EP1311712A2 - Method for increasing compression stress or reducing internal tension stress of a cvd, pcvd or pvd layer and cutting insert for machining - Google Patents

Method for increasing compression stress or reducing internal tension stress of a cvd, pcvd or pvd layer and cutting insert for machining

Info

Publication number
EP1311712A2
EP1311712A2 EP01991711A EP01991711A EP1311712A2 EP 1311712 A2 EP1311712 A2 EP 1311712A2 EP 01991711 A EP01991711 A EP 01991711A EP 01991711 A EP01991711 A EP 01991711A EP 1311712 A2 EP1311712 A2 EP 1311712A2
Authority
EP
European Patent Office
Prior art keywords
layer
substrate body
cvd
cutting insert
pcvd
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP01991711A
Other languages
German (de)
French (fr)
Inventor
Hartmut Westphal
Volkmar Sottke
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Widia GmbH
Original Assignee
Widia GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from DE10123554A external-priority patent/DE10123554B4/en
Application filed by Widia GmbH filed Critical Widia GmbH
Publication of EP1311712A2 publication Critical patent/EP1311712A2/en
Withdrawn legal-status Critical Current

Links

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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5886—Mechanical treatment
    • 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
    • C23C14/58—After-treatment
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/56—After-treatment
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
    • Y10T428/2495—Thickness [relative or absolute]
    • Y10T428/24967—Absolute thicknesses specified
    • Y10T428/24975—No layer or component greater than 5 mils thick
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
    • Y10T428/264—Up to 3 mils
    • Y10T428/265—1 mil or less

Definitions

  • the invention relates to a method for increasing the residual compressive stress or for lowering the internal tensile stress of an outer or an outer hard material layer applied by means of CVD, PCVD or PVD to a hard metal, cermet or ceramic substrate body, in which the coated substrate body after coating is subjected to a dry blasting treatment Using a granular abrasive.
  • the invention further relates to a cutting insert for machining, which consists of a hard metal, cermet or ceramic substrate body with a single or multi-layer coating of carbides, nitrides, carbonitrides, oxicarbonitrides and / or borides of the elements of the IVa to Vla group of the periodic table, boron-containing hard material compounds and / or oxidic compounds of aluminum and / or zirconium, which have been applied by means of a PCVD or CVD process.
  • Hard metals have a binding phase consisting of cobalt and / or nickel as well as a hard material phase, which can have, for example, WC, TiC, TaC, NbC, VC and / or Cr 3 C 2 .
  • the cermets differ in that they have a large proportion of a TiCN phase, but other carbides and / or nitrides can also belong to them.
  • binder metals are the elements of the iron group, mostly Co and / or Ni. Ceramics, in particular for machining purposes, usually consist of A1 2 0 3 and / or Zr0 2 .
  • the wear resistance can be increased by single- or multi-layer coatings of the above composition.
  • the coating can be applied by means of a physical vapor deposition process (PVD) or a chemical vapor deposition process (CVD), whereby the CVD process or - in a further development - the so-called plasma-assisted CVD process (PCVD) has the advantage of a more uniform deposition, which the Avoid shading effects that occur with PVD processes.
  • PVD physical vapor deposition process
  • CVD chemical vapor deposition process
  • PCVD plasma-assisted CVD process
  • the outer layer (top layer) consists of a single or multi-phase layer of carbides, nitrides or carbonitrides based on Zr or Hf, which has been applied by means of CVD and which has internal compressive stresses, and the layer or layers underneath, also applied by means of CVD all have internal tensile stresses, at least one or the only underlying layer consisting of TiN, TiC and / or Ti (C, N).
  • the compressive stresses measured in the outer layers or the outer layer are between -500 and -2500 MPa (compressive stresses are defined by definition with negative values in contrast to tensile stresses for which positive values are used).
  • the blasting medium has a maximum diameter of 150 ⁇ m, preferably a maximum of 100 ⁇ m.
  • the internal tension of the layers lying under the cover layer also changes in a uniform manner to the extent that the edge zones of the substrate body near the surface are influenced.
  • a composite body with a multi-layer coating can thus be produced by dry mechanical blasting treatment, the layers of which, without exception, have internal compressive stresses, the top layer having undergone intensive consolidation and thus increased wear resistance.
  • the fine-grained powdery abrasives are also essentially not, but at least significantly less abrasive, than the coarser grains previously used in the prior art.
  • a further advantage of this dry blasting treatment is that the layer surface is smoothed considerably better than was previously possible with blasting treatment or brushing.
  • WO 99/23275 describes the use of a beam consisting of Al 2 0 3 particles with a size of 30 ⁇ m. proposed, but this should be used in the form of a suspension as a wet blasting agent, which should be used under a pressure of 2 to 6 bar (x 10 5 Pa), preferably 3 bar.
  • the wet jet treatment described there relates exclusively to the specific layer sequence with a lower ⁇ l 2 0 3 layer on which an outer layer has been applied, which consists of TiN or a multi-layer layer of TiN / TiC.
  • the CVD process used for coating apparently leads to (tensile) stresses, which should be minimized by means of wet blasting.
