WO2013091601A2 - Surfaces autonettoyantes et superhydrophobes à base de nanotubes en tio2 - Google Patents

Surfaces autonettoyantes et superhydrophobes à base de nanotubes en tio2 Download PDF

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Publication number
WO2013091601A2
WO2013091601A2 PCT/DE2012/001183 DE2012001183W WO2013091601A2 WO 2013091601 A2 WO2013091601 A2 WO 2013091601A2 DE 2012001183 W DE2012001183 W DE 2012001183W WO 2013091601 A2 WO2013091601 A2 WO 2013091601A2
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WO
WIPO (PCT)
Prior art keywords
metallic substrate
self
superhydrophobic coating
fluoride
cleaning properties
Prior art date
Application number
PCT/DE2012/001183
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German (de)
English (en)
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WO2013091601A3 (fr
Inventor
Tobias Mertens
Dominik Raps
Jürgen Wehr
Original Assignee
Eads Deutschland Gmbh
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Publication date
Application filed by Eads Deutschland Gmbh filed Critical Eads Deutschland Gmbh
Priority to EP12820852.7A priority Critical patent/EP2794966A2/fr
Priority to US14/367,667 priority patent/US20150299889A1/en
Publication of WO2013091601A2 publication Critical patent/WO2013091601A2/fr
Publication of WO2013091601A3 publication Critical patent/WO2013091601A3/fr

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/26—Anodisation of refractory metals or alloys based thereon

Definitions

  • the invention relates to a method for producing a superhydrophobic coating with self-cleaning properties on a metallic substrate, a metallic substrate with superhydrophobic coating and self-cleaning properties obtainable by such a method, the use of an electrolyte solution comprising ammonium sulfate and
  • Ammonium fluoride for producing a superhydrophobic coating with self-cleaning properties on a metallic substrate and the use of the metallic substrate for protection against icing in an aircraft or for protection against contamination and / or erosion in an aircraft.
  • buoyancy or flow elements such as wing, engine or
  • the air flow over the affected surfaces can be so unfavorably influenced that the aerodynamics of an aircraft impaired and, in particular in icing, in the worst case can lead to stall and loss of buoyancy.
  • icing or contamination of these systems can also increase the weight of the aircraft.
  • the contamination e.g. with insects the realization of a laminar wing are severely limited.
  • CONFIRMATION COPY During the flight of an aircraft, other techniques are used to prevent ice formation.
  • the leading edge of a wing with hot bleed air can be heated by engines, so as to perform a de-icing or to keep the wing ice-free.
  • engine bleed air may reduce the effective power of engines by about 3% and must not be activated during the takeoff phase.
  • inflatable elastic mats can be used with which formed ice is to be blasted off.
  • inflatable mats need a certain amount of time, until by the internal pressure
  • Geometry change can be achieved, leading to a blasting of the
  • Ice crystals leads. Furthermore, the surface quality of mat systems is very limited.
  • De-icing means actively removing ice and snow from the wing. On the ground this happens, for example, by spraying with 70-80 ° C warm de-icing liquids, during the flight, for example, with warm branch air or by electric heaters in the wing edges.
  • de-icing measures require either a considerable effort on the ground or an enormous energy expenditure during the flight.
  • special deicing vehicles is required on the ground, for which purpose appropriate logistics, such as the availability of the deicing vehicles, service schedules or maintenance of the deicing vehicles, must be available.
  • the use of these de-icing vehicles is also of environmental concern, as the
  • Deicing fluids are often based on ethylene glycol or propylene glycol, which are environmentally hazardous.
  • the operation of the deicing vehicles due to their size and weight leads to a significant fuel consumption.
  • Insect contamination have a significantly negative influence on the flow around and the friction losses. The same effects are also observed on surfaces exposed to erosion by air, rain and / or sand.
  • coated structures and thus represents a health hazard.
