EP1144341A1 - Procede pour produire des surfaces ultraphobes a base de carbure de tungstene - Google Patents

Procede pour produire des surfaces ultraphobes a base de carbure de tungstene

Info

Publication number
EP1144341A1
EP1144341A1 EP99968356A EP99968356A EP1144341A1 EP 1144341 A1 EP1144341 A1 EP 1144341A1 EP 99968356 A EP99968356 A EP 99968356A EP 99968356 A EP99968356 A EP 99968356A EP 1144341 A1 EP1144341 A1 EP 1144341A1
Authority
EP
European Patent Office
Prior art keywords
ultraphobic
laser
microns
tungsten carbide
coating
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Withdrawn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
EP99968356A
Other languages
German (de)
English (en)
Inventor
Karsten Reihs
Daniel-Gordon Duff
Georg Wiessmeier
Burkhard KÖHLER
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.)
Sunyx Surface Nanotechnologies GmbH
Original Assignee
Sunyx Surface Nanotechnologies 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 Sunyx Surface Nanotechnologies GmbH filed Critical Sunyx Surface Nanotechnologies GmbH
Publication of EP1144341A1 publication Critical patent/EP1144341A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/0036—Laser treatment
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/203—Oil-proof or grease-repellant materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials

Definitions

  • the present invention relates to an ultraphobic surface, its manufacture and
  • the method is characterized in that an essentially smooth surface made of tungsten carbide is structured by means of laser ablation, wherein periodically recurring depressions are formed along the surface with a depth in the range from 10 ⁇ m to 500 ⁇ m, preferably from 50 ⁇ m to 250 ⁇ m.
  • the surface is then optionally coated with an adhesion promoter layer and then provided with a hydrophobic or in particular oleophobic coating.
  • Ultraphobic surfaces are characterized by the fact that the contact angle of a drop of a liquid, usually water, lying on the surface is significantly more than 90 ° and that the roll angle does not exceed 10 °. Ultraphobic surfaces with a contact angle> 150 ° and the above Roll-off angles have a very high technical benefit because they e.g. cannot be wetted with water or oil, dirt particles adhere very poorly to these surfaces and these surfaces are self-cleaning. Self-cleaning is understood here to mean the ability of the surface to easily release dirt or dust particles adhering to the surface to liquids that flow over the surface.
  • EP 476 510 AI discloses a method for producing an ultraphobic surface, in which a metal oxide film is applied to a glass surface and then etched using an Ar plasma.
  • the surfaces produced using this method have the disadvantage that the contact angle of a drop lying on the surface is less than 150 °.
  • US Pat. No. 5,693,236 also teaches a number of processes for the production of ultraphobic surfaces, in which zinc oxide microneedles are brought onto a surface with a binder and are then partially exposed in different ways (for example by plasma treatment). The surface structured in this way is then coated with a water-repellent agent. To this
  • Wise structured surfaces however, also only have contact angles of up to 150 °.
  • the roll angle here is understood to be the angle of inclination of a basically planar but structured surface with respect to the horizontal, at which a standing water drop of volume 10 ⁇ l is moved due to gravity when the
  • the object is achieved according to the invention by the provision of a method for producing an ultraphobic surface which is the subject of the invention, characterized in that an essentially smooth surface is made of
  • Tungsten carbide is structured by means of laser ablation, with periodically recurring depressions in particular being formed along the surface with a depth in the range from 10 ⁇ m to 500 ⁇ m, preferably from 50 ⁇ m to 250 ⁇ m and an average distance between adjacent depressions from 10 to 500 ⁇ m, preferably from 50 up to 250 ⁇ m, the surface is then optionally coated with an adhesion promoter layer and then provided with a hydrophobic or in particular oleophobic coating.
  • a foam body that is to be provided with the surface according to the invention either consists entirely of tungsten carbide or has a surface
  • Tungsten carbide the surface being coated with any can be applied by way of driving.
