Classifications

• • 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
• • 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
  • 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
• • 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
  • 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
  • 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

Definitions

• the present invention relates to a coated cutting tool comprising a nanomultilayer of (Ti,AI)N and (Ti,AI,Si)N.
• a cutting tool for metal machining comprises a hard substrate material such as cemented carbide which has a thin hard wear resistant coating.
• a cutting tool generally has at least one rake face and at least one flank face. A cutting edge is present where a rake face and flank face meet.
• Nano-multilayered coatings are commonly used in the area of cutting tools for metal machining. In these coatings at least two sublayers which are different in some respect alternate forming a coating of a stack of nanolayers. Various metal nitrides are commonly used in wear resistant coatings of cutting tools.
• Metal machining operations include, for example, turning, milling, and drilling.
• a coated cutting tool such as an insert, should have high resistance against different types of wear, e.g., flank wear resistance, crater wear resistance, chipping resistance and flaking resistance.
• Flank wear obviously takes place on a flank face of the cutting edge, mainly from an abrasive wear mechanism.
• the flank face is subjected to workpiece movement and too much flank wear will lead to poor surface texture of the workpiece, inaccuracy in the cutting process and increased friction in the cutting process. If a better flank wear resistance is provided longer tool life is provided for certain metal machining operations.
• a coating must also remain adherent to the substrate, i.e., not flake off, during a machining operation.
• Some workpiece material types such as ISO-M (stainless steel) and ISO-S (heat resistant super alloys and, e.g., titanium), are so called sticky materials and induce flaking more than other workpiece material types. These material types also have a smearing behaviour which means that workpiece material is smeared onto the cutting tool surface which eventually may lead to the formation of a built-up edge (BUE) of workpiece material on the cutting edge. Such a BUE may cause the coating to flake off or even rip off a part of the edge of the cutting tool.
• BUE built-up edge
• average layer period thickness is meant the average thickness of a combination A-B in the nano-multilayer coating of a first nanolayer A and second nanolayer B in a nano-multilayer A-B-A-B-A... If the deposition process is known the calculation can be made by dividing the total thickness of the nano-multilayer by the number of A-B depositions (which corresponds to the number of revolutions when depositing a substrate in a rotating manner).
• the calculation being made by using TEM analysis of a cross-section of the nano-multilayer counting the number of consecutive A-B nanolayer combinations over a length of at least 200 nm and calculating an average value.
• the nano-multilayer has a total thickness of only 0.5 pm then the measuring places are located just below the outer surface of the nanomultilayer.
• methods of analysis include transmission electron microscopy (TEM).
• FWHM Full Width at Half Maximum
• the present invention relates to a coated cutting tool comprising a substrate and a coating, wherein the coating comprises a nano-multilayer of alternating layers of a first nanolayer being Tii- X AI X N, 0.55 ⁇ x ⁇ 0.70, and a second nanolayer being Tii- y -zAl y SizN, 0.20 ⁇ y ⁇ 0.50, 0.13 ⁇ z ⁇ 0.25, 0.46 ⁇ y+z ⁇ 0.65, a sequence of one first nanolayer and one second nanolayer forms a layer period, the average layer period thickness in the nano-multilayer is ⁇ 20 nm.