  • Another object is to provide a substrate having a superhydrophobic coating and self-cleaning properties which has a high hydrophobicity
  • a solution according to the invention consists in a process for producing a superhydrophobic coating with self-cleaning properties on a metallic substrate, comprising
  • step d) anodizing the metallic substrate from step c) to produce a nanoporous layer comprising titanium dioxide-containing nanotubes on the metallic substrate, and
  • nanoporous layer comprising titania-containing nanotubes
  • the electrolyte solution comprises another water-soluble salt selected from the group consisting of ammonium sulfate, sodium sulfate, sodium bisulfate, potassium sulfate, potassium bisulfate, and mixtures of these.
  • the invention enables the production of metallic substrates having a superhydrophobic coating and self-cleaning properties.
  • the present invention enables the production of metallic substrates with superhydrophobic coating and self-cleaning
  • the resulting metallic substrate having superhydrophobic coating and self-cleaning properties has high resistance to icing and / or contamination and / or erosion.
  • the surface of the metallic substrate having superhydrophobic coating and self-cleaning properties has a contact angle to water of more than 140 °.
  • an electrolyte solution comprising 50 to 250 g / l, in particular 120 to 140 g / l, ammonium sulfate and 0.5 to 10 g / l, in particular 4 to 6 g / l of ammonium fluoride in such Method provided.
  • a metallic substrate having superhydrophobic coating and self-cleaning properties for protection against icing in an aircraft.
  • the metallic substrate is a titanium alloy.
  • the alloy additionally comprises at least one further metal selected from the group consisting of V, Fe, Sn, Ni, Nb, Mo, Zr, Y, Hf, Ta, Ce, Tb, Nd, Gd, Dy, Ho and Er and / or additionally at least one further element selected from the group comprising Zn, Mn, Ag, Li, Cu, Si, Al or Ca.
  • the metallic substrate additionally comprises Al and V.
  • the fluoride salt is selected from the group comprising ammonium fluoride,
  • Ammonium bifluoride potassium fluoride, sodium fluoride, calcium fluoride,
  • the fluoride salt is ammonium fluoride.
  • the further water-soluble salt is ammonium sulfate.
  • the anodization is carried out in an electrolyte solution comprising 50 to 250 g / l, in particular 120 to 140 g / l ammonium sulfate and 0.5 to 10 g / l, in particular 4 to 6 g / l Ammonium fluoride, at a temperature in a range of 10 to 60 ° C, in particular 20 to 30 ° C and a voltage of preferably 2 to 50 volts, in particular 10 to 20 volts for 5 to 480 minutes, in particular 20 to 40 minutes.
  • the titania-containing nanotubes have a diameter in a range of 10 to 300 nm, preferably 20 to 220 nm, more preferably 30 to 180 nm, still more preferably 30 to 140 nm, and most preferably 30 to 100 nm up.
  • the titanium dioxide-containing nanotubes have a diameter in a range of 30 to 60 nm.
  • the superhydrophobic coating having self-cleaning properties on the metallic substrate has a layer thickness between 100 nm and 10 ⁇ m, preferably between 200 nm and 1 ⁇ m, more preferably between 250 nm and 800 nm more preferably between 280 nm and 600 nm and in particular between 300 nm and 500 nm.
  • the superhydrophobic coating comprises a fluoroalkyl functional silane.
  • the contacting of the metallic substrate surface with the electrolyte solution and / or the application of the superhydrophobic coating on the nanoporous layer by means of dipping, spinning, flooding, brushing or spraying.
  • a “superhydrophobic coating” or “superhydrophobic coating” is meant a coating that repels water
  • Coating "or" superhydrophobic coating understood a coating having a contact angle to water of more than 140 °.
  • “superhydrophobic coating” means a coating which has repellent properties with respect to dirt and gas components in the air or rainwater, such as SO 2, NO xl salts and hygroscopic dust or by residues of chlorides, sulfides, sulfates or acids or insects. Due to the small contact surface between the superhydrophobic material and these impurities, they can adhere worse to the surface. Does the metallic substrate such a superhydrophobic
  • the superhydrophobic coating also has self-cleaning
  • metal substrate is to be understood as meaning any substrate which consists entirely of metal or at least has a metallic layer on its surface.
  • metal not only pure metals, but also mixtures of metals and metal alloys.
