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WO2015036427A1 - Procédé au laser pour la modification de nanoparticules métalliques sur des substrats en verre de grande dimension - Google Patents

Procédé au laser pour la modification de nanoparticules métalliques sur des substrats en verre de grande dimension Download PDF

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Publication number
WO2015036427A1
WO2015036427A1 PCT/EP2014/069274 EP2014069274W WO2015036427A1 WO 2015036427 A1 WO2015036427 A1 WO 2015036427A1 EP 2014069274 W EP2014069274 W EP 2014069274W WO 2015036427 A1 WO2015036427 A1 WO 2015036427A1
Authority
WO
WIPO (PCT)
Prior art keywords
containing layer
laser line
glass substrate
nanoparticle containing
laser
Prior art date
Application number
PCT/EP2014/069274
Other languages
English (en)
Inventor
Li-Ya Yeh
Michael BEHMKE
Lorenzo CANOVA
Nicolas Nadaud
Original Assignee
Saint-Gobain Glass France
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Saint-Gobain Glass France filed Critical Saint-Gobain Glass France
Priority to EP14777281.8A priority Critical patent/EP3044176A1/fr
Publication of WO2015036427A1 publication Critical patent/WO2015036427A1/fr

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/26—Thermography ; Marking by high energetic means, e.g. laser otherwise than by burning, and characterised by the material used
    • B41M5/262—Thermography ; Marking by high energetic means, e.g. laser otherwise than by burning, and characterised by the material used recording or marking of inorganic surfaces or materials, e.g. glass, metal, or ceramics
    • 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
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
    • 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
    • C03C17/06—Surface treatment of glass, not in the form of fibres or filaments, by coating with metals
    • C03C17/09—Surface treatment of glass, not in the form of fibres or filaments, by coating with metals by deposition from the vapour phase
    • 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