  • Tungsten carbide in the sense of the invention means not only pure tungsten carbide but also alloys or mixtures in which the proportion of tungsten carbide is> 30% by weight, preferably> 45% by weight.
  • the tungsten carbide can be structured with any laser suitable for laser ablation.
  • the wavelength of the laser light is preferably between 500 and 550 nm.
  • a Nd: YAG laser is particularly preferably used for this.
  • the laser also preferably has a beam diameter on the sample surface of 30 to 70 ⁇ m, particularly preferably 45 to 55 ⁇ m.
  • the power density of the laser on the substrate surface is preferably 10 4 to 10 7 W / cm 2 , particularly preferably 10 5 to 10 6 W / cm 2 .
  • the scanning speed is preferably 30 to 50 mm / s, particularly preferably 35 to 45 mm / s.
  • the line offset of adjacent scanning lines is preferably 5 to 500 ⁇ m, particularly preferably 8 to 250 ⁇ m.
  • the surfaces thus obtained are provided with a hydrophobic or in particular oleophobic coating.
  • a hydrophobic material in the sense of the invention is a material which shows a contact angle with respect to water of greater than 90 ° on a flat, non-structured surface.
  • An oleophobic material in the sense of the invention is a material which, on a flat, non-structured surface, has a contact angle with respect to long-chain n-alkanes, such as n-decane, of greater than 90 °.
  • the ultraphobic surface preferably has a coating with a hydrophobic phobicization aid, in particular an anionic, cationic, amphoteric or nonionic, surface-active compound.
  • These compounds are preferably cationic, anionic, amophotere or non-ionic surface-active compounds, such as those e.g. in the directory “Surfactants Europa, A Dictionary of Surface Active Agents available in Europe, Edited by Gordon L. Hollis, Royal Socity of Chemistry, Cambridge, 1995.
  • anionic phobicization aids alkyl sulfates, ether sulfates, ether carboxylates, phosphate esters, sulfosucinates, sulfosuccinatamides, paraffin sulfonates, olefin sulfonates, sarcosinates, isothionates, taurates and Linginian compounds.
  • Quaternary alkylammonium compounds and imidazoles may be mentioned as cationic phobicization aids
  • Amphoteric phobicization aids are, for example, betaines, glycinates, propionates and imidazoles.
  • nonionic phobing aids examples include: alkoxylates, alkyloamides, esters, amine oxides and alkypolyglycosides. Also suitable are: reaction products of alkylene oxides with alkylatable compounds, such as. B. fatty alcohols, fatty amines, fatty acids, phenols, alkylphenols, arylalkylphenols, such as styrene-phenol condensates, carboxamides and resin acids.
  • Phobicization aids are particularly preferred in which 1 to 100%, particularly preferably 60 to 95%, of the hydrogen atoms are substituted by fluorine atoms.
  • Examples include perfluorinated alkyl sulfate, perfluorinated alkyl sulfonates, and perfluorinated Called alkyl phosphonates, perfluorinated alkyl phosphinates and perfluorinated carboxylic acids.
  • polymeric phobicization aids for hydrophobic coating or as polymeric hydrophobic material for the surface.
  • These polymeric phobicization aids can be nonionic, anionic, cationic or amphoteric compounds.
  • these polymeric phobicization aids can be homopolymers and copolymers, graft and graft copolymers and random block polymers.
  • Particularly preferred polymerizing auxiliaries are those of the type AB, BAB and ABC block polymers.
  • the A segment is a hydrophilic homopolymer or copolymer and the B block is a hydrophobic homopolymer or copolymer or a salt thereof.
  • Anionic, polymeric phobing aids are also particularly preferred, in particular condensation products of aromatic sulfonic acids with formaldehyde and alkylnaphthalenesulfonic acids or from formaldehyde, naphthalenesulfonic acids and / or benzenesulfonic acids, condensation products from optionally substituted phenol with formaldehyde and sodium bisulfite.
  • condensation products which can be obtained by reacting naphthols with alkanols, additions of alkylene oxide and at least partial conversion of the terminal hydroxyl groups into sulfo groups or half esters of maleic acid and phthalic acid or succinic acid.
  • the phobicization aid is from the group of the sulfosuccinic acid esters and alkylbenzenesulfonates.
  • Sulfated, alkoxylated fatty acids or their salts are also preferred.
  • alkoxylated fat Acid alcohols are understood in particular to be those with 5 to 120, with 6 to 60, very particularly preferably with 7 to 30 ethylene oxide units, C 6 -C 22 fatty acid alcohols which are saturated or unsaturated, in particular stearyl alcohol.