  • the method of the invention can be applied to metallic substrates comprising titanium, although the scope of the present invention is not limited to this metal.
  • the method according to the invention is applied to a metallic substrate which consists of titanium.
  • the metallic substrate comprises a titanium alloy.
  • the amount of titanium in the alloy is at least 50% by weight, based on the total mass of the alloy, for example between 50 and 98% by weight. or 60 and 98% by weight.
  • the alloy comprises titanium in an amount of 85 to 95 wt .-%, based on the total mass of the alloy.
  • Titanium alloy additionally at least one other metal, this
  • V is selected from the group consisting of V, Fe, Sn, Ni, Nb, Mo, Zr, Y, Hf, Ta, Ce, Tb, Nd, Gd, Dy, Ho and Er.
  • Titanium alloys which may particularly benefit from the present invention are e.g. B. vanadium and aluminum-containing titanium alloys.
  • the process according to the invention is suitable for the production of superhydrophobic coatings with self-cleaning properties for the protection of titanium substrates and their alloys.
  • the titanium alloy additionally comprises at least Al as a further element.
  • the titanium alloy comprises AI as a further element in an amount of, for example, 1 to 10 wt .-% or 3 to 9 wt .-%, based on the total mass of the alloy.
  • the titanium alloy V comprises as further metal in an amount of, for example, 0.5 to 8 wt .-% or 1 to 6 wt .-%, based on the total mass of the alloy.
  • the titanium alloy additionally comprises at least V as a further metal and additionally at least AI as a further element.
  • the titanium alloy V comprises as further metal in an amount of, for example, 0.5 to 8 wt .-% or 1 to 6 wt .-%, based on the total mass of the alloy, and AI as another element in an amount of for example 1 to 10 wt .-% or 3 to 9 wt .-%, based on the total mass of the alloy.
  • the metallic substrate provides a
  • a requirement of the method according to the invention is that at least part of the metallic substrate surface is brought into contact with an electrolyte solution.
  • Electrolyte solution is brought into contact, which is to be protected by the superhydrophobic coating with self-cleaning properties from icing and / or contamination and / or erosion.
  • the entire coating with self-cleaning properties from icing and / or contamination and / or erosion.
  • the electrolyte solution comprises a fluoride salt.
  • the fluoride salt is selected from the group comprising
  • Ammonium fluoride ammonium bifluoride, potassium fluoride, sodium fluoride,
  • the fluoride salt is ammonium fluoride
  • the electrolyte solution may be provided in the form of an aqueous solution.
  • the total amount of fluoride salt in the electrolyte solution may be between 0.5 and 10 g / l.
  • the electrolytic solution contains the fluoride salt in an amount of 4 to 6 g / l.
  • Electrolyte solution another water-soluble, salt to improve the
  • the further water-soluble salt is ammonium sulfate.
  • the total amount of further water-soluble salt in the electrolyte solution may be between 50 and 250 g / l.
  • the electrolytic solution contains the further water-soluble salt in an amount of 120 to 140 g / l.
  • the electrolyte solution comprises
  • the electrolyte solution is water
  • the electrolyte solution comprises 50 to 250 g / l, in particular 120 to 140 g / l, preferably about 130 g / l of ammonium sulfate and 0.5 to 10 g / l,
  • the electrolyte solution contains no hydrofluoric acid.
  • the electrolyte solution can be applied by means of dipping, spinning, flooding, brushing or spraying.
  • the surface of the metallic substrate is pretreated before the application of the electrolyte solution.
  • the substrate is first cleaned and then etched or pickled. Suitable means for purification are, for example
  • Ethanol / Tensidgemische or alkaline cleaning agents such as. B. P3 Almeco 18 (Henkel Technologies).
  • the etching or acid pickling of the substrate can be carried out, for example, with an aqueous solution containing hydrofluoric acid
  • the surface of the substrate becomes acidic or basic conditioned by the substrate is immersed briefly in an alkaline cleaning bath.
  • the method comprises anodizing the with the
  • Electrolytic solution coated metallic substrate for producing a nanoporous layer on the metallic substrate comprises anodizing the entire electrolyte-coated metallic substrate to form a nanoporous layer on the metallic substrate.
