasma(-jet) sources arranged along the lateral direction y laterally offset to one another such that plasma cones in a sideview overlap only partially in the surface plane S.
  • the plasma(-jet) source(s) may comprise a grounded housing forming a plasma chamber.
  • the housing is connectable to a gas supply and has a nozzle with a plasma channel ending with a plasma outlet aperture.
  • the essentially closed housing can form a plasma chamber to ignite and maintain the plasma to supply the plasma(-jet) and can comprise an electrically isolated electrode in the plasma chamber, the electrode being connectable to a high voltage supply of alternating current.
  • the nozzle can be rotatable around a central nozzle axis R and the plasma outlet aperture can be eccentric relative to the central nozzle axis R, where R usually corresponds to an axis Z vertical/perpendicular to the basic plane B.
  • the aperture can be provided with its outer diameter r I still comprising the centre of the nozzle defined by the central nozzle axis R, or preferably just touching the central nozzle axis R, or completely outside the central region of the nozzle.
  • the plasma cone can produce a disc, ring or ring-like surface treated area when it rotates without linear movement of the plasma source.
  • the diameter of the nozzle r can, as an example, be chosen in a range from 15 to 30 mm, the diameter r I of the plasma outlet aperture can be in a range from 5 to 15 mm.
  • the actual diameter r of the nozzle and the plasma outlet aperture r I , respectively, as used with the examples mentioned below were about 20 mm and about 9 mm, respectively.
  • the plasma channel can be funnel- shaped with the smaller diameter ending with the plasma outlet aperture.
  • the larger diameter end of the funnel may encompass symmetrically the axis R. Due to that the axis F of the funnel is slanted with respect to the axis R, comprising a radial direction away from the axis R and a vertical direction z towards the surface of the glass product to be treated which also defines the direction of the plasma torch. Thereby, a ring-like surface treated area is produced when the plasma torch rotates without linear movement of the plasma source and overheating in a central area can be avoided.
  • the electrode of the plasma(-jet) source may comprise a free end piece directed towards the centre of the plasma channel.
  • the end piece can be cone or truncated cone shaped with the narrower end directed towards the plasma channel.
  • the apparatus may comprise means to control the working distance automatically at a distance di above the surface plane.
  • the means to control the working distance di together with d2 may comprise a vertical drive effectively connected to the at least one plasma-jet source and a distance meter, e.g., a laser distance meter, effectively connected to an electronic control circuit to control the vertical drive.
  • Protective films to be removed or etched away can be, as an example, carbon containing films, e.g., a diamond like carbon (DLC) film which may contain hydrogen or may be essentially free of hydrogen.
  • DLC diamond like carbon
  • the invention further pertains to a flat glass in-line coating system comprising a series of consecutive vacuum processing or coating chambers succeeded by an apparatus as specified above, wherein one of the last vacuum coating chambers, in particular the last vacuum coating chamber, in a downstream direction is adapted to deposit a carbon containing film, e.g., a diamond like carbon (DLC) film, and comprises at least one gas inlet and a vacuum-plasma source, the last vacuum coating chamber in particular being operatively connected via a vacuum to vacuum port or lock to a preceding vacuum coating chamber and via a vacuum to atmosphere lock to the succeeding apparatus for removing the carbon containing (e.g., DLC) coating/film and for measuring the optical properties of the glass product of the coating/film as described above.
  • a carbon containing film e.g., a diamond like carbon (DLC) film
  • a vacuum to atmosphere lock is a vacuum tight feedthrough to transfer a flat glass product from vacuum to atmosphere, the same applies to a vacuum to vacuum lock for the transfer from one vacuum, chamber to the next chamber, e.g. deposition chambers, whereas the term vacuum port refers to feedthroughs from one vacuum chamber to the next which need not be vacuum tight but may provide means to avoid free exchange of process gases between respectively linked chambers.
  • Vacuum chambers can be equipped beneficially with a separate vacuum pump for each chamber.
  • the vacuum-plasma source may comprise at least one plasma source chamber having an inductively coupled plasma (ICP) electrode and at least one plasma window in parallel to a substrate plane to couple a plasma inductively into a process compartment of the last vacuum coating chamber.
  • ICP inductively coupled plasma
  • the preceding vacuum coating chamber of the inventive coating system can be a sputter chamber comprising at least one transition metal (TM) and/or silver (containing) target and at least one gas inlet for inert gas and a carbon containing gas.
  • TM transition metal
  • containing silver
  • the preceding vacuum coating chamber can be further coupled to a last vacuum coating chamber of a number of operatively connected vacuum coating chambers all together adapted to form an antireflective, solar coating, low-emissivity, decorative or functional coating system, wherein the system comprises at least one vacuum coating chamber adapted to deposit a dielectric coating, e.g., via sputtering of a dielectric or a metal target in an oxygen containing atmosphere, further at least one coating chamber to deposit a silver or a silver containing coating, e.g., via sputtering of a silver target in an inert gas atmosphere, and optionally one or more further coating chambers adapted to deposit at least one further functional layer, e.g., a metallic or nitride containing adsorption layer or an adhesion layer to provide adhesion of the layer system on the glass substrate or provide adhesion of the silver layer within the coating system, e.g., on a preceding dielectric layer.
  • a dielectric coating e.g.
  • each vacuum coating chamber is equipped with a separate vacuum pump and each coating chamber is equipped with a respective sputter target and an electric sputter supply, an inert sputter gas supply, and optionally with a reactive gas supply in case of coating chambers for the deposition of carbon, nitrogen or oxygen containing coatings, as for the deposition of dielectric, transition metal or certain oxygen or nitrogen containing adhesion or barrier or anti-reflective layers.
  • the invention furthermore pertains to a method for measuring optical properties of a flat glass product extending in a longitudinal direction x and a lateral direction y provided with an optical coating system which is protected by a final protective film, adapted to protect the coating system during transportation, handling and final production steps like trimming, creating phases, framing and the like.
  • the method comprises the following steps:
  • the method may further comprise providing an oxygen containing gas at a pressure in a range from 1 to 200 bar, in particular in a range from 1.5 to 10 bar, e.g., compressed air, to the plasma(-jet) source from a connected gas supply.
  • An electrode of the plasma(-jet) source can be driven with alternating current, at a frequency in a range from 18 to 25 kHz, at a power in a range from 400 to 800 W and an operating voltage in a range from 1.5 to 2.5 kV.
  • an ignition voltage of 20 ⁇ 5 kV can be used to ignite the plasma.
  • a working distance di between the outlet aperture and the surface of the glass product can be set to a distance in a range from 1 to 30 mm and can be held constant by means for controlling a pre-set distance, preferably automatically.
  • a transverse speed in a range from 0.5 to 300 m/minute, in particular in a range from 3 to 24 m/minute, can be set between the surface of the glass product and the plasma-jet source and the following optical spectrometer to etch the protective film away without harm of the underlaying solar control coating.
  • the outlet aperture can be rotated eccentrically round an axis R of a rotating nozzle, the latter comprising a plasma channel ending in the outlet aperture, whereby a speed in a range from 1'500 to 3'000 revolutions per minute (rpm) can be set.
