WO2021053072A1 - Substrat mit einem molydännitrid schichtsystem, sowie beschichtungsverfahren zur herstellung eines schichtsystems - Google Patents
Substrat mit einem molydännitrid schichtsystem, sowie beschichtungsverfahren zur herstellung eines schichtsystems Download PDFInfo
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- WO2021053072A1 WO2021053072A1 PCT/EP2020/075978 EP2020075978W WO2021053072A1 WO 2021053072 A1 WO2021053072 A1 WO 2021053072A1 EP 2020075978 W EP2020075978 W EP 2020075978W WO 2021053072 A1 WO2021053072 A1 WO 2021053072A1
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
- C23C28/046—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material with at least one amorphous inorganic material layer, e.g. DLC, a-C:H, a-C:Me, the layer being doped or not
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/0605—Carbon
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
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- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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- C23C28/044—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material coatings specially adapted for cutting tools or wear applications
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
- C23C28/048—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material with layers graded in composition or physical properties
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
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- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
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- C23C28/343—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one DLC or an amorphous carbon based layer, the layer being doped or not
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
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- C23C28/347—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with layers adapted for cutting tools or wear applications
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
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- C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
- C23C30/005—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process on hard metal substrates
Definitions
- the invention relates to a substrate with a multi-layer layer system designed as a surface coating, in particular on a surface of a wear part such as a tool or a machine part, as well as a method for producing a surface coating according to the preamble of the independent claim of the respective category.
- Substrates include tools or parts of machines, for example internal combustion engines, or in particular also tools for forming, cutting tools and other components, especially wear parts for machines in all possible embodiments.
- Typical substrate materials that are coated in practice include all types of steel, tool steels or hard metals, but also all possible other substrate materials, such as ceramics in particular.
- Steels with a low tempering temperature, around 200 ° C, such as ball bearing steels, are also particularly important in order to increase their performance for components such as motorized components. The reduction in friction and the compatibility with lubricants as well as adequate resistance at the operating temperature play a role here.
- nitridic layers for example CrN, or oxynitridic layers such as CrNO, or carbonitridic layers such as TiCN and various DLC layers are applied.
- ceramic cutting bodies for example based on cubic boron nitride, are preferably used for the hard machining of steels.
- the hard machining of steels are preferably used for the hard machining of steels.
- One class of layers concerns Al-containing base layers such as AITiN and AICrN, whereby additional elements can be added depending on the requirements.
- Typical compounds from this area are compounds of the form AITiXNCO, where X is, for example, Cr or another metal.
- cubic BN has the decisive disadvantage that it is extremely complicated to represent. This is primarily due to difficulties in the layer growth itself, but also to the high internal stresses in the layers.
- WO 2016/188632 A1 which refer to pure MoN layers.
- DLC layers amorphous (diamond-like) carbon layers
- the layers in particular the DLC layers with hardnesses of more than 30 GPa, often have strong internal compressive stresses, so that the layer thickness that can be used sensibly is significantly limited.
- the mechanical load is also limited, in particular on soft substrates that have a much lower hardness and modulus of elasticity than the corresponding coating.
- the functionality is only limited to the layer volume of the DLC layers.
- the mostly metallic adhesive layer e.g. Cr
- the object of the invention is therefore to provide an improved surface coating for a substrate, in particular for a wear part, such as a tool or a machine part or another, in particular mechanically, tribologically or thermally stressed wear part, which has the problems known from the prior art overcomes, and in particular has a tribologically positive effect, improved mechanical properties, especially, but not only, with regard to the hardness and internal compressive stresses and can also be used at elevated temperatures.
- Another object of the invention is to provide a method for producing such an improved coating, in particular which is suitable for coating in the temperature range from 100 to 300 ° C, in particular approx. 150-200 ° or around 200 ° C.
- the invention thus relates to a coating method for producing a layer system on a substrate, as well as a substrate with a multilayer layer system designed as a surface coating, which has an outer cover layer comprising amorphous carbon.
- the substrate coated according to the invention can in particular be a component of a component subject to wear and / or friction, in particular a component of a motor vehicle or an internal combustion engine, in particular a piston, or a piston ring, a valve, a valve disk, or another component of an internal combustion engine or a tool, such as a cutting tool, a molding tool, a cutting tool, or another tool subject to wear and / or friction or other component subject to wear.
- the present invention has shown that the above-described problems with the DLC layer systems known from the prior art can be avoided to a very large extent and a layer system according to the invention is used particularly advantageously in particular with the aforementioned parts and components.
- MoN support layers overcomes the disadvantages mentioned above, in particular also with the extremely hard tetrahedral amorphous carbon layers (ta-C layers), which are mostly in the hardness range above 30 GPa and moduli of elasticity, measured with the nano hardness , of over 300 GPa.
