EP1920276A1 - Verfahren zur herstellung einer strukturierten sol-gel-schicht. - Google Patents

Verfahren zur herstellung einer strukturierten sol-gel-schicht.

Info

Publication number
EP1920276A1
EP1920276A1 EP06776593A EP06776593A EP1920276A1 EP 1920276 A1 EP1920276 A1 EP 1920276A1 EP 06776593 A EP06776593 A EP 06776593A EP 06776593 A EP06776593 A EP 06776593A EP 1920276 A1 EP1920276 A1 EP 1920276A1
Authority
EP
European Patent Office
Prior art keywords
substrate
soi
vibrated
substrates
sol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP06776593A
Other languages
German (de)
English (en)
French (fr)
Inventor
Michael Ukelis
Monika Kursawe
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Merck Patent GmbH
Original Assignee
Merck Patent GmbH
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 Merck Patent GmbH filed Critical Merck Patent GmbH
Publication of EP1920276A1 publication Critical patent/EP1920276A1/de
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C03C17/25—Oxides by deposition from the liquid 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
    • C03C17/001—General methods for coating; Devices therefor
    • C03C17/002—General methods for coating; Devices therefor for flat glass, e.g. float glass
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
    • 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
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/02—Diffusing elements; Afocal elements
    • G02B5/0205—Diffusing elements; Afocal elements characterised by the diffusing properties
    • G02B5/021—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place at the element's surface, e.g. by means of surface roughening or microprismatic structures
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/02—Diffusing elements; Afocal elements
    • G02B5/0205—Diffusing elements; Afocal elements characterised by the diffusing properties
    • G02B5/021—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place at the element's surface, e.g. by means of surface roughening or microprismatic structures
    • G02B5/0221—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place at the element's surface, e.g. by means of surface roughening or microprismatic structures the surface having an irregular structure
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/02—Diffusing elements; Afocal elements
    • G02B5/0268—Diffusing elements; Afocal elements characterized by the fabrication or manufacturing method
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/02—Diffusing elements; Afocal elements
    • G02B5/0273—Diffusing elements; Afocal elements characterized by the use
    • G02B5/0278—Diffusing elements; Afocal elements characterized by the use used in transmission
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/02—Diffusing elements; Afocal elements
    • G02B5/0273—Diffusing elements; Afocal elements characterized by the use
    • G02B5/0284—Diffusing elements; Afocal elements characterized by the use used in reflection
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/21—Oxides
    • C03C2217/213—SiO2
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/113—Deposition methods from solutions or suspensions by sol-gel processes