  • the protective film to be removed or etched away can be a carbon containing film, e.g., a diamond like carbon (DLC) film which may contain hydrogen or may be essentially free of hydrogen.
  • DLC diamond like carbon
  • the etching rate to be achieved is defined through the width of the glass pane, production speed and distance between glasses and the thickness of the protection layer. Therefore, multiple jets can be mounted to achieve the required etching rates in a range from 30 to 300 nm-m/min. for DLC-coatings, e.g., DLCH coatings, whereat the underlaying TM-inclusive layer can be partially or fully oxidized at least at the surface and in a surface near region, but is substantially not etched away. Thereby, the hardness of the transition metal (TM)-inclusive layer can be increased to protect the underlaying (solar control) coating and at the same time the optical properties can be improved.
  • TM transition metal
  • DLC films in a range from 5 to 50 nm could be reliably removed in one run (20 to 30 s, depending on the actual width of the glass product and on the thickness of the protective layer) and optical measurements performed at the same time over a treated flat glass product width in a range from 0.4 to 3.3 m in lateral direction (variable y coordinate) or diagonally along and across (variable x and y coordinates) the glass panel of up to 12 m in length.
  • Fig. 1 a schematic side view of an inventive apparatus
  • Fig. 2 detail A from Fig. 1;
  • Fig. 3 a schematic top view of an inventive apparatus
  • Fig. 4 detail B from Fig. 3;
  • Fig. 5 details of the function of the plasma-jet sources
  • Fig. 6 a schematic side view of a plasma-jet source
  • Fig. 7 a schematic top view of an inventive in-line coating system
  • Fig. 8 a a schematic perspective view of an inventive in-line coating system with the plasma-jet source(s) and the optical spectrometer(s) being moved laterally across the glass panel;
  • Fig. 8 b a schematic perspective view of the inventive in-line coating system with the plasma-jet source(s) and the optical spectrometer(s) being moved diagonally across and along the glass panel;
  • Fig. 9 a schematic cross-sectional view of a coating system before and after plasma-jet treatment.
  • Fig. 1 shows an exemplary embodiment of an inventive apparatus 1 in a schematic side view.
  • Fig. 2 shows detail A from Fig. 1 referring to the positioning of the plasma-jet source 2, respectively the tip of the nozzle 8 towards the glass product 25.
  • the apparatus 1 comprises a horizontal glass support, here a roller table 22 comprising respective rollers 23 to move the flat glass product 25 in a longitudinal direction x into processing position with reference to the plasma-jet sources 2 and the optical spectrometer 16 (cf. Fig. 3).
  • Plasma-jet sources 2 and the optical spectrometer(s) 16 are mounted together on a carriage 28 (cf. Fig. 7) which is mounted movably in a vertical direction z to a vertical linear guide 19 to set distances di and d2 between the plasma outlet aperture 10 of the nozzles 8 and the surface plane S of the glass product 25 and between the gauge heads (not shown) of the optical spectrometer 16 and the surface plane S, respectively, where the surface plane S is located a thickness distance t above and essentially parallel to the basic plane B given by the support area of the glass support 22.
  • the thickness distance t may vary due to different glass types to be (de-)coated or due to minor geometric surface variations of the flat glass product 25.
  • a laser distance meter 41 which is also mounted on the vertical linear guide 19, can be used to set/adjust the distance di automatically.
  • the distance d2 of the optical spectrometer 16 to the surface plane S is defined, which can be the same or different to di.
  • the vertical linear guide 19 itself is mounted movably in a lateral direction y to a horizontal linear guide 18.
  • the horizontal linear guide 18 therewith moves the plasma-jet sources 2 and optical spectrometer 16 synchronously and staggered, i.e., one after the other as shown in Fig. 3 and Fig.
  • the horizontal linear guide 18 extending in a lateral direction y is mounted together with the vertical linear guide 19, which carries the de-coating/measuring ensemble 2, 16, 41 is mounted to a portal carrier or forms the crossbar of a portal carrier.
  • the portal carrier, the horizontal linear guide 18, and the vertical linear guide 19 thereby form the carrier ensemble 17.
  • horizontal movement in the lateral direction y and up-/downward movement in the vertical direction z can be performed by drives (not shown) being operatively connected to the vertical linear guide 19 and the carriage 28, and being controllable by at least one electronic control circuit, e.g., by a pre-programmed lateral speed v y and repetition frequency or a bounce signal from the laser distance meter 41 or a separate presence sensor (not shown) for the glass product 25.
  • the signal from the laser distance meter can be fed to and processed by the control circuit to hold the working distance di constant over the width of the glass product 25.
  • Such a control circuit can be foreseen separate with apparatus 1 or integrated into a central processing unit (CPU) of the in-line coating system 30 which can be manually programmed via a control unit 42 (cf. Fig. 7).
  • Drives can be designed as belt or spindle drives, for example a belt drive for the horizontal movement and a spindle drive for the vertical movement.
  • a nozzle 8 of the plasma-jet source 2 is shown.
  • the nozzle 8 is rotatable at high speed around the axis R and has a funnel like plasma channel 9 which ends in a plasma outlet aperture 10 eccentric to the central and rotational nozzle axis R. Due to the plasma channel being slanted away from the axis R in a flow direction and the centripetal force due to the high rotational speed a static plasma track 14 as shown in Fig. 5 can be produced by the leaving plasma flame, e.g., at distance di to the surface B of the glass product 25. Due to the staggered arrangement of the plasma-jet sources 8 with an offset s in longitudinal direction x as shown in Fig.
  • a plasma treated area 15 can be produced when the source ensemble is moved in working distance di over the surface B of the glass product 25.
  • the optical spectrometer 16 is mounted to follow in line behind the source ensemble and measure as mentioned parameters of the optical coating.
  • each plasma-jet source 8 is provided by a separate power and gas line and is controlled by a separate controller under a central process control.
  • power and gas lines as well as separate control lines can be foreseen in a cable trailing fashion as known to those skilled in the art.
  • the plasma-jet source 2 consists of a rotating, cylindrical nozzle 8 into which a process gas is fed into through the gas inlet 5.
  • An electric current is fed through the current feedthrough 4 to the electrode 6 with an end piece 7.
  • the electric potential difference between the housing 3 and the electrode 6 with the end piece 7 which are insulated from the housing by an insulator 11, leads to a plasma discharge 12.
  • the plasma-jet exits the funnel-shaped nozzle 8 through a plasma channel 9 with a plasma outlet aperture 10 and hits the coated glass product 25 at a distance in the range from 5 to 15 mm.
  • Fig. 7 schematically illustrates a top view of an inventive in-line coating system 26 for producing coated flat glass products 25.
  • the flat glass pane/substrate 24 is conveyed by a transport system 29 (e.g., comprising rollers 23) through a system of consecutive vacuum chambers 31-37 (and optionally 27), whereby in the last coating chamber 37 a carbon containing film, such as a diamond like carbon (DLC) film is deposited to make the coated flat glass product 25 scratch-resistant (especially for later handling).
  • a transport system 29 e.g., comprising rollers 23
  • a carbon containing film such as a diamond like carbon (DLC) film
  • the coating, such as a solar control coating, of the flat glass product 25 must be checked, i.e., its properties must be measured in order to verify whether the in-line coating process was performing as desired, and to adjust the process parameters if necessary for subsequent coating.
