Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
  • B23B—TURNING; BORING
  • B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
  • B23B27/14—Cutting tools of which the bits or tips or cutting inserts are of special material
  • B23B27/148—Composition of the cutting inserts
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • 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
  • C23C28/044—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
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • 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
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • 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
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • 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
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • 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
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • 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
  • C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • 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
  • C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
  • C23C28/42—Coatings including alternating layers following a pattern, a periodic or defined repetition characterized by the composition of the alternating layers
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • 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
  • C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
  • C23C28/44—Coatings including alternating layers following a pattern, a periodic or defined repetition characterized by a measurable physical property of the alternating layer or system, e.g. thickness, density, hardness
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • 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
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
  • B23B—TURNING; BORING
  • B23B2224/00—Materials of tools or workpieces composed of a compound including a metal
  • B23B2224/24—Titanium aluminium nitride
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
  • B23B—TURNING; BORING
  • B23B2228/00—Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner
  • B23B2228/10—Coatings
  • B23B2228/105—Coatings with specified thickness
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
  • B23B—TURNING; BORING
  • B23B2228/00—Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner
  • B23B2228/36—Multi-layered
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
  • B23B—TURNING; BORING
  • B23B2228/00—Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner
  • B23B2228/44—Materials having grain size less than 1 micrometre, e.g. nanocrystalline