Definitions

  • the present invention relates to a method for producing a structured surface on a substrate, wherein a substrate is introduced into a vibrated SoI, in particular immersed, or a vibrated substrate is introduced into an optionally vibrated SoI, in particular immersed, is. Structured substrates in this way and their use in optical applications are also the subject of the present invention.
  • Structured surfaces play a role in a variety of applications and processes.
  • Surface-structured substrates are also becoming increasingly important in optical applications, e.g. as diffusers or as reflectors.
  • Optical diffusers are scattered surfaces where incident light diffuses diffusely. Common examples of the use of optical diffusers are, for example, focusing screens in photography or projection technology onto which an image is projected. The light that strikes the screen for imaging is scattered by it, ie deflected in different directions. This scattering ensures that the image projected onto the ground-glass screen can be recognized from different directions. Diffusers are also finding increasing use in liquid crystal displays (LCD), e.g. for generating a planar illumination. Thus, there is a need for methods that can provide diffuse scattering surfaces.
  • LCD liquid crystal displays
  • the present invention accordingly provides methods for producing a structured surface on a substrate, wherein a substrate is introduced, in particular dipped, in or introduced into a vibrated sol
  • Vibrated substrate is placed in an optionally vibrated SoI introduced, in particular submerged, is.
  • a structured surface in the sense of the present invention is a surface which has a regular or irregular structure, in particular in the form of grooves, depressions or protrusions of any kind.
  • the depressions and bulges can assume any shape and are in the nanometer to millimeter size range.
  • the method according to the invention has the advantage that it is simple to carry out and offers the possibility of producing a wide variety of structuring.
  • a simple step the structure is preserved directly in a stable coating and requires no further additional stabilization.
  • structures can be produced in the one-step process on the surface of a substrate.
  • suitable mixing of appropriate sols for example of T ⁇ O 2 - and SiO 2 sols, a refractive index adjustment for controlling the optical effects can be achieved.
  • the processes according to the invention are suitable for the production of diffusers for liquid crystal displays.
  • a backlight for LCDs which ensures a sufficient contrast.
  • battery-LCD's for example in laptops
  • reflectors that should fulfill at least the following requirements:
  • Suitable substrates in the present invention are glass substrates, ceramic substrates, metal substrates or plastic substrates, preferably glass, metal or ceramic substrates and very particularly preferably glass substrates or metal substrates. Glass substrates or metal substrates having structured surfaces are particularly suitable for optical applications, in particular for LCD 's.
  • Suitable materials for the glass substrates are all known glasses, for example float glass, cast glass from all glass compositions known to those skilled in the art, A, C, D, E, ECR, R or S glasses.
  • metal substrates are, for example, polished or blank drawn metal sheets with a mean roughness of ⁇ 1 micron.
  • Suitable plastic substrates consist for example of PMMA or polycarbonate.
  • Suitable ceramic substrates are all ceramics known to the person skilled in the art, in particular transparent ceramics, which can be structured by one of the methods mentioned below.
  • the sols which are suitable in the process according to the invention can be all sols known to the person skilled in the art, for example sols of compounds of the elements titanium, zirconium, silicon, aluminum and / or mixtures thereof.
  • silicon sols are used. Sols or precursors of this type are known and commercially available.
  • the silicon sols are those in which the SiO 2 particles have been obtained by hydrolytic polycondensation of tetraalkoxysilane, in particular tetraethoxysilane (TEOS), in an aqueous-alcoholic-ammoniacal medium.
  • TEOS tetraethoxysilane
  • aqueous and / or solvent-containing sols prepared in another way can also be used as the coating solution.
  • the coating solution may additionally contain surfactants.
  • the employable sol-gel coating solutions may contain other components, e.g. Leveling agent or complexing agent.
  • the respective solids content in the coating solution is usually in the range of 0.1 to 20 wt .-%, preferably 2 to 10 wt .-%.
  • the coating of the substrate is preferably carried out by dip coating, wherein the sol or the substrate or optionally both is vibrated.
  • the substrate is coated with the sol, wherein the applied layer has a structuring, which is caused by the vibrations of the sol and / or the substrate.
  • the SoI is vibrated.
  • the oscillations can be achieved by both mechanical and electromechanical oscillation oscillations.
  • mechanical vibration generators consist of a rotating balancing mass driven by a motor, wherein the balancing in the simplest case is transmitted mechanically to the container containing the sol, for example a cuvette, and / or the substrate. The drive of the mechanical
  • Vibration generator can be electrically, pneumatically, hydraulically or by an internal combustion engine, depending on the desired application.
  • the substrate is dipped with a lifting device into a SoI filled cuvette, whereby the cuvette and thus the SoI or SoI alone is vibrated. Subsequently, the substrate is withdrawn from the cuvette at a uniform rate. If the substrate is immersed in the vibrating SoI and pulled out again, there is an uneven coating of the substrate with the coating solution. In this way, a structured surface is created, the type and degree of structuring depends significantly on the set frequency of the vibration and the sols and equipment used. By expertly adjusting the aforementioned parameters, the structuring obtained can be adapted to the needs. Since the structuring takes place directly on the surface of the substrate by coating in a vibrating SoI, the structures have "smooth" transitions without edges and corners.The period of structuring can also be controlled by the frequency of the oscillation used and thus also the needs are adjusted.
  • Electromechanical vibration generators usually consist of an electromagnetic system or piezo system, which is excited by high-frequency alternating voltage to vibrate. These vibrations are characterized by a very wide possible frequency spectrum.
  • the individual types and variants of vibration generators and their structural design are the One skilled in the art and can be easily adapted to the particular needs. For example, when ultrasound is used, it may be a corresponding ultrasonic bath into which the container containing the sol is introduced. The vibrations are transferred to the SoI in the container.
  • an ultrasonic generator directly in the SoI used is conceivable, e.g. in the form of a sonotrode, which is immersed in the SoI.
  • Vibrational excitation of SoIs are at 5 Hz to 50 KHz, preferably at 5 to 500 Hz.
  • the thickness of the deposited layer depends essentially on the pull rate of the substrate during coating. The higher the pulling speed, the thicker the layer obtained. Usually, the drawing speeds are in the range of 0.01 to 250 mm / sec, and preferably in the range of 1 to 20 mm / sec, and most preferably in the range of 2 to 10 mm / sec. Of course, the coating process can also be repeated one or more times until the desired thickness is reached. Preferably, the individual parameters are coordinated so that the structured surface fulfills the desired conditions.
  • the structured substrate can be calcined. Calcination removes the residual solvent content from the applied layer.
  • the calcination temperatures are usually from 300 to 700 ° C., in particular from 500 to 600 ° C.
  • the structured surface is additionally coated with a metal layer.
  • This additional step follows the coating in the SoI-GeI process and can be carried out at any time afterwards.
  • the coating with a metal layer can be carried out wet-chemically, for example by suitable reduction methods, in the CVD and / or PVD method, the PVD methods being preferred.
  • Suitable metals for the additional metal layer are, for example, aluminum, silver, chromium, nickel or other reflective metal layers.
  • the metal layer is aluminum.
  • the thickness of the additional metal layer depends on the material and the desired properties and is usually in the range of 10 to 150 nm and in particular in the range of 30 to 100 nm.
  • substrates with a structured surface prepared by one of the processes according to the invention.
  • Another object of the present invention is the use of structured surface substrates obtainable according to the methods described above as diffusers and / or reflectors in optical applications.
  • the optical applications can be any of the optical applications known to the person skilled in the art, for example cameras of all types, projection devices and screens, liquid crystal displays, magnification systems, eg microscopes etc.
  • the substrates according to the invention are preferably used in liquid crystal displays.
  • the structured substrates according to the present invention can be used particularly advantageously, for example as a reflective background, to replace a backlight and thus reduce the energy consumption of the display can. Further fields of application of the structured substrates according to the The present invention will be apparent to those skilled in the art without inventive step.
  • Example 1 A CrNi steel cuvette measuring 250 ⁇ 30 ⁇ 350 mm is filled with an aqueous-alcoholic SiO 2 sol (solids content: 3% by weight). On the cuvette, a mechanical vibration generator is mounted at the top in the middle.
  • the oscillator is a commercial electric motor with imbalance weight (mass of imbalance weight about 10 g), which is attached via a clamping device on the cuvette.
  • An approximately 1 mm thick float glass is attached to a lifting device and immersed in the cuvette. After switching on the oscillator (frequency: 120 Hz), the glass sheet is pulled out of the cuvette with the lifting device at a speed of 5 mm / sec. The glass sheet is dried for 10 minutes at room temperature.
  • a coated float glass pane is obtained, the coating having a diffusely scattering surface structuring.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Optics & Photonics (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Dispersion Chemistry (AREA)
  • Composite Materials (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Chemically Coating (AREA)
  • Surface Treatment Of Glass (AREA)
  • Colloid Chemistry (AREA)
  • Oxygen, Ozone, And Oxides In General (AREA)
  • Silicon Compounds (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Optical Elements Other Than Lenses (AREA)
EP06776593A 2005-08-31 2006-08-04 Verfahren zur herstellung einer strukturierten sol-gel-schicht. Withdrawn EP1920276A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102005041243A DE102005041243A1 (de) 2005-08-31 2005-08-31 Verfahren zur Herstellung einer strukturierten Sol-Gel-Schicht
PCT/EP2006/007709 WO2007025629A1 (de) 2005-08-31 2006-08-04 Verfahren zur herstellung einer strukturierten sol-gel-schicht.