  • Anodizing is an electrochemical process in which an oxide layer on titanium and alloys thereof can be produced by anodic oxidation.
  • the anodization takes place by means of a three-electrode arrangement.
  • a three-electrode arrangement Such three-electrode arrangements are known per se, so that they need not be shown and explained in detail.
  • the anodization takes place at a voltage between 2 volts and 50 volts, for example at a voltage between 10 and 20 volts.
  • the anodization step is carried out at a temperature between 10 ° C and 60 ° C or between 20 ° C and 30 ° C.
  • the anodization is carried out at room temperature, for example between 21 ° C and 25 ° C.
  • the anodization must be done for a period of time which leads to the formation of the desired surface structure.
  • the anodizing is carried out for a period of at least 5 minutes.
  • anodizing is performed for a period of 5 minutes to 480 minutes or 20 minutes to 40 minutes.
  • the anodization is carried out for a period of about 30 minutes.
  • the anodization step according to the invention leads to the formation of a
  • nanoporous layer on the metallic substrate is nanoporous
  • anodizing the metal substrate treated with the electrolytic solution results in the formation of nanotubes containing titanium dioxide ( ⁇ 2 ).
  • the nanoporous layer on the metallic substrate has a structure comprising a plurality of
  • Titanium dioxide-containing nanotubes includes.
  • the layer thickness of the nanoporous layer is preferably adjusted to a layer thickness between 100 nm and 10 ⁇ m.
  • the layer thickness of the nanoporous layer is preferably set to a layer thickness between 200 nm and 1 ⁇ m, preferably between 250 nm and 800 nm and more preferably between 280 nm and 600 nm.
  • the layer thickness of the nanoporous layer is adjusted to a layer thickness between 300 nm and 500 nm.
  • the nanotubes containing titanium dioxide contained in the nanoporous layer are adjusted to a specific pore diameter.
  • nanotube Having set nanotube to a diameter between 10 nm and 300 nm, preferably to a diameter between 20 nm and 220 nm or between 30 nm and 180 nm
  • Diameter of the nanotubes between 30 nm and 140 nm.
  • the nanotubes containing titanium dioxide produced during anodization are preferably evenly distributed on the metal surface.
  • the anodization step may be performed once or more than once.
  • a superhydrophobic coating is applied to the nanoporous layer.
  • the structure of the nanoporous layer comprising titanium dioxide-containing nanotubes is not changed during the application of the superhydrophobic coating.
  • sol / gel coatings SAM's [self-assembled
  • amphiphilic block copolymers siloxanes, long chain
  • Hydrocarbons and any other coating materials are used which form very thin superhydrophobic layers.
  • superhydrophobic coatings are suitable, with which a
  • Layer thickness between 0.1 nm and 200 nm can be adjusted, preferably a layer thickness between 1 nm and 100 nm or between 2 nm and 70 nm. Particularly preferred is a layer thickness between 3 nm and 50 nm or between 5 nm and 30 nm.
  • amphiphilic block copolymers selected from the group consisting of hydrophilic block copolymers, such as Polyethylene oxide (PEO), hydrophobic block copolymers such as polyethylene (PE), polybutadiene (PB) and mixtures of these.
  • hydrophilic block copolymers such as Polyethylene oxide (PEO)
  • PEO Polyethylene oxide
  • hydrophobic block copolymers such as polyethylene (PE), polybutadiene (PB) and mixtures of these.
  • siloxanes e.g. oligomeric alkylalkoxysiloxanes or polymeric siloxanes, long chain hydrocarbons, e.g. Octyltriethoxysilane, or silane-siloxane mixtures.
  • a sol / gel coating is applied to the nanoporous layer.
  • Suitable sol / gel coatings are, for example, optionally fluorinated, alkylsilane compounds.
  • Tetraalkoxysilanes alkyltrialkoxysilanes, aryltrialkoxysilanes, alkenyltrialkoxysilanes, glycidoxyalkyltrialkoxysilanes, aminoalkyltrialkoxysilanes and
  • fluoroalkyl-functional silanes include fluorinated tetraalkoxysilanes,
  • the sol / gel coating comprises (tridecafluoro-1,1,2,2-tetrahydrooctyl) triethoxysilane.