  • the sulfated alkoxylated fatty acid alcohols are preferably in the form of a salt, in particular in the form of alkali or amine salts, preferably in the form of the diethylamine salt.
  • an adhesion promoter layer is therefore optionally applied between the surface and the hydrophobic or oleophobic coating.
  • any substance which is familiar to the person skilled in the art and which increases the bond between the surface and the respective hydrophobic or oleophobic coating is suitable as an adhesion promoter.
  • Preferred adhesion promoters, e.g. for thiols as a hydrophobic coating noble metal layers are e.g. made of Au, Pt or Ag or those made of GaAs, especially gold.
  • Adhesion promoter layer is preferably from 10 to 100 nm.
  • ultraphobic surfaces can be produced in which the contact angle of a drop lying on the surface is> 155 °.
  • the invention therefore also relates to the ultraphobic surfaces obtained by the process according to the invention.
  • ultraphobic surfaces have the advantage, among other things, that they are self-cleaning, and the self-cleaning can be carried out by exposing the surface to rain or moving water from time to time.
  • ship hulls With the ultraphobic surface produced by the method according to the invention, ship hulls can be coated in order to reduce their frictional resistance.
  • sanitary facilities in particular toilet bowls, can be provided with the ultraphobic surface produced by the process according to the invention in order to reduce their susceptibility to contamination.
  • ultraphobic surface is the coating of surfaces on which no water should adhere in order to avoid icing.
  • the surfaces of heat exchangers are an example here. in refrigerators or the surfaces of aircraft called.
  • the surfaces produced with the method according to the invention are also suitable for attachment to house facades, roofs, monuments in order to make them self-cleaning.
  • the ultraphobic surfaces produced by the method according to the invention are also particularly suitable for coating shaped articles whose surface is subjected to high mechanical stress.
  • the ultraphobic surfaces produced using the method according to the invention are also particularly suitable for coating shaped articles which are translucent. In particular, it is translucent glazing of buildings, vehicles, solar panels.
  • a thin layer of the ultraphobic surface according to the invention is evaporated onto the molded body.
  • the invention also relates to a material or building material having an ultraphobic surface according to the invention.
  • Another object of the invention is the use of the ultraphobic surface according to the invention for the friction-reducing lining of vehicle bodies, aircraft or ship hulls.
  • the invention also relates to the use of the ultraphobic surface according to the invention as a self-cleaning coating or planking of
  • the invention further relates to the use of the ultraphobic surface according to the invention as a rust-protecting coating of metal objects.
  • a tungsten carbide substrate (WC 64%, Co 6%, grade: THM SPUN 633 (US); K10-K25 190412; WIDIA, 19x19 mm 2 , 5mm thick) is covered on an area of 10x10 mm 2 with the following registration conditions by a Nd : YAG laser structured:
  • Laser power 3 W (pulse length 100 ns, frequency 4 kHz) Beam diameter: 50 ⁇ m
  • the inscribed pattern has approximately square columns in the format 67 x 67 ⁇ m 2 , the height of which is 200 ⁇ m. The distance between the columns is approximately 200 ⁇ m.
  • the tungsten carbide surface is roughened due to melting or condensation processes in the area of the inscribed areas.
  • the substrate treated in this way was coated with an approximately 50 nm thick gold layer by sputtering.
  • This coating corresponds to the method which is also common for preparation in electron microscopy and according to Klaus Wetzig, Dietrich Schulze, "In situ Scanning Electron Microscopy in Material Research",
  • the gold layer of the sample was coated with a few drops of a solution of n-decanethiol in ethanol (1 g / 1) at room temperature in a closed vessel for 24 hours, then rinsed with ethanol and dried.
  • the surface has a static contact angle of 155 ° for water. If the straight surface is inclined by ⁇ 10 °, a drop of water with a volume of 10 ⁇ l will roll off spontaneously.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