  • the scratch-resistant carbon containing film must be removed as described above by means of plasma-jet processing (etching), in order to provide direct access to the underlying (e.g., solar control) coating for subsequent measurements with the optical spectrometer(s) 16.
  • Fig. 8 a) & b) show in a schematic perspective view an in-line coating system 26 with rollers 23 for transporting the flat glass substrate 24 into the in-line coating system 26 comprising multiple vacuum processing/coating chambers, out of which come coated glass products 25 with a protective, e.g., scratch-resistant top layer.
  • the plasma-jet source 2 operated at ambient environment is moved laterally (i.e., in y direction) across the glass panel 25 while exiting the in-line coating system 26.
  • the rollers 23 do not move the glass panel 25 while the plasma-jet source 2 laterally traverses the glass panel 25 to remove the protective top layer at the plasma-treated area A.
  • the optical properties of the glass panel 25 are measured by the optical spectrometer 16, which is mounted on the same carrier and moved together with the plasma-jet source 2, but arranged in a set back position relative to the plasma-jet source 2.
  • the optical properties of the preceding glass panel 25' can be measured ex-situ by the optical spectrometer 16' located downstream of the plasma-jet source 2 and mounted on a separate carrier, which is moved (simultaneously/synchronously with the plasma-jet source 2 operating on the succeeding glass panel 25) laterally (i.e., in y direction) across the glass panel 25' while the rollers do not move the glass panel 25'.
  • the optical spectrometer 16' located downstream of the plasma-jet source 2 and mounted on a separate carrier, which is moved (simultaneously/synchronously with the plasma-jet source 2 operating on the succeeding glass panel 25) laterally (i.e., in y direction) across the glass panel 25' while the rollers do not move the glass panel 25'.
  • the plasma-jet source 2 operated at ambient environment is moved diagonally (i.e., in x & y direction) along and across the glass panel 25 while exiting the in-line coating system 26.
  • the rollers 23 are moving forward the glass panel 25 in x direction while the plasma-jet source 2 laterally traverses the glass panel 25 and at the same time moved along with the glass panel 25, which is also moving forward in the x direction, thereby removing the protective top layer at the plasma-treated area A limited across the forward end of the glass panel 25.
  • the optical properties of the glass panel 25 are measured by the optical spectrometer 16, which is mounted on the same carrier and moved together with the plasma-jet source 2, but arranged in a set back position relative to plasma-jet source 2.
  • the optical properties of the preceding glass panel 25' where the protective top layer has already been removed at the plasma-treated area A limited across the forward end of the glass panel 25', can be measured ex-situ by the optical spectrometer 16' located downstream of the plasma-jet source 2 and mounted on a separate carrier, which is also moved (simultaneously/synchronously with the plasma-jet source 2 operating on the succeeding glass panel 25) diagonally (i.e., in x & y direction) along and across the glass panel 25' while the rollers 23 are moving the glass panel 25' forward in the x direction.
  • a total of four optical spectrometers 16 in a typical measurement setup.
  • sheet resistance should be measured in the range from 10 mQ to 100 Q for instance based on Eddie currents.
  • Fig. 9 shows on the left side a coated flat glass product 25 (as disclosed in WO2020164735A1), where a substrate S is coated with a solar control coating 40 coated which is topped by a transition metal (TM), carbon and oxygen containing layer 36', and an immediately consecutive DLCH layer 37', both increasing the scratch resistance of the solar coating.
  • TM transition metal
  • the latter is implemented in a configuration comprising two reflective silver layers 32', 34' sandwiched by three dielectric layers 31', 33', 35'.
  • a respective plasma treated glass product 25 can be seen on the right side of Fig. 9, a respective plasma treated glass product 25 can be seen. Due to the oxygen plasma flame expanding with high speed into atmosphere through the plasma aperture the DLC layer and the carbon content is burnt or etched away at least at and near the surface of the now treated TM layer 39. Thereby optical properties and hardness of the TM layer 39 are enhanced.

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Abstract

The present invention provides an apparatus (1) for removing a protective film from a coated flat glass product (25) extending in a longitudinal direction (x) and a lateral direction and subsequently measuring optical properties of the glass product (25). The apparatus (1) comprises a glass support (22) defining a basic plane at which the glass product (25) is supported; at least one plasma source (2) movable relative to the glass product (25) in at least one of the lateral direction, the longitudinal direction (x) and a vertical direction (z), in particular movable parallel to the basic plane, the at least one plasma source (2) having a plasma outlet aperture adjustable in a working distance above a surface plane, the surface plane being substantially parallel and at a thickness distance above the basic plane in which the glass product (25) is supported; at least one optical spectrometer or at least one optical fibre connected to the at least one optical spectrometer movable relative to the glass product (25) in at least one of the lateral direction, the longitudinal direction (x) and the vertical direction (z) and adjustable at a distance above the surface plane together or synchronized with the at least one plasma source (2) and, with respect to a working direction, in line and set back to the at least one plasma source (2). Furthermore, the present invention includes a flat glass in-line coating system comprising such an apparatus (1) as well as a method for measuring optical properties of a flat glass product (25) provided with an optical coating system which is protected by a final protective film.

Description

APPARATUS FOR REMOVING A PROTECTIVE FILM FROM AND MEASURING OPTICAL PROPERTIES OF A COATED FLAT GLASS PRODUCT
The present invention relates to an apparatus for removing a protective film from a coated flat glass product and subsequently measuring optical properties of the glass product and to a flat glass in-line coating system comprising such an apparatus. The invention further pertains to a method for measuring optical properties of a flat glass product provided with an optical coating system which is protected by a final protective, e.g., scratch-resistant film.
DESCRIPTION OF THE RELATED ART
Established plasma-treatments for removing protective carbon or carbon containing films from flat glass products precoated with optical films for different purposes have certain disadvantages when it comes to removing such films quickly and only locally from a predefined surface area. Known plasma procedures act either on the whole surface of the flat glass product, are difficult to restrict to a certain target area and do not provide high etching. Such area-unspecific treatments are typically used for the pre-cleaning conditioning of glass substrates prior to further processing like coating, printing, laminating and so forth. A CO2 laser is typically applied for the removal of a temporary organic protecting layer from a specific area. However, operating such a laser is associated with high expenses, multiple runs for broader areas and requires safety measures.
SUMMARY OF THE INVENTION
It is an object of the present invention to avoid the disadvantages of the state of the art and to provide an apparatus as well as a method for removing a protective film from a coated flat glass product in a fast and reliable manner within a locally delimited area and without the risk of negatively influencing the properties of underlaying optical coatings, like antireflective, solar control, low-emissivity, decorative (e.g., colour) or functional coatings.
It is a further object of the present invention to provide an apparatus as well as a method to allow in parallel, i.e., at the same time, to perform optical measurements (transmission, reflection, colour, etc.) in the locally delimited area after the protective top layer has been removed. Thereby, it is also desirable to additionally perform measurements of physical properties, such as electrical sheet resistance or hardness, and/or of chemical properties.
It is a further object of the present invention to provide an apparatus as well as a method which allows respective locally delimited film removal and measurement over the full width of a flat glass product and can be integrated at the end of an in-line coating system in a single film removal and measuring apparatus or station.