  • the sol / gel coating comprises (tridecafluoro-1,1,2,2-tetrahydrooctyl) triethoxysilane.
  • the commercially available Dynasylan ® F 8261 (Evonik Industries).
  • the properties of the coating, for. As hardness, can be increased by the addition of silicon-free precursors. examples for this are
  • organometallic compounds such as tetra-iso-propoxytitanium, tri-isopropoxyaluminum, tri-sec-butoxyaluminum, tetrabutoxyzirconium and
  • sol-gel matrix small particles such.
  • metal oxides metal carbides and metal nitrides are added. Suitable materials are, for example, SiC, Si 3 N 4 , Al 2 O 3, ZrO 2 , TiO 2 or SiO 2 .
  • nanoparticles can increase the resistance of the coating.
  • the particles may optionally be functionalized.
  • the functionalization can be carried out, for example, by chemo-mechanical processes during the milling of the particles.
  • a suitable for the functionalization of nanoparticles compound is z. B.
  • the hydrolysis of the sol-gel forming components can be accomplished by the addition of water.
  • the processing properties of the sol-gel material can be adjusted via solvents and additives.
  • Suitable as a solvent are, for.
  • the additives may, for example, wetting agents, flow control agents, foam suppressants, dispersants, UV stabilizers and silicones and condensation catalysts such.
  • acids or bases to be adjusted via solvents and additives.
  • the finished sol can also be provided with organic polymers.
  • the sol-gel material is prepared from (tridecafluoro- 1, 1, 2,2-tetrahydrooctyl) triethoxysilane and isopropanol, wherein the hydrolysis is effected by adding water and 37% strength hydrochloric acid.
  • the superhydrophobic coating can be applied by conventional application methods such as dipping, spinning, flooding, brushing or spraying.
  • the sol / gel coating may be thermal, e.g. Example, at a temperature between 40 ° C and 180 ° C, are cured, preferably at a temperature between 60 ° C and 120 ° C.
  • the sol / gel coating becomes one
  • the coating may alternatively or additionally by irradiation, for. B. with UV light, infrared or the like.
  • the sol / gel coating is adjusted to a layer thickness between 0.1 nm and 200 nm, preferably to a layer thickness between 1 nm and 100 nm or between 2 nm and 70 nm. More preferably, the layer thickness between 3 nm and 50 nm or between 5 nm and 30 nm.
  • the layer thickness may be further increased if necessary.
  • the metallic substrates with superhydrophobic coating and self-cleaning properties obtained by the process according to the invention can be used in particular in aircraft such as aircraft and helicopters.
  • Coating and self-cleaning properties can also be used in land vehicles, rail vehicles or ships.
  • the resulting metallic substrates with superhydrophobic coating and self-cleaning properties have in particular a contact angle to water of more than 140 °.
  • the obtained metallic substrate with superhydrophobic coating and self-cleaning properties has a contact angle to water between 140 ° and 170 ° or between 150 ° and 160 °.
  • the metallic substrate to which the inventive superhydrophobic coating with self-cleaning is provided.
  • the metallic substrate to which the superhydrophobic coating of the invention having self-cleaning properties is applied is selected from rotor blades of wind turbines, house facades, bridges, power lines and the like.
  • Aircraft in which the metallic substrates of the invention having superhydrophobic coating and self-cleaning properties are used are protected against erosion and / or contamination by insects and / or organic and inorganic materials such as dirt and gas components in the air or rainwater.
  • contamination in particular with organic materials, can take place first.
  • These adhering contaminants are under UV irradiation by the metallic substrate with superhydrophobic coating and self-cleaning properties are decomposed and removed from the coated substrate surface.
  • Aircraft provided. Further, in another aspect of the present invention, the use of a metallic substrate having superhydrophobic coating and self-cleaning properties for protection against
  • an electrolyte solution comprising 50 to 250 g / l, in particular 120 to 140 g / l, ammonium sulfate and 0.5 to 10 g / l, in particular 4 to 6 g / l ammonium fluoride in one method for producing a superhydrophobic coating with self-cleaning
  • the embodiments of the method also apply to the metallic substrate obtainable by the method as well as the uses and vice versa.