  • wet blasting with an Al 2 0 3 abrasive primarily serves to smooth the surface, whereas the achievable change in internal stresses compared to dry blasting treatment is significantly minimized.
  • the K-aluminum oxide present on the surface should finally be heat-treated at a temperature of 900 ° C to 1100 ° C for 0.3 to 10 hours in order to convert the wet-blasted K-aluminum oxide into ⁇ -aluminum oxide.
  • the blasting agent has at least essentially a rounded grain shape, the diameter of which is preferably between see 5 to 150 microns, further preferably between 10 to 100 microns.
  • the blasting agent has at least essentially a rounded grain shape, the diameter of which is preferably between see 5 to 150 microns, further preferably between 10 to 100 microns.
  • Pressure-atomized steel, cast iron granules, heavy metal powder or alloys or carbide granules and / or break-resistant ceramics produced therefrom are preferably used as blasting agents. These abrasives are characterized by a high breaking strength, so that the grains do not crack into smaller, sharp-edged grains, which can then damage the composite surface more severely.
  • the abrasive is or are directed onto the coated substrate body by means of compressed air under a pressure of at least 5 ⁇ 10 5 Pa to a maximum of 10 6 Pa, preferably between 6 ⁇ 10 5 Pa and 7 ⁇ 10 5 Pa.
  • the jet prints used are therefore considerably higher than the pressures usually used according to the prior art (when using a coarser-sized blasting agent).
  • blasting media it is possible that blasting media ; to be directed at the composite surface at any angle, but the effect increases if the abrasive is directed essentially perpendicular to the composite surface.
  • the blasting treatment is carried out until the one under an external one Layer or an outermost layer lying areas or layers, preferably up into the near-surface zones of the substrate body, have experienced a change in the internal stresses, ie either an increase in the compressive stresses or a minimization of the tensile stresses.
  • the jet pressure and duration of treatment the internal tensions of the layers lying under the cover layer can also be influenced in a targeted manner.
  • the substrate body can be a hard metal, a hard metal with an edge zone gradient, a cermet or an oxide or nitride ceramic.
  • the substrate body is preferably coated with a coating of carbides, nitrides, carbonitrides, oxicarbonitrides and / or borides of the elements of the IVa to Vla group of the periodic table, boron-containing hard material compounds and / or oxidic compounds of aluminum and / or zirconium.
  • the layer thickness of a single layer is between 0.1 ⁇ m and a maximum of 10 ⁇ m.
  • the total layer thickness of a multilayer coating should preferably be ⁇ 20 ⁇ m.
  • the residual compressive stresses are measured by X-ray analysis using the sin 2 ⁇ method.
  • the method is described, for example, in the publication HTM43 (1988) 4, pages 208 to 211, "Roentgenographic residual stress measurements on texture-based PVD layers made of titanium carbide" by B. Eigenmann, B. Scholtes and E. Macherauch.
  • the residual stress values measured according to the invention are achieved on at least one grid level.
  • the proposed beam treatment covers at least the entire cutting area of a cutting insert used for the respective machining operations.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)
  • Chemical Vapour Deposition (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

The invention relates to a method for increasing internal pressure stress or for reducing the internal tension stress of an outer or outermost hard material layer that is applied on a hard metal, cermet or ceramic substrate body by means of CVD, PCVD or PVD. After coating, the coated substrate body is subjected to dry shot blasting using a granular shot blasting agent, which, according to the invention, has a maximum diameter of 150 mu m.

Description

Beschreibung description
Verfahren zur Erhöhung der Druckspannung oder zur Erniedrigung der Zugeigenspannung einer CVD-, PCVD- oder PVD-Schicht und Schneideinsatz zum ZerspanenProcess for increasing the compressive stress or reducing the tensile residual stress of a CVD, PCVD or PVD layer and cutting insert for machining
Die Erfindung betrifft ein Verfahren zur Erhöhung der Druckeigenspannung oder zur Erniedrigung der Zugeigenspannung einer äußeren oder einer äußersten, mittels CVD, PCVD oder PVD auf einen Hartmetall-, Cermet- oder Keramiksubstratkörper aufgetragenen Hartstoffschicht, bei dem der beschichtete Substratkörper nach dem Beschichten einer trockenen Strahlbehandlung unter Verwendung eines körnigen Strahlmittels unterzogen wird.The invention relates to a method for increasing the residual compressive stress or for lowering the internal tensile stress of an outer or an outer hard material layer applied by means of CVD, PCVD or PVD to a hard metal, cermet or ceramic substrate body, in which the coated substrate body after coating is subjected to a dry blasting treatment Using a granular abrasive.
Die Erfindung betrifft ferner einen Schneideinsatz zum Zerspanen, der aus einem Hartmetall-, Cermet- oder Keramiksubstratkörper mit einer ein- oder mehrlagigen Beschichtung aus Carbi- den, Nitriden, Carbonitriden, Oxicarbonitriden und/oder Bori- den der Elemente der IVa bis Vla-Gruppe des Periodensystems, borhaltigen Hartstoffverbindungen und/oder oxidischen Verbindungen des Aluminiums und/oder des Zirkoniums besteht, die mittels eines PCVD- oder CVD-Verfahrens aufgetragen worden sind.The invention further relates to a cutting insert for machining, which consists of a hard metal, cermet or ceramic substrate body with a single or multi-layer coating of carbides, nitrides, carbonitrides, oxicarbonitrides and / or borides of the elements of the IVa to Vla group of the periodic table, boron-containing hard material compounds and / or oxidic compounds of aluminum and / or zirconium, which have been applied by means of a PCVD or CVD process.