Definitions

  • the invention relates to a laser process for the modification of metallic nanoparticles into the surface of large size glass substrates and its use.
  • Modern architecture often contains large glass surfaces, which are often colored to give an appealing impression.
  • Manufacturing of colored glass is usually done by addition of colorants, e.g. metals or metal oxides, to the molten glass or the raw materials for glass production. Changing the color or the composition of the glass is extremely time consuming and expensive as the float glass process is a continuous process and large scales of rejects are produced.
  • colorants e.g. metals or metal oxides
  • WO 2010/106370 describes a process for coloration of glass, in which a precursor containing metallic nanoparticles is sprayed onto a hot glass substrate.
  • the glass substrates are heated to a temperature of 350°C to 550 °C.
  • the tempering has to done for several minutes due to the time dependency of the diffusion process. Hence the process is rather time consuming.
  • Another method for coating glass substrates is flame spraying. Such a flame spraying process is for example disclosed in WO 2008/099048.
  • a precursor comprising coloring transition metal oxides is flame sprayed onto the substrate followed by a reduction step.
  • Another process leading to colored glass or glass with optically modified properties is alternating sputtering and co-sputtering of a dielectric matrix containing nanoparticles onto
  • the mechanical stability and resistivity of the obtained coating is quite low due to the low layer thickness between 10 nm and 500 nm.
  • US 2004/01 18157 A1 discloses a process for laser beam-assisted implementation of metallic nano particles into glass surfaces.
  • the object of the invention is to develop a method for marking glass or to produce multi colored decorations.
  • the laser processing is preferably realized by a C0 2 laser, whereat the deposition area is limited by the size of the laser spot.
  • the size of the processing area of such laser arrangements is typically limited between 10 ⁇ and several millimeters. Hence the laser process described in US 2004/01 18157 A1 is not suitable for processing of large sheets of glass.
  • the object of the present invention is to provide a profitable laser process for modification of metallic nanoparticles on coated glass substrates, wherein also large size substrates can be processed.
  • the solution of the object of the present invention is a laser process for modification of metallic nanoparticles on large size glass substrates and its use according to independent claims 1 and 9.
  • the method according to the invention for modification of optical properties of a glass substrate by modification of nanoparticles comprises the following steps:
  • a) at least one nanoparticle containing layer is applied onto the glass substrate, b) a laser line is focused onto this nanoparticle containing layer,
  • the glass substrate is moved in a direction x relative to the laser line and the glass substrate with nanoparticle containing layer is laser processed, wherein the glass substrate has got a width of 0.10 m to 5.00 m perpendicular to the direction x.
  • the laser processing during step c) leads to a modification of the optical properties of the nanoparticle containing layer.
  • the method according to the invention enables a homogeneous and time-saving laser processing of large size substrates.
  • the nanoparticle containing layer is heated by carefully targeted laser processing, whereas an increase of the core temperature of the glass substrate can be mostly avoided and only the temperature within the surface near region of the glass substrate is slightly raised.
  • a local heat treatment of the nanoparticle containing layer leads to the modification of their optical properties.
  • the process according to the invention is especially advantageous for the production of large-scale sheets of colored glass or diffractive glazing.
  • optical properties or color is governed by the size, number, depth and allocation of the nanoparticles. These values can be controlled by the heating process. Therefore the precise adjustment of the laser heating process allows a defined modification of the optical properties.
  • the change in optical properties or color of the modified glass is defined by the wavelength of the Surface Plasmon Resonance (SPR). This is manly governed on the material of the nanoparticles. For example cobalt leads to bluish, copper to ruby, nickel to grey and silver to yellow color change.
  • SPR Surface Plasmon Resonance
  • Oven processes according to the state of the art are rather time consuming, in general a few minutes are needed per substrate, whereas laser processes according to the state of the art use lasers providing a laser spot of very limited size, typically 10 pm to a few millimeters. Thus these processes are not suitable for processing of large size substrates.
  • the method according to the invention enables a fast processing of large substrates, in which a single substrate is typically processed within a few seconds, preferably a fraction of seconds.
  • the direction x is defined as the direction of relative movement between the laser line and the substrate during processing.
  • the glass substrates are placed onto a conveyor, which is spanned by a stationary laser arrangement generating the laser line.
  • the glass substrates are transported in direction x via the conveyor and processed by crossing the laser line. This embodiment is especially advantageous as the process could be performed in line with a float process and a deposition process.
  • the laser arrangement is mounted on a moveable track system while the glass substrates are held stationary.
  • the direction x is solely defined as positive value as the transportation of the glass sheet only takes place in one direction.
  • a backward transport of the glass substrate in direction -x is not necessary as the laser line covers the width of the substrate and the entire surface of the substrate is treated within one cycle. A time- consuming repeated passage of substrates is not required.
  • Nanoparticles which are already implemented in coatings of glass substrates or within the surface near-region of glass substrates can be modified by a second heating process according to the invention. It is possible to perform this post heating very precise by the method according to the invention. The modification of the nanoparticles leads to a change in optical properties of the glazing.
  • a first process for implementation of nanoparticles can be an oven process, laser process, physical or chemical vapor deposition process or other
  • the nanoparticle containing layer could for example be generated by a sputtering process, in which a metal compound containing layer is deposited.
  • the nanoparticles could be formed within the sputtering process by dewetting. Alternatively the sputtering could be followed by an oven process for generating nanoparticles.
  • An application of the method according to the invention is laser treatment of nanoparticles to gain colored glass.
  • the method according to the invention is especially advantageous within the production of mirrors, wherein the reflection properties of the mirrors are changed yielding a slightly pink reflection. The color of human skin appears more vivid in such mirrors.
  • the nanoparticle containing layer contains a transition metal or a transition metal compound, preferably silver, gold, iron, copper, chromium, cobalt, nickel, molybdenum, palladium, platinum, manganese, vanadium, rare earth metals or compounds or mixtures thereof, more preferably cobalt, nickel, palladium, silver, gold, copper or compounds or mixtures thereof.