Definitions

• the invention relates to a coated cutting tool comprising a substrate and a coating comprising a first, a second, and a third layer.
• a cutting tool for metal machining comprises a hard substrate material such as cemented carbide coated with a thin hard wear resistant coating such as a titanium aluminium nitride (Ti,AI)N coating deposited by means of a PVD method.
• a hard substrate material such as cemented carbide coated with a thin hard wear resistant coating such as a titanium aluminium nitride (Ti,AI)N coating deposited by means of a PVD method.
• Ti,AI titanium aluminium nitride
• a single phase cubic crystal structure is generally desired but a threshold with respect to aluminium content to provide such single phase cubic structure rather than a mixed structure comprising both cubic and hexagonal structure exists which may vary to some extent depending on, for example, the deposition conditions.
• thicker coatings may impart increased service life up to a certain limit at which high undesired stress concentrations arise in e.g. the coating-to-substrate interface.
• a further objective of the present invention is to provide a coated cutting tool with excellent flank wear resistance.
• a further objective is to provide universally operable tools such as solid carbide drills applicable in any machining operation including drilling in various steel grades.
• the present invention relates to a coated cutting tool comprising a substrate and a coating comprising a first, a second and a third layer, wherein i) the first layer is a (Ti, AI)N layer adhered to the substrate, said first layer having a. an atomic ratio AI/(Ti+AI) of 0.3 to 0.65, preferably from 0.4 to 0.65, more preferably from 0.5 to 0.65 b. a fracture toughness ranging from 3.5 to 6 MPa m, preferably from 4 to 5 MPa m c.
• the second layer is a (Ti, AI)N layer adhered to the first layer having a.
• the third layer is composed of a nitride of one or more elements belonging to group 4, 5 or 6 of the periodic table of elements, or a nitride of Al and/or Si together with one or more elements belonging to group 4, 5 or 6 of the periodic table of elements, said third layer having a substantially homogenous residual stress o 3 ⁇ -1200 MPa, preferably o 3 ⁇ -1400 MPa, more preferably -5000 MPa ⁇ o 3 ⁇ -1500 MPa.
• substantially homogeneous residual stress is meant a maximum variation of 15 % or preferably a maximum variation of 5 % from an average value of the residual stress.
• grade is also meant to include the increase may be stepwise and not necessarily continuously increasing.
• gradient is preferably meant a continuous and regular increase, such as a continuous linear increase.
• the second layer is a cubic (Ti, AI)N layer.
• the third layer which can be a single layer or a multilayer, is composed of a nitride containing at least one of Al, Zr, Ti, Nb and Cr, or a nitride of Al and/or Si together with at least one of Zr, Ti, Nb, and Cr .
• the third layer may suitably be composed of (Ti,AI)N, (Cr,AI)N, (Ti,Si)N, CrN, TiN, or NbN.
• the third layer is a cubic (Ti, AI)N layer or a (Ti, Si)N layer having an atomic ratio AI/(Ti+AI) of 0.67 to 0.85 or an atomic ratio Si/(Ti+Si) of 0.05 to 0.2.
• the atomic ratio AI/(Ti+AI) of the second layer gradually increases from the interface with the first layer to the interface with the third layer, for example from 0.5 to 0.8 or from 0.55 to 0.75.
• the gradual increase in Al content in the second layer can be achieved in several ways.
• an increase of the Al content can be achieved by the selection of the types and number of targets containing certain amounts of Al and Ti during the progress of the deposition process.
• the Al and Ti contents in the deposited coating layers can be varied by varying the deposition condition, such as bias voltage and arc current.
• At least one of the first, second and third layers is a multilayer composed of two or more alternating (Ti, AI)N sub-layer types different in their composition with an overall atomic ratio as specified herein.
• At least one of the first, second, and third (Ti , Al) N layer is a multilayer of two or more alternating (Ti , Al) N sub-layer types different in their composition of which at least one (Ti, Al) N sub-layer type has an atomic ratio AI/(Ti+AI) of 0.50-0.67, preferably 0.55-0.67, most preferably 0.60-0.67, and at least one (Ti ,AI)N sub-layer type has an atomic ratio AI/(Ti+AI) of 0.70-0.90, preferably 0.75-0.85.
• the (Ti ,AI) N sub-layer type in a multilayer suitably is a nanolayer which may have an average thickness of 1-100 nm, preferably 1.5-50 nm, most preferably 2-20 nm.
• the first, second and third layers are single layers.
• the third layer is a (Ti, AI)N layer having an atomic ratio AI/(Ti+AI) ranging from 0.70 to 0.85.
• the atomic ratio AI/(AI+Ti) of the second layer is 0.7 to 0.85.
• the mean grain size of the first layer ranges from 50 to 500 nm, preferably from 50 to 200 nm, and most preferably from 70 to 150 nm.
• the thickness of the first layer ranges from 1 pm to 20 pm, for example from 2 pm to 10 pm such as from 3 pm to 8 pm.
• the coating has a thickness of 3-25 pm, preferably 5-15 pm, most preferably 7-12 pm.
• the first layer shows a distribution of 311 misorientation angles.
• a 311 misorientation angle is an angle between a normal vector to the surface of the first layer and the ⁇ 311 > direction that is closest to the normal vector to the surface of the first layer.
