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WO2019078729A2 - Procédé de fabrication d'un agencement protégé contre le givrage et agencement protégé contre le givrage - Google Patents

Procédé de fabrication d'un agencement protégé contre le givrage et agencement protégé contre le givrage Download PDF

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Publication number
WO2019078729A2
WO2019078729A2 PCT/NO2018/050249 NO2018050249W WO2019078729A2 WO 2019078729 A2 WO2019078729 A2 WO 2019078729A2 NO 2018050249 W NO2018050249 W NO 2018050249W WO 2019078729 A2 WO2019078729 A2 WO 2019078729A2
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WIPO (PCT)
Prior art keywords
graphene
coating
icing
substrate
fluorinated
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Ceased
Application number
PCT/NO2018/050249
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English (en)
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WO2019078729A3 (fr
Inventor
Bodil HOLST
Naureen AKTHAR
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Vestlandets Innovasjonsselskap AS
Original Assignee
Bergen Teknologioverforing AS
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Publication of WO2019078729A2 publication Critical patent/WO2019078729A2/fr
Publication of WO2019078729A3 publication Critical patent/WO2019078729A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
    • C23C16/0281—Deposition of sub-layers, e.g. to promote the adhesion of the main coating of metallic sub-layers
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/56—After-treatment

Definitions

  • the invention relates to a method for producing an icing protected arrangement. Furthermore, the invention relates to an icing protected arrangement, comprising a substrate coated by an anti-icing coating.
  • icing of surfaces can be a problem. Sensors, surveillance cameras, windows or other critical surfaces must be free of ice for proper operation. This requires for example heating, manual cleaning or chemical cleaning, which is power consuming and thus to be avoided.
  • the wings or rotors and/or some other critical parts i.e. rudder, elevators, stabilizers, propeller, swatch plates etc. of aircrafts have to be de-iced during flight or prior to the take-off in winter or in harsh environments. For that reason the aircraft is sprayed with a special de-icing solution and/or heated. This is time consuming and expensive.
  • the problem to be solved is to provide a method for producing an icing protected arrangement and such an icing protected arrangement which is capable to at least reduce the need for additional de-icing provisions like heating or spraying with de-icing solutions or manual cleaning.
  • the problem is solved by a method as mentioned above comprising the steps forming graphene coating on a substrate
  • an icing protected arrangement as mentioned above with its anti-icing coating comprising a one side fluorinated graphene layer with a saturation of 20 % to 50 %.
  • Fluorinated graphene shows good anti-icing properties.
  • Using this icing protected arrangement keeps the windows of sensors or surveillance cameras or other windows or critical surfaces free of ice, even in hash or arctic environment for example for environmental monitoring or in the oil and gas industry. Further, by using this icing protected arrangement there is no or at least a reduced need of de-icing of aircrafts during flight or before take-off.
  • said graphene coating or said anti-icing coating is comprising one or more layers, preferably monolayers. This results in a good coverage of the surface to be kept free of ice.
  • said graphene coating is formed by mechanical cleavage, epitaxial growth, chemical vapor deposition (CVD), plasma enhanced chemical vapor deposition (PECVD), unzipping of carbon nanotubes, carbon nanotube slicing, arc discharge, thermal graphitization of silicon carbide, growth from polymerized self-assembled monolayers followed by thermal treatment, growth from the thermal decomposition of chemisorbed fullerene molecules, intercalation of graphite, spraying, dip coating, spin coating, spray coating, spray drying, layer- by- layer self-assembly, painting or using polydimethylsiloxane (PDMS) stamps.
  • PDMS polydimethylsiloxane
  • the method comprises the step of forming an intermediate layer, preferably between said substrate and said graphene coating, more preferably the intermediate layer forms a catalyst layer and/or an adhesion layer and/or is made of metals such as Cu, Ni, Fe, Pt, Ru, Ir, Co, Au, oxides such as CuO x , SiO x , Co y O x , Al y O x , composite material or graphene.
  • the intermediate layer is removed with an etchant, preferably 1 M solution of ferric chloride in water Concerning the arrangement it is to be preferred that said anti-icing coating comprising an intermediate layer, preferably from ruthenium or graphene.
  • the intermediate layer can give a more accurate connection between the substrate and the coating.
  • the graphene is placed directly on the surface without an intermediate layer or the intermediate layer used for growing the graphene layer is removed before or after fluorination, preferably removed before fluorination step.
  • the method comprises the steps forming the graphene coating (14, 15) on a growth substrate, preferably the intermediate layer, transferring the graphene coating (14, 15), preferably as graphene sheets, from said growth substrate to said substrate (11), curing of liquid polydimethylsiloxane (PDMS) on graphene followed by fast release of graphene from substrate though wet-etching- assisted mechanical peeling.
  • PDMS liquid polydimethylsiloxane
  • Another advantage results from the step of producing a heating element from said graphene coating or that intermediate layer. Accordingly, it is of advantage, if said anti- icing coating comprising a heating element from graphene, preferably from one or more graphene layers. In case of remaining moisture or ice on the surface this results in an easy and direct heating, which is highly transparent.