• the first nanolayer Tii - X AI X N suitably 0.56 ⁇ x ⁇ 0.65, preferably 0.58 ⁇ x ⁇ 0.63, most preferably 0.58 ⁇ x ⁇ 0.61.
• the second nanolayer Tii- y -zAl y SizN suitably 0.25 ⁇ y ⁇ 0.45 and 0.13 ⁇ z ⁇ 0.20, preferably 0.28 ⁇ y ⁇ 0.40 and 0.14 ⁇ z ⁇ 0.18, most preferably 0.33 ⁇ y ⁇ 0.40 and 0.14 ⁇ z ⁇ 0.17.
• the second nanolayer Tii- y-z Al y SizN suitably 0.46 ⁇ y+z ⁇ 0.60, preferably 0.47 ⁇ y+z ⁇ 0.55.
• the average layer period thickness of the nano-multilayer is suitably from 2 to 15 nm, for example from 3 to 10 nm, or from 3 to 7 nm.
• the nano-multilayer has a columnar microstructure. This means that there are crystallites, or "grains”, of columnar shape in the nano-multilayer which are generally elongated in their growth direction.
• the nano-multilayer has a 200 crystallographic preferred orientation.
• the intensity ratio l(200)/l( 111 ) in a theta-2theta X-ray diffraction analysis is suitably >5, for example >10, or >20.
• the nano-multilayer has a FWHM value for the cubic (200) peak in X-ray diffraction being from 0.4 to 1 degrees (2theta), for example from 0.5 to 0.9 degrees (2theta), or from 0.6 to 0.8 degrees (2theta).
• the (200) peak in XRD used for determining the FWHM value is Cu-Ka2 stripped.
• the thickness of the nano-multilayer is suitably from about 0.5 to about 15 pm, preferably from about 1 to about 10 pm, more preferably from about 1 to about 7 pm, most preferably from about 1 .5 to about 4 pm.
• the nano-multilayer is suitably a cathodic arc evaporation deposited layer.
• the coating comprises a layer of TiN, (Ti,AI)N or (Cr,AI)N below the nano-multilayer, suitably closest to the substrate.
• the innermost layer is (Ti,AI)N. If (Ti,AI)N is used then the (Ti,AI)N is suitably Tii- V AI V N, 0.35 ⁇ v ⁇ 0.70, preferably 0.45 ⁇ v ⁇ 0.65, most preferably 0.55 ⁇ v ⁇ 0.65.
• the Ti-AI relation in the (Ti,AI)N is the same as the Ti-AI relation in the first nanolayer of the nanomultilayer, i.e., in the Tii- V AI V N, suitably 0.55 ⁇ v ⁇ 0.70, for example 0.56 ⁇ v ⁇ 0.65, or 0.58 ⁇ v ⁇ 0.63, or 0.58 ⁇ v ⁇ 0.61 .
• the thickness of this innermost layer can be from about 0.1 to about 3 m, from about 0.2 to about 2 pm, most preferably from about 0.5 to about 1 .5 pm.
• the coating comprises a nano-multilayer of alternating layers of a first nanolayer being Tii- X AI X N, 0.55 ⁇ x ⁇ 0.65, and a second nanolayer being Tii- y -zAl y SizN, 0.25 ⁇ y ⁇ 0.45 and 0.13 ⁇ z ⁇ 0.20, 0.46 ⁇ y+z ⁇ 0.65, the average layer period thickness of the nano-multilayer is from 3 to 10 nm, the thickness of the nano-multilayer is from about 1 to about 7 pm, there is an innermost layer of (Ti,AI)N below the nano-multilayer closest to the substrate having a thickness of from about 0.5 to about 1 .5 pm.
• the coating comprises a nanomultilayer of alternating layers of a first nanolayer being Tii- X AI X N, 0.55 ⁇ x ⁇ 0.63, and a second nanolayer being Tii- y-z Al y SizN, 0.28 ⁇ y ⁇ 0.40 and 0.13 ⁇ z ⁇ 0.17, 0.47 ⁇ y+z ⁇ 0.55, the average layer period thickness of the nano-multilayer is from 3 to 10 nm, the thickness of the nano-multilayer is from about 1 to about 7 pm, there is an innermost layer of (Ti,AI)N below the nano-multilayer closest to the substrate having a thickness of from about 0.5 to about 1 .5 pm.
• the substrate of the coated cutting tool can be selected from the group of cemented carbide, cermet, ceramic, cubic boron nitride and high speed steel.
• the substrate is a cemented carbide comprising from 5 to 18 wt% Co and from 0 to 10 wt% carbides nitrides or carbonitrides of group 4 to 5 in the periodic table of elements.
• the coated cutting tool is suitably a cutting tool insert, a drill, or a solid end-mill, for metal machining.
