EP3200931B1 - Composite formé d'un substrat, d'une couche plasma polymère, d'une couche mixte et d'une couche de couverture - Google Patents

Composite formé d'un substrat, d'une couche plasma polymère, d'une couche mixte et d'une couche de couverture Download PDF

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Publication number
EP3200931B1
EP3200931B1 EP15775176.9A EP15775176A EP3200931B1 EP 3200931 B1 EP3200931 B1 EP 3200931B1 EP 15775176 A EP15775176 A EP 15775176A EP 3200931 B1 EP3200931 B1 EP 3200931B1
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EP
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Prior art keywords
layer
plasma
substrate
cover layer
plasma polymer
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German (de)
English (en)
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EP3200931A1 (fr
Inventor
Ralph Wilken
Thomas WÜBBEN
Jost Degenhardt
Jörg IHDE
Kira ROSANOVA
Uwe Lommatzsch
Christoph Regula
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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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
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/50—Multilayers
    • B05D7/56—Three layers or more
    • 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
    • B05D2451/00—Type of carrier, type of coating (Multilayers)
    • 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
    • B05D2490/00—Intermixed layers
    • B05D2490/50—Intermixed layers compositions varying with a gradient perpendicular to the surface

Definitions

  • the present invention relates to a composite of a substrate, a plasma polymeric layer, a cover layer and a mixed layer arranged between the cover layer and the plasma polymeric layer. It also relates to the use of a plasma polymer layer and a mixed layer to improve adhesion between a substrate and a cover layer, and to a method for producing a corresponding mixed layer.
  • Coated objects are used in many technical areas.
  • the coatings have the function of imparting certain properties to a substrate. These can be optical or anti-corrosion properties, e.g. in the case of paints, or dirt-repellent, adhesion-reducing properties such as a PTFE coating, or adhesion-promoting properties as required when applying adhesives and paints.
  • a critical point is to ensure sufficient adhesion to the substrate or between the individual layers.
  • solvent-based adhesion promoters are often used, also in the form of adhesion-promoting layers. These layers are intended to prepare a substrate that is not suitable for the subsequent coating in such a way that adequate, long-term and media-stable adhesion is ensured.
  • Plasma processes are also known in which good adhesive properties of the material surfaces are generated without the deposition of adhesion-promoting layers (e.g DE4325377C1 ) and other documents on certain pre-treatments, e.g EP0761415B9 , DE4407478A1 .
  • adhesion-promoting layers e.g DE4325377C1
  • other documents on certain pre-treatments e.g EP0761415B9 , DE4407478A1 .
  • This is particularly interesting for materials that have poor adhesive properties: polyolefins (PP, PE), fluoro-organic polymers (PTFE, ETFE, PVDF), silicones, etc.
  • Plasma polymer coatings are also known that have an adhesion-promoting effect (e.g WO2004035857A2 , JP6200217 ). These layers have good adhesive properties on the one hand to the substrate and on the other hand to subsequently applied adhesives, paints or sealants.
  • WO 02/05972 A2 discloses a method for producing a permanent release layer by plasma polymerisation on the surface of a molding tool, with a gradient layer structure being produced in the release layer by varying the polymerisation conditions over time.
  • EP 1 852 522 A1 discloses a film evaporated on a base material surface formed by a plasma CVD method using an organic metal compound and an oxidizing gas as a reactive gas.
  • the evaporated film has three sections: an adhesive layer on the base material side containing 5% or more carbon, a barrier interlayer containing less than 5% carbon, and a surface protective film containing 5% or more carbon by element concentration in terms of the total amount of one Metal element (M), oxygen (O) and carbon (C) derived from the organic metal compound.
  • M Metal element
  • O oxygen
  • C carbon
  • this object is achieved by a composite comprising a substrate and arranged on the substrate a plasma polymer layer and a cover layer as defined in the claims, wherein between the cover layer and the plasma polymer layer there is a mixed layer which, in terms of its material composition, has a gradient of the composition of the plasma polymeric layer to the composition of the cover layer.
  • the adhesion promotion between the substrate and the top layer by means of a plasma polymer layer works particularly well if the layer deposited from a precursor by a plasma process is on its surface at the time the top layer is applied not yet reached the plasma polymer state Has.