Definition: In the following the term DLC film is used in the sense of any DLC (diamond like carbon) coating known from the state of the art. This may comprise hydrogen rich (DLCH) or hydrogen poor DLC films, as well as pure carbon films, or films comprising other elements such as a-C:H- or MeC:H films and the like.
According to the present invention an apparatus for removing a protective film from a coated flat glass product extending in a longitudinal direction x and a lateral direction y and for measuring optical properties of the glass product (and/or a remaining optical coating after plasma treatment) comprises: a glass support, such as a roller table, defining a basic plane B at which the glass product is supported; - at least one plasma source, in particular a plasma-jet source, movable relative to the glass product, in particular in the lateral direction y and optionally also in the longitudinal direction x and/or a vertical direction z, in particular movable parallel to the basic plane B, the at least one plasma(-jet) source having a plasma outlet aperture adjustable in a first distance di above a surface plane S, the surface plane S being substantially parallel and at a thickness distance t of the glass product above the basic plane B in which the glass product is supported;
- at least one optical spectrometer or at least one optical fibre connected to the at least one optical spectrometer movable relative to the glass product, in particular in the lateral direction y and optionally also in the longitudinal direction x and/or the vertical direction z, and adjustable at a second distance d2 above the surface plane S together or synchronized with the at least one plasma(-jet) source and, with respect to a working direction, in line and set back to (or alternatively downstream of) the at least one plasma(-jet) source.
The glass product may be a float glass with a thickness in a range from 3 to 19 mm, or could even be a thin or ultra-thin glass product with a thickness in a range from 0.2 to 3 mm or from 0.01 to 0.2 mm, respectively. Furthermore, flat "glass-like" products, for instance based on a transparent plastic substrate, also fall within the scope of the present invention.
The thickness distance t hereby equals substantially the thickness of the coated glass product and surfaces of the flat glass product will in many cases be parallel to each other. However, with reference to the term substantially parallel, it should be expressed that certain flat glass products may comprise steps, areas of diminished or increased thickness t or comprise areas of decreasing/increasing thickness, for instance from the coordinates yi to y2, which may be coordinates ya to yz defining the glass product's boundaries (sides) in the lateral y direction. Flat glass products according to the present invention will in this sense also encompass glass products with respectively varying thickness and/or bow and/or warpage.
The plasma source(s) and the glass product can be moved relative to each another. This is also true for the optical spectrometer(s) and the glass product. Movements of the plasma source(s) and optical spectrometer(s) relative to the glass product may for instance be achieved by either moving the plasma source(s) and optical spectrometer(s), e.g., be means for an appropriate transport mechanism onto which the plasma source(s) and optical spectrometer(s) are mounted, and/or by moving the glass product, e.g., by means of one or more roller tables, which for instance can themselves be moved in order to change the direction in which the glass product is moved. In this way the plasma source(s) and together with them the optical spectrometer(s) may be moved along and/or across, e.g., diagonally over, the glass product in any desired manner. Accordingly, it is for instance possible to mount the plasma source(s) and optical spectrometer(s) at (a) fixed location(s) and move the glass product about this/these location(s) in order to treat by the plasma a certain desired area of the glass product and subsequently measure the optical properties of the glass product in this treated area. Conversely, it is also possible not to move the glass product whilst the plasma source(s) and optical spectrometer(s) are moved over the glass product in order to treat by the plasma a certain desired area of the glass product and subsequently measure the optical properties of the glass product in this treated area. Alternatively, both the glass product as well as the plasma source(s) and optical spectrometer(s) may be moved in order to treat by the plasma a certain desired area of the glass product and subsequently measure the optical properties of the glass product in this treated area. For reasons of conciseness, all these various options are collectively referred to (especially in the claims) by the expression that the at least one plasma source / optical spectrometer (or optical fibre connected to the optical spectrometer) is movable relative to the glass product. The working direction is a direction during which the plasma source(s) are turned on and moved in a working distance di over the surface plane, e.g., when the plasma source(s) and spectrometer(s) are moved from a start position, e.g., near or at ya, to an end position, e.g., near or at yz. When the plasma source(s) and spectrometer(s) are moved back from an end to a start position, the plasma source(s) can be turned off and/or lifted away from the surface plane S in a greater vertical distance. The working distance d2 above the surface plane of the spectrometer(s) can be equal to or different from the working distance di above the surface plane of the plasma source(s).
The optical spectrometer(s) can be a single or multichannel spectrometer comprising one or several gauge/measurement heads. The optical spectrometer(s) cover the wavelength range of interest, in particular the visible and near-infrared (NIR) range, e.g., from 330 to 2100 nm. The measurement can include one or multiple measurement points at the glass plane. To perform measurements at the desired positions at the glass panel/ pane, one or more measurement heads can be fixedly arranged above the glass panel which is then moved, or the one or more measurement heads are moved across the glass panel to the desired measurement positions. Alternatively, the optical spectrometer(s) can be fixedly mounted and measurements can be conducted via optical fibre(s) connected to the optical spectrometer(s), whereby the optical fibre(s) are moved across the glass panel to the desired measurement position(s) or measurements are collected from a plurality of fixed fibre positions by means of multiplexing. Instead of optical spectrometer(s) or in addition thereto, single wavelength or broadband photodiodes/detectors may be employed.
The following optical spectroscopy measurements can for instance be performed: transmission (T), reflection from the coated side (Rc), reflection from the glass side (Rg), or in case of a double-sided coating (i.e., on both sides of the glass panel), transmission (T), reflection from the first/front coated side (Rci), reflection from the second/rear coated side (RC2). Each of the optical measurements can be performed under multiple angles and/or polarizations. It is advantageous to perform multiple optical measurements at various angles and/or polarizations, i.e., at two or more angles and/or polarizations. Additional measurement heads for measurement of glass thickness and/or electrical sheet resistance of the coating can be used. The distance from the measurement head to the glass panel during measurement may be in a range from 1 to 30 mm. Depending on the number of desired measurement positions at the glass panel, the optical spectroscopy measurement should not take longer than one minute per measurement position, preferably not longer than 30 seconds per measurement position. It is of advantage for the quality control of architectural glass coatings to perform measurement at multiple measurement points (i.e., at several different x, y coordinates) across the glass panel. The location of the measurement points is chosen such as to characterize a coating distribution 1) across the width of the glass in one line, i.e., x held constant, y variable, or 2) across the length of the glass in one line, i.e., x variable, y held constant, or 3) in a mixed way, both x and y variable, e.g., diagonally along and across the glass panel. The optical measurement can be performed simultaneously with the plasma treatment downstream thereof (i.e., position shifted) or after plasma treatment (i.e., time-shifted/delayed).
As indicated above (in parentheses), apart from measuring optical properties of the glass product, the optical spectrometer(s) can also be used to determine the effectiveness of removing by means of the plasma(-jet) source(s) the protective (scratch-resistant DLC) film on top of the glass product by measuring the properties of the remaining top protective coating. The apparatus according to the invention may comprise two or more plasma(-jet) sources arranged along the lateral direction y laterally offset to one another such that plasma cones in a sideview overlap only partially in the surface plane S.