- ta-C layers extremely hard tetrahedral amorphous carbon layers
- the layer system according to the invention comprising at least one Mo a N x support layer and a hard amorphous carbon layer or also diamond-like carbon layer, which for the sake of simplicity are also referred to synonymously as a DLC layer for the sake of simplicity, e.g. a hydrogen-free aC cover layer or a ta -C-
- Cover layer or another type of layer made of amorphous carbon as a cover layer that closes off from the outside serves primarily, but not exclusively, to reduce wear and friction in connection with lubricants on components such as automotive components, tools or other heavily stressed components or wear parts of any kind
- the deposition takes place particularly preferably by means of methods known per se, such as by means of a PVD method, CVD method, PA-CVD method, sputtering method, preferably HIPMS sputtering method, in particular filtered or unfiltered arc coating process, or by means of a combination or hybrid process comprising one or more of the aforementioned coating processes.
- this layer structure compared to the prior art are, above all, the improved support effect, which increases it Total layer thickness enables and higher point loads are possible.
- a layer system according to the invention a significantly improved functionality in the event of layer wear or flaking due to the formation of Magneli phases due to oxidation at sufficient operating temperatures is guaranteed.
- molybdenum can form a large number of compounds or modifications, also called phases, with nitrogen, which can have different crystal structures and properties.
- phase mixtures of metallic molybdenum Mo plus Mo2N phases can arise.
- Mo 2 N phases arise, and with a further increase in nitrogen phase mixtures of Mo 2 N plus MoN can form.
- MoN emerges.
- overstoichiometric MoN with (N / Mo> 1) has also been reported.
- a MoN-based hard material layer which at least for the most part comprises the hexagonal phase of the molybdenum nitride d-MoN, the intensity ratio of the two peaks (ö - MoN 220) / (d - MoN 200)> 3, preferably> 10, particularly preferably> 30, is most suitable.
- the maximum nitrogen content of the MoN layers is up to 55 at%, depending on the phase composition.
- the layers always have MoN x phases except for a minority proportion of metallic molybdenum.
- the layers can consist of pure Mo 2 N phases consist, or be Mo2N / MoN phase mixtures, or consist of pure MoN. With regard to the composition, the MoN sub-layers can be designed in multiple layers.
- the first Mo a N x support layers according to the invention or the second Mo N y support layers, which are described in greater detail below, can be deposited in separate processes under the DLC cover layer that closes off to the outside. Or the layer according to the invention can also be deposited in one process.
- a d-MoN (delta - molybdenum nitride) can also be used, for example, for tribological applications in a layer system according to the invention under the cover layer made of amorphous carbon.
- MoN phases can also be advantageously suitable.
- the MoN support layers can also be multilayer systems, which consist of MoN in combination with other nitrides such. B. CrN, Cr 2 N or TiN can be produced. It is also possible to dop the MoN support layers with elements such as copper, oxygen or carbon. (The generalized designation MoN support layers in the context of this application means: MoN regardless of the nitrogen content and / or phase composition).
- metallic elements such as Al or other elements such as B and Si can also be used for modification.
- a preferred embodiment of a layer system according to the invention is the use of a support layer which at least for the most part comprises the hexagonal phase of the molybdenum nitride d-MoN and / or consists of pure molybdenum nitride d-MoN.
- a support layer which at least for the most part comprises the hexagonal phase of the molybdenum nitride d-MoN and / or consists of pure molybdenum nitride d-MoN.
- an intermediate layer under a MoN support layer in the direction of the substrates.
- This can be a CrN x layer, for example. It can also often make sense to deposit a metallic adhesive layer on the substrates, such as a Cr adhesive layer.
- the nitrogen content x of the first Mo a N x support layer is in the range of 30 at% ⁇ x ⁇ 53 at% and is particularly advantageously approx.
- the hardness of the first Mo a N x support layer, which is arranged closer to the cover layer of the system, is particularly preferably greater than the hardness of the second support layer, which is arranged closer to the substrate, as will be shown below with reference to the special exemplary embodiments according to FIG. 5a and 5b or by FIG. 6 will be explained in more detail.
- the first Mo a N x support layer and / or the second Mo b N y support layer contain a proportion of metallic Mo.
- the first Mo a N x support layer and / or the second Mo N y support layer can also consist of pure Mo 2 N phases and their phase mixtures ⁇ -Mo 2 N and g-Mo 2 N, and / or also of Mo 2 N / MoN phase mixtures and / or be composed of pure MoN phases, in particular of cubic MoN and / or hexagonal d-MoN phases or phase mixtures.
- the g-Mo 2 N and the pure hexagonal phase of the d-MoN are particularly preferred.