Hartmetalle besitzen eine aus Cobalt und/oder Nickel bestehende Bindephase sowie eine Hartstoffphase, die z.B. WC, TiC, TaC, NbC, VC und/oder Cr3C2 aufweisen kann.Hard metals have a binding phase consisting of cobalt and / or nickel as well as a hard material phase, which can have, for example, WC, TiC, TaC, NbC, VC and / or Cr 3 C 2 .
Demgegenüber unterscheiden sich die Cermets durch einen starken Anteil einer TiCN-Phase, der jedoch auch andere Carbide und/oder Nitride zugehören können. Bindemetalle sind auch hier die Elemente der Eisengruppe, zumeist Co und/oder Ni. Keramiken, insbesondere für Zerspanungszwecke bestehen meist aus A1203 und/oder Zr02. Je nach Zerspanungsoperation und zu bearbeitendem Werkstück kann die Verschleißbeständigkeit (Standzeit) durch ein- oder mehrlagige Beschichtungen der obengenannten Zusammensetzung gesteigert werden. Die Beschichtung läßt sich mittels eines physikalischen Aufdampfverfahrens (PVD) oder eines chemischen Aufdampfverfahrens (CVD) auftragen, wobei das CVD-Verfahren oder - in einer Weiterentwicklung - das sogenannte plasmaunterstützte CVD-Verfahren (PCVD) den Vorteil einer gleichmäßigeren Ablagerung hat, die die bei PVD-Verfahren auftretenden Schattierungseffekte vermeiden.In contrast, the cermets differ in that they have a large proportion of a TiCN phase, but other carbides and / or nitrides can also belong to them. Here too, binder metals are the elements of the iron group, mostly Co and / or Ni. Ceramics, in particular for machining purposes, usually consist of A1 2 0 3 and / or Zr0 2 . Depending on the machining operation and the workpiece to be machined, the wear resistance (service life) can be increased by single- or multi-layer coatings of the above composition. The coating can be applied by means of a physical vapor deposition process (PVD) or a chemical vapor deposition process (CVD), whereby the CVD process or - in a further development - the so-called plasma-assisted CVD process (PCVD) has the advantage of a more uniform deposition, which the Avoid shading effects that occur with PVD processes.
Die MikroStruktur, die Eigenspannungen und die Haftfestigkeit von ein- oder mehrlagigen Schichten ist stark von den jeweils angewandten Beschichtungsverfahren und den verwendeten Beschichtungspara etern abhängig. In der Vergangenheit gewonnene Erfahrungen zeigen, daß mittels CVD abgeschiedene Beschichtungen im Regelfall Zugspannungen aufweisen, während durch PVD-Verfahren aufgetragene Beschichtungen Druckspannungen besitzen. Zur Verbesserung der Bruchfestigkeit wird beispielsweise in der WO 92/05296 vorgeschlagen, eine CVD-Schicht bzw. mehrere CVD-Schichten mit einer oder mehreren durch PVD abgeschiedenen Schichten zu kombinieren, wobei als Material für die inneren, mittels CVD abgeschiedene Schicht, Nitride des Titans, Hafniums und/oder Zirkoniums und für die mittels PVD abgeschiedene Schicht Nitride und Carbonitride der genannten Metalle vorgeschlagen werden. Eine solche Beschichtung muß jedoch nachteiligerweise in unterschiedlichen Apparaturen durchgeführt werden, was arbeitsaufwendig und kostspielig ist.The microstructure, the residual stresses and the adhesive strength of single or multi-layer layers depend heavily on the coating processes used and the coating parameters used. Experience gained in the past shows that coatings deposited by means of CVD generally have tensile stresses, while coatings applied by PVD processes have compressive stresses. To improve the breaking strength, it is proposed, for example, in WO 92/05296 to combine a CVD layer or a plurality of CVD layers with one or more layers deposited by PVD, nitrides of titanium being used as the material for the inner layer deposited by means of CVD , Hafnium and / or zirconium and for the layer deposited by means of PVD nitrides and carbonitrides of the metals mentioned. However, such a coating must disadvantageously be carried out in different apparatuses, which is labor-intensive and expensive.