• a cumulative frequency distribution of the 311 misorientation angles is such that are less than 12.5°.
• 311 misorientation angle is meant the smallest angle, i.e., the angle between a normal vector to the (Ti,AI)N layer and the ⁇ 311> direction that is closest to the normal vector to the (Ti, Al) N layer.
• the cumulative frequency distribution of the 311 misorientation angles is such that more than 50%, such as more than 55 % are less than 12.5°.
• the cumulative frequency distribution of the 311 misorientation angles is such that than 95%, such as less than 85% or less than 75% are less than 12.5°.
• the cumulative frequency distribution of the 311 misorientation angles is such that 40 to 85%, for example from 50 to 75% are less than 12.5°.
• the cumulative frequency distribution of the 311 misorientation angles is such that 5 to 40%, for example 8 to 25% or for example from 10 to 15%, are less than 5°.
• the distribution of 311 misorientation angles can be determined in an electron backscatter analysis (EBSD).
• EBSD electron backscatter analysis
• the columnar grain width is generally increasing by increasing the thickness of the (Ti, Al) N layer, especially for the first micrometers of the (Ti , Al) N layer and EBSD analysis may not be suitable if the grain width is too small. Therefore, in the case of a (Ti , Al) N layer of a thickness of 2 pm or less, the distribution of 311 misorientation angles is preferably determined in an transmission electron microscope (TEM) analysis, if the grain size is regarded to be too small for EBSD analysis.
• TEM transmission electron microscope
• the EBSD or TEM analysis is suitably made within a distance of 0.7 mm from the cutting edge.
• the third layer is the outermost layer.
• the first layer (Ti ,AI) N has a Vickers hardness of 2400 HV (15 mN load), preferably 2500 to 2800 HV (15 mN load).
• the first layer (Ti, Al) N has a plane strain modulus of 450 GPa, preferably 500 GPa, for example from 450 to 550 or from 450 to 500 GPa.
• the third (Ti,AI)N layer has preferably a plane strain modulus of 450 to 530 GPa, more preferably 480 to 510 GPa.
• the substrate of the coated cutting tool can be of any kind common in the field of cutting tools for metal machining.
• the substrate is suitably selected from cemented carbide, cermet, cubic boron nitride (cBN), ceramics, polycrystalline diamond (PCD) and high speed steel (HSS).
• the substrate is cemented carbide.
• the coated cutting tool of the invention obtained by the process as further described herein has a low residual stress first layer. This is obtained by depositing the first layer on the substrate at the selected process conditions including a high temperature. The process also imparts increased fracture toughness to the first layer. The process also involves deposition of a second layer which is deposited while the temperature is linearly ramped down as further explained in the working example. This also results in a residual stress gradient across the second layer. The third layer is deposited at the lowest temperature used for the second layer whereby a single phase cubic structure of a (Ti, AI)N composition with high aluminium content can be deposited as an outermost layer. To improve the surface roughness and lower the surface adhesion of workpiece material, wet blasting and drag finishing can be performed.
• the coated cutting tool manufactured is preferably an insert for drilling such as a solid carbide drill, an insert for turning or end mill, or other indexable insert.
• Figure 1 shows a schematic view of one embodiment of a cutting tool being a milling insert.
• Figure 2 shows a schematic view of the coated cutting tool and the temperature used during the deposition of the three layers.
• Figure 1 shows a schematic view of one embodiment of a cutting tool (1) having a rake face (2), a flank face (3) and a cutting edge (4).
• the cutting tool (1) is in this embodiment a milling insert.
• Figure 2 shows a schematic view of a cross section of an embodiment of the coated cutting tool of the present invention having a substrate body (5) and first (6), second (7) and third (8) coating layers.
• a cumulative frequency distribution of 311 misorientation angles was calculated as follows: For each spot measurement of the total EBSD scan (representing an incremental surface area of the overall analyzed surface region) the crystallographic direction perpendicular to the surface plane of the (Ti,AI)N layer, is derived from the absolute crystallographic orientation measured (i.e. the orientation data in Euler angles).
• the vector angle between this crystallographic direction and the closest ⁇ 311 >-type direction is calculated.
• “closest” refers to the ⁇ 311>-type direction (among all twelve crystallographically equivalent possibilities) that includes the smallest possible angle with the surface normal. This angle is defined as the 311 misorientation angle.
• the relative frequency distribution of these angular misorientation values characterizes the overall degree of the 311 surface texture.
• the sample is suitably analysed in cross-section, i.e., the incident electron beam is parallel to the film plane.
• different methods can be used, i) classical preparation including mechanical cutting, gluing, grinding and ion polishing and ii) using a FIB to cut the sample and make a lift out to make the final polishing.