The plasma(-jet) source(s) may comprise a grounded housing forming a plasma chamber. The housing is connectable to a gas supply and has a nozzle with a plasma channel ending with a plasma outlet aperture. The essentially closed housing can form a plasma chamber to ignite and maintain the plasma to supply the plasma(-jet) and can comprise an electrically isolated electrode in the plasma chamber, the electrode being connectable to a high voltage supply of alternating current.
The nozzle can be rotatable around a central nozzle axis R and the plasma outlet aperture can be eccentric relative to the central nozzle axis R, where R usually corresponds to an axis Z vertical/perpendicular to the basic plane B. Thereby, the aperture can be provided with its outer diameter rI still comprising the centre of the nozzle defined by the central nozzle axis R, or preferably just touching the central nozzle axis R, or completely outside the central region of the nozzle. Thereby, the plasma cone can produce a disc, ring or ring-like surface treated area when it rotates without linear movement of the plasma source. The diameter of the nozzle r can, as an example, be chosen in a range from 15 to 30 mm, the diameter rI of the plasma outlet aperture can be in a range from 5 to 15 mm. The actual diameter r of the nozzle and the plasma outlet aperture rI, respectively, as used with the examples mentioned below were about 20 mm and about 9 mm, respectively.
In a further embodiment of the present invention the plasma channel can be funnel- shaped with the smaller diameter ending with the plasma outlet aperture. Thereby, in a preferred embodiment, the larger diameter end of the funnel may encompass symmetrically the axis R. Due to that the axis F of the funnel is slanted with respect to the axis R, comprising a radial direction away from the axis R and a vertical direction z towards the surface of the glass product to be treated which also defines the direction of the plasma torch. Thereby, a ring-like surface treated area is produced when the plasma torch rotates without linear movement of the plasma source and overheating in a central area can be avoided.
The electrode of the plasma(-jet) source may comprise a free end piece directed towards the centre of the plasma channel. The end piece can be cone or truncated cone shaped with the narrower end directed towards the plasma channel.
The apparatus may comprise means to control the working distance automatically at a distance di above the surface plane. The means to control the working distance di together with d2 may comprise a vertical drive effectively connected to the at least one plasma-jet source and a distance meter, e.g., a laser distance meter, effectively connected to an electronic control circuit to control the vertical drive.
Protective films to be removed or etched away can be, as an example, carbon containing films, e.g., a diamond like carbon (DLC) film which may contain hydrogen or may be essentially free of hydrogen.
The invention further pertains to a flat glass in-line coating system comprising a series of consecutive vacuum processing or coating chambers succeeded by an apparatus as specified above, wherein one of the last vacuum coating chambers, in particular the last vacuum coating chamber, in a downstream direction is adapted to deposit a carbon containing film, e.g., a diamond like carbon (DLC) film, and comprises at least one gas inlet and a vacuum-plasma source, the last vacuum coating chamber in particular being operatively connected via a vacuum to vacuum port or lock to a preceding vacuum coating chamber and via a vacuum to atmosphere lock to the succeeding apparatus for removing the carbon containing (e.g., DLC) coating/film and for measuring the optical properties of the glass product of the coating/film as described above. A vacuum to atmosphere lock is a vacuum tight feedthrough to transfer a flat glass product from vacuum to atmosphere, the same applies to a vacuum to vacuum lock for the transfer from one vacuum, chamber to the next chamber, e.g. deposition chambers, whereas the term vacuum port refers to feedthroughs from one vacuum chamber to the next which need not be vacuum tight but may provide means to avoid free exchange of process gases between respectively linked chambers. Vacuum chambers can be equipped beneficially with a separate vacuum pump for each chamber.
In an embodiment of the in-line coating system the vacuum-plasma source may comprise at least one plasma source chamber having an inductively coupled plasma (ICP) electrode and at least one plasma window in parallel to a substrate plane to couple a plasma inductively into a process compartment of the last vacuum coating chamber.
The preceding vacuum coating chamber of the inventive coating system can be a sputter chamber comprising at least one transition metal (TM) and/or silver (containing) target and at least one gas inlet for inert gas and a carbon containing gas.
The preceding vacuum coating chamber can be further coupled to a last vacuum coating chamber of a number of operatively connected vacuum coating chambers all together adapted to form an antireflective, solar coating, low-emissivity, decorative or functional coating system, wherein the system comprises at least one vacuum coating chamber adapted to deposit a dielectric coating, e.g., via sputtering of a dielectric or a metal target in an oxygen containing atmosphere, further at least one coating chamber to deposit a silver or a silver containing coating, e.g., via sputtering of a silver target in an inert gas atmosphere, and optionally one or more further coating chambers adapted to deposit at least one further functional layer, e.g., a metallic or nitride containing adsorption layer or an adhesion layer to provide adhesion of the layer system on the glass substrate or provide adhesion of the silver layer within the coating system, e.g., on a preceding dielectric layer.
In an embodiment of the system each vacuum coating chamber is equipped with a separate vacuum pump and each coating chamber is equipped with a respective sputter target and an electric sputter supply, an inert sputter gas supply, and optionally with a reactive gas supply in case of coating chambers for the deposition of carbon, nitrogen or oxygen containing coatings, as for the deposition of dielectric, transition metal or certain oxygen or nitrogen containing adhesion or barrier or anti-reflective layers.
The invention furthermore pertains to a method for measuring optical properties of a flat glass product extending in a longitudinal direction x and a lateral direction y provided with an optical coating system which is protected by a final protective film, adapted to protect the coating system during transportation, handling and final production steps like trimming, creating phases, framing and the like. The method comprises the following steps:
- removing the protective film linearly and in a defined width by moving at least one plasma outlet aperture of a plasma(-jet) source in a working distance di above a surface plane S in particular in the lateral direction y across an essential or the full width of the flat glass product to produce a protective film free linear section, and
- measuring at the same time or subsequently (e.g., offset in time / after a delay), but with reference to a working direction linearly offset behind and following the plasma(-jet) source in the lateral direction y, the optical properties of the coated glass product along the protective film free linear section with at least one optical spectrometer. The method may further comprise providing an oxygen containing gas at a pressure in a range from 1 to 200 bar, in particular in a range from 1.5 to 10 bar, e.g., compressed air, to the plasma(-jet) source from a connected gas supply.
An electrode of the plasma(-jet) source can be driven with alternating current, at a frequency in a range from 18 to 25 kHz, at a power in a range from 400 to 800 W and an operating voltage in a range from 1.5 to 2.5 kV. Usually, an ignition voltage of 20±5 kV can be used to ignite the plasma.
A working distance di between the outlet aperture and the surface of the glass product can be set to a distance in a range from 1 to 30 mm and can be held constant by means for controlling a pre-set distance, preferably automatically.
A transverse speed in a range from 0.5 to 300 m/minute, in particular in a range from 3 to 24 m/minute, can be set between the surface of the glass product and the plasma-jet source and the following optical spectrometer to etch the protective film away without harm of the underlaying solar control coating.
In an embodiment of the present invention the outlet aperture can be rotated eccentrically round an axis R of a rotating nozzle, the latter comprising a plasma channel ending in the outlet aperture, whereby a speed in a range from 1'500 to 3'000 revolutions per minute (rpm) can be set.