In der DE 197 19 195 AI wird daher vorgeschlagen, eine mehrlagige Beschichtung durch einen ununterbrochenen CVD-Prozeß bei Temperaturen zwischen 900°C und 1100°C durch jeweiligen Wechsel der Gaszusammensetzung abzuscheiden. Die äußere Schicht (Deckschicht) besteht aus einer ein- oder mehrphasigen Schicht aus Carbiden, Nitriden oder Carbonitriden auf Zr- oder Hf-Basis, die mittels CVD aufgetragen worden ist und die innere Druckspannungen aufweist und deren darunterliegende, ebenfalls mittels CVD aufgetragene Schicht oder Schichten ausnahmslos innere Zugspannungen aufweisen, wobei mindestens eine oder die einzige darunterliegende Schicht aus TiN, TiC und/oder Ti(C,N) besteht. Die in den äußeren Schichten oder der äußeren Schicht gemessenen Druckspannungen liegen zwischen -500 und -2500 MPa (Druckspannungen werden definitionsgemäß mit negativen Werten im Gegensatz zu Zugspannungen, für die positive Werte angesetzt werden, benannt) .DE 197 19 195 AI therefore proposes a multi-layer coating through an uninterrupted CVD process Separate temperatures between 900 ° C and 1100 ° C by changing the gas composition. The outer layer (top layer) consists of a single or multi-phase layer of carbides, nitrides or carbonitrides based on Zr or Hf, which has been applied by means of CVD and which has internal compressive stresses, and the layer or layers underneath, also applied by means of CVD all have internal tensile stresses, at least one or the only underlying layer consisting of TiN, TiC and / or Ti (C, N). The compressive stresses measured in the outer layers or the outer layer are between -500 and -2500 MPa (compressive stresses are defined by definition with negative values in contrast to tensile stresses for which positive values are used).
Nach dem Stand der Technik ist es weiterhin bekannt, beschichtete Substratkörper nach der Beschichtung einer Oberflächenbehandlung zu unterziehen. Gängige mechanische Behandlungsverfahren sind das Bürsten und die Strahlbehandlung, bei der die verwendeten kugelförmigen Strahlmittel mit Korngrößen von 300 μm bis 600 μm mittels Preßluft unter einem Druck von 2 x 105 Pa bis 4 x 105 Pa auf die Oberfläche gerichtet werden. Eine solche Oberflächenbehandlung erhöht die Druckeigenspannungen der äußersten Schicht durch eintretende Verfestigung geringfügig. Hiermit will man störenden Rißbildungen und Ausbreitungen, Korrosion und Abplatzungsreaktionen entgegenwirken.According to the prior art, it is also known to subject coated substrate bodies to a surface treatment after coating. Common mechanical treatment methods are brushing and blasting, in which the spherical blasting media used with grain sizes of 300 μm to 600 μm are directed onto the surface by means of compressed air under a pressure of 2 x 10 5 Pa to 4 x 10 5 Pa. Such a surface treatment slightly increases the residual compressive stresses of the outermost layer as it solidifies. This is intended to counteract disruptive cracking and spreading, corrosion and spalling reactions.
Es ist Aufgabe der vorliegenden Erfindung, die Rißanfälligkeit, Korrosionsbeständigkeit und Verschleißbeständigkeit von beschichteten Verbundwerkstoffen, insbesondere Schneidkörpern, durch geeignete Maßnahmen zu erhöhen und einen verbesserten Schneideinsatz zu schaffen.It is an object of the present invention to determine the susceptibility to cracking, corrosion resistance and wear resistance of coated composite materials, in particular cutting bodies, through suitable measures and to create an improved cutting insert.
Diese Aufgabe wird durch das Verfahren nach Anspruch 1 gelöst. Erfindungsgemäß besitzt das Strahlmittel einen maximalen Durchmesser von 150 μm, vorzugsweise von maximal 100 μm. Überraschenderweise führt die Verwendung von derart feinkörnigen Strahlmitteln, die trocken ohne Wasser oder sonstigen Flüssigkeitszusatz verwendet werden, zu dem überraschenden Ergebnis, daß die Druckspannungen der äußeren Schicht in weitaus stärkerem Maße erhöht werden bzw., sofern die äußere Schicht innere Zugspannungen aufweist, die Zugspannungen mittels der trockenen Strahlbehandlung deutlich minimiert werden können bis hin zur Umkehrung in eine Druckspannung in der äußeren Schicht. Je nach Dauer und Intensität der Strahlbehandlung ändert sich auch in gleichförmiger Weise die innere Spannung der unter der Deckschicht liegenden Schichten bis hin zur Beeinflussung der oberflächennahen Randzonen des Substratkörpers. Im Idealfall kann somit ein Verbundkörper mit einer mehrlagigen Beschichtung durch trockene mechanische Strahlbehandlung erzeugt werden, dessen Schichten ausnahmslos innere Druckspannungen aufweisen, wobei die Deckschicht eine intensive Verfestigung und damit erhöhte Verschleißbeständigkeit erfahren hat. Die feinkörnigen pulverartigen Strahlmittel sind auch im wesentlichen nicht, zumindest aber deutlich weniger abrasiv als die bisher nach dem Stand der Technik verwendeten gröberen Körnungen. Ein weiterer Vorteil dieser trockenen Strahlbehandlung liegt darin, daß die Schichtoberfläche erheblich besser geglättet wird als dies durch bisherige Strahlbehandlung oder Bürsten erreichbar war.This object is achieved by the method according to claim 1. According to the invention, the blasting medium has a maximum diameter of 150 μm, preferably a maximum of 100 μm. Surprisingly, the use of such fine-grained abrasives, which are used dry without water or other liquid addition, leads to the surprising result that the compressive stresses of the outer layer are increased to a much greater extent or, if the outer layer has internal tensile stresses, the tensile stresses by means of dry blasting treatment can be significantly minimized up to a reversal of compressive stress in the outer layer. Depending on the duration and intensity of the blasting treatment, the internal tension of the layers lying under the cover layer also changes in a uniform manner to the extent that the edge zones of the substrate body near the surface are influenced. In the ideal case, a composite body with a multi-layer coating can thus be produced by dry mechanical blasting treatment, the layers of which, without exception, have internal compressive stresses, the top layer having undergone intensive consolidation and thus increased wear resistance. The fine-grained powdery abrasives are also essentially not, but at least significantly less abrasive, than the coarser grains previously used in the prior art. A further advantage of this dry blasting treatment is that the layer surface is smoothed considerably better than was previously possible with blasting treatment or brushing.