  • said fluorination comprising at least one of the following fluorination methods Exposure to fluorine gas, preferably at high temperatures, more preferred with fluorine gas diluted in noble gas, most preferred in Xenon
  • F-based plasma preferably using SF6, CF 4 or Ar/F2
  • Exfoliation of graphite fluoride or fluorinated graphite preferably sonochemical exfoliation, more preferably liquid phase exfoliation assisted by ultrasonication, using most preferably ethanol, isopropanol, acetonitrile, ionic liquids, surfactants as intercalating agents or thermal exfoliation
  • CF X with 0 ⁇ x ⁇ 1 For partially fluorinated graphene (CF X with 0 ⁇ x ⁇ 1), a certain amount of carbon atoms are bonded to fluorine atoms with bonding character varying from ionic to semi-ionic to covalent. Control of the C-F bonding character and the mole ratio of fluorine to carbon is important for tuning the electrical conductivity in fluorinated graphene and can be achieved through optimizing the fluorination conditions including pressure, temperature, the species of fluorination agents and treatment time with fluorination agent [Adv. Sci. 2016, 3, 1500413].
  • the method according to the invention comprises a one side fluorination of the graphene coating with a surface saturation of 25 % to 50 %, preferably with a saturation of 25 %, more preferably one carbon atom per every two primitive graphene unit cells in the graphene coating surface is fluorinated.
  • said anti-icing coating comprises a one side fluorinated graphene coating with a saturation of 20% to 50%.
  • said anti-icing coating comprises a one side fluorinated graphene coating with a saturation of 25 % to 50 %, more preferably with a saturation of 25 %, most preferably one carbon atom per every two primitive graphene unit cells in the graphene coating surface is fluorinated. This yields proper anti-icing properties with little influence of the fluorination to the bulk as well as the sticking of the coating to the substrate.
  • the method comprises the step of producing an anti-icing coating on the surface of an aircraft, preferably on a wing or rotors and/or some other critical parts i.e. rudder, elevators, stabilizers, propeller, swatch plates etc. of the aircraft.
  • said substrate of the arrangement is an aircraft, preferably a wing or rotors and/or some other critical parts i.e. rudder, elevators, stabilizers, propeller, swatch plates etc. of an aircraft. In that case de-icing during flight or prior to take-off can be avoided.
  • the method according to invention comprises the step of producing an anti-icing coating on a optically transparent surface, a lens or a window, preferably on an sapphire substrate, lens or window. It is in the same way to be preferred, if said substrate of said arrangement is a window, preferably a sapphire window.
  • Fig. 1 a schematically view of an icing protected arrangement according to the invention
  • Fig. 2 a number of images with a cross-sectional view of water droplets resting on different arrangements, and at different temperatures,
  • Fig. 3 a table (Tab. 1), representing the onset of freezing and the delay of freezing for the water droplets resting on the different arrangements from Fig. 2,
  • Fig. 4 a diagram showing the variation of the static contact angle as a function of the arrangement surface temperature, by applying water droplets on different arrangements
  • Fig. 5 a diagram showing the contact angle hysteresis data, in accordance to Fig. 4, and
  • Fig. 6 a schematically view similar to Fig. 1 of another embodiment of an icing protected arrangement according to the invention.
  • Fig. 1 shows a schematically view of an icing protected arrangement 10 according to the invention.
  • the icing protected arrangement 10 comprises a substrate 1 1 covered by a coating 12.
  • An intermediate layer 13 is arranged between the substrate 1 1 and the coating 12.
  • the substrate 1 1 is a window 1 1 , in detail it is a sapphire window 1 1.
  • the intermediate layer 13 of the embodiment is a ruthenium layer 13.
  • the intermediate layer 13 can be made of other material as for example graphene. It can be omitted as well.
  • the coating 12 of the shown embodiment is an anti-icing coating 12, comprising a graphene layer 14 adjacent to the intermediate layer 13 and opposite to the substrate.
  • the anti-icing coating 12 comprises several layers graphene as graphene layer 14. A monolayer of graphene or more than one layer of graphene can be intended.
  • the graphene layer 14 is fluorinated, thus forming a fluorinated graphene CxF layer 15.
  • the shown anti-icing coating 12 is hydrophobic.
  • the anti-icing coating 12 has icephobic properties.
  • Fig. 2 shows a number of images with a cross-sectional view of water droplets, resting on different substrates, and at different temperatures.
  • the substrates are sapphire samples.
  • the sapphire samples are designed as sapphire windows.
  • twelve images are shown, grouped into four lines and three columns: The first line shows water droplets, resting on sapphire windows without any surface treatment; the second line shows water droplets, resting on sapphire windows providing a graphene coating; and the third and fourth line shows water droplets, resting on sapphire windows providing a fluorinated graphene coating, with two different fluorine contents.
  • the third line shows a sapphire window providing a graphene coating, which is fluorinated for 30 seconds and the fourth line shows a sapphire window providing a graphene coating, which is fluorinated for 1200 seconds.
  • the left, middle and right columns represent the water droplets resting on the sapphire windows at room temperature (left), at a temperature where freezing begins (middle) and at a temperature after freezing (right), respectively.
  • Fig. 3 shows Tab. 1 , representing the onset of freezing and the delay of freezing for water droplets resting on different substrates.
  • these substrates represent sapphire windows without any surface treatment or with varying coating.