• the position of the analysis is, for example, near the substrate, about 200 nm from the substrate.
• SAED data are then obtained for the sample. From the SAED data a diffraction intensity profile is provided along the 311 ring that is centered around the angular position that corresponds to the coating normal. Then normalized integrations are made both at the 311 diffraction spot and the -3-1-1 diffraction spot, respectively, going to 45 degrees misorientation angle. The two integrations are then combined into one intensity distribution curve. The intensity distribution data from both the 311 diffraction spot and the -3-1-1 diffraction spot are used in order to increase the number of data points thereby reducing the signal to noise ratio as much as possible.
• the Vickers hardness was measured by means of nanoindentation (load-depth graph) using a Picodentor HM500 of Helmut Fischer GmbH, Sindelfingen, Germany.
• the Oliver and Pharr evaluation algorithm was applied, wherein a diamond test body according to Vickers was pressed into the layer and the force-path curve was recorded during the measurement.
• the maximum load used was 15 mN (HV 0.0015) and the time period for load increase and load decrease was 20 seconds each. From this curve, the hardness was calculated.
• the elastic properties of the coating samples were characterized by the so-called plane strain modulus E ps as derived by nanoindentation via the Oliver and Pharr method.
• the nanoindentation data was obtained from indentation as described for Vickers hardness above.
• the mean grain size is determined from SEM images by means of the stereological line intersection method: A line grid is overlaid to the micrograph of interest and the intersections of the lines with the grain boundary network are marked. The statistics of the distances between adjacent intersections reflect the size of the three-dimensional grains (e.g. H.E. Exner, Quantitative Description of Microstructures by Image Analysis, in: Mater. Sci.
• the respective SEM micrographs are taken from the flank face of three-fold rotated test inserts made of cemented carbide (substrate surface repeatedly facing the arc sources during deposition). They stem from a distance of 100 pm from the substrate edge. The grain width was determined at a defined coating height of 2 pm. A minimum of 380 spacing measurements were collected.
• coating material is removed above the layer to be measured. Care has to be taken to select and apply a method for the removal of material which does not significantly alter the residual stress within the remaining nitride multilayer material.
• a suitable method for the removal of deposited coating material may be polishing, however, gentle and slow polishing using a fine-grained polishing agent should be applied. Strong polishing using a coarse grained polishing agent will rather increase the residual stress, as it is known in the art.
• Other suitable methods for the removal of deposited coating material are ion etching and laser ablation.
• the thickness of a layer was determined by calotte grinding using a steel ball having a diameter of 30 mm for grinding the dome shaped recess and further the ring diameters were measured, and the layer thicknesses were calculated therefrom. Measurements of the layer thickness on the rake face (RF) of the cutting tool were carried out at a distance of 2000 pm from the corner, and measurements on the flank face (FF) were carried out in the middle of the flank face. Fracture
• the micro-pillar splitting technique as developed by Sebastiani et al. [1 , 2 and 4] was applied.
• a sharp indenter tip is centered on the top face of a micron-scale pillar of the sample material.
• the force is continuously increased until failure - i.e. splitting - of the pillar occurs.
• the critical stress intensity factor for cracks to emanate from the indenter contact, i.e. the splitting fracture toughness Kc can then be derived from the critical splitting force Pc via the following equation:
• the pillars were micro-machined from the coatings of interest by means of focused ion beam (FIB) milling.
• FIB focused ion beam
• a single-pass milling strategy that utilizes concentric ring patterns of continuously decreasing diameter was used to minimize taper of the pillars. Accordingly, the FIB probe currents were successively lowered from 15 nA (initial roughing) to a final polishing current of 300 pA.
• All of the tested pillars featured a diameter of 7 pm and an aspect ratio of ⁇ 1.3 (height-to-diameter ratio, > 1 is required by the pillar splitting technique [2]).
• the sample surfaces to be structured Prior to any FIB milling the sample surfaces to be structured were carefully polished using a colloidal silica suspension with a nominal grain size of 40 nm (Struers OPS 0.04 pm). This step served to remove any roughness present on the as deposited coating surface. No more than 100 nm of the top coating is removed by this procedure. After this surface preparation the micro-pillars were consistently placed at a distance of -120 pm from the cutting edges, near a “nose radius” of the carrying substrates. Loading of the pillars was performed in a Fischer Picodenter HM500 nanoindentation system (Helmut Fischer GmbH, Sindelfingen, Germany) using a three-sided, pyramidal cube corner diamond indenter (nominal surface angle of 35.26°).