- the first Mo a N x support layer and / or the second Mo b N y support layer can additionally contain one or more elements from the group consisting of [Ag, Cr, Ti, Cu, Al, Si, B , O, C] and / or an element from the 4th, 5th or 6th group of the Periodic Table of the Elements.
- an adhesive layer can be provided, which is especially alloyed with one or more elements from the group consisting of [C, N, O].
- the adhesive layer can advantageously also contain one or more elements of the 4th, 5th or 6th group of the periodic table of the elements, in particular also one of the elements Cr, Ti, Cu, Al, or Mo include.
- a layer system according to the invention can additionally also comprise one or more intermediate layers under the support layer.
- the intermediate layer can in particular comprise, for example, single-phase metal nitrides, metal carbides and metal carbonitrides and / or phase mixtures of metal nitrides, metal carbides and metal carbonitrides, the intermediate layer specifically comprising a single-phase Cr 2 N or CrN layer or a phase mixture of CrN and Cr 2 N.
- the first Mo a N x support layer and / or the second Mo N y support layer and / or the intermediate layer and / or the adhesive layer can be designed in the form of a gradient layer in relation to the chemical composition or in relation to another physical or chemical property whereby, in particular, an adaptation between two different types of layers in the layer system can be carried out optimally through the gradient layer.
- a thickness d of the first Mo a N x support layer and / or the second Mo b N y support layer and / or the intermediate layer can be in the range of O.Odmhh ⁇ d ⁇ 50pm, preferably in the range of 0.03pm ⁇ d ⁇ 30miti, im Specifically in the range of 0.2miti ⁇ d ⁇ 25miti, or in the range of 0.3miti ⁇ d ⁇ 10miti.
- first Mo a N x or second Mo b N y support layers and / or by one or more adhesive layers and / or intermediate layers in a layer system according to the invention, among other things
- Layer properties such as stability, hardness, and above all temperature resistance, adaptation to impact loads or also ductility etc., depending on can be individually adapted or further improved according to application and substrate.
- compositions of the individual layers of the layer system under the top layer can be set in practice, for example, as follows.
- a certain layer composition can be achieved in which Coating chamber, the nitrogen partial pressure, the bias on the substrate, or, for example, the substrate temperature or another relevant parameter can be set in a suitable manner known per se to the person skilled in the art or varied according to a predeterminable scheme during the coating process.
- Layer composition or lead to the desired layer structure As a rough guideline, it can be assumed in special cases, for example, that with nitrogen partial pressures of up to approx. 0.4Pa and / or higher substrate bias voltages of up to 250V and more, the formation of phase mixtures of Mo + Mo 2 N in the layers tends to occur is favored. At nitrogen partial pressures up to for example, about 1 Pa, the formation of MO 2 N phases tends to be favored, while preferred at higher nitrogen partial pressures of approximately 2Pa up to about 2Pa and substrate bias voltages to about 150 V Mo 2 N + MoN phases are formed.
- phase mixtures can be detected in the deposited layer systems in a manner known per se, for example by means of X-ray diffraction and other methods known per se, and the element compositions with corresponding methods such as EDX, WDX, SIMS or other measurement and analysis methods well known to the person skilled in the art .
- the outer cover layer comprising the amorphous carbon of a layer system according to the invention is a known amorphous carbon layer of the aC type, an amorphous carbon layer of the aC type doped with an element X, a tetrahedral amorphous carbon layer of the ta-C type doped with an element X: X, an amorphous carbon layer of the aC: Me type doped with a metal, a tetrahedral amorphous carbon layer of the ta-C: Me type doped with a metal, an amorphous carbon layer of the aC: H: Me type doped with a metal and hydrogen or one with a metal and hydrogen doped tetrahedral amorphous carbon layer of the ta-C: H: Me type.
- the cover layer can of course comprise one or more of the aforementioned types of amorphous carbon layers.
- X is preferably an element from the group of elements consisting of [F, CI, B, N, O, Si] and Me, one or more elements from the 4th, 5th or 6th group of the Periodic Table of the Elements, and Me can furthermore also comprise Al or Cu, preferably one of the elements Mo, Cr, Ti, W, Al.
- the top layer of a layer system according to the invention can consist of two or more layer layers each comprising an amorphous carbon layer of type aC, or of type aC: X, or of type ta-C: X, or of type aC: Me, or of type ta- C: Me, or of type aC: H: Me, or of the type ta-C: H: Me.
- cover layer and / or a layer layer of the cover layer may comprise a gradient layer which is an amorphous carbon layer of the aC type, or of the aC: X type, or of the ta-C: X type, or of the aC: ME type , or of the type ta-C: Me, or of the type a-C: H: Me, or of the type ta-C: H: Me.
- Two different layers of layers can have a different sp 3 / sp 2 ratio, for example, depending on the requirements
- Temperature resistance etc. can be individually adapted depending on the application, substrate or other special boundary conditions.