  • a transition metal or a transition metal compound preferably silver, gold, iron, copper, chromium, cobalt, nickel, molybdenum, palladium, platinum, manganese, vanadium, rare earth metals or compounds or mixtures thereof, more preferably cobalt, nickel, palladium, silver, gold, copper or compounds or mixtures thereof.
  • the nanoparticle containing layer is one layer within a stack of multiple layers, at least two layers.
  • at least one nanoparticle containing layer is arranged alternating with at least two intermediate layers, wherein the intermediate layers are dielectric layers and/or TCO-layers.
  • the dielectric layers contain Si 3 N 4 , Si0 2 , Ti0 2 , Al 2 0 3 or compounds or mixtures thereof, more preferably Si 3 N 4 .
  • the TCO-layers (TCO: transparent conductive oxide) contain indium tin oxide (ITO).
  • nanoparticle containing layer consisting of a 2 nm silver layer applied in an alternate sputtering process with two dielectric layers of 10 nm Si 3 N 4 , wherein the nanoparticle containing layer is embedded between the dielectric layers.
  • the length of the laser line is defined as its maximum dimension, while the width of the laser line is its minimum dimension.
  • the laser line runs along direction y, perpendicular to direction x, so that the width of the laser line is measured along direction x, while the length of the laser line is measured along direction y.
  • a diagonal progression of the laser line is also possible.
  • the laser line according to the invention is preferably generated by a series of laser assemblies, mounted besides each other.
  • the areas illuminated by the single laser assemblies add up to the laser line.
  • the single laser assemblies can be operated independently, e.g. the power density could be modulated within the laser line.
  • the laser line is generated by a single laser.
  • the laser assemblies comprise diode lasers, fiber lasers and/or disk lasers, most preferably diode lasers.
  • the laser line has got a length of 0.10 m to 5.00m, preferably 0.25 m to 3.50 m, more preferably of 0.60 m to 3.30 m.
  • the general standard size of float glass sheets is 6 m x 3 m, the method according to the invention enables homogeneous and fast processing of such sheets.
  • the laser line has got a width of 10 ⁇ to 500 ⁇ , preferably 20 ⁇ to 250 ⁇ , most preferably 20 ⁇ to 100 ⁇ .
  • the power density of the laser line is between 50 W/mm 2 and 3000 W/mm 2 , preferably 300 W/mm 2 to 2000 W/mm 2 , most preferably 500 W/mm 2 to 1700 W/mm 2 .
  • the line width of the laser line is 40 ⁇ .
  • the line width should be chosen as small as possible to maximize the energy input per unit area.
  • a large energy input per surface area means that the processing time can be kept short. Hence only the surface area of the substrate is heated and the temperature rise of the glass is minimized.
  • the wave length of the laser line is between 250 nm to 2000 nm, preferably 500 nm to 1700 nm, most preferably 700 nm to 1300 nm.
  • the method according to the invention is suitable for heat treatment within the temperature range of 80 °C to 700 °C, preferably 100 °C to 600 °C.
  • the maximum core temperature of the glass substrate is 250 °C, preferably 100 °C, most preferably 80 °C.
  • the core temperature of the glass substrate is defined as the temperature outside the surface near region, wherein during processing the temperature of the surface near region is equal to or higher than the core temperature.
  • the surface near region has got a thickness of 1 ⁇ to 500 ⁇ , preferably 1 ⁇ to 100 ⁇ .
  • the laser line is turned off at least once during step c) and/or the power density of the laser line is modified during step c).
  • a modulation of the power density leads to a structuring of the substrate as nanoparticles are only modified in some regions, e.g. when the laser line is turned off during processing, or nanoparticles with different properties are formed. This could be desirable in terms of design aspects, for the production of diffractive glazing or other linear designs for gaining optical effects.
  • the power density along the laser line is not homogeneous and/or the power density along the laser line is modified during step c).
  • Such an embodiment of the process is for example advantageous in production of glazing with an inhomogeneous appearance or color.
  • Another solution of the present invention is the use of the method according to the invention for the production of colored glass substrates, preferably for processing of large-scale glass substrates with a size of at least 1 m 2 .
  • Figure 1 a and 1 b depict a glass substrate with a nanoparticle containing layer and a method for modification of the nanoparticle containing layer.
  • Figure 2 depicts a glass substrate with a stack of nanoparticle containing layers and intermediate layers and a method for modification of the nanoparticle containing layers.
  • Figure 3 depicts a flow chart of the method according to the invention.
  • Figure 1 a depicts a cross sectional view of a glass substrate (1 ) with a nanoparticle containing layer (2.2).
  • the nanoparticle containing layer (2.2) is deposited by sputtering of silver in step a).
  • a laser line (4) is focused onto the nanoparticle containing layer (2.2) in step b) and the glass substrate (1 ) is processed by moving the glass substrate in direction x relative to the laser line (4) in step c).
  • the laser line (4) runs along direction y, perpendicular
  • the laser line (4) has got a length of 3.1 m and runs along the width of the glass substrate (1 ), having a width of 3.0 m, along direction y, perpendicular to direction x.
  • the laser line (4) has got a line width of 40 ⁇ , a power density of 1000 W/mm 2 and a wave length of 980 nm.
  • Laser treatment of the nanoparticle containing layer (2.2) leads to a temperature increase, which leads to a change in optical properties and formation of a nanoparticle containing layer with modified optical properties (2.2').
  • Figure 1 b shows a top view of the glass substrate (1 ) with nanoparticle containing layer (2.2) according to Figure 1 a.
  • the laser line (4) runs along the direction x and covers the whole width of the glass substrate (1 ).
  • the glass substrate (1 ) is laser processed by transport of the substrate in direction x via a conveyor.
  • Figure 2 depicts a cross sectional view of a glass substrate (1 ) with a stack of nanoparticle containing layers (2.2) and intermediate layers (3) and a method for modification of the nanoparticle containing layers (2.2).
  • the nanoparticle containing layer (2.2) consists of a 3 nm gold layer applied in an alternate sputtering process with an intermediate layer (3) of 30 nm Ti0 2 .
  • the upper layer of the stack and the layer directly applied onto the glass substrate (1 ) are intermediate layers (3). Between this top and bottom intermediate layers (3) an alternating stack of three nanoparticle containing layers (2.2) and two intermediate layers (3) is applied.
  • the properties of the laser line (4) and the dimensions of the substrate are those already described in Figure 1 a.
  • Laser treatment of the nanoparticle containing layer (2.2) leads to a temperature increase, which leads to a change in optical properties and formation of a nanoparticle containing layer with modified optical properties (2.2').
  • Figure 3 shows a flow chart of the method according to the invention.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Dispersion Chemistry (AREA)
  • Composite Materials (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

