WO2013072293A1 - Structure de surface nanométrique pour améliorer l'adhérence - Google Patents

Structure de surface nanométrique pour améliorer l'adhérence Download PDF

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Publication number
WO2013072293A1
WO2013072293A1 PCT/EP2012/072447 EP2012072447W WO2013072293A1 WO 2013072293 A1 WO2013072293 A1 WO 2013072293A1 EP 2012072447 W EP2012072447 W EP 2012072447W WO 2013072293 A1 WO2013072293 A1 WO 2013072293A1
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WO
WIPO (PCT)
Prior art keywords
layer
agglomerate
ali
substrate
nanostructured
Prior art date
Application number
PCT/EP2012/072447
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German (de)
English (en)
Inventor
Rudolf Emmerich
Matthias Graf
Helfried Urban
Rüdiger BRÄUNING
Klaus-Dieter Nauenburg
Ralf Dreher
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Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e. V.
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Publication of WO2013072293A1 publication Critical patent/WO2013072293A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/62—Plasma-deposition of organic layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/10—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an adhesive surface
    • 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
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/401—Oxides containing silicon
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/02—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain a matt or rough surface

Definitions

  • composite materials are required in which a first material component, e.g. a polymer component, with a second material component, e.g. Also, a polymer part or other substance such as ceramic, glass or metal, is connected, i. have a common interface. So far it has been e.g. usual that the applied material such. a polymer was melted onto a substrate only partially (partly by means of a primer) or glued to this substrate. An adhesive or primer was incorporated between the fabrics or the surface was modified such that the two members were joined by chemical bonds. An increase in the applied material such. a polymer was melted onto a substrate only partially (partly by means of a primer) or glued to this substrate. An adhesive or primer was incorporated between the fabrics or the surface was modified such that the two members were joined by chemical bonds. An increase in the applied material such. a polymer was melted onto a substrate only partially (partly by means of a primer) or glued to this substrate. An adhesive or primer was incorporated between the fabrics or the surface was
  • Adhesive strength was in some cases by a simple roughening of the surface and the associated increase in surface area. However, there are also substances that can be due to their chemical inertness very poorly or not stick together.
  • liquid material eg liquid polymer
  • adhesives to bond material components such as polymers to other components has a number of disadvantages, such as chemical surface pretreatment, limited dripping time, or environmental impact.
  • the gecko's paws which have a nanostructured and adhesion-promoting surface, enable the gecko to climb close to smooth walls.
  • the gecko's paws which have a nanostructured and adhesion-promoting surface, enable the gecko to climb close to smooth walls.
  • Lithography process done. It should be noted, however, that it is not possible with lithographic methods to apply the nanostructured layer directly to the substrate, so that further method steps would be necessary for this purpose. Also, no nano undercuts are possible.
  • a support material comprising a substrate on which optionally one or more layers may be applied
  • the spaced, upwardly at least partially widening agglomerates comprises, wherein the porous, column having agglomerate layer ALI due to the spaced agglomerates a mean column width ⁇ di> in the range of 3-500 nm , determined on a scanning electron micrograph in plan view, has.
  • the agglomerate layer ALI present on the carrier material thus consists predominantly of discrete agglomerates, which are spaced apart from their neighboring agglomerates, whereby three-dimensionally bent interspaces or
  • a liquid material such as e.g. a
  • Agglomerate ALI penetrate and thus fill the existing there columns or cavities.
  • By selecting an appropriate range for the middle Column width ⁇ di> penetrates a subsequently applied liquid material sufficiently in the gaps between the agglomerates and adheres after its solidification particularly well on the nanostructured layer system.
  • the agglomerates deposited on the surface of the carrier material via suitable process parameters widen at least in sections (ie have an increasing diameter at least in sections as the distance from the carrier material surface increases), an intensive interlocking between the nanostructure and a subsequently applied material occurs
  • the agglomerates show a high cohesive load-bearing capacity and are simultaneously stabilized by the resulting composite, in particular against side forces.
