• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    sliding element, in particular a piston ring, having a coating. the present application relates to a sliding element, in particular a piston ring, with at least one sliding surface, which comprises a coating comprising, from the inside out, a metal-containing adhesive layer and a dlc layer, where the layer dlc is a hydrogen-free amorphous diamond-like carbon layer that has a main dlc layer that extends from the adhesive layer to an adjacent dlc overlay layer and has a carbon content greater than about 98.5 at%, oxygen and/or hydrogen and/or nitrogen in a proportion, in each case, less than about 0.5 at% and one to sp2/sp3 ratio of carbon in the range of about 1 to about 3, and a layer of dlc coating that extends from the main dlc layer to the surface of the slip element and compared to the main layer has a lower carbon content and/or higher oxygen content and/or higher hydrogen content as well as metals and/or metal oxides and a relationship the sp2/sp3 of carbon in the range of about 1 to about 3.
    公开号:BR112015009584B1
    申请号:R112015009584-4
    申请日:2013-10-31
    公开日:2021-06-15
    发明作者:Kennedy Marcus；Lammers Ralf；Ivanov Yuriy；Zinnabold Michael
    申请人:Federal-Mogul Burscheid Gmbh；
    IPC主号:
    专利说明:

    Technical Field of the Invention
    [0001] The invention relates to a sliding element, in particular a piston ring with at least one sliding surface having a coating comprising, from the inside out, an adhesive layer containing a metal and a DLC layer consisting of a cover layer and a main layer. State of the Art
    [0002] Increasingly stricter legal provisions and high customer desires for lower fuel consumption by internal combustion engines demand a sustainable reduction of losses by mechanical friction. However, this is also accompanied by a significant increase in component requirements, due to the introduction of performance optimizations such as direct injection and turbocharging, which in turn require particularly wear-resistant components.
    [0003] To safeguard the life of piston rings with high service stress, carbide coatings are being used more and more, as described in DE 44 19 713. Thus, metal nitrides, such as, for example, CrN and TiN, are configured as a single or as multiple layers, primarily through physical vapor deposition.
    [0004] In order to reduce friction in the piston ring/cylinder slip band system, amorphous DLC (diamond type carbon) coatings (standard VDI 2840) are used. However, these have a service life that is still very short. And, due to the formation of internal stresses, which reduce adhesiveness and thus the service life, the thickness of the layers to be applied is limited to about 5 µm, as described in DE 10 2005 063 123 B.
    [0005] The documents DE 40 40 456 C1 and DE 198 50 218 C1 describe the production of hydrogen-free amorphous diamond-type carbon layer systems, using conventional spray processes or so-called vacuum arc processes. The high degree of hardness of the layers promises better wear values. Hardness is thus substantially determined by the bonding character, that is, the ratio of sp2 to sp3 carbon bonds. The higher the sp3 content, the harder and stiffer the DLC layer.
    [0006] The production of hydrogen-free or oxygen- and hydrogen-free amorphous diamond-like carbon is described in documents DE 10 2008 022 039 A1 and EP 0 724 023 A1.
    [0007] The high degree of hardness and the high modulus of elasticity of the hydrogen-free amorphous diamond-like carbon layers, however, are also accompanied by some technological problems. On the one hand, the surfaces of the very hard layers must be very smooth, in order to prevent, under high surface pressure, the occurrence of surface cracks and thus the failure of the layer system. Furthermore, a so-called bimetallic effect occurs due to different coefficients of thermal expansion of the base materials of the piston ring and its coating. This bimetallic effect is intensified due to the differences in the modulus of elasticity of the two materials. As a result, with an increase in temperature, there is an increase in pressure in the piston ring joint area, which can cause increased wear. Furthermore, the partner element (cylinder liner) can be damaged by spline formation and high wear. Description of the Invention
    [0008] It is up to the invention the task of creating a sliding element, in particular a piston ring for internal combustion engines with excellent mechanical and tribological properties. More precisely, the objective is to provide a sliding element whose surface ensures the least possible friction and/or the least possible wear and/or a high resistance to abrasion and/or an optimal sealing and oil pickling effect through a high strength of geometry and thus allow a piston ring with a long service life. Compared to hard material systems, an increase in hardness and/or a high wear resistance with sufficient shear strength and/or low friction and/or existing inertia is thus required. Furthermore, the bimetallic effect should be avoided as far as possible.