  • the onset of freezing was identified as a change in the optical appearance of the droplet.
  • the onset of freezing was shifted towards lower temperatures for water droplets, resting on sapphire windows providing a graphene coating.
  • the onset of freezing was lowered further for water droplets, resting on sapphire windows providing a fluorinated graphene layer.
  • the displayed water droplets have a volume of 4 ⁇ _, each.
  • Fig. 4 shows the variation of the static contact angle as a function of the substrate surface temperature, by applying water droplets on different substrates.
  • the substrates used for this study are designed as sapphire windows.
  • the sapphire windows are provided (1) without any surface treatment, (2) with a graphene coating and (3) with a fluorinated graphene coating. Measurements were done in ambient air with about 50 % relative humidity at 23° C.
  • the used water droplets have a volume of 4 ⁇ _, each.
  • Static contact angles measurements were done by placing the sapphire windows on a cooling stage. Water droplets were dispensed on the surface of the sapphire window. Afterwards, the temperature was lowered from room temperature to the desired low temperature. All low temperature measurements were performed in dry nitrogen (N2) atmosphere to avoid water condensation at temperatures below zero degrees.
  • N2 dry nitrogen
  • ACA Advancing
  • RCA receding
  • Fig. 5 shows contact angle hysteresis data, in accordance to Fig. 4.
  • the contact angle hysteresis data were calculated as difference between advancing and receding contact angles at corresponding tilting angles of sample.
  • a 4 ⁇ _ water droplet was deposited at the surface of the substrate, which is designed as sapphire windows, at 0° tilt. Measurements were done in ambient air with about 50 % relative humidity at 23° C.
  • the hysteresis was observed to reduce for water droplets, resting on sapphire windows providing a graphene coating.
  • the hysteresis was observed to reduce further for water droplets, resting on sapphire windows providing a fluorinated graphene layer.
  • Graphene is produced using various methods such as mechanical cleavage, epitaxial growth, chemical vapor deposition (CVD), carbon nanotube slicing and intercalation of graphite.
  • Fluorination is the process in which a Fluoride ion bonds to a sp2 orbital of graphene that is only bonded to one carbon atom of the graphene substrate. Bond character can vary from ionic to semi-ionic to covalent. It is different from the approach in which graphene sheet/ribbons are functionalized with fluorocarbon alkyl chains. Usually, in this case, alkyl chains covalently bond to the edges only. However, in case of fluorination, fluoride ions are distributed over the whole sheet and the functionalisation consists of fluor only without any alkyl or other chain.
  • Graphene coated sapphire windows were fluorinated using the Xactix® XeF2 etching system.
  • the XeF2 gas exposure times were 30 seconds and 1200 seconds, using a temperature of approximately 30° C.
  • the XeF2 treatment is shown to fluorinate graphene without etching.
  • the fluorine content was observed (Nano Lett. 2010, 10, 3001-3005) to saturate at 25 % coverage or C 4 F, which corresponds to one atom per every two primitive graphene unit cells in graphene.
  • Fluorination of graphene can be achieved through number of techniques including exposure to fluorine gas (F2) at high temperatures and F-based plasma. Exfoliation of graphite fluoride has also been used to get fluorinated graphene sheets.
  • Sapphire windows were characterized using a DataPhysics OCA 20 instrument (DataPhysics GmbH, Germany). The system is equipped with a high speed CCD camera, a computer programmable droplet-dispensing unit, a Peltier cooling stage and an electronic tilt table. The electronic tilt table can tilt the sample stage up to 90°. Data were analyzed utilizing the SCA 20 software.
  • Graphene was deposited through chemical vapor deposition (CVD) method on sapphire windows.
  • the sapphire windows used for the examples of Fig. 1 to 5 have an Ru(0001) intermediate layer 13.
  • Ru(0001) was deposited followed by graphene via CVD. It is also possible to place the graphene directly on the substrates or to use an intermediate layer which can be removed after deposition.
  • Fig. 6 shows a schematically view similar to Fig. 1 of another embodiment of an icing protected arrangement 16 according to the invention.
  • the icing protected arrangement 16 is similar to the icing protected arrangement 10. Similar elements have the same reference numerals.
  • the icing protected arrangement 16 does not comprise the intermediate layer 13.
  • An anti-icing coating 17 similar to the anti-icing coating 12 is directly arranged on the substrate.
  • the graphene layer 14 is directly attached to the substrate 11 with the fluorinated graphene layer 15 on top.
  • Direct gas fluorination such as F2 and XeF2
  • plasma fluorination such as SF6, CF 4 , Ar/F 2
  • hydrothermal and photochemical synthesis
  • Graphene is grown directly on the surfaces using CVD method or with an intermediate metal layer (metals such as Cu, Ni, Fe, Pt, Ru, Ir, Co, Au, oxides such as CuO x , SiO x , CoyOx, AlyOx, composite materials).
  • the intermediate layer may be removed prior to fluorination step.
  • Xactix® XeF2 etching system was used for fluorination. Other methods as described above could also be employed.
  • An intermediate adhesion layer may also be used to ensure good adhesion of coating to the target surface.
  • Exfoliated fluorinated graphene micro/nano sheets can be deposited to target surface using methods such as dip coating, spin coating, spray coating, spray drying, layer-by layer self-assembly.
  • An intermediate adhesion layer may also be used to ensure good adhesion of coating to the target surface.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Materials Applied To Surfaces To Minimize Adherence Of Mist Or Water (AREA)
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Abstract