  • the three-dimensionally highly branched, fissured and nanoscale-porous agglomerate layer ALI has an extremely large surface, resulting in a good and deep at the same time
  • this porous, columnar agglomerate layer ALI is prepared by plasma assisted chemical vapor deposition (PECVD) (hereinafter also referred to as PECVD agglomerate layer ALI).
  • PECVD plasma assisted chemical vapor deposition
  • the porous, columnar agglomerate layer (preferably PECVD agglomerate layer) has ALI due to the spaced apart ones
  • the average column width ⁇ di> is in the range of 10-200 nm, more preferably in the range of 20-150 nm.
  • the column width di between two adjacent agglomerates corresponds to the shortest connecting line between their agglomerate edges in the SEM photograph. Averaged over many adjacent agglomerates, ⁇ di> is obtained.
  • a suitable magnification in order to carry out a corresponding optical evaluation and thus a determination of the mean column width.
  • Suitable e.g. a SEM image with 20,000 times
  • the term "agglomerate” is understood to mean a clustering of smaller particles into a solid composite.
  • the agglomerates are thus composed of smaller particles, which in turn may be composed of even smaller particles
  • the term fractal-like structure of the agglomerates produced here means "agglomerate” in the following, the largest possible individually recognizable structural unit.
  • Agglomerate layer ALI has a mean diameter ⁇ Di> in the range of 10-1000 nm, more preferably in the range of 50 to 600 nm, determined on a SEM image in plan view, on.
  • Hydrocarbons, alcoholates, acetylacetonates or alkyl compounds of suitable metals e.g., Ti, Zn, Sn, Ta, Si, etc.
  • suitable metals e.g., Ti, Zn, Sn, Ta, Si, etc.
  • siloxanes e.g.
  • HMDSO Hexamethylsisiloxane
  • silazanes metal carbonyls or comparable compounds
  • reactive gases such as oxygen
  • PECVD Hydrogen and / or nitrogen
  • inert gases such as argon, helium
  • the substrate may be e.g. may be a metal substrate, plastic substrate, ceramic substrate, glass substrate, carbon substrate, or a combination of these substrate materials.
  • the substrate may be e.g. may be a metal substrate, plastic substrate, ceramic substrate, glass substrate, carbon substrate, or a combination of these substrate materials.
  • the substrate may be a rigid plate or alternatively a flexible film.
  • the carrier material comprises a substrate and one or more substrate layers attached to the substrate, wherein the substrate layer SL1 in contact with the first agglomerate layer ALI is preferably likewise a PECVD-producible layer ("PECVD substrate layer")
  • PECVD substrate layer a PECVD-producible layer
  • this PECVD substrate layer SL1 is made up of agglomerates which can be detected in an SEM image, these agglomerates, unlike the first agglomerate layer ALI, are preferably predominantly in contact with each other, see above a substantially closed PECVD substrate layer SL1 is present, in which preferably ⁇ di> / ⁇ Di> ⁇ 0.01, more preferably ⁇ 0.001
  • the quantities ⁇ di> and ⁇ Di> have the same meaning with respect to this substrate layer SL1
  • the preparation is carried out
  • Such a closed substrate layer SLl preferably overlaps in time (eg at the same time) with the production of the first agglomerate
  • the first agglomerate layer ALI present on the carrier material has an average height ⁇ H> in the range of 50-1500 nm.
  • the mean height ⁇ H> is determined in the rupture edge image in the SEM or by an interferometer. Such a break edge image is shown in FIG.
  • the mechanical stability of the agglomerates can be further optimized. This in turn has an advantageous effect on the mechanical stability of a composite material which comprises the nanostructured layer according to the invention.
  • the ratio of ⁇ H> / ⁇ Di> is in the range of 0.5 to 5, more preferably in the range of 1.5 to 3.
  • Agglomerate be applied, which are also the agglomerates already described above or alternatively to other agglomerate or
  • Particle layers can act.
  • this additional layer (s) is preferably selected so that their surface energy is adapted to a subsequently applied polymer material, so as to ensure the best possible wetting.
  • the adaptation of the surface energy can, for example, by adaptation of the monomer in the production of the agglomerates; and / or treatment with a gas plasma.
  • Agglomerate layer ALI is only attached to one side of the carrier material.
  • the carrier material of the nanostructured layer system may have the first agglomerate layer ALI both on its front side and on its rear side.
  • Adhesion promoter plate or bonding agent film act when the nanostructured surface is to effect an adhesion mediation between polymers that are not accessible for a plasma coating.
  • Nanostructured layer system a substrate, an adhesive layer (preferably a temporary adhesive layer) and a functional layer.
  • the substrate may be rigid or flexible (e.g., in the form of a foil).
  • the functional layer may be, for example, a catastrophic layer (e.g.
  • the applied to the nanostructured layer system and adhering to this material may be a polymer, a metal or a
  • Metal alloy an inorganic material, an organic-inorganic