    [0009] According to the invention, the objective is achieved by the sliding element according to claim 1. Advantageous embodiments and other developments of the invention can be achieved with the features cited in the dependent claims.
    [0010] The sliding element, in particular a piston ring, has at least one sliding surface, on which a coating is applied which comprises, from the inside out, a binding layer containing a metal and a DLC layer, wherein the DLC layer is an amorphous, hydrogen-free, diamond-like carbon layer which comprises a main DLC layer that extends from the adhesive layer to a subsequent DLC overlay layer and has a carbon content greater than about 98, 5 at%, oxygen and/or hydrogen and/or nitrogen in a ratio in each case of less than about 0.5 at% and an sp2/sp3 ratio of carbon of between about 1 and about 3, and a DLC cover layer that extends from the main DLC layer to the surface of the slip element and has, compared to the main layer, a lower carbon content and/or higher oxygen content and/or higher hydrogen content , as well as metals and/or metal oxides and an sp2/sp3 ratio of carbon from about 1 to about 3.
    [0011] The described sliding element has proven to be advantageous with regard to reducing friction and wear due to the high degree of hardness and the good inertia properties of the DLC layer. The sp2/sp3 ratio according to the invention is particularly advantageous for reducing the average wear of the ring along the circumference of the ring and the wear in the area of the piston ring joint due to the reduction of the bimetallic effect, namely by reducing the modulus of elasticity. The geometry's robustness thus increased furthermore contributes to obtaining an optimized sealing and oil pickling.
    [0012] Furthermore, in particular, the sp2/sp3 ratio range according to the invention is advantageous since it allows the definition of a better combination of hardness and elasticity properties of the DLC layer. For optimal tribological properties, the metal is advantageously predominantly present in the DLC coating layer as metal oxide and thus acts as a solid lubricant. In general, therefore, this results in a sliding element with high wear resistance and an extended service life.
    Advantageously, the DLC layer has an sp2/sp3 ratio of carbon preferably from about 1.05 to about 2. This preferred range allows the DLC layer to adapt well to the base material of the slip element. The modulus of elasticity can in particular be advantageously reduced and thus the elasticity of the DLC layer can be improved and, for example, the bimetallic effect reduced.
    [0014] The DLC cover layer, in another preferred embodiment, contains iron and iron oxides, where these iron oxides can be FeO and Fe3O4, as demonstrated by means of x-ray diffraction. The DLC cover layer, furthermore, advantageously comprises an iron content of about 30 at % or less. It is known from the literature that iron oxides as solid lubricants can result in a reduction in friction. They are, in addition, significantly softer materials than hydrogen-free DLC coatings, whereby the starting behavior can be considerably improved. A defined surface portion of these metals and metal oxides leads to an optimization of wear, starting behavior and friction. From scanning electron microscopy measurements in the so-called BSE (Back Scattered Electrons) mode, the surface portion of metals and metal oxides directly on the surface can be determined according to a preferred embodiment of the invention. The surface portion is about 5 to 40%, preferably about 5 to 25%.
    [0015] It is particularly preferred that the metals and/or metal oxides comprising the DLC overlay layer are present or more specifically incorporated, in particular, in the valleys of the roughness of the DLC overlay layer. Furthermore, it is preferable that metals and/or metal oxides are only present in the cover layer.
    [0016] The DLC overlay layer preferably furthermore has a carbon content of about 25 at% or less and an oxygen content of preferably about 50 at% or less.