• Fischer Picodenter HM500 nanoindentation system Helmut Fischer GmbH, Sindelfingen, Germany
• the experiment were performed in a load-controlled manner using a constant loading rate of 1 mN/s. For each coating and sample state a minimum of 12 tests were performed to account for the intrinsic scatter of the fracture experiments (20 tests in most cases). The accuracy of the sample stage and tip positioning was experimentally validated to be within 10% of the used pillar radius to not distort the measurement results [3], To calculate the fracture toughness according to equation (1) the coating specific /-coefficient was derived from data published by Ghidelli et al. in ref [4], Measurements can be performed by preparing a cross-section of an already coated tool or by carefully removing the top layers via mechanical polishing or focused ion-beam machining.
• Pillar indentation splitting test for measuring fracture toughness of thin ceramic coatings Philos. Mag. 95 (2015) 1928-1944. https://doi.org/10.1080/14786435.2014.913110.
• a WC-Co substrate was pretreated by means of plasma etching (central beam etching) prior to deposition of the coating to remove about 1 pm to eliminate organic residues and mitigate surface damage and residual stress due to prior grinding of the substrate.
• the etching was performed at a temperature of 600 °C at the following further process conditions:
• An arc-deposited (Ti, AI)N three-layered coating was prepared by depositing on a cemented carbide substrate a first base layer, a second intermediate layer and a third top layer in the mentioned order.
• the first and the second layers were prepared from a Tio.4oAlo.eo target deposited onto a WC-Co based substrate.
• the substrate had a composition of 6 wt% Co and balance WC.
• the deposition was made using cathodic arc deposition in a Balzers Innova Arc-PVD system (Oerlikon Balzers Coating AG, Balzers, Liechtenstein) with the following process parameters:
• Target material Tio.4oAlo.6O
• Target size circular 150 mm
• a layer thickness of about 3.1 pm was deposited.
• Target material Tio.4oAlo.6O
• Target size circular 150 mm
• Bias potential -40 V Source configuration APO, mag 14
• the temperature was linearly ramped down from 600 °C to 300 °C during the coating step.
• the second layer was grown to a thickness of 1.5 pm.
• Target material Tio.27Alo.73
• Target size circular 150 mm
• a layer thickness of 1.4 pm was deposited. A coating with a total thickness of 6 pm was thus prepared.
• Residual stress of first layer - 600 MPa
• Fracture toughness of first layer 4.1 MPa m
• Plane strain modulus of the first layer 520 GPa
• Electron backscatter diffraction (EBSD) analysis was made on the first (base) layer of (Ti,AI)N.
• a cumulative frequency distribution of 311 misorientation angles was calculated, as described in the "Methods" section.
• the first (base) layer of (Ti,AI)N shows a cumulative frequency distribution of the 311 misorientation angles such that about 62% of the 111 misorientation angles are less than 12.5 degrees, and about 13% of the 311 misorientation angles are less than 5 degrees.
• the third (top) layer of (Ti,AI)N shows a 111-texture.
• a cumulative frequency distribution of 111 misorientation angles for the third (top) layer of (Ti,AI)N is such that a cumulative frequency distribution of the 111 misorientation angles is such that >50% of the 111 misorientation angles are less than 10 degrees.
• a base layer was prepared as a comparison according to the preparation of the first (base) layer of example 1 with the exception that it was prepared with a thickness of 5.9 pm to make the coating thickness comparable to the total thickness of the coating of example 1.
• Drilling tests were performed for various work piece materials according to the below in a DMG MORI DMLI65 MonoBlock vertical 3-axis machine.
• steel was machined with coated cutting tools prepared with coatings prepared in accordance with the coatings of examples 1 and 2.
• the number of holes to critical flank wear is indicated for the tested tools in table 1 below:
• Drilling depth 30 mm
• a three-layered tool with the coating according to example 1 has extended tool life compared to the single-layered coating of example 2 (reference).
• Drilling depth 30 mm
• KSS emulsion, 6%; 40 bar

Landscapes

• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Mechanical Engineering (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Materials Engineering (AREA)
• Metallurgy (AREA)
• Organic Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Cutting Tools, Boring Holders, And Turrets (AREA)
• Physical Vapour Deposition (AREA)
• Drilling Tools (AREA)

Priority Applications (4)

Applications Claiming Priority (2)

Publications (1)

Family

ID=81448600

Family Applications (1)

Country Status (6)

Cited By (1)

Citations (4)

• 2022
  • 2022-04-29 EP EP22170878.7A patent/EP4269655A1/en active Pending
• 2023
  • 2023-04-13 JP JP2024563027A patent/JP2025513585A/ja active Pending
  • 2023-04-13 KR KR1020247035603A patent/KR20250004245A/ko active Pending
  • 2023-04-13 US US18/861,086 patent/US20250345860A1/en active Pending
  • 2023-04-13 CN CN202380035511.4A patent/CN119013435A/zh active Pending
  • 2023-04-13 WO PCT/EP2023/059666 patent/WO2023208597A1/en not_active Ceased

Patent Citations (4)

Non-Patent Citations (5)

Also Published As

Similar Documents

Legal Events