L'invention concerne un procédé pour la modification de propriétés optiques d'un substrat en verre (1) par la modification de nanoparticules comprenant a) l'application d'au moins une couche contenant des nanoparticules (2.2) sur le substrat en verre (1), b) la focalisation d'une raie laser (4) sur la couche contenant des nanoparticules (2.2), c) le traitement au laser du substrat en verre (1) présentant la couche contenant des nanoparticules (2.2) par le mouvement du substrat en verre (1) dans la direction x par rapport à la raie laser (4), le substrat en verre (1) présentant une largeur de 0,10 m à 5,00 m perpendiculairement à la direction x et les propriétés optiques de la couche contenant des nanoparticules (2.2) étant modifiées dans l'étape c).
PCT/EP2014/069274 2013-09-10 2014-09-10 Procédé au laser pour la modification de nanoparticules métalliques sur des substrats en verre de grande dimension WO2015036427A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP14777281.8A EP3044176A1 (fr) 2013-09-10 2014-09-10 Procédé au laser pour la modification de nanoparticules métalliques sur des substrats en verre de grande dimension

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP13183701.5 2013-09-10
EP13183701 2013-09-10

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WO2015036427A1 true WO2015036427A1 (fr) 2015-03-19

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EP (1) EP3044176A1 (fr)
WO (1) WO2015036427A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018019374A1 (fr) 2016-07-27 2018-02-01 Trumpf Laser Gmbh Éclairage de ligne laser
WO2019149352A1 (fr) 2018-01-31 2019-08-08 Trumpf Laser Gmbh Source d'éclairage de ligne à base de diode laser et éclairage à ligne laser