    Advantageously, a surface of the cover layer has, under normal atmospheric conditions, about 20 at% to about 30 at% CO bonds, about 8 at% to about 15 at%, preferably about 10 at% to about 15 at% C=O bonds, and about 6 at% at approximately 10 at% OC=O bonds. The increased CO bond ratio in the layer, in particular according to the invention, leads to an increase in the saturation of the carbon bond and advantageously to a reduction in wear and friction.
    [0018] The DLC overlay layer has a thickness of up to about 2 µm, preferably about 1 µm, and the main DLC layer has a thickness of up to about 5 µm to about 40 µm. The preferred thicknesses positively ensure a long service life and uptime of the coating and therefore lasting protection against abrasive and adhesive wear and component failure.
    [0019] Advantageously, in the DLC cover layer, the metal content and/or the oxygen content and/or the hydrogen content increase towards the outside of it. The preferential enrichment of the concentration of these elements on the outer side leads to advantageous tribological properties of the coating and to a reduction in average ring wear along the ring circumference and wear in the piston ring joint area.
    [0020] The DLC layer preferably has a hardness of about 1800 to 3500 HV0.02 and/or even more preferably a modulus of elasticity of about 150 to 320 GPa. The combination of a high degree of hardness compared to Conventional cemented carbide materials and reduced modulus of elasticity compared to previously known, in particular, hydrogen-free DLC materials is particularly advantageous since the wear resistance and geometry robustness are increased and the bimetallic effect is reduced in this way.
    Advantageously, the DLC layer further has an average roughness depth of Rz < about 2 µm, preferably Rz < about 1 µm, and a reduced peak height Rpk < about 0.15 µm, preferably Rpk < about 0.1 µm. This low roughness, which can be achieved on softer surface areas with little technical effort, is particularly advantageous, since a failure of the layer system due to a breakdown caused by irregularities in the hard carbon layers can be reduced.
    [0022] The adhesive layer preferably has a thickness of about 0.05 to about 1.0 µm and, in addition, preferably contains chromium or titanium. Furthermore, the base material of the sliding element is preferably cast iron or steel. This embodiment according to the invention firstly ensures an optimized and sustainable connection of the wear-reducing DLC layers with the base material of the sliding element and therefore significantly contributes to their functionality. Brief Description of Drawings Figure 1 shows a schematic representation of the structure of a coating of a sliding element. Figure 2 shows a scanning electron micrograph in BSE (Back Scattered Electron) Mode of the rupture of an amorphous carbon-free hydrogen-free polished layer diamond. Figure 3 shows the mean relative wear values along the ring circumference of the slip elements described and tested in Table 1. Figure 4 shows the mean relative wear values of the ring in the region of the junction of the slip elements described and tested in Table 1. Detailed Description of Embodiments of the Invention
    [0023] Figure 1 shows the structure according to the invention of a coating of a sliding element. The adhesive layer (1) is directly bonded to the base material of the sliding element. Over this adhesive layer the main DLC layer (2) is applied, and over the latter the DLC cover layer (3) is applied as a surface layer.
    [0024] Figure 2 shows a scanning electron microscopy photograph of the coating, in a side view. In contrast material-dependent BSE (Back Scattered Electrons), the carbon-containing material (4) appears grayish black. In addition, white areas are apparent near the surface of the layer, which represent the iron-containing material (5). Each of the arrows (6) and (7) indicates the thickness of the iron-containing material at selected measurement points provided as examples.
    [0025] Table 1 presents an overview of three different coatings of a sliding element, in particular a piston ring, and lists their names, manufacturing processes, layer thicknesses, mechanical properties and sp2/sp3 ratios. The layer system "PtaC2" corresponds to a preferred embodiment of the present invention.