In der WO 99/23275 wird zwar die Verwendung eines aus Al203-Partikeln mit einer Größe von 30 μm bestehenden Strahl- mittels vorgeschlagen, jedoch soll dies in Form einer Suspension als Naßstrahlmittel angewendet werden, das unter einem Druck von 2 bis 6 bar (x 105 Pa) , vorzugsweise 3 bar benutzt werden soll. Die dort beschriebene Naßstrahlbehandlung bezieht sich jedoch ausschließlich auf die konkrete Schichtfolge mit einer unteren Αl203-Schicht, auf der eine äußere Schicht aufgetragen worden ist, die aus TiN oder einer Viellagenschicht aus TiN/TiC besteht. Das zur Beschichtung verwendete CVD-Verfahren führt augenscheinlich zu (Zug-) Spannungen, die mittels des Naßstrahlens minimiert werden sollen. Das Naßstrahlen mit einem Al203-Abrasionsmittel dient jedoch primär der Ober- flächenglättung, wohingegen die erzielbare Änderung der inneren Spannungen gegenüber einer Trockenstrahlbehandlung deutlich minimiert ist.WO 99/23275 describes the use of a beam consisting of Al 2 0 3 particles with a size of 30 μm. proposed, but this should be used in the form of a suspension as a wet blasting agent, which should be used under a pressure of 2 to 6 bar (x 10 5 Pa), preferably 3 bar. The wet jet treatment described there, however, relates exclusively to the specific layer sequence with a lower Αl 2 0 3 layer on which an outer layer has been applied, which consists of TiN or a multi-layer layer of TiN / TiC. The CVD process used for coating apparently leads to (tensile) stresses, which should be minimized by means of wet blasting. However, wet blasting with an Al 2 0 3 abrasive primarily serves to smooth the surface, whereas the achievable change in internal stresses compared to dry blasting treatment is significantly minimized.
Dies wird auch daran deutlich, daß in dieser Druckschrift die Befürchtung ausgesprochen wird, daß eine unmittelbar auf eine Al203-Schicht abgeschiedene TiN-Schicht eine nur geringe Haftfestigkeit hat, weshalb vorzugsweise eine Zwischenlage aus (Ti,Al) (C,0,N) bevorzugt werden sollen.This is also evident from the fact that this document expresses the fear that a TiN layer deposited directly on an Al 2 0 3 layer has only a low adhesive strength, which is why an intermediate layer of (Ti, Al) (C, 0 , N) should be preferred.
Entsprechendes gilt auch für das in der EP 0 727 510 A2 beschriebene Naßstrahlbehandeln einer Aluminiumoxid-Beschichtung. Das an der Oberfläche vorliegende K-Aluminiumoxid soll abschließend bei einer Temperatur von 900°C bis 1100°C für 0,3 bis 10 Stunden wärmebehandelt werden, um das naßgestrahlte K-Aluminiumoxid in α-Aluminiumoxid umzuwandeln.The same also applies to the wet jet treatment of an aluminum oxide coating described in EP 0 727 510 A2. The K-aluminum oxide present on the surface should finally be heat-treated at a temperature of 900 ° C to 1100 ° C for 0.3 to 10 hours in order to convert the wet-blasted K-aluminum oxide into α-aluminum oxide.
Weiterbildungen der Erfindung sind in den ünteransprüchen beschrieben.Further developments of the invention are described in the subordinate claims.
So weist das Strahlmittel zumindest im wesentlichen eine rundliche Korngestalt auf, dessen Durchmesser vorzugsweise zwi- sehen 5 bis 150 μm, weiterhin vorzugsweise zwischen 10 bis 100 μm liegt. Bei jeweils größeren Körnungen besteht die Gefahr einer stärkeren Abrasion der aufgetragenen Deckschicht bis hin zu einem völlig unerwünschten Abtragen dieser äußeren Deckschicht sowie angrenzender darunterliegender Schichten. Bei kleineren Strahlmittel-Korngrößen reduziert sich demgegenüber die abrasive Wirksamkeit der trockenen Strahlmittelbehandlung erheblich.The blasting agent has at least essentially a rounded grain shape, the diameter of which is preferably between see 5 to 150 microns, further preferably between 10 to 100 microns. With larger grits, there is a risk of greater abrasion of the applied top layer to a completely undesired removal of this outer top layer and adjacent layers underneath. In contrast, with smaller abrasive grain sizes, the abrasive effectiveness of the dry abrasive treatment is considerably reduced.