Publications (1)

Publication Number Publication Date
EP1920276A1 true EP1920276A1 (de) 2008-05-14

Family

ID=37103058

Family Applications (1)

Application Number Title Priority Date Filing Date
EP06776593A Withdrawn EP1920276A1 (de) 2005-08-31 2006-08-04 Verfahren zur herstellung einer strukturierten sol-gel-schicht.

Country Status (9)

Country Link
US (1) US20080204885A1 (zh)
EP (1) EP1920276A1 (zh)
JP (1) JP2009505936A (zh)
KR (1) KR20080046692A (zh)
CN (1) CN101253422B (zh)
AU (1) AU2006286835B2 (zh)
DE (1) DE102005041243A1 (zh)
TW (1) TWI415673B (zh)
WO (1) WO2007025629A1 (zh)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009035585A1 (de) * 2009-07-31 2011-02-03 Krones Ag Inspektionsvorrichtung und Inspektionsverfahren zum Erkennen von Fremdkörpern in einem gefüllten Behälter
CN110565037A (zh) * 2019-10-19 2019-12-13 广西凯威铁塔有限公司 一种具有表面均匀纹路热浸锌工件的生产方法

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EP0545135B1 (de) * 1991-11-30 1998-06-17 MERCK PATENT GmbH Herstellung von Metalloxidsolen durch Elektrolyse
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JP2003167101A (ja) * 2001-03-01 2003-06-13 Nippon Sheet Glass Co Ltd 光学素子の製造方法
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JP2003186004A (ja) * 2001-12-14 2003-07-03 Nippon Sheet Glass Co Ltd 凸状膜の形成方法
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Also Published As

Publication number Publication date
WO2007025629A1 (de) 2007-03-08
AU2006286835A1 (en) 2007-03-08
TW200719955A (en) 2007-06-01
US20080204885A1 (en) 2008-08-28
KR20080046692A (ko) 2008-05-27
DE102005041243A1 (de) 2007-03-01
CN101253422B (zh) 2012-02-22
CN101253422A (zh) 2008-08-27
TWI415673B (zh) 2013-11-21
AU2006286835B2 (en) 2012-02-09
JP2009505936A (ja) 2009-02-12

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