    [0026] All sliding elements have been validated in an engine test, that is, in a highly demanded diesel engine having a combustion pressure of 200 bar and a specific power of 71 kW/liter cylinder capacity. Figures 3 and 4 show a comparison of the mean relative wear of the ring along the circumference of the ring and the mean relative wear of the ring in the joint region, after 500 hours of running time, in which the prior art under the shape of the CrN coating was used as reference (100%). The preferred embodiment proves to be particularly advantageous, i.e. comparatively low wear. Since the reduced sp3 content causes this, it is unusual compared to the prior art that the "PtaC2" coating has a lower degree of hardness and a lower elastic modulus than "PtaC1".
    [0027] In addition, the sealing effect of the piston rings produced from the liners in Table 1 was determined by means of a contour plot on fixed rings. The radial pressure over the entire circumference of the ring is then determined.
    [0028] Compared to "PtaC1", the preferred embodiment "PtaC2" is characterized by an almost pressure-free area with a low indentation in the ring joint and is light slit-proof. This suggests good geometry strength and sealing effect also at higher temperatures.
    [0029] Furthermore, the necessary surface treatment of the layers designated "PtaC" can change their surface composition and microstructure. Thus, it was measured by means of SIMS (Secondary Ion Mass Spectrometry) that, after processing/smoothing, the oxygen content in the layers "PtaC1" and "PtaC2" increased from about < 0.5 at%, at a depth of about 500 nm for the base material, up to approximately 47 at% in the region near the surface. The iron content also increased from < approximately 1 at% to up to about 23 at% and the carbon content decreased from approximately 99 at% in the depth of the DLC layer to approximately 30 at% in the region near the surface.

    [0030] Table 2 specifies, based on REM (Scanning Electron Microscopy) examinations, the Fe surface portions for the "PtaC1" and "PtaC2" coatings. Table 2 further specifies, based on measurements by XPS (X-Ray PhotoElectronic Spectroscopy) and therefore for a region of approximately 10 nm thickness of the surface, ie, the covering layer (3), the carbon-oxygen bond relationships.
    [0031] Compared to "PtaC1", the coating "PtaC2", which corresponds to a preferred embodiment of the invention, is characterized by a relatively large Fe surface portion, as well as by a higher proportion of single CO bonds. It is expected that, in a normal atmosphere, carbon not bonded to oxygen will bond to hydrogen, which has a lower enthalpy of formation than a CO bond, and therefore "PtaC1" will have a lower resistance to wear and a higher friction than "PtaC2" as according to the invention. This type of connection, however, is not detectable using XPS.

    [0032] The sliding element according to the invention can be produced by means of PVD processes, whereby, for example, chromium as the adhesive layer and carbon are vaporized, and ionized by means of electromagnetic fields deposited on a base material of the sliding element. Further processing of the slip element is carried out by means of a subsequent process, in which, in connection with a thermochemical process, for example a temperature-induced oxidation, the transfer of material from a metallic processing material takes place. As a result, corresponding metal and/or metal oxides are deposited in the roughness valleys of the DLC cover layer, as is clearly evident from the white areas in Figure 2.
    权利要求:
    Claims (18)
    [0001]
    1. Sliding element, in particular a piston ring, having at least one sliding surface that has a coating that has, from the inside out, a metal-containing adhesive layer and a DLC layer, characterized in that the DLC layer is a layer of hydrogen-free diamond-like amorphous carbon, which comprises a main DLC layer (2) that extends from the adhesive layer to a subsequent DLC cover layer (3) and has a carbon content greater than 98.5 at %, oxygen and/or hydrogen and/or nitrogen in a proportion, in each case, less than 0.5 to % and a carbon sp2/sp3 ratio of between 1 and 3, and a DLC cover layer extending from the main DLC layer to the surface of the sliding element and has, compared to the main layer, a lower carbon content and/or higher oxygen content and/or higher hydrogen content, as well as metals and/or metal oxides and an sp2/sp3 carbon ratio of between 1 and 3.