Als Strahlmittel wird vorzugsweise druckverdüster Stahl, Gußeisengranulat, Schwermetallpulver oder hieraus hergestellte Legierungen oder Hartmetallgranulate und/oder bruchfeste Keramik verwendet. Diese Strahlmittel zeichnen sich durch eine große Bruchfestigkeit aus, so daß ein Zerspringen der Körner zu scharfkantigen kleineren Körnern, die dann die Verbundkörperoberfläche stärker beschädigen können, vermieden wird.Pressure-atomized steel, cast iron granules, heavy metal powder or alloys or carbide granules and / or break-resistant ceramics produced therefrom are preferably used as blasting agents. These abrasives are characterized by a high breaking strength, so that the grains do not crack into smaller, sharp-edged grains, which can then damage the composite surface more severely.
Nach einer weiteren Erkenntnis der Erfindung wird das oder werden die Strahlmittel mittels Preßluft unter einem Druck von mindestens 5 x 105 Pa bis maximal 106 Pa, vorzugsweise zwischen 6 x 105 Pa bis 7 x 105 Pa auf den beschichteten Substratkörper gerichtet. Die verwendeten Strahldrucke liegen damit erheblich über den üblicherweise nach dem Stand der Technik (bei Verwendung eines grobkörnigeren Strahlmittels) verwendeten Drucken.According to a further finding of the invention, the abrasive is or are directed onto the coated substrate body by means of compressed air under a pressure of at least 5 × 10 5 Pa to a maximum of 10 6 Pa, preferably between 6 × 10 5 Pa and 7 × 10 5 Pa. The jet prints used are therefore considerably higher than the pressures usually used according to the prior art (when using a coarser-sized blasting agent).
Grundsätzlich ist es möglich, daß Strahlmittel; unter beliebigen Winkeln auf die Verbundkörperoberfläche zu richten, jedoch erhöht sich die Wirkung, wenn das Strahlmittel im wesentlichen senkrecht auf die Verbundkörperoberfläche gerichtet wird.Basically, it is possible that blasting media ; to be directed at the composite surface at any angle, but the effect increases if the abrasive is directed essentially perpendicular to the composite surface.
Nach einer Weiterbildung der Erfindung wird die Strahlbehandlung so lange durchgeführt, bis auch die unter einer äußeren Schicht oder einer äußersten Schicht liegenden Bereiche bzw. Schichten, vorzugsweise bis in die oberflächennahen Zonen des Substratkörpers hinein, eine Veränderung der inneren Spannungen, d.h. entweder Erhöhung der Druckspannungen oder Minimierung der Zugspannungen erfahren haben. Durch entsprechende Wahl des Strahldruckes und Behandlungsdauer lassen sich somit gezielt auch die inneren Spannungen der unter der Deckschicht liegenden Schichten beeinflussen.According to a development of the invention, the blasting treatment is carried out until the one under an external one Layer or an outermost layer lying areas or layers, preferably up into the near-surface zones of the substrate body, have experienced a change in the internal stresses, ie either an increase in the compressive stresses or a minimization of the tensile stresses. By appropriate selection of the jet pressure and duration of treatment, the internal tensions of the layers lying under the cover layer can also be influenced in a targeted manner.
Überraschenderweise konnten mit einem Schneideinsatz gemäß Anspruch 7 erheblich verbesserte Standzeiten beim Zerspanen erreicht werden. Erstmals ist es gelungen, in einer äußeren bzw. äußersten Schicht, die mittels PCVD oder CVD aufgetragen worden ist, Druckeigenspannungen zu erzeugen, die > 4 GPa, vorzugsweise 4,5 bis 10 GPa betragen. Solche Druckeigenspannungen waren bisher allenfalls in PVD-Schichten, die nachbehandelt worden sind, erreichbar.Surprisingly, with a cutting insert according to claim 7, significantly improved tool life could be achieved. For the first time, it has been possible to generate residual compressive stresses in an outer or outermost layer, which has been applied by means of PCVD or CVD, which are> 4 GPa, preferably 4.5 to 10 GPa. Previously, such residual compressive stresses could only be achieved in PVD layers that have been post-treated.
Der Substratkörper kann ein Hartmetall, ein Hartmetall mit einem Randzonengradienten, ein Cermet oder eine Oxid- oder Nitridkeramik sein. Der Substratkörper wird vorzugsweise mit einer Beschichtung aus Carbiden, Nitriden, Carbonitriden, Oxi- carbonitriden und/oder Boriden der Elemente der IVa bis Vla-Gruppe des Periodensystems, borhaltigen HartstoffVerbindungen und/oder oxidischen Verbindungen des Aluminiums und/oder Zirkoniums beschichtet. Die Schichtdicke einer einzelnen Schicht liegt zwischen 0,1 μm und maximal 10 μm. Die Gesamtschichtdicke einer mehrlagigen Beschichtung soll bevorzugt < 20 μm betragen.The substrate body can be a hard metal, a hard metal with an edge zone gradient, a cermet or an oxide or nitride ceramic. The substrate body is preferably coated with a coating of carbides, nitrides, carbonitrides, oxicarbonitrides and / or borides of the elements of the IVa to Vla group of the periodic table, boron-containing hard material compounds and / or oxidic compounds of aluminum and / or zirconium. The layer thickness of a single layer is between 0.1 μm and a maximum of 10 μm. The total layer thickness of a multilayer coating should preferably be <20 μm.