The protective film to be removed or etched away can be a carbon containing film, e.g., a diamond like carbon (DLC) film which may contain hydrogen or may be essentially free of hydrogen. Within the production line, the etching rate to be achieved is defined through the width of the glass pane, production speed and distance between glasses and the thickness of the protection layer. Therefore, multiple jets can be mounted to achieve the required etching rates in a range from 30 to 300 nm-m/min. for DLC-coatings, e.g., DLCH coatings, whereat the underlaying TM-inclusive layer can be partially or fully oxidized at least at the surface and in a surface near region, but is substantially not etched away. Thereby, the hardness of the transition metal (TM)-inclusive layer can be increased to protect the underlaying (solar control) coating and at the same time the optical properties can be improved.
When applying such parameters with an apparatus provided with five plasma-jet sources similar to the apparatus as discussed below, DLC films in a range from 5 to 50 nm could be reliably removed in one run (20 to 30 s, depending on the actual width of the glass product and on the thickness of the protective layer) and optical measurements performed at the same time over a treated flat glass product width in a range from 0.4 to 3.3 m in lateral direction (variable y coordinate) or diagonally along and across (variable x and y coordinates) the glass panel of up to 12 m in length.
BRIEF DESCRIPTION OF THE DRAWINGS
Embodiments of the present invention are described in more detail in the following with reference to the attached figures which show:
Fig. 1 a schematic side view of an inventive apparatus;
Fig. 2 detail A from Fig. 1;
Fig. 3 a schematic top view of an inventive apparatus;
Fig. 4 detail B from Fig. 3;
Fig. 5 details of the function of the plasma-jet sources;
Fig. 6 a schematic side view of a plasma-jet source; Fig. 7 a schematic top view of an inventive in-line coating system;
Fig. 8 a) a schematic perspective view of an inventive in-line coating system with the plasma-jet source(s) and the optical spectrometer(s) being moved laterally across the glass panel;
Fig. 8 b) a schematic perspective view of the inventive in-line coating system with the plasma-jet source(s) and the optical spectrometer(s) being moved diagonally across and along the glass panel;
Fig. 9 a schematic cross-sectional view of a coating system before and after plasma-jet treatment.
DETAILED DESCRIPTION OF THE FIGURES
Fig. 1 shows an exemplary embodiment of an inventive apparatus 1 in a schematic side view. Fig. 2 shows detail A from Fig. 1 referring to the positioning of the plasma-jet source 2, respectively the tip of the nozzle 8 towards the glass product 25.
The apparatus 1 comprises a horizontal glass support, here a roller table 22 comprising respective rollers 23 to move the flat glass product 25 in a longitudinal direction x into processing position with reference to the plasma-jet sources 2 and the optical spectrometer 16 (cf. Fig. 3).
Plasma-jet sources 2 and the optical spectrometer(s) 16 are mounted together on a carriage 28 (cf. Fig. 7) which is mounted movably in a vertical direction z to a vertical linear guide 19 to set distances di and d2 between the plasma outlet aperture 10 of the nozzles 8 and the surface plane S of the glass product 25 and between the gauge heads (not shown) of the optical spectrometer 16 and the surface plane S, respectively, where the surface plane S is located a thickness distance t above and essentially parallel to the basic plane B given by the support area of the glass support 22. The thickness distance t may vary due to different glass types to be (de-)coated or due to minor geometric surface variations of the flat glass product 25. A laser distance meter 41, which is also mounted on the vertical linear guide 19, can be used to set/adjust the distance di automatically. At the same time, the distance d2 of the optical spectrometer 16 to the surface plane S is defined, which can be the same or different to di. The vertical linear guide 19 itself is mounted movably in a lateral direction y to a horizontal linear guide 18. The horizontal linear guide 18 therewith moves the plasma-jet sources 2 and optical spectrometer 16 synchronously and staggered, i.e., one after the other as shown in Fig. 3 and Fig. 4, from a start position yi to an end position y2, which can be terminal positions ya and yz defining the lateral dimension y of the flat glass product 25 as shown in Fig. 3. Thereby, the optical quality can be measured over the full width of the flat glass product 25.
Finally, the horizontal linear guide 18 extending in a lateral direction y is mounted together with the vertical linear guide 19, which carries the de-coating/measuring ensemble 2, 16, 41 is mounted to a portal carrier or forms the crossbar of a portal carrier. The portal carrier, the horizontal linear guide 18, and the vertical linear guide 19 thereby form the carrier ensemble 17.
In any embodiment of the present invention horizontal movement in the lateral direction y and up-/downward movement in the vertical direction z can be performed by drives (not shown) being operatively connected to the vertical linear guide 19 and the carriage 28, and being controllable by at least one electronic control circuit, e.g., by a pre-programmed lateral speed vy and repetition frequency or a bounce signal from the laser distance meter 41 or a separate presence sensor (not shown) for the glass product 25. For the vertical movement the signal from the laser distance meter can be fed to and processed by the control circuit to hold the working distance di constant over the width of the glass product 25. Such a control circuit can be foreseen separate with apparatus 1 or integrated into a central processing unit (CPU) of the in-line coating system 30 which can be manually programmed via a control unit 42 (cf. Fig. 7). Drives can be designed as belt or spindle drives, for example a belt drive for the horizontal movement and a spindle drive for the vertical movement.
From detail A as shown in Fig. 2, the principle of a preferred design of a nozzle 8 of the plasma-jet source 2 is shown. The nozzle 8 is rotatable at high speed around the axis R and has a funnel like plasma channel 9 which ends in a plasma outlet aperture 10 eccentric to the central and rotational nozzle axis R. Due to the plasma channel being slanted away from the axis R in a flow direction and the centripetal force due to the high rotational speed a static plasma track 14 as shown in Fig. 5 can be produced by the leaving plasma flame, e.g., at distance di to the surface B of the glass product 25. Due to the staggered arrangement of the plasma-jet sources 8 with an offset s in longitudinal direction x as shown in Fig. 4, referring to detail B of Fig. 3, a plasma treated area 15 can be produced when the source ensemble is moved in working distance di over the surface B of the glass product 25. The optical spectrometer 16 is mounted to follow in line behind the source ensemble and measure as mentioned parameters of the optical coating.
An AC power supply 20 and a gas supply 21 to the plasma-jet sources 2 are shown only schematically in Fig. 3. Preferably each plasma-jet source 8 is provided by a separate power and gas line and is controlled by a separate controller under a central process control. Such power and gas lines as well as separate control lines can be foreseen in a cable trailing fashion as known to those skilled in the art.
As illustrated in Fig. 6, the plasma-jet source 2 consists of a rotating, cylindrical nozzle 8 into which a process gas is fed into through the gas inlet 5. An electric current is fed through the current feedthrough 4 to the electrode 6 with an end piece 7. The electric potential difference between the housing 3 and the electrode 6 with the end piece 7 , which are insulated from the housing by an insulator 11, leads to a plasma discharge 12. The plasma-jet exits the funnel-shaped nozzle 8 through a plasma channel 9 with a plasma outlet aperture 10 and hits the coated glass product 25 at a distance in the range from 5 to 15 mm.