  • Fig. 1 shows the top view of a coated titanium substrate in one
  • Fig. 2 shows the side view of a coated titanium substrate in one
  • FIG. 3 shows a schematic representation of a metallic substrate having a superhydrophobic coating with self-cleaning properties.
  • Titanium alloy TiAl6V4 with the commercially available alkaline cleaner P3 Almeco 18 (Henkel Technologies) degreased at a concentration of 30 g / l at 70 ° C for 15 min and cleaned. Subsequently, the substrate was etched at a concentration of 500 g / l of the commercially available stain Turco® 5578 (Henkel Technologies) at about 95 ° C for 5 min, cleaned with deionized water and dried in air.
  • the anodization of the cleaned substrate was carried out in the electrolytic solution using a three-electrode arrangement with TiAl6V4 as the cathode at a voltage of 15 volts for 30 minutes at about 22 ° C.
  • a substrate with a nanoporous layer which had a layer thickness of 300 nm to 350 nm, was obtained.
  • the nanoporous layer was uniformly distributed over the treated substrate and had a multiplicity of nanotubes with a pore diameter of about 40 to 50 nm.
  • the anodized substrate was then cleaned with deionized water and dried in a stream of nitrogen.
  • the substrate with the commercially available fluorosilane Dynasylan ® F 8261 (Evonik Industries) was treated.
  • fluorosilane coating was carried out by dip coating for 2 min and subsequent purification with deionized water for 30 s.
  • the resulting substrates were cured at 80 ° C. for 1 h.
  • the edge regions of the Ti0 2- containing nanotubes were treated with a thin layer (a few nm) of the fluorosilane coating.
  • a substrate with a nanoporous layer which had a layer thickness of 300 nm to 350 nm, was obtained.
  • the nanoporous layer of Ti0 2 - containing nanotubes on the titanium substrate and the structure of the obtained nanotubes are in the
  • FIG. 2 Scanning electron micrograph shown in Fig. 2. As shown in Fig. 2, the TiO 2 -containing nanotubes are not closed.
  • Fig. 3 shows a schematic representation of the titanium substrate with a superhydrophobic coating and self-cleaning properties.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

L'invention concerne un procédé permettant de fabriquer un revêtement superhydrophobe doté de propriétés autonettoyantes sur un substrat métallique, un substrat métallique pourvu d'un revêtement superhydrophobe, présentant des propriétés autonettoyantes et pouvant être obtenu par un tel procédé. L'invention concerne également l'utilisation d'une solution électrolytique comprenant du sulfate d'ammonium et du fluorure d'ammonium pour fabriquer un revêtement superhydrophobe présentant des propriétés autonettoyantes sur un substrat métallique. L'invention concerne également l'utilisation d'un substrat métallique pour empêcher un givrage dans un aéronef et/ou pour empêcher des impuretés de pénétrer dans l'aéronef et/ou empêcher une érosion de se former dans l'aéronef.
PCT/DE2012/001183 2011-12-22 2012-12-11 Surfaces autonettoyantes et superhydrophobes à base de nanotubes en tio2 WO2013091601A2 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP12820852.7A EP2794966A2 (fr) 2011-12-22 2012-12-11 Surfaces autonettoyantes et superhydrophobes à base de nanotubes en tio2
US14/367,667 US20150299889A1 (en) 2011-12-22 2012-12-11 Self-Cleaning and Superhydrophobic Surfaces Based on TIO2 Nanotubes

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE102011122084 2011-12-22
DE102011122084.8 2011-12-22
DE102012001912.2 2012-02-02
DE102012001912A DE102012001912A1 (de) 2011-12-22 2012-02-02 Selbstreinigende und superhydrophobe Oberflächen auf Basis von TiO2-Nanotubes

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WO2013091601A2 true WO2013091601A2 (fr) 2013-06-27
WO2013091601A3 WO2013091601A3 (fr) 2013-08-22

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