    [0002]
    2. Sliding element according to claim 1, characterized in that the DLC layer has a carbon sp2/sp3 ratio preferably from 1.05 to 2.
    [0003]
    3. Sliding element according to claim 1 or 2, characterized in that the DLC covering layer comprises iron and/or iron oxides.
    [0004]
    4. Sliding element according to claim 3, characterized in that the iron oxides are FeO and/or Fe3O4.
    [0005]
    5. Sliding element according to any one of claims 1 to 4, characterized in that the DLC cover layer has an iron content of 30 at% or less.
    [0006]
    6. Sliding element according to any one of claims 1 to 5, characterized in that the DLC cover layer has a carbon content of 25 at% or more.
    [0007]
    7. Sliding element according to any one of claims 1 to 6, characterized in that the DLC cover layer has an oxygen content of 50 at% or less.
    [0008]
    8. Sliding element according to any one of claims 1 to 7, characterized in that a surface of the DLC cover layer has the following CO:• CO bond ratios from 20 at% to 30 at%, • C= O from 8 at% to 15 at%, preferably from 10 at% to 15 at%, • OC=O from 6 at% to 10 at%.
    [0009]
    9. Sliding element according to any one of claims 1 to 8, characterized in that the metals and/or metal oxides disposed on the coating surface have a surface proportion of 5 to 40 at%, preferably of 5 at 25 to %.
    [0010]
    10. Sliding element according to any one of claims 1 to 9, characterized in that the DLC cover layer has a thickness of up to 2 µm, preferably 1 µm.
    [0011]
    11. Sliding element according to any one of claims 1 to 10, characterized in that the main DLC layer has a thickness of 5 μm to 40 μm.
    [0012]
    12. Sliding element according to any one of claims 1 to 11, characterized in that in the DLC covering layer the metal content and/or the oxygen content and/or the hydrogen content increases/increases towards the outside of it.
    [0013]
    13. Sliding element according to any one of claims 1 to 12, characterized in that the DLC layer has a hardness of 1800 to 3500 HV0.02.
    [0014]
    14. Sliding element according to any one of claims 1 to 13, characterized in that the DLC layer has an elastic modulus of 150 to 320 GPa.
    [0015]
    15. Sliding element according to any one of claims 1 to 14, characterized in that the DLC layer has an average roughness depth Rz of < 2 μm, preferably an Rz < 1 μm, and a reduced peak height of Rpk < 0.15 µm, preferably Rpk < 0.1 µm.
    [0016]
    16. Sliding element according to any one of claims 1 to 15, characterized in that the adhesive layer has a thickness of 0.05 μm to 1.0 μm.
    [0017]
    17. Sliding element according to any one of claims 1 to 16, characterized in that the adhesive layer comprises chromium or titanium.
    [0018]
    18. Sliding element according to any one of claims 1 to 17, characterized in that a base material of the sliding element is cast iron or steel.
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    同族专利:
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    DE102020124180A1|2020-09-16|2022-03-17|Federal-Mogul Burscheid Gmbh|Sliding element, in particular a piston ring|
    法律状态:
    2018-03-06| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|
    2018-03-13| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|
    2018-03-20| B06I| Publication of requirement cancelled [chapter 6.9 patent gazette]|Free format text: ANULADA A PUBLICACAO CODIGO 6.6.1 NA RPI NO 2462 DE 13/03/2018 POR TER SIDO INDEVIDA. |
    2019-10-15| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|
    2021-04-06| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2021-06-15| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 31/10/2013, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
    申请号 | 申请日 | 专利标题
    DE102012219930.6|2012-10-31|
    DE102012219930.6A|DE102012219930A1|2012-10-31|2012-10-31|Sliding element, in particular piston ring, with a coating|
    PCT/EP2013/072781|WO2014068040A1|2012-10-31|2013-10-31|Sliding element, in particular a piston ring, having a coating|
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