- a thickness Dd of the top layer and / or a layer layer of the top layer is advantageously in the range of 0.05 pm ⁇ Dd ⁇ 50 pm, preferably in the range of 0.05 pm ⁇ Dd ⁇ 30 mhh, in particular in the range of
- 0.1 pm ⁇ Dd ⁇ 20miti or in the range of 0.5pm ⁇ Dd 10pm, preferably in the range of 1 pm ⁇ Dd ⁇ 5pm, particularly preferably the thickness Dd is approx.
- a total thickness of Gd of a layer system of the present invention is in a range of 0.1 pm ⁇ Gd ⁇ 100 pm, preferably in the range of 0.5 pm ⁇ Gd ⁇ 50 pm, in particular in the range of 1 pm ⁇ Gd ⁇ 10 pm, particularly preferably around 4 pm selected, with a ratio of the thickness Dd of the cover layer to the total thickness of the Gd of the entire layer system in the range of 1% ⁇ (Dd / Gd) ⁇ 1000%, preferably in the range of 10% ⁇ (Dd / Gd) ⁇ 500%, in particular in the range of
- a hardness Hd of the cover layer is in a range of 8GPa ⁇ Hd ⁇ 80GPa, in particular in the range of 10GPa ⁇ Hd ⁇ 70GPa, or in the range of 25GPa ⁇ Hd ⁇ 60GPa, and is particularly preferably about 50GPa.
- the hardness can be determined by nano-penetration, in particular according to ISO 14577.
- a chromium-based substructure can be provided as the adhesive layer on the substrate, the adhesive layer essentially consisting of chromium with a thickness of the chrome layer of approximately 0.1 ⁇ m.
- the chromium bonding layer is followed by a CrN intermediate layer, preferably in the form of a Cr 2 N + CrN phase mixture with a thickness of 0.5 ⁇ m.
- a support layer made of d-MoN with a thickness of approx. 2 ⁇ m is also provided on the intermediate layer.
- the entire layer system can, for example, with one per se known arc (ARC) coating processes can be deposited on the substrate.
- ARC se known arc
- a cover layer made of amorphous carbon, as already mentioned, of the aC, ta-C, aC: X, ta-C: X, aC: Me, ta-C: Me, aC: H, a-C: H type, is particularly advantageous : X, aC: H: Me and had a layer thickness in the range from at least 100 nm to 20 ⁇ m.
- the cover layer can be a single-layer monolayer, a multi-layer layer or a gradient layer. Different types of cover layers made of amorphous carbon, as they have already been explicitly mentioned and listed several times, can also be combined in one and the same cover layer.
- the multilayer cover layer or the cover layer in the form of a gradient layer can be implemented by changing the sp3 / sp2 content of CC bonds by changing process parameters or by combining different types, e.g. ta-C with ta-C: N.
- That layer of the layer system which is arranged immediately adjacent to the cover layer made of amorphous carbon is in practice in the vast majority of cases a MoN layer. So preferably a first Mo a N x support layer or a second Mo b N y support layer.
- the cover layer made of amorphous carbon is then deposited directly on the MoN layer with suitable parameters.
- MoN has a particularly positive effect under the top layer of amorphous carbon if it is very hard and has a high modulus of elasticity. The positive effect becomes particularly clear when hardening ta-C layers, ie with layers with moduli of elasticity above 300 GPa.
- aC: Me layers can also be provided in a particularly advantageous manner as a cover layer for a layer system according to the invention.
- These layers contain at least one metal as a doping element and have different property profiles compared to the aC and ta-C layers without a doping element, for example the electrical conductivity is greater. This can therefore be advantageous in certain applications. Since the lower layer contains at least Mo or also Cr, it can be advantageous in terms of the process to use Mo and / or Cr as Me.
- the hydrogen-free, amorphous layer is an a-C: X layer, where X is preferably an element from the group of elements consisting of [F,
- non-metallic elements can also be added as doping elements for layer optimization depending on the application.
- These non-metallic elements can be boron, silicon, fluorine, or others.
- Si leads to a reduction in stress and F to a change in the Wetting properties, in particular to a larger contact angle.
- the hydrogen-free, amorphous layer is designed as a multi-layer layer, the multi-layer layer structure comprising alternately arranged individual layers of a type A and a type B, the individual layers of type A consisting of aC or ta-C and the individual layers of type B are made from Me or from aC: Me.
- Mo can be used as Me, so that a multi-layer layer of the type aC / Mo or aC / aC: Mo, or ta-C / Mo or ta-C / aC: Mo or ta-C / ta- C: Mo or aC / ta-C: Mo is formed.