Die Druckeigenspannungen werden röntgenographisch nach dem sin2ψ-Verfahren gemessen. Das Verfahren wird beispielsweise in der Veröffentlichung HTM43 (1988) 4, Seiten 208 bis 211, "Röntgenographische Eigenspannungsmessungen an texturbehafteten PVD-Schichten aus Titancarbid" von B. Eigenmann, B. Scholtes und E. Macherauch.The residual compressive stresses are measured by X-ray analysis using the sin 2 ψ method. The method is described, for example, in the publication HTM43 (1988) 4, pages 208 to 211, "Roentgenographic residual stress measurements on texture-based PVD layers made of titanium carbide" by B. Eigenmann, B. Scholtes and E. Macherauch.
Die erfindungsgemäß gemessenen Eigenspannungswerte werden an mindestens einer Gitterebene erreicht. Die vorgeschlagene Strahlbehandlung erfaßt zumindest den gesamten für die jeweiligen Zerspanungsoperationen verwendeten Schneidenbereich eines Schneideinsatzes.The residual stress values measured according to the invention are achieved on at least one grid level. The proposed beam treatment covers at least the entire cutting area of a cutting insert used for the respective machining operations.
Die Erfindung wird im folgenden anhand von Ausführungsbeispielen näher erläutert:The invention is explained in more detail below on the basis of exemplary embodiments:
Beispiel 1example 1
Schneidkörper des Typs CNMG 120412 mit Spanformrille für mittlere bis mittelschwere Schnittbedingungen aus P 20 Hartmetall (WC/TaC/NbC/TiC/7, 5% Co) mit mischcarbidfreier Randzone und einer am Substrat beginnenden CVD-Beschichtung TiN-TiCN(MT CVD) -Al203-ZrCN bei einer Gesamtschichtdicke von 18 μm wurden nach der Beschichtung einer Trockenstrahlbehandlung nach dem Injektor-Gravitations-Strahlverfahren mit Zir- konoxidkeramik-Granulat, druckverdüstem Stahlpulver und gesintertem Hartmetallsprühgranulat unterworfen, die Eigenspannungen nach dem sin2ψ-Verfahren röntgendiffraktometrisch an jeweils mindestens zwei Gitterebenen bestimmt (die darauf gebildeten Mittelwerte sind in der Tabelle 1 angegeben) und im Drehtest mit stark unterbrochenen Schnitt (Leistendrehtest) auf rostfreiem martensitischem Stahl auf Schneidhaltigkeit geprüft (v = 150 m/min, ap = 2,0 mm, f = 0,35 mm/U): Tabelle 1CNMG 120412 cutting body with chip-forming groove for medium to medium-heavy cutting conditions made of P 20 hard metal (WC / TaC / NbC / TiC / 7.5% Co) with mixed carbide-free edge zone and a CVD coating TiN-TiCN (MT CVD) beginning on the substrate - Al 2 0 3 -ZrCN with a total layer thickness of 18 μm were subjected to a dry blast treatment after the coating with the injector gravitational blasting method with zirconium oxide ceramic granulate, pressure-atomized steel powder and sintered hard metal spray granulate, the residual stresses according to the sin 2 ψ method by X-ray diffraction at least two grating planes were determined (the mean values formed on them are given in Table 1) and tested for cutting stability in the rotary test with a strongly interrupted cut (last turning test) on stainless martensitic steel (v = 150 m / min, a p = 2.0 mm, f = 0.35 mm / rev): Table 1
vOvO
Vorzeichen + steht für Zugeigenspannungen, - steht für Druckeigenspannungen Sign + stands for residual tensile stress, - stands for residual compressive stress
Beispiel 2Example 2
Zur Verbesserung des Glätteffektes wurde für die Stahlbehandlung mit Hartmetallgranulat gemäß obenstehender Tabelle ca. 5 % Gußhartmetallsplitt in der Körnung 50 - 100 μm als abrasiv wirkende Komponente zugemischt. Unter den gleichen Bedingungen, wie sie für Hartmetallgranulat oben beschrieben sind, vermindert sich die Rauhtiefe um ca. 1/3. Die Änderung der Eigenspannungen bleibt davon unbeeinflußt.In order to improve the smoothing effect, approx. 5% cast hard metal chippings with a grain size of 50 - 100 μm were added as an abrasive component for the steel treatment with hard metal granules according to the table above. Under the same conditions as described for hard metal granulate, the roughness depth is reduced by approx. 1/3. The change in the residual stresses remains unaffected.