  • suitable deposition conditions cf. also below
  • a plasma-oligomeric state within the meaning of this text is present if a drop of water applied to the layer reduces the thickness of the (plasma polymers/plasma oligomers) layer applied by means of PECVD (plasma enhanced chemical vapor deposition) by ⁇ 2 nanometers within ten minutes.
  • PECVD plasma enhanced chemical vapor deposition
  • this test is done at room temperature and with deionized water.
  • the change in layer thickness is measured by means of reflectometry or preferably ellipsometry. From the point in time at which a layer is removed by ⁇ 2 nanometers per ten minutes under the aforementioned conditions, the (plasma polymer) coating is no longer considered a plasma oligomer, but a finished plasma polymer.
  • the coating according to the invention (or composite according to the invention) is only successful if the time between application of the coating using plasma coating processes (atmospheric pressure plasma is preferred here) and the subsequent application of the cover layer material is so short that there is still a plasma oligomer on the surface of the later plasma polymeric layer applied by means of PECVD present.
  • This makes it possible for the plasma oligomer to mix with the material for the top layer.
  • This results in a mixed layer of material from the top layer and material that would have become part of the plasma polymer layer if the top layer had been delayed for too long.
  • the mixed layer is formed from parts of the plasma polymer layer (plasma oligomers) that has not yet completely formed and parts of the cover layer material. It is also possible - and often desirable - for the plasma oligomers to react with the components of the top layer in the mixed layer.
  • a mixed layer in the sense of the present text always consists of a mixture of the upper components of a previously deposited plasma polymeric layer and the components of the cover layer deposited or applied directly thereon.
  • the mixed layer is a transition zone that is formed from components still present in the plasma-oligomeric state on the surface of the deposited plasma-polymeric layer and components of the top layer applied subsequently.
  • a separate layer application/layer deposition process is therefore not used to produce the mixed layer/transition zone, and the parameters of a deposition process are also not varied for the formation of this layer, in order to produce a gradient layer, for example.
  • a mixed layer in the sense of this invention is thus created by mixing plasma oligomeric components on the surface of the plasma polymeric layer with components of the subsequently applied top layer during the application of the components or the precursor components of the top layer.
  • Cover layers which are applied in the liquid state or gaseous state are of course particularly suitable here, with the liquid state being according to the invention.
  • the boundary between the plasma polymer layer and the mixed layer is determined by means of TEM on lamellar sections across the composite. The same also applies to the boundary between the mixed layer and the top layer.
  • the limit should be set at the point at which at least one component of the plasma polymer layer or the top layer deviates by ⁇ 5 atom % measured by TEM.
  • the course of the concentration of the individual elements in the mixed layer will change from the concentration in the plasma polymer layer in each case within the framework of a gradient to the concentration of the cover layer. This change will regularly result in a constant increase or decrease in the respective element content.
  • the boundary layer between cover layer and transition layer or plasma-polymeric layer and transitional layer begins where a chemical element is present for the first time that is not present in the plasma-polymeric layer or the cover layer.
  • the person skilled in the art determines the concentration curves of the individual elements in a meaningful way: It is possible, for example, for the top layer to be a dispersion layer, in particular a suspension layer or an emulsion layer. This can mean that there are also two phases in the mixed layer. Of course, when determining the concentration, the person skilled in the art will take into account the typical droplet size of the corresponding phases or also particle sizes. He can do this by choosing a sufficient slice width for the TEM determination so that any inhomogeneities that may be caused by the top layer in the mixed layer are statistically averaged out. It is preferred here that the person skilled in the material composition considers a TEM section with a width of at least five times the size of the material inhomogeneities caused by the cover layer.