- the hydrogen-free, amorphous layer is designed as a multilayer layer, the multilayer layer structure comprising alternately arranged individual layers of a type A and a type B, the individual layers of type A being made up of aC or ta-C and the individual layers of type B from aC: X are.
- silicon can be used as X, for example.
- the addition of silicon also helps to minimize stress in the layers through the formation of the aC: Si structure.
- Additional arc evaporators can be used to deposit such layers, which evaporate the graphite cathodes alloyed with the X element, or other suitable PVD methods can also be used, for example sputter sources which sputter off the X element.
- the thickness of the individual layers of type A is preferably not more than 1000 nm and not less than 10 nm.
- the thickness of the individual layers of type B is also preferably not more than 1000 nm and not less than 10 nm. This embodiment is also particularly advantageous the possibility of combining greater layer thicknesses with a simultaneously optimized stress ratio within the same coating.
- the invention further relates to a coating method for producing a layer system of the invention on a substrate, the coating method being a PVD method, a CVD method, a PA-CVD method, a sputtering method, preferably a HIPMS sputtering method, in particular a filtered or unfiltered one Arc coating process, or a combination or hybrid process, which comprises at least one of the aforementioned coating processes.
- the coating of the entire layer system can be deposited on the substrate by means of the unfiltered or filtered arc evaporator.
- Substrate surface and / or a surface of the first Mo a N x support layer and / or a surface of the second Mo b N y support layer and / or the intermediate layer and / or the adhesive layer prior to coating by means of argon ions and / or hydrogen ion cleaning using an AEGD (Are Enhanced Glow Discharge) technology are treated, wherein in a subsequent step an ion treatment can preferably also be carried out, for example with Cr ions or Mo ions.
- the first Mo a N x support layer and / or the second Mo b N y support layer and the Cover layer made of amorphous carbon in a PVD system by means of a coating process according to the invention carried out as follows.
- a temperature-sensitive steel is selected as the substrate, which only allows coating temperatures of up to 200 ° C (e.g. ball bearing steel 100 Cr6).
- a PVD machine is used, which is
- a coating system for carrying out the coating process according to the invention comprises various coating sources (e.g. arc evaporators) in a coating chamber, as well as, inter alia, an AEGD source, heaters and pumps in a manner known per se.
- a coating system is usually designed in an octagonal design with two doors.
- Round evaporators are used as arc evaporators, several of which are arranged in a row one above the other.
- the system has at least 3 flanges to accommodate the arc sources.
- At least one row is equipped with Cr targets, Mo targets and C targets.
- the turbo pumps are installed on the chamber side. Sufficient heating power is installed.
- An AEGD device consisting of the necessary components is also installed.
- the substrate is heated by means of integrated radiant heating in the coating system under a high vacuum, e.g. to 150 ° C.
- a high vacuum e.g. to 150 ° C.
- the substrate is rotated in different degrees of freedom, single, double or triple rotation.
- Ion purification is preferably carried out in two steps. First, the substrates are etched with argon ions plus hydrogen. This is done by the known so-called AEGD technology and the application of a negative bias voltage to the substrates. This cleaning of the substrate surface is achieved.
- a chromium MIE chromium metal ion etching
- the chrome targets are ignited.
- a negative BIAS voltage of at least -600 V on the substrate strongly accelerates the chromium ions (Cr +) from the target to the substrate.
- Cr + chromium ions
- a bias voltage of at least 10 V is applied to the substrates.
- a Cr layer is deposited with a layer thickness of approx. 10 nm to 200 nm using the Cr evaporators.
- nitrogen is let into the system in order to deposit a CrN layer with a layer thickness of approx. 50 nm to 500 nm.
- the Mo evaporators are then ignited and the Cr evaporators switched off.
- a MoN coating is created.
- the process parameters are chosen so that the coating temperature is a maximum of 200 ° C.
- the layer thickness is chosen between 500 nm and 5000 nm.
- the Mo evaporators are first switched off and the nitrogen supply is interrupted.
- a sufficiently high voltage of at least -200V is applied to the substrates in order to bombard the previously deposited MoN layer with C ions. Then the voltage is gradually decreased to deposit the ta-C layer.
- voltages in the range from 10 to 100 V are applied and coating temperatures from 100 ° C to 200 ° C are selected.
- a delta-MoN layer with a hardness of 33 GPa and a modulus of elasticity of 320 GPa with a total layer thickness was used of 2.2 m ⁇ h deposited on a substrate made of temperature-sensitive ball bearing steel with a hardness of approx. 63 HRC in a first coating system.
- the layer structure consisted of a Cr adhesive layer with a layer thickness of 100 nm followed by a 200 nm thick CrN layer and a 1.9 ⁇ m thick d-MoN layer.