Fig. 7 schematically illustrates a top view of an inventive in-line coating system 26 for producing coated flat glass products 25. In such an in-line coating system 26 the flat glass pane/substrate 24 is conveyed by a transport system 29 (e.g., comprising rollers 23) through a system of consecutive vacuum chambers 31-37 (and optionally 27), whereby in the last coating chamber 37 a carbon containing film, such as a diamond like carbon (DLC) film is deposited to make the coated flat glass product 25 scratch-resistant (especially for later handling). After exiting the last coating chamber 37, the coating, such as a solar control coating, of the flat glass product 25 must be checked, i.e., its properties must be measured in order to verify whether the in-line coating process was performing as desired, and to adjust the process parameters if necessary for subsequent coating. To measure the optical properties of the resulting flat glass product 25, the scratch-resistant carbon containing film must be removed as described above by means of plasma-jet processing (etching), in order to provide direct access to the underlying (e.g., solar control) coating for subsequent measurements with the optical spectrometer(s) 16.
Fig. 8 a) & b) show in a schematic perspective view an in-line coating system 26 with rollers 23 for transporting the flat glass substrate 24 into the in-line coating system 26 comprising multiple vacuum processing/coating chambers, out of which come coated glass products 25 with a protective, e.g., scratch-resistant top layer. As indicated in Fig. 8 a) by the arrows in the y direction, the plasma-jet source 2 operated at ambient environment is moved laterally (i.e., in y direction) across the glass panel 25 while exiting the in-line coating system 26. In the case of Fig. 8 a) the rollers 23 do not move the glass panel 25 while the plasma-jet source 2 laterally traverses the glass panel 25 to remove the protective top layer at the plasma-treated area A. After removing the protective top layer by plasma treatment, the optical properties of the glass panel 25 are measured by the optical spectrometer 16, which is mounted on the same carrier and moved together with the plasma-jet source 2, but arranged in a set back position relative to the plasma-jet source 2. Alternatively, the optical properties of the preceding glass panel 25', where the protective top layer has already been removed at the plasma-treated area A, can be measured ex-situ by the optical spectrometer 16' located downstream of the plasma-jet source 2 and mounted on a separate carrier, which is moved (simultaneously/synchronously with the plasma-jet source 2 operating on the succeeding glass panel 25) laterally (i.e., in y direction) across the glass panel 25' while the rollers do not move the glass panel 25'. As indicated in Fig. 8 b) by the arrows in the diagonal (x & y) direction, the plasma-jet source 2 operated at ambient environment is moved diagonally (i.e., in x & y direction) along and across the glass panel 25 while exiting the in-line coating system 26. In the case of Fig. 8 b) the rollers 23 are moving forward the glass panel 25 in x direction while the plasma-jet source 2 laterally traverses the glass panel 25 and at the same time moved along with the glass panel 25, which is also moving forward in the x direction, thereby removing the protective top layer at the plasma-treated area A limited across the forward end of the glass panel 25. After removing the protective top layer by plasma treatment, the optical properties of the glass panel 25 are measured by the optical spectrometer 16, which is mounted on the same carrier and moved together with the plasma-jet source 2, but arranged in a set back position relative to plasma-jet source 2. Alternatively, the optical properties of the preceding glass panel 25', where the protective top layer has already been removed at the plasma-treated area A limited across the forward end of the glass panel 25', can be measured ex-situ by the optical spectrometer 16' located downstream of the plasma-jet source 2 and mounted on a separate carrier, which is also moved (simultaneously/synchronously with the plasma-jet source 2 operating on the succeeding glass panel 25) diagonally (i.e., in x & y direction) along and across the glass panel 25' while the rollers 23 are moving the glass panel 25' forward in the x direction. The "continuous" diagonal scheme employed in Fig. 8 b) results in a higher through-put of the in-line process compared with the "stop-and-go" schema employed in Fig. 8 a). When employing the "continuous" scheme of Fig. 8 b) the plasma-jet source 2 and the optical spectrometer 16 (or 16') need to be moved backwards towards the in-line coating system 26 quickly in the short time interval between the back end of a glass panel 25 exiting the in-line coating system 26 and the following front end of the next glass panel 25 exiting the in-line coating system 26.
It is proposed to employ a total of four optical spectrometers 16 in a typical measurement setup. For instance, a first diode array spectrometer for the 380-2150 nm range with a measuring head for measuring transmission T at an angle of 0°, a second diode array spectrometer for the 380-2150 nm range with a measuring head for measuring the reflection on the glass side at an angle of 8°, a third diode array spectrometer for the 380-2150 nm range with a measuring head for measuring the reflection on the coated side at an angle of 8°, and a fourth diode array spectrometer for spectral reflection in the 380-2150 nm range with a measuring head for measuring the reflection on the coated side at an angle of 55°. Furthermore, sheet resistance should be measured in the range from 10 mQ to 100 Q for instance based on Eddie currents.
Fig. 9 shows on the left side a coated flat glass product 25 (as disclosed in WO2020164735A1), where a substrate S is coated with a solar control coating 40 coated which is topped by a transition metal (TM), carbon and oxygen containing layer 36', and an immediately consecutive DLCH layer 37', both increasing the scratch resistance of the solar coating. The latter is implemented in a configuration comprising two reflective silver layers 32', 34' sandwiched by three dielectric layers 31', 33', 35'.
On the right side of Fig. 9, a respective plasma treated glass product 25 can be seen. Due to the oxygen plasma flame expanding with high speed into atmosphere through the plasma aperture the DLC layer and the carbon content is burnt or etched away at least at and near the surface of the now treated TM layer 39. Thereby optical properties and hardness of the TM layer 39 are enhanced.
LIST OF REFERENCE SIGNS
1 apparatus 25' previously plasma-treated glass
2 plasma-jet source product (downstream)
3 housing 26 in-line coating system
5 gas inlet 27 further processing/coating
4 feedthrough chamber
6 electrode 28 carriage
7 end piece 29 transport system
8 nozzle 30 multi-chamber vacuum system
9 plasma channel (MCVS)
10 plasma outlet aperture 31-37 processing/coating chambers
11 insulator 31-36' layers of the coating system
12 plasma discharge 37' top protective layer/film (e.g.,
13 offset DLCH)
14 plasma track 38 coating system before plasma
15 plasma-treated area treatment
16 optical spectrometer 39 coating system after plasma
16' optical spectrometer located treatment downstream of plasma-jet 40 solar control coating
17 carrier 41 laser distance meter
18 horizontal guide (in y direction) 42 control unit
19 vertical guide (in z direction) A plasma-treated area
20 AC power supply B basic plane
21 plasma gas supply d distance between aperture and
22 roller table / glass support surface
23 roller di first distance (above S) of the
24 flat glass substrate plasma outlet aperture
25 coated flat glass product d2 second distance (above S) of the optical spectrometer
R central nozzle axis
S surface plane s offset between plasma-jet sources t thickness of glass product x longitudinal direction y lateral direction z vertical direction

Claims

1. An apparatus (1) for removing a protective film (37') from a coated flat glass product (25) extending in a longitudinal direction (x) and a lateral direction (y) and for measuring optical properties of the glass product (25), the apparatus (1) comprising:
- a glass support (22) defining a basic plane (B) at which the glass product (25) is supported;
- at least one plasma source (2), in particular a plasma-jet source, movable relative to the glass product (25) in at least one of the lateral direction (y), the longitudinal direction (x) and a vertical direction (z), in particular movable parallel to the basic plane (B), the at least one plasma source (2) having a plasma outlet aperture (10) adjustable in a first distance (di) above a surface plane (S), the surface plane (S) being substantially parallel and at a thickness distance (t) above the basic plane (B) in which the glass product (25) is supported;
- at least one optical spectrometer (16) or at least one optical fibre connected to the at least one optical spectrometer (16) movable relative to the glass product (25) in at least one of the lateral direction (y), the longitudinal direction (x) and the vertical direction (z) and adjustable at a second distance (d2) above the surface plane (S) together or synchronized with the at least one plasma source (2) and, with respect to a working direction, in line and set back to the at least one plasma source (2).