  • Hybrid material or a mixture thereof.
  • the polymer present on the nanostructured layer system may be a thermoplastic, a thermoset, an elastomer, or mixtures of these polymers.
  • Suitable polymers may be e.g. from a polyolefin, an epoxy resin, a fluoropolymer, a polyamide, a polyacrylate, polymethacrylate, polycarbonate, rubber, thermoplastic olefin (TPO), or mixtures of these polymers.
  • Procedural steps such as a sol-gel process is solidified or cured.
  • the material applied to the nanostructured layer system may also be substances or mixtures of substances with a specific functionality. Such materials may be applied to the nanostructured layer system alone or in combination with other materials (e.g., a matrix, particularly a polymer matrix in which the material is dissolved or dispersed). As possible substances or materials with specific functionality, for example, pharmaceutically or biochemically active substances or
  • Active ingredients Active ingredients, biological cells, chemical sensors, UV absorbers, self-healing polymers, by oxidation and / or hydrolysis polymerizable monomers, oils (which are preferably highly viscous) and / or lubricants, metal particles (preferably metal nanoparticles) are called.
  • oils which are preferably highly viscous
  • metal particles metal nanoparticles
  • these substances may optionally be dissolved or dispersed in a suitable matrix (e.g., a polymer matrix).
  • the cavities of the nanostructured layer system can be advantageously used to take up materials or substances such as those mentioned above and to temporarily or permanently deposit them.
  • biochemically active substances or substances or substance mixtures By means of an additionally deposited layer, these active substances can be released again over a definable period of time.
  • the Active substances can be dissolved or dispersed in a matrix material (eg a polymer).
  • UV absorbers for protection against weathering damage (especially scratch-resistant coatings on PC) - This is preferred
  • Scratch-resistant are sealed.
  • Such a barrier layer can be applied, for example, by PECVD.
  • Incorporation e.g. of self-healing polymers or of monomers which can be polymerized by oxidation or hydrolysis into the nanolayer for producing a self-healing surface. Subsequently, it is preferably sealed with a barrier layer (preferably via PECVD). In case of injury, the surface is closed by the embedded polymers / monomers by itself.
  • Nanostructure e.g. by adding appropriate starting compounds toward the end of the PECVD process, to produce catalysts (e.g., Pd catalyst membranes for fuel cells).
  • catalysts e.g., Pd catalyst membranes for fuel cells.
  • Tube / vascular systems e.g. of heat exchangers or coolers for transporting liquids to surfaces by capillary action / wetting.
  • nanostructured layer system as anti-fogging or
  • the present invention therefore relates to an antifogging coating which contains the nanostructured layer system or composite material according to the invention. Furthermore, the present invention relates to the use of the invention
  • nanostructured layer system or composite material for producing an antifogging coating is a nanostructured layer system or composite material for producing an antifogging coating.
  • the material applied to the nanostructured layer contacts at least a portion of the cavity surface formed by the gaps of the first agglomerate layer ALI and therefore at least partially fills in the interstices or cavities present between the spaced agglomerates. Moreover, since the agglomerates widen upwards over at least a certain agglomerate length, an effective entanglement between the polymer and the nanostructured layer system occurs (formation of undercuts). Preferably, at least 50%, more preferably at least 70%, even more preferably at least 90% or even nearly 100% of the cavity surface of the first agglomerate layer ALI present on the carrier material is in contact with the applied material.
  • the cavity surface is understood as meaning the surface of the adhesion-promoting agglomerate layer ALI which is provided by the three-dimensionally shaped cavities or gaps in this porous layer.
  • agglomerate layer ALI is used as an extremely effective primer layer between support material and a post-applied material such as e.g. a polymer, it is no longer necessary, an additional
  • the nanostructured composite does not have an adhesive layer between the substrate and the applied layer of material (e.g., polymer layer).
  • the composite material is free of adhesive.
  • the present invention relates to the use of the above-described nanostructured layer system as a bonding agent between a substrate or support material and a material subsequently applied to this nanostructured layer system.
  • Agglomerate layer ALI adhere particularly well to this substrate, can be made to the above statements.
  • the deposition of a first agglomerate layer ALI on the surface of the carrier material preferably takes place by means of a plasma-assisted chemical
  • the optional layers may be applied to the substrate by conventional coating methods known to those skilled in the art.