L'invention concerne un procédé pour produire une surface présentant des propriétés ultraphobes, selon lequel une surface pratiquement lisse, constituée de carbure de tungstène est structurée par ablation au laser. Ledit procédé consiste à ménager des évidements en particulier récurrents le long de la surface, présentant une profondeur comprise entre 10 νm et 500 νm, puis à revêtir éventuellement la surface avec une couche d'agent adhésif et à appliquer un revêtement hydrophobe ou oléophobe.
EP99968356A 1998-12-24 1999-12-20 Procede pour produire des surfaces ultraphobes a base de carbure de tungstene Withdrawn EP1144341A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19860135 1998-12-24
DE1998160135 DE19860135C2 (de) 1998-12-24 1998-12-24 Ultraphobe Oberfläche auf Basis von Wolframcarbit, ein Verfahren zu ihrer Herstellung und ihre Verwendung
PCT/EP1999/010113 WO2000039051A1 (fr) 1998-12-24 1999-12-20 Procede pour produire des surfaces ultraphobes a base de carbure de tungstene

Publications (1)

Publication Number Publication Date
EP1144341A1 true EP1144341A1 (fr) 2001-10-17

Family

ID=7892710

Family Applications (1)

Application Number Title Priority Date Filing Date
EP99968356A Withdrawn EP1144341A1 (fr) 1998-12-24 1999-12-20 Procede pour produire des surfaces ultraphobes a base de carbure de tungstene

Country Status (4)

Country Link
EP (1) EP1144341A1 (fr)
AU (1) AU2538100A (fr)
DE (1) DE19860135C2 (fr)
WO (1) WO2000039051A1 (fr)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19947788A1 (de) * 1999-10-05 2001-04-12 Bayer Ag Verfahren und Vorrichtung zum Bewegen von Flüssigkeiten
DE10004724A1 (de) * 2000-02-03 2001-08-09 Bayer Ag Rohrleitung mit ultraphober Innenwand
DE10005600A1 (de) 2000-02-09 2001-08-16 Bayer Ag Ultraphobes Flächengebilde mit einer Vielzahl von hydrophilen Bereichen
DE10028772B4 (de) * 2000-06-07 2005-03-17 Technische Universität Dresden Aluminiumwerkstoff mit ultrahydrophober Oberfläche, Verfahren zu dessen Herstellung sowie Verwendung
FR2830008B1 (fr) 2001-09-21 2004-06-11 Alstom Procede pour ameliorer les proprietes d'adhesion d'un substrat ceramique de la famille des non-oxydes en vue de son collage
DE10162816A1 (de) * 2001-12-19 2003-07-03 Sunyx Surface Nanotechnologies Optischer Schalter
US7456392B2 (en) 2002-02-22 2008-11-25 Qiagen Gmbh Use of ultraphobic surfaces having a multitude of hydrophilic areas for analyzing samples
EP2157432A1 (fr) 2008-08-15 2010-02-24 Qiagen GmbH Procédé d'analyse d'un échantillon complexe par spectrométrie de masse
WO2015003333A1 (fr) * 2013-07-10 2015-01-15 公凖精密工业股份有限公司 Procédé de traitement antiadhérence pour moule et moule traité à l'aide dudit procédé
ES2697919A1 (es) * 2017-07-28 2019-01-29 Bsh Electrodomesticos Espana Sa Metodo para fabricar un componente de aparato domestico, componente de aparato domestico, aparato domestico, y dispositivo de microestructuracion por laser
CN114315428B (zh) * 2020-09-29 2024-03-08 航天特种材料及工艺技术研究所 一种去除多孔石英陶瓷透波材料锈渍的方法
CN114178709A (zh) * 2021-12-29 2022-03-15 陕西科技大学 一种纯钛表面的二维码激光标刻方法

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JPH04124047A (ja) * 1990-09-17 1992-04-24 Nissan Motor Co Ltd ガラス表面の撥水処理方法
DE4125165A1 (de) * 1991-07-30 1993-02-04 Hoechst Ceram Tec Ag Gebranntes, keramisches erzeugnis mit strukturierter oberflaeche und verfahren zu seiner herstellung
US5473138A (en) * 1993-07-13 1995-12-05 Singh; Rajiv K. Method for increasing the surface area of ceramics, metals and composites
JPH07316546A (ja) * 1994-05-23 1995-12-05 Matsushita Electric Ind Co Ltd 撥水表面構造及びその形成方法

Non-Patent Citations (1)

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Also Published As

Publication number Publication date
AU2538100A (en) 2000-07-31
WO2000039051A1 (fr) 2000-07-06
DE19860135C2 (de) 2003-02-06
DE19860135A1 (de) 2000-06-29

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