2. The apparatus (1) according to claim 1, wherein two or more plasma sources (2) are arranged along the lateral direction (y) laterally offset to one another such that plasma cones in a sideview overlap only partially in the surface plane (S). The apparatus (1) according to claim 1 or 2, wherein the at least one plasma source (2) comprises a grounded housing (3) forming a plasma chamber, the housing (3) being connectable to a gas supply (21) and having a nozzle (8) with a plasma channel ending with a plasma outlet aperture (10), the plasma chamber comprising an electrically isolated electrode (6) which is connectable to a high voltage supply of alternating current (20). The apparatus (1) according to claim 3, wherein the nozzle (8) is rotatable around a central nozzle axis (R) and the plasma outlet aperture (10) is eccentric relative to the central nozzle axis (R). The apparatus (1) according to claim 3 or 4, wherein the plasma channel (9) is funnel shaped with the smaller diameter ending with the plasma outlet aperture (10). The apparatus (1) according to claim 5, wherein the larger diameter end of the funnel encompasses symmetrically the central nozzle axis (R). The apparatus (1) according to one of claims 3 to 6, wherein the electrode (6) comprises a free end piece (7) directed towards the centre of the plasma channel (9). The apparatus (1) according to claim 7, wherein the end piece (7) is cone or truncated cone shaped with the narrower end directed towards the plasma channel (9). The apparatus (1) according to one of claims 1 to 8, further comprising means to control the first distance (di) above the surface plane (S) automatically. The apparatus (10) according to claim 9, wherein the means to control the first distance (di) comprise a vertical drive operatively connected to the at least one plasma source (2) and a distance sensor (41) operatively connected to an electronic control circuit (42) to control the vertical drive. A flat glass in-line coating system (26) comprising a series of consecutive vacuum processing or coating chambers (31-37, 27) succeeded by an apparatus (1) according to one of claims 1 to 10, wherein one of the last vacuum coating chambers, in particular the last vacuum coating chamber (37), in a downstream direction is adapted to deposit a carbon containing film, e.g., a diamond like carbon film (371), and comprises at least one gas inlet and a vacuum-plasma source, the last vacuum coating chamber (37) in particular being operatively connected via a vacuum to vacuum port or lock to a preceding vacuum coating chamber (36) and via a vacuum to atmosphere lock to the succeeding apparatus (1) according to one of claims 1 to 10. The system (26) according to claim 11, wherein the vacuum-plasma source comprises at least one plasma source chamber having an inductively coupled plasma electrode and at least one plasma window in parallel to a substrate plane to couple a plasma inductively into a process compartment of the one, in particular the last, vacuum coating chamber (37). The system (26) according to claim 11 or 12, wherein the preceding vacuum coating chamber (36) is a sputter chamber comprising at least one transition metal and/or silver target and at least one gas inlet for inert gas and a carbon containing gas. The system (26) according to one of claims 11 to 13, wherein the preceding vacuum coating chamber (36) is coupled to a last vacuum coating chamber (35) of a number of operatively connected vacuum coating chambers (31-35) all together adapted to form an antireflective, solar control, low-emissivity, decorative or functional coating system, wherein the system (26) comprises at least one vacuum coating chamber to deposit a dielectric coating, at least one vacuum coating chamber adapted to deposit a silver or a silver containing coating, and optionally one or more further coating chambers adapted to deposit at least one further functional layer. The system (26) according to claim 11, wherein each vacuum coating chamber (31-37) is equipped with a separate vacuum pump, a respective sputter target and an electric sputter supply, an inert sputter gas supply, and optionally with a reactive gas supply. A method for measuring optical properties of a flat glass product (25) extending in a longitudinal direction (x) and a lateral direction (y) provided with an optical coating system (40) which is protected by a final protective film (37'), comprising the steps:
- removing the protective film (371) linearly and in a defined width by moving at least one plasma outlet aperture (10) of a plasma source (2) in a working distance (di) above a surface plane (S) in particular in the lateral direction (y) across an essential or the full width of the flat glass product (25) to produce a protective film free linear section (15, A), and
- measuring at the same time or subsequently, but with reference to a working direction linearly offset behind and following the plasma source (2) in the lateral direction (y), the optical properties of the coated glass product along the protective film free linear section (15, A) with an optical spectrometer (16). The method according to claim 16, wherein the plasma source is connected to a gas supply (21) providing an oxygen containing gas at a pressure in a range from 1 to 200 bar, in particular from 1.5 to 10 bar. The method according to one of claims 16 to 17, wherein an electrode of the plasma source (2) is driven with alternating current, at a frequency from 18 to 25 kHz, at a power from 400 to 800 W and an operating voltage from 1.5 to 2.5 kV. The method according to one of claims 16 to 18, wherein the working distance (di) between the plasma outlet aperture (10) and a surface (S) of the glass product (25) is set to a distance in the range from 1 to 30 mm. The method according to one of claims 16 to 19, wherein a transverse speed in the range from 0.5 to 300 m/minute, in particular from 3 to 24 m/minute, is set between the surface (S) of the glass product (25) and the plasma source (2) and the same or a different transverse speed in the range from 3 to 24 m/minute is set between the surface (S) of the glass product (25) and the optical spectrometer (16). The method according to one of claims 16 to 19, wherein the plasma outlet aperture (10) is rotated eccentrically round an axis (R) of a nozzle (8) at a speed in a range from 1'500 to 3'000 revolutions per minute. The method according to one of claims 16 to 19, wherein the protective film (37') is a carbon containing film, in particular a diamond like carbon film.
PCT/EP2022/068097 2022-06-30 2022-06-30 Apparatus for removing a protective film from and measuring optical properties of a coated flat glass product WO2024002484A1 (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012083542A1 (en) * 2010-12-23 2012-06-28 深圳市华星光电技术有限公司 Device for repairing alignment layer and method for repairing alignment layer
WO2020164735A1 (en) 2019-02-15 2020-08-20 Glas Trösch Ag Functional coated article

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012083542A1 (en) * 2010-12-23 2012-06-28 深圳市华星光电技术有限公司 Device for repairing alignment layer and method for repairing alignment layer
WO2020164735A1 (en) 2019-02-15 2020-08-20 Glas Trösch Ag Functional coated article
US20220144698A1 (en) * 2019-02-15 2022-05-12 Glas Trösch Ag Functional Coated Article

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