• the cutting tool insert is, for example, a turning insert or a milling 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 one embodiment of a cutting tool being a turning insert.
• Figure 3 shows a schematic view of a cross section of an embodiment of the coated cutting tool of the present invention showing a substrate and a coating comprising different layers.
• Figure 1 shows a schematic view of one embodiment of a cutting tool (1 ) having a rake face (2) and flank faces (3) and a cutting edge (4).
• the cutting tool (1 ) is in this embodiment a milling insert.
• Figure 2 shows a schematic view of one embodiment of a cutting tool (1 ) having a rake face (2) and flank faces (3) and a cutting edge (4).
• the cutting tool (1 ) is in this embodiment a turning insert.
• Figure 3 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 a coating (6).
• the coating consisting of a first (Ti, Al) N innermost layer (7) followed by a nano-multilayer (8) of alternating nanolayers being Tii - X AI X N (9) and nanolayers being Tii- y -zAl y SizN (10).
• the uncoated blanks were mounted on pins that undergo a three-fold rotation in the PVD chamber.
• the chamber was pumped down to high vacuum (less than 10’ 2 Pa) and heated to 450-550°C by heaters located inside the chamber.
• the blanks were then etched for 60 minutes in an Ar plasma.
• an innermost, about 1 pm thick, layer of Ti0.40AI0.60N was deposited by using only the Ti-AI targets, which were Ti0.40AI0.60 targets.
• the process conditions when depositing the innermost (Ti,AI)N layer were: a chamber pressure (reaction pressure) of 4 Pa of N2 gas, and a DC bias voltage of -70 V (relative to the chamber walls) applied to the blank assembly.
• the cathodes were run in an arc discharge mode at a current of 150 A (each).
• both the Ti-AI targets and the Ti-AI-Si targets were employed.
• the chamber pressure (reaction pressure) was set to 4 Pa of N2 gas, and a DC bias voltage of -70 V (relative to the chamber walls) was applied to the blank assembly.
• the cathodes were run in an arc discharge mode at a current of 150 A (each) for 75 minutes (4 flanges).
• a nano-multilayer coating having a thickness of about 3 pm was deposited on the blanks.
• Depositions were made with combinations of Ti-AI-Si targets being Ti0.50AI0.35Si0.15, Tio.5oAlo.3oSio.2o, Tio.35Alo.55Sio.1o and Ti0.30AI0.60Si0.10, and Ti-AI targets being Ti0.40AI0.60.
• the total thickness of the deposited nano-multilayers were about 3 pm (as measured on the flank face).
• the rotational speed correlates to a certain period thickness. In the specific equipment used the rotational speed 5 rpm used correlates to a nanolayer period thickness of about 5 nm.
• sample 1 Invention
• Sample 2 Invention
• Sample 3 Comparative
• Sample 4 Comparative
• a coating comprising a nano-multilayer of (Ti,AI)N and (Ti,Si)N was deposited on sintered cemented carbide cutting tool insert blanks of the geometries SNMA120408, CNMG120408MM and R390-11.
• the composition of the cemented carbide was the same as for samples 1-4.
• the cemented carbide blanks were coated by cathodic arc evaporation in a vacuum chamber comprising four arc flanges.
• Targets of Ti-Si were mounted in two of the flanges opposite each other.
• Targets of Ti-AI were mounted in the two remaining flanges opposite each other.
• the targets were circular and planar with a diameter of 100 mm available on the open market. Suitable target technology packages for arc evaporation are available from suppliers on the market such as IHI Hauzer Techno Coating B.V., Kobelco (Kobe Steel Ltd.) and Oerlikon Balzers.
• the uncoated blanks were mounted on pins that undergo a three-fold rotation in the PVD chamber.
• the chamber was pumped down to high vacuum (less than 10’ 2 Pa) and heated to 450-550°C by heaters located inside the chamber.
• the blanks were then etched for 60 minutes in an Ar plasma.