- a ta-C with a layer thickness of 1.2 ⁇ m and a hardness of 55 GPa and a modulus of elasticity of 370 GPa was then deposited in a second coating system.
- FIGS. 5a-5b two further exemplary embodiments with at least a first and a second support layer.
- FIG. 6 shows an example of the course of the hardness and the modulus of elasticity in a special layer system of the invention.
- 1a to 1d show by way of example some preferred exemplary embodiments of the present invention with simple layer structures which comprise only molybdenum Mo or molybdenum support layers MoN between the cover layer made of amorphous carbon and the substrate.
- Such layers are very simple, relatively quick and thus also inexpensive to produce and are therefore particularly suitable for coatings on inexpensive mass products.
- cover layer 3 for the production of the remaining parts of the layer system 2, in addition to the process gas nitrogen, in principle only one Mo evaporation source has to be provided, which means minimal expenditure in terms of the equipment of the coating chamber and the The coating process itself is very simplified.
- MoN layer or simply “MoN” is used in the context of the present application for the sake of simplicity, this means a chemical composition or a layer comprising at least Mo and N any composition with respect to Mo and N is meant.
- MoN or a MoN layer within the meaning of this application can thus be, for example, a first Mo a N x support layer 4 or a second Mo N y support layer 5 or any other layer or composition of the MoN type within the meaning of this application .
- MoN is to be understood as a kind of generic term for the molybdenum-nitrogen layers or molybdenum-nitrogen compositions defined in this application.
- the MoN layer layers shown are each first Mo a N x support layers 4.
- the outer cover layer 3 comprising the amorphous carbon can be any type of amorphous carbon layer.
- a very simple amorphous carbon layer of the aC type, or an amorphous carbon layer of the aC: X type doped with an element X, or a tetrahedral amorphous carbon layer of the ta-C: X type doped with an element X an amorphous carbon layer doped with a metal of the a-C: Me type, a tetrahedral amorphous carbon layer doped with a metal of the ta-C: Me type, or an amorphous carbon layer of the aC: H: Me type doped with a metal and hydrogen or, for example, one doped with a metal and hydrogen tetrahedral amorphous carbon layer of the type ta-C: H: Me.
- the cover layer 3 could also be designed as a multilayer layer, formed from one or more of the aforementioned amorphous carbon layer types, or be formed in the form of one or more gradient layers or in any other way designed as an amorphous carbon layer, as within the scope of the description and the claims of this Registration specified.
- the thickness or thickness ratios and hardness or hardness ratios of the individual layers of the layer system 2, as shown schematically in the figures of the present application, can assume all suitable values, as they are explained in the present description and the claims.
- the layer thicknesses or layer thickness ratios of the individual layers of the layer systems 2 shown or of the substrate 1 shown in all figures are of course to be understood as purely schematic and do not reflect actual thicknesses or actual layer thickness ratios.
- the substrate can, in particular, be a component of a component subject to wear and / or friction, in particular a component of a motor vehicle or an internal combustion engine, in particular a piston, or a piston ring, a valve, a valve disk, or another component of an internal combustion engine, or also a tool , such as a cutting tool, a forming tool, a cutting tool, or another tool subject to wear and / or friction, or any other substrate that can advantageously be provided with a coating of the present invention.
- a tool such as a cutting tool, a forming tool, a cutting tool, or another tool subject to wear and / or friction, or any other substrate that can advantageously be provided with a coating of the present invention.
- Thickness ratios as well as the hardness and hardness ratios of the layers of the layer system 2 also apply to all other special layer systems of the invention discussed below and therefore need in the discussion of the following figures Fig. 2a to Fig. 2e, Fig. 3a to Fig 4a and 4b, as well as for the layer systems in FIGS. 5a and 5b, not to be repeated again explicitly. Therefore, in the following discussion of further layer systems of the invention, for the sake of simplicity, only one cover layer 3 or one substrate 4 is spoken of, without having to specify these in more detail. Referring back to the special exemplary embodiments according to FIGS. 1a to 1d, the simplest type of layer of a layer system 2 of the present invention is exemplarily shown on the basis of FIG.
- first Mo a N x support layer 4 which is distinguished by the fact that exactly one first Mo a N x support layer 4, and no further layer is provided.
- This type of layer which can be produced easily and inexpensively, is particularly well suited when, in the application of the coated substrate 1, there are no particularly high requirements for the adhesion of the first Mo a N x support layer 4 on the substrate or the cover layer 3 on the first Mo a N x Support layer 4 exist.
- a Mo adhesive layer is additionally provided between the substrate 1 and the first Mo a N x support layer 4 compared to that of FIG. 1a. In particular, this improves the adhesion of the first Mo a N x support layer 4 to the substrate.
- the adhesive layer 6 made of Mo is provided between the cover layer 3 and the first Mo a N x support layer 4, so that above all the adhesion of the cover layer to the layer system 2 below with substrate 1 is improved.