  • the “size of the material inhomogeneities” means the longest diameter of the respective inhomogeneity, determined by means of transmission electron microscopy.
  • the lamella section In preferred methods of determination, those skilled in the art will consider the lamella section to be ⁇ 6 microns wide. This width relates to the x-axis of the TEM observation volume, while the y-axis is perpendicular to the substrate surface and the distance along the y-axis must of course be long enough to use the composition of the plasma polymer layer and the top layer as the respective reference layers to determine.
  • the x-axis in this image corresponds to the penetration depth of the selected TEM measurement method and is preferably 100 nanometers.
  • the inventors of the present invention have surprisingly found that it is possible to specifically control the deposition of plasma oligomers. By means of this control, it is possible to achieve very good adhesion promotion via the mixed layer to be used according to the invention.
  • a gas phase deposition is used, such as can be used for coating semi-finished products made of different materials.
  • the deposited coating has a high chemical reactivity immediately after deposition, if the deposition conditions are chosen appropriately, and is not yet fully crosslinked (plasma oligomer).
  • oligomeric components are extracted from the layer or oligomeric components of the layer are extracted in water or possibly another Solvent dissolved. In extreme cases, the layer can even be completely removed from the substrate.
  • the person skilled in the art applies the covering layer in good time so that a plasma oligomer is still present.
  • this can be determined with a drop test, which means that a plasma oligomer is present in the sense of this text as long as a drop of water removes a layer thickness of two nanometers from the layer within ten minutes when it is wetted.
  • the top layer is also important for the formation of the composite according to the invention: the top layer must be applied in a state that allows the top layer material to be mixed with the plasma oligomers to form the mixed layer.
  • the covering layer is deposited in liquid form (according to the invention) and/or as a gas phase deposition (not according to the invention).
  • the material for the top layer is preferably solvent-based, with at least part of the solvent being particularly preferably water.
  • Polyurethane skins can be used, but in some cases it may be preferred that the skin in the composite of the invention is not polyurethane.
  • the adhesion-promoting area used consisting of a plasma polymer layer and a mixed layer, can be used for economic surface functionalization, with both a flat and a local treatment of the surface to be coated being possible. They can be used as a substitute for solvent-based adhesion promoters and/or primer layers.
  • the cover layer is a polymeric layer.
  • a polymeric layer is a layer formed from typical polymers as the main component. Of course, such layers can also contain other components, such as particles or fillers.
  • a composite according to the invention is preferred in which the mixed layer has a thickness of 2-1200 nm, preferably 20-500 nm, particularly preferably 50-200 nm.
  • a composite according to the invention is also preferred within the meaning of the invention, in which case the substrate contains metal or consists of metal.
  • the plasma polymer layer to be used according to the invention consists of Si, C, O, N, H and/or F.
  • Plasma polymer layers of these elements can be deposited particularly well by means of a process that also promotes the formation of plasma oligomers in the context of the above invention.
  • the atomic percentages are based on the atoms that can be measured using XPS (H is not taken into account). In order to ensure reproducibility, the measurement using XPS is only carried out when there are no longer any plasma oligomers. In case of doubt, this means that a drop of water no longer causes a thinning of the layer within ten minutes if it has been applied to the plasma polymer layer.
  • Layers of the compositions mentioned result in particularly good adhesion promotion and particularly good plasma oligomer formation (during the deposition) for the composites according to the invention.
  • Also part of the invention is the use of a plasma polymeric layer formed from plasma oligomers as described above and an intermediate layer as described above to improve adhesion between a substrate and a cover layer.
  • a plasma-oligomeric layer is a layer deposited by means of PECVD which has not yet fully reacted and in which a drop of water (or another solvent) removes a layer thickness of ⁇ 2 nm within ten minutes.
  • Also part of the invention is a composite comprising a mixed layer produced or producible by a method according to the invention.