• an innermost, about 1 pm thick, layer of Ti0.40AI0.60N was deposited by using only the Ti-AI targets, which were Ti0.40AI0.60 targets.
• the process conditions when depositing the innermost (Ti,AI)N layer were: a chamber pressure (reaction pressure) of 4 Pa of N2 gas, and a DC bias voltage of -70 V (relative to the chamber walls) applied to the blank assembly.
• the cathodes were run in an arc discharge mode at a current of 150 A (each).
• both the Ti-AI targets and the Ti-Si targets were employed.
• the chamber pressure (reaction pressure) was set to 4 Pa of N2 gas, and a DC bias voltage of -70 V (relative to the chamber walls) was applied to the blank assembly.
• the cathodes were run in an arc discharge mode at a current of 150 A (each) for 75 minutes (4 flanges).
• a nano-multilayer coating having a thickness of about 3 pm was deposited on the blanks.
• the rotational speed correlates to a certain period thickness.
• the rotational speed 5 rpm used correlates to a nanolayer period thickness of about 5 nm.
• the samples made are called "Sample 5 (comparative)".
• X-ray diffraction (XRD) analysis was conducted on the flank face of coated inserts using a PANalytical CubiX3 diffractometer equipped with a PIXcel detector.
• the coated cutting tool inserts were mounted in sample holders that ensure that the flank face of the samples were parallel to the reference surface of the sample holder and also that the flank face was at appropriate height.
• Cu-K a radiation was used for the measurements, with a voltage of 45 kV and a current of 40 mA.
• Anti-scatter slit of 1/2 degree and divergence slit of 1/4 degree were used.
• the diffracted intensity from the coated cutting tool was measured around 29 angles where relevant peaks occur.
• An FWHM value reflects both the grain size of crystallites in the coating and the point defect density in that the smaller the grain size and/or the greater the point defect density the larger the FWHM value.
• the coatings of the invention show a quite small value of FWHM.
• the cut-off criteria for tool life is a flank wear VB of 0.15 mm.
• the evaluation was made through turning test in austenitic steel. In order to provoke adhesive wear and flaking of the coating the depth of cut a P was varied between 4 to 0 and 0 to 4 mm (in one run during radial facing). The inserts were evaluated through SEM analysis.
• Depth of cut a P 4 to 0, 0 to 4 mm
• Feed rate f z 0.36 mm/rev
• the cut-off criteria are chipping of at least 0.5 mm of the edge line or a measured depth of 0.2 mm at either the flank- or the rake phase. Tool life is presented as the number of cut entrances in order to achieve these criteria.
• Sample 1 and Sample 2 perform excellent, although a difference is seen for Sample 2 between the flaking test run at 100 m/min and 140 m/min. In this flaking test in stainless steel machining using 100 m/min is the most severe test since more smearing is induced than when using 140 m/min.
• Sample 3 and Sample 4 comprising nano-multilayers of (Ti,AI)N and (Ti,AI,Si)N with higher Al content in the (Ti,AI,Si)N nanolayers perform much worse in the flaking resistance test at both 100 m/min and 140 m/min.

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• 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)

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Citations (4)

• 2023
  • 2023-05-31 KR KR1020247037481A patent/KR20250011624A/ko active Pending
  • 2023-05-31 JP JP2024570257A patent/JP2025518128A/ja active Pending
  • 2023-05-31 EP EP23729759.3A patent/EP4532794A1/en active Pending
  • 2023-05-31 US US18/869,881 patent/US20250326038A1/en active Pending
  • 2023-05-31 WO PCT/EP2023/064546 patent/WO2023232869A1/en not_active Ceased
  • 2023-05-31 CN CN202380037118.9A patent/CN119053728A/zh active Pending

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