- the layer system according to FIG. 1d then combines the advantages of the exemplary embodiments according to FIGS. 1b and 1c, in that both the cover layer 3 and the first Mo a N x support layer 4 and between the first Mo a N x support layer 4 and the Substrate 1, an adhesive layer 6 made of molybdenum is provided so that very good adhesion of all layers involved to one another as well as good adhesion of the first Mo a N x support layer 4 on the substrate 1 is achieved.
- FIGS. 1a to 1d are shown schematically.
- the adhesive layers 6 according to FIGS. 1 a to 1b are partially or completely made up of adhesive layers made of a different metal, in the present examples in FIGS. 2a to 2b replaced by adhesion layers made of Cr.
- an adhesive layer 6 made of Mo is provided between the cover layer 3 and the first Mo a N x support layer 4 and an adhesive layer 6 made of Cr is provided between the first Mo a N x support layer 4 and the substrate 1.
- the two exemplary embodiments according to FIG. 2d and FIG. 2e are thus two further advantageous modifications of FIG. 1d, between which the person skilled in the art can select in practice based on the specific application of the coated substrate 1, depending on the requirements.
- FIGS. 3a to 3c further developments of the layer systems 2 according to the special exemplary embodiments described above are schematically sketched, which between the cover layer 3 and the substrate 1 in addition to the at least one first Mo a N x support layer 4 and in addition to the at least one Adhesive layer 6 also include an intermediate layer 7.
- an intermediate layer 7 can be softer, not only when, but in particular, when used
- Steels for the substrate 1 are additionally advantageously provided in the layer system 2, with an additional intermediate layer 7 particularly preferably under a MoN support layer, for example under a first Mo a N x support layer 4 or a second Mo N y support layer 5, very particularly preferably in the direction of the substrate 1 can be provided.
- an additional intermediate layer 7 particularly preferably under a MoN support layer, for example under a first Mo a N x support layer 4 or a second Mo N y support layer 5, very particularly preferably in the direction of the substrate 1 can be provided.
- layer properties such as stability, hardness, above all temperature resistance, adaptation to impact loads or also ductility etc. can be achieved in a layer system 2 according to the invention
- Application and substrate can be individually adapted or further improved.
- the modulus of elasticity and the hardness of the sub-layers or sub-areas of the layer system preferably become increasingly greater in the direction of the top layer.
- the modulus of elasticity and the hardness of the intermediate layer 7 are particularly preferably smaller than the modulus of elasticity and the hardness of the first Mo a N x support layer 4 and / or the second Mo b N y support layer 5 and / or the cover layer 3. This The relationship will be explained in more detail below with reference to FIG. 6.
- intermediate layers 7 for the production of a layer system 2 according to the invention, such as, for example, from intermediate layers comprising single-phase metal nitrides and / or metal carbides and metal carbonitrides and / or phase mixtures of metal nitrides, metal carbides and metal carbonitrides, wherein the intermediate layer 7 in particular can be a single-phase Cr 2 N or a single-phase CrN layer, as in the exemplary embodiments of FIGS. 3a to 3c, or a phase mixture of CrN and Cr 2 N and otherwise special properties and May have configurations as they have already been described in detail elsewhere in the context of this application.
- an additional intermediate layer 7 made of CrN is deposited between the adhesive layer 6 made of Cr provided on the substrate 1 and the first Mo a N x support layer 4 provided under the cover layer 3.
- the exemplary embodiment in FIG. 3a can thus be understood as a further development and further improvement of the exemplary embodiment according to FIG. 2a.
- an additional intermediate layer 7 made of CrN is also deposited between the adhesive layer 6 made of Cr provided on the substrate 1 and under the first Mo a N x support layer 4, with an additional adhesive layer 6 in this exemplary embodiment compared to FIG. 3a is provided between the cover layer 3 and the first Mo a N x support layer 4.
- the exemplary embodiment according to FIG. 3c can be understood as a further development of the exemplary embodiment in FIG. 2e.
- an intermediate layer made of CrN is additionally deposited between the adhesive layer 6 made of Cr provided on the substrate 1 and the first Mo a N x support layer 4.
- Layer systems 2 according to the present invention are layer systems which additionally comprise multilayer layers 71.
- a multilayer layer 71 is to be understood as meaning a sub-layer of the layer system 2 that comprises a plurality of individual different sub-layers 4, 5, 6, 7, the individual thicknesses of which are each relatively small compared to the thickness of the entire layer system 2 or in comparison to the thickness of most of the other partial layers of the layer system 2 or in comparison to the thickness of the entire multilayer layer 71.