L'invention concerne un agencement protégé contre le givrage (10) comprenant un substrat (11) couvert d'un revêtement antigivrage (12)capable d'au moins réduire les besoins en termes de moyens de dégivrage supplémentaires comme le chauffage ou la pulvérisation de solutions de dégivrage, ledit revêtement antigivrage (12) comprenant une couche de graphène fluoré (15).
PCT/NO2018/050249 2017-10-20 2018-10-19 Procédé de fabrication d'un agencement protégé contre le givrage et agencement protégé contre le givrage Ceased WO2019078729A2 (fr)

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NO20171683 2017-10-20
NO20171683 2017-10-20

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WO2019078729A2 true WO2019078729A2 (fr) 2019-04-25
WO2019078729A3 WO2019078729A3 (fr) 2019-05-31

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Cited By (4)

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CN114104299A (zh) * 2021-11-26 2022-03-01 中国人民解放军空军工程大学 超疏水涂层等离子体与石墨烯电热复合防除冰装置及方法
CN114152365A (zh) * 2022-02-07 2022-03-08 中国空气动力研究与发展中心低速空气动力研究所 一种临界防冰保护的光纤结冰传感器、系统和方法
CN116179218A (zh) * 2022-12-15 2023-05-30 东北农业大学 一种防冰除冰皮克林乳液及其制备与应用方法
WO2024105038A1 (fr) 2022-11-15 2024-05-23 Paragraf Limited Méthodes de formation de graphène sur un substrat

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US9028969B2 (en) * 2010-07-27 2015-05-12 United Technologies Corporation Composite article having protective coating
US10850496B2 (en) * 2016-02-09 2020-12-01 Global Graphene Group, Inc. Chemical-free production of graphene-reinforced inorganic matrix composites

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114104299A (zh) * 2021-11-26 2022-03-01 中国人民解放军空军工程大学 超疏水涂层等离子体与石墨烯电热复合防除冰装置及方法
CN114104299B (zh) * 2021-11-26 2024-03-12 中国人民解放军空军工程大学 超疏水涂层等离子体与石墨烯电热复合防除冰装置及方法
CN114152365A (zh) * 2022-02-07 2022-03-08 中国空气动力研究与发展中心低速空气动力研究所 一种临界防冰保护的光纤结冰传感器、系统和方法
CN114152365B (zh) * 2022-02-07 2022-04-12 中国空气动力研究与发展中心低速空气动力研究所 一种临界防冰保护的光纤结冰传感器、系统和方法
WO2024105038A1 (fr) 2022-11-15 2024-05-23 Paragraf Limited Méthodes de formation de graphène sur un substrat
CN116179218A (zh) * 2022-12-15 2023-05-30 东北农业大学 一种防冰除冰皮克林乳液及其制备与应用方法

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