  • one or more of these optional layers may be applied by PECVD.
  • CVD Gas phase deposition
  • at least one reactive starting compound or monomer compound is in the gaseous state sufficient energy input (eg thermal energy or the energy of accelerated electrons as in the case of the PECVD method) with a
  • the deposition of the agglomerate layer ALI and the deposition of the substrate layer SL1 in contact therewith may be temporally overlapping (for example simultaneous), wherein preferably the optional substrate layer SL1 is also deposited by the plasma enhanced chemical vapor deposition.
  • the process parameters such as pressure, gas flow and the power of the plasma-assisted chemical vapor deposition PECVD are preferably selected such that, on the one hand, particle or agglomeration already takes place in the gas phase, while at the same time an optional substrate layer SL1, preferably a closed substrate layer SL1, is formed on the carrier material by the PECVD.
  • an optional substrate layer SL1 preferably a closed substrate layer SL1 is formed on the carrier material by the PECVD.
  • the plasma-assisted chemical vapor deposition may be continued until the agglomerates present on the optional substrate layer SL1 satisfy the conditions described above with respect to the agglomerate layer ALI.
  • PECVD Microwave System A microwave duo- lin plasma coating system with an active plasma area of 20 x 20 cm consisting of four plasma quartz tubes arranged in an array, a usable coating area of 18 x 18 cm, a lower gas shower underneath the quartz tubes and a space between the upper edge of the quartz tubes and the substrate surface of 95 mm supported over the quartz tubes.
  • a vacuum pumping station consisting of a Roots pump (pumping speed 250 m 3 / h) and a rotary vane pump (pumping speed 65 m 3 / h), which is connected via a DN63 flange of the plasma source, above the substrate to the recipient.
  • PECVD microwave systems are also useful in the present invention. If necessary, the parameters given above (gas flow, pressure, plasma power, etc.) must then be modified accordingly to realize the agglomerate layer ALI according to the invention on the carrier material.
  • the provision of the nanostructured layer system described above preferably takes place by means of plasma-assisted chemical vapor deposition
  • the liquid precursor of a polymer material can be, for example, organic starting compounds which must first be subjected to polymerization or crosslinking in order to form the polymer component of the composite material.
  • the solidification of the liquid polymer material or of the liquid precursor of a polymer material can be achieved, for example, by changing the temperature (eg cooling the
  • a further layer e.g. by PECVD, is applied to the nanostructured layer system whose
  • the process gas exclusively hexamethyldisiloxane (optionally argon), while for the production of an amphiphilic sample, the process gas additionally contained oxygen (and optionally argon).
  • the supply of the process gas was carried out via a lower feed line and a lower gas shower (below the plasma source). Alternatively or additionally, the supply of the process gas can also take place via an upper feed line and an upper gas shower (above the plasma source).
  • the distance between the lower gas shower / upper edge of the quartz tubes was 46 mm.
  • the diameter of the quartz tubes was 15 mm and the distance h from the upper edge of the quartz tubes / substrate surface was 95 mm.
  • the reaction chamber is connected to a vacuum pump.
  • Suction capacity / vacuum pump level 250 m 3 / h, connected by a DN63 suction pipe, whereby the following stated process pressure is realized.
  • Microwave power P 2 x 1, 5 kW cw
  • the ratio of ⁇ di> to ⁇ Di> is in the range of 0.05-1.5.
  • the contact angles to water, diiodomethane and paraffin oil were each 0 °.
  • Molten polypropylene was applied to the nanostructured amphiphilic layer system described above. Because the agglomerates are spaced apart, the polymer melt can be incorporated into the material provided thereby
  • Figures 6 and 7 show an SEM side view of a fracture edge of a material, wherein the liquid polypropylene (PP) on a inventive
  • Agglomerate was applied (substrate: glass) and penetrated into the gaps of this layer, which was then pulled on the solidified polypropylene so strong that an adhesion failure has just begun, as can be seen in the SEM images on the basis of threading.
  • Liability failure is here with appropriate deduction on a
  • Such a peel fracture pattern is characteristic of the nanostructured layer according to the invention if a polymer such as PP is melted into the layer and removed again after cooling. Even after the demolition or withdrawal of such a polymer layer still remains
  • Comparative Sample 1 whose SEM micrograph is shown in Figure 4, there is a "substantially dense" layer of polyorganosiloxane agglomerates Since the agglomerates deposited on the substrate are densely packed and in contact with each other, ⁇ di> and thus also the ratio ⁇ di> / ⁇ Di> ⁇ 0.
  • a chemically inactive polymer melt eg PP