- a multilayer layer 71 is provided between the two adhesive layers 6 made of Cr instead of a simple first Mo a N x support layer 4, which alternates between a multitude of individual thin layers of CrN intermediate layers and first Mo a N x support layer 4.
- a further second multilayer layer 71 is provided on the adhesive layer 6 made of Cr deposited on the substrate 1, which alternately contains a large number of individual thin layer layers made of a first CrN1 with a first composition of Cr and nitrogen and further comprises a plurality of individual thin layers of a second CrN2 with a second composition of Cr and nitrogen different from the first composition according to CrN1.
- the multilayer layer 71 according to the present invention can also comprise more than two different types of partial layers or a layer system 2 according to the invention can also comprise more than two identical or different multilayer layers 71, which can be provided at different positions in the layer system 2.
- a multilayer layer 71 it is also possible for a multilayer layer 71 to be designed partially or entirely as a gradient layer in which the chemical composition changes more or less continuously in a characteristic manner with respect to a coating direction.
- FIGS. 5a and 5b are provided under the cover layer 3 with at least a first and a second support layer.
- the nitrogen content x of the first Mo a N x support layer 4 is in the range of 30 at% ⁇ x ⁇ 53 at% and is particularly advantageously around 50 at%.
- the first Mo a N x support layer 4 is, for example, a gradient layer
- the hardness of the first Mo a N x support layer 4 can preferably increase due to an increasing nitrogen content in the direction of the cover layer 3.
- the second Mo b N y supporting layer 5 for example, a gradient layer
- the hardness H is the second Mo b N y backing layer 5 by an increasing nitrogen content towards the coating layer 3 is preferred to increase, so in the direction of substrate 1 decrease.
- an adhesive layer 6 made of Cr is additionally provided to improve the adhesion between substrate 1 and second Mo b N y support layer 5. And also between the first Mo a N x support layer 4 and the second Mo b N y support layer 5, as well as between the first Mo a N x support layer 4 and the cover layer 3, a further adhesive layer 6 made of Mo + Mo 2 N is provided, this being the case are each preferably designed as a Mo layer with a Mo 2 N minor phase.
- the special layer system 2 of FIG. 6 comprises an adhesive layer 6 arranged on the substrate 1, a subsequent intermediate layer 7 and a MoN support layer system 4, 5 arranged on a further adhesive layer 6, which lies directly below the cover layer 3.
- the hardness in GPa is plotted on the left of the ordinate of the diagram in FIG. 6, the modulus of elasticity in GPa on the right, and the thickness D of the layer system in nm is plotted on the abscissa.
- the intermediate layer 7 has a lower hardness H and a lower modulus of elasticity E than the MoN support system 4, 5 comprising the first Mo a N x support layer 4 and / or the second Mo b N y support layer 5, and also the hardness of the MoN support system 4, 5 comprising the first Mo a N x support layer 4 and / or the second Mo b N y support layer 5 increases in the direction of the cover layer.
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Abstract
Description
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KR1020227010077A KR20220066077A (ko) | 2019-09-19 | 2020-09-17 | 몰리브데넘 질화물 코팅 시스템을 구비한 기재 및 코팅 시스템을 생성하기 위한 코팅 프로세스 |
JP2022517183A JP2022548893A (ja) | 2019-09-19 | 2020-09-17 | 窒化モリブデンコーティングシステムを備えた基材、およびコーティングシステムを製造するコーティング方法 |
CN202080077101.2A CN114641588A (zh) | 2019-09-19 | 2020-09-17 | 具有氮化钼层体系的基底和用于制造层体系的涂覆方法 |
US17/761,777 US20220372629A1 (en) | 2019-09-19 | 2020-09-17 | Substrate with a molybdenum nitride layer system, and coating method for producing a layer system |
EP20771569.9A EP4031690A1 (de) | 2019-09-19 | 2020-09-17 | Substrat mit einem molydännitrid schichtsystem, sowie beschichtungsverfahren zur herstellung eines schichtsystems |
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2020
- 2020-09-17 EP EP20771569.9A patent/EP4031690A1/de active Pending
- 2020-09-17 JP JP2022517183A patent/JP2022548893A/ja active Pending
- 2020-09-17 CN CN202080077101.2A patent/CN114641588A/zh active Pending
- 2020-09-17 WO PCT/EP2020/075978 patent/WO2021053072A1/de unknown
- 2020-09-17 KR KR1020227010077A patent/KR20220066077A/ko unknown
- 2020-09-17 US US17/761,777 patent/US20220372629A1/en active Pending
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Also Published As
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CN114641588A (zh) | 2022-06-17 |
US20220372629A1 (en) | 2022-11-24 |
KR20220066077A (ko) | 2022-05-23 |
EP4031690A1 (de) | 2022-07-27 |
JP2022548893A (ja) | 2022-11-22 |
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