  • this mixed layer is the decisive factor in the composite according to the invention, since the use of this layer enables particularly good adhesion promotion through the plasma polymer layer.
  • Example according to the invention To create the example according to the invention, a polished aluminum substrate AA1050 with a thickness of 1 mm was treated as follows: Step 1: Plasma cleaning and activation
  • a plasma system using a transformer HGR12 (manufacturer: Plasmatreat) and a generator FG5001 (manufacturer: Plasmatreat) was used.
  • the substrate temperature was room temperature (23°C) at the beginning of the treatment and was kept at ⁇ 40°C during the plasma cleaning and activation.
  • the frequency set on the generator was 19 kHz.
  • the plasma cycle time (PCT) to be set on the generator was 100%.
  • a voltage of 280 V was set on the generator.
  • the resulting current depends on the parameters mentioned.
  • the nozzle used consisted of PT21836 and PT21837 (Part numbers, manufacturer Plasmatreat also referred to as PAD-10 in offers). This is the one in the DE 10 2006 038 780 A1 described nozzle.
  • step 1 the distance between the nozzle and the substrate was 6 mm, the nozzle was scanned in parallel lines and with a line spacing of 4 mm over the substrate at a speed of 20 m/min. Only 1 cycle was carried out, i.e. the entire surface was only swept over once with the nozzle in the manner described above.
  • the process gas used was compressed air with a process gas flow of 29 l/min.
  • Step 2 Deposition of the plasma oligomer
  • the substrate pretreated from step 1 was placed in a coating system that contained a transformer HGR12 (manufacturer: Plasmatreat) and a generator FG5001 (manufacturer: Plasmatreat).
  • the nozzle used was the nozzle described in step 1.
  • the substrate temperature at the beginning of the coating process was room temperature (23°C). Care was taken during the coating that the substrate temperature did not exceed 50°C. All temperature measurements (as in step 1) were carried out using an IR thermometer.
  • the system was operated at a frequency of 19 kHz, a plasma cycle time (PCT) of 100% and at a voltage of 280 V. The amperage resulted from the settings of the system.
  • PCT plasma cycle time
  • the nozzle was guided over the substrate at a distance of 6 mm from the substrate in parallel lines with a line spacing of 4 mm and at a speed of 30 m/min. 1 coating cycle was carried out, the process gas was compressed air, the precursor used was HMDSO. The precursor was fed in at the nozzle head in the area of the relaxing plasma after preheating to 110° C. (gaseous) with a precursor flow rate of 24 g/h.
  • the carrier gas was nitrogen with a gas flow of 2 l/min.
  • the process gas flow compressed air see above was 29 l/min.
  • the layer thickness (including the plasma oligomer) is 150 nm +/- 15 nm
  • Step 3 Applying the top coats
  • the above aluminum substrate was treated as follows: A Teflon system as in the application was used as the top coating WO 2013/030503A1 applied as described in the examples for the mixture CP1 and as a finish mixture the mixture CF1. The application took place 30 seconds after step 2.
  • Example not according to the invention Step 1 as in example 1, but plasma generator FG3001 and process gas 10 l/min: The nozzle does not ignite, no usable plasma was created.
  • Measurement parameters The XPS investigations were carried out using a Thermo K-Alpha K1102 system with an upstream argon glove box for handling air-sensitive samples. Parameters: acceptance angle of the photoelectrons 0°, monochromatized Al K ⁇ excitation, constant analyzer energy mode (CAE) with 150 eV pass energy in overview spectra and 40 eV in energetically high-resolution line spectra, analysis area: 0.40 mm diameter. Electronically non-conductive samples are neutralized by a combination of low-energy electrons and low-energy argon ions. An argon ion sputtering source can be used for removal.
  • CAE constant analyzer energy mode
  • Example 7 The layer from Example 7 was coated with a drop of water as described in Example 7 after the following standing times after deposition. This resulted in the following static water contact angles, measured with the MobileDrop GH11 system from Krüss and according to the instructions for this device. time water edge angle 20 seconds 4° 30 seconds 26.6 degrees 2 mins 53.3 degrees 5 mins 65.6 degrees 20 min. 67.5 degrees
  • the water contact angle of the coating rose to 85.5°.
  • the contact angle measurements were carried out using the MobileDrop GH11 system from Krüss.
  • Example 10 Compositions by means of infrared spectra
  • the IR spectra were recorded using the Vertex 80 device (manufacturer: Bruker) at an angle of 45° and with an aperture of 0.5 mm.
  • the layer composition was determined via an IR spectrum immediately after deposition, after treatment with a drop of water according to Example 7a.) and in both cases after storage under standard conditions for 30 minutes in each case.