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Laminated Bodies (AREA)

Abstract

La présente invention concerne un système de couches poreuses à structure nanométrique comprenant un support qui présente un substrat sur lequel une ou plusieurs couches peuvent être appliquées en option. Sur le support, au moins une première couche AL1 poreuse présentant des fentes et obtenue par séparation chimique en phase gazeuse assistée par plasma (PECVD), comprend des agglomérés écartés s'élargissant du moins partiellement vers le haut. La couche d'aggloméré PECVD poreuse AL1 présentant des fentes en raison des agglomérés écartés possède une largeur de fente moyenne <d1> dans la plage 3-500 nm, déterminée selon une micrographie électronique à balayage en vue de dessus.
PCT/EP2012/072447 2011-11-15 2012-11-13 Structure de surface nanométrique pour améliorer l'adhérence WO2013072293A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE201110086399 DE102011086399B4 (de) 2011-11-15 2011-11-15 Nanoskalige Oberflächenstruktur zur Verbesserung der Adhäsion sowie Verfahren zu deren Herstellung
DE102011086399.0 2011-11-15

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WO2017003791A1 (fr) * 2015-06-30 2017-01-05 3M Innovative Properties Company Revêtements discontinus et leurs procédés de formation
DE102018202438B4 (de) 2018-02-19 2022-11-10 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zum Verbinden eines Trägermaterials mit einem weiteren Material
DE102019200291A1 (de) * 2019-01-11 2020-07-16 Bos Gmbh & Co. Kg Haftvermittler für den Einbau eines Bauteils im Fahrzeugbau

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US20060121080A1 (en) * 2002-11-13 2006-06-08 Lye Whye K Medical devices having nanoporous layers and methods for making the same

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PEI-ZHI YANG ET AL: "Characterization of PECVD grown porous SiO2 thin films with potential application in an uncooled infrared detector", SEMICONDUCTOR SCIENCE AND TECHNOLOGY, IOP PUBLISHING LTD, GB, vol. 25, no. 4, 1 April 2010 (2010-04-01), pages 45017, XP020172899, ISSN: 0268-1242 *
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DE102011086399A8 (de) 2013-08-29

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