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040118157A1 (en) 2001-04-19 2004-06-24 Reinhard Borek Method for laser beam-assisted application of metal ions in glass for producing colorless and color pixels
US20050044895A1 (en) * 2002-04-16 2005-03-03 Central Glass Company, Limited Method for putting color to glass or erasing color from colored glass
US20050124712A1 (en) * 2003-12-05 2005-06-09 3M Innovative Properties Company Process for producing photonic crystals
US20050239004A1 (en) * 2002-10-29 2005-10-27 Siegfried Gahler Coating composition, particularly for glass surfaces, and methods for the production and use thereof
GB2431892A (en) * 2002-09-26 2007-05-09 Printable Field Emitters Ltd Creating layers in thin-film structures
WO2008099048A1 (fr) 2007-02-12 2008-08-21 Beneq Oy Procédé de dopage du verre
US20080268165A1 (en) * 2007-04-26 2008-10-30 Curtis Robert Fekety Process for making a porous substrate of glass powder formed through flame spray pyrolysis
US20090104436A1 (en) * 2005-06-03 2009-04-23 Boraglas Gmbh Low-E Layered Systems Comprising Coloured Structures, Method for Producing the Latter and Use of Said Systems
WO2010106370A1 (fr) 2009-03-20 2010-09-23 University College London Substrat enduit
WO2013050337A2 (fr) * 2011-10-06 2013-04-11 Solvay Sa Composition de revêtement et revêtement antireflet préparé à partir de celle-ci

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CN101689376B (zh) * 2007-09-28 2012-07-11 Hoya株式会社 磁盘用玻璃基板及其制造方法、磁盘

Patent Citations (10)

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Publication number Priority date Publication date Assignee Title
US20040118157A1 (en) 2001-04-19 2004-06-24 Reinhard Borek Method for laser beam-assisted application of metal ions in glass for producing colorless and color pixels
US20050044895A1 (en) * 2002-04-16 2005-03-03 Central Glass Company, Limited Method for putting color to glass or erasing color from colored glass
GB2431892A (en) * 2002-09-26 2007-05-09 Printable Field Emitters Ltd Creating layers in thin-film structures
US20050239004A1 (en) * 2002-10-29 2005-10-27 Siegfried Gahler Coating composition, particularly for glass surfaces, and methods for the production and use thereof
US20050124712A1 (en) * 2003-12-05 2005-06-09 3M Innovative Properties Company Process for producing photonic crystals
US20090104436A1 (en) * 2005-06-03 2009-04-23 Boraglas Gmbh Low-E Layered Systems Comprising Coloured Structures, Method for Producing the Latter and Use of Said Systems
WO2008099048A1 (fr) 2007-02-12 2008-08-21 Beneq Oy Procédé de dopage du verre
US20080268165A1 (en) * 2007-04-26 2008-10-30 Curtis Robert Fekety Process for making a porous substrate of glass powder formed through flame spray pyrolysis
WO2010106370A1 (fr) 2009-03-20 2010-09-23 University College London Substrat enduit
WO2013050337A2 (fr) * 2011-10-06 2013-04-11 Solvay Sa Composition de revêtement et revêtement antireflet préparé à partir de celle-ci

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Title
BERG K-J ET AL: "Small silver particles in glass surface layers produced by sodium-silver ion exchange-their concentration and size depth profile", INSPEC, 1990, XP002329493 *
H. HOFMEISTER ET AL.: "Oriented prolate silver particles in glass - characteristics of novel dichroic polarizers", NANOSTRUCTURED MATERIALS, vol. 12, 1999, pages 207 - 210, XP022455228, DOI: 10.1016/S0965-9773(99)00100-2 *
M. KAEMPFE ET AL.: "Ultrashort laser pulse induced deformation of silver nanoparticles in glass", APPLIED PHYSICS LETTERS, vol. 74, no. 9, March 1999 (1999-03-01), pages 1200 - 1202, XP012023327, DOI: 10.1063/1.123498 *
See also references of EP3044176A1 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018019374A1 (fr) 2016-07-27 2018-02-01 Trumpf Laser Gmbh Éclairage de ligne laser
US11407062B2 (en) 2016-07-27 2022-08-09 Trumpf Laser Gmbh Laser line illumination
US11759886B2 (en) 2016-07-27 2023-09-19 Trumpf Laser Gmbh Laser line illumination
EP4331768A2 (fr) 2016-07-27 2024-03-06 TRUMPF Laser GmbH Éclairage de ligne laser
WO2019149352A1 (fr) 2018-01-31 2019-08-08 Trumpf Laser Gmbh Source d'éclairage de ligne à base de diode laser et éclairage à ligne laser

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