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Laminated Bodies (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
  • Chemical Vapour Deposition (AREA)

Claims (9)

  1. Composite, comprenant un substrat et agencées sur le substrat une couche plasma polymère et une couche de recouvrement, dans lequel une couche mixte est présente entre la couche de recouvrement et la couche plasma polymère, laquelle présente en ce qui concerne sa composition de matériau un gradient de la composition de la couche plasma polymère jusqu'à la composition de la couche de recouvrement, dans lequel la couche de recouvrement est une couche polymère, caractérisé en ce que la couche de recouvrement est une couche de recouvrement déposée sous la forme liquide.
  2. Composite selon la revendication 1, dans lequel le matériau pour la couche de recouvrement contient du solvant.
  3. Composite selon l'une quelconque des revendications précédentes, dans lequel la couche polymère est un vernis, un revêtement anti-adhérent, une colle, une masse de scellement ou une masse d'étanchéité.
  4. Composite selon l'une quelconque des revendications précédentes, dans lequel la couche mixte possède une épaisseur de 2 - 1 200 nm, de préférence de 20 - 500 nm, de manière particulièrement préférée de 50 - 200 nm.
  5. Composite selon l'une quelconque des revendications précédentes, dans lequel le substrat contient du métal ou se compose de métal.
  6. Composite selon l'une quelconque des revendications précédentes, dans lequel la couche plasma polymère se compose de Si, C, O, N, H et/ou F.
  7. Composite selon l'une quelconque des revendications précédentes ; dans lequel la couche plasma polymère contient
    C : 5 - 45 %at, de manière particulièrement préférée 10 - 25 %at
    O : 30 - 65 %at, de manière particulièrement préférée 50 - 60 %at
    Si : 20 - 35 %at, de manière particulièrement préférée 24 - 30 %at mesuré par XPS.
  8. Utilisation de la couche plasma polymère et de la couche mixte telles que décrites dans l'une des revendications précédentes pour l'amélioration de l'adhérence entre un susbtrat et une couche de recouvrement, dans laquelle la couche de recouvrement est une couche polymère, dans laquelle la couche de recouvrement est une couche de recouvrement déposée sous la forme liquide.
  9. Procédé pour la génération d'une couche mixte telle que définie dans l'une des revendications 1 à 8 comprenant les étapes :
    a) la fourniture d'un substrat,
    b) la séparation d'une couche plasma oligomère sur le substrat,
    c) l'application du matériau pour la couche de recouvrement sur la couche plasma oligomère, avant la réaction de la couche plasma oligomère pour former une couche plasma polymère,
    dans lequel la couche de recouvrement est une couche polymère, dans lequel la couche de recouvrement est une couche de recouvrement déposée sous la forme liquide.
EP15775176.9A 2014-10-01 2015-10-01 Composite formé d'un substrat, d'une couche plasma polymère, d'une couche mixte et d'une couche de couverture Active EP3200931B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102014219979.4A DE102014219979A1 (de) 2014-10-01 2014-10-01 Verbund aus Substrat, plasmapolymerer Schicht, Mischschicht und Deckschicht
PCT/EP2015/072741 WO2016050937A1 (fr) 2014-10-01 2015-10-01 Composite formé d'un substrat, d'une couche plasma polymère, d'une couche mixte et d'une couche de couverture

Publications (2)

Publication Number Publication Date
EP3200931A1 EP3200931A1 (fr) 2017-08-09
EP3200931B1 true EP3200931B1 (fr) 2022-08-24

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EP (1) EP3200931B1 (fr)
DE (1) DE102014219979A1 (fr)
ES (1) ES2927149T3 (fr)
WO (1) WO2016050937A1 (fr)

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DE102017130353A1 (de) 2017-12-18 2019-06-19 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Sol-Gel-basierte Haftvermittlungsschicht für PTFE-basierte Beschichtungen und Verfahren zur Herstellung derselben
DE102018131228A1 (de) 2018-12-06 2020-06-10 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung eingetragener Verein Kontaktstelle für einen elektrischen Kontakt

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EP3200931A1 (fr) 2017-08-09
WO2016050937A1 (fr) 2016-04-07
ES2927149T3 (es) 2022-11-02
DE102014219979A1 (de) 2016-04-07

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