Beispiel 3Example 3
Schneidkörper des Typs SEKN 1203 AF.N mit umlaufender Spanflächenfase (15°/0,2 mm) aus K 20 Hartmetall ( C/6,2%Co) mit einer am Substrat beginnenden CVD-Beschichtung TiN-TiCN(MT CVD) -Al203-TiN mit einer Gesamtschichtdicke von 11 μm wurden nach der Beschichtung einer Trockenstrahlbehandlung nach dem Injektor-Gravitations-Strahlverfahren mit Stahlkies, Hartmetallgranulat und Wolframmetallpulver unterworfen, wie in Beispiel 1 beschrieben, Eigenspannungen bestimmt und im Einzahn-Frästest (Planfräsen) auf Kugelgraphitguss GGG60 auf Schneidhaltigkeit geprüft (v = 250 m/min, ap = 2,0 mm, fz = 0,25 mm/Zahn, vf = 200 mm/min) (siehe Tabelle 2): SEKN 1203 AF.N cutter body with all-round rake face (15 ° / 0.2 mm) made of K 20 hard metal (C / 6.2% Co) with a CVD coating TiN-TiCN (MT CVD) -Al beginning on the substrate 2 0 3 -TiN with a total layer thickness of 11 μm were subjected, after coating, to a dry blast treatment using the injector gravitational blasting method with steel gravel, hard metal granules and tungsten metal powder, as described in Example 1, residual stresses were determined and in the single-tooth milling test (face milling) on spheroidal graphite cast iron GGG60 tested for cutting edge stability (v = 250 m / min, a p = 2.0 mm, f z = 0.25 mm / tooth, v f = 200 mm / min) (see table 2):
Tabelle 2Table 2
Vorzeichen + steht für Zugeigenspannungen, - steht für Druckeigenspannungen Sign + stands for residual tensile stress, - stands for residual compressive stress
Die vorstehenden Tabellen zeigen, daß eine Trockenstrahlbehandlung erhebliche Standzeitverbesserungen der Schneidkörper bewirkt. Die besten Ergebnisse konnten mit druckverdüstem Stahlpulver, Hartmetallgranulat und Wolframpulver erreicht werden. The tables above show that dry blast treatment brings about considerable improvements in the service life of the cutting bodies. The best results were achieved with pressure-atomized steel powder, hard metal granulate and tungsten powder.

Claims

Patentansprüche claims
1. Verfahren zur Erhöhung der Druckeigenspannung oder zur Erniedrigung der Zugeigenspannung einer äußeren oder einer äußersten, mittels CVD, PCVD oder PVD auf einen Hartmetall-, Cermet-, oder Keramiksubstratkörper aufgetragenen Hartstoffschicht r bei dem der beschichtete Substratkörper nach dem Beschichten einer Trockenstrahlbehandlung unter Verwendung eines körnigen Strahlmittels unterzogen wird, d a d u r c h g e k e n n z e i c h n e t, daß das Strahlmittel einen maximalen Durchmesser von 150 μm, vorzugsweise von maximal 100 μm aufweist.1. A method for increasing the compressive residual stress or for lowering the tensile residual stress of an outer or an outermost hard layer r applied by means of CVD, PCVD or PVD on a hard metal, cermet or ceramic substrate body, in which the coated substrate body after coating a dry blasting treatment using a granular abrasive is subjected to, characterized in that the abrasive has a maximum diameter of 150 microns, preferably a maximum of 100 microns.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Strahlmittel zumindest im wesentlichen eine rundliche Korngestalt aufweist, dessen Durchmesser vorzugsweise zwischen 5 bis 150 μm, weiterhin vorzugsweise 10 bis 100 μm liegt.2. The method according to claim 1, characterized in that the blasting agent has at least substantially a rounded grain shape, the diameter of which is preferably between 5 to 150 microns, further preferably 10 to 100 microns.
3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß als Stahlmittel druckverdüster Stahl, Gußeisengranulat, Schwermetallpulver oder hieraus hergestellte Legierungen oder Hartmetallgranulate und/oder bruchfeste Keramiken verwendet werden.3. The method according to claim 1 or 2, characterized in that pressure-atomized steel, cast iron granules, heavy metal powder or alloys or carbide granules and / or break-resistant ceramics produced therefrom are used as the steel medium.
4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß das oder die Strahlmittel mittels Preßluft unter einem Druck von mindestens 5 x 105 Pa bis maximal 106 Pa, vorzugsweise 6 x 105 Pa bis 7 x 105 Pa auf den beschichteten Substratkörper gerichtet wird. 4. The method according to any one of claims 1 to 3, characterized in that the or the blasting agent by means of compressed air under a pressure of at least 5 x 10 5 Pa to a maximum of 10 6 Pa, preferably 6 x 10 5 Pa to 7 x 10 5 Pa the coated substrate body is directed.
5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß das Strahlmittel im wesentlichen senkrecht auf die Substratkörperoberfläche gerichtet wird.5. The method according to any one of claims 1 to 4, characterized in that the blasting agent is directed substantially perpendicular to the substrate body surface.
6. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß die Strahlbehandlung so lange durchgeführt wird, bis auch die unter einer äußeren Schicht oder einer äußersten Schicht liegenden Bereiche, vorzugsweise bis in die oberflächennahen Zonen des Substratkörpers hinein, eine Absenkung der inneren Zugspannungen (entweder Erhöhung der Druckspannungen oder Minimierung der Zugspannungen) erfahren haben.6. The method according to any one of claims 1 to 5, characterized in that the blasting treatment is carried out until the areas lying under an outer layer or an outermost layer, preferably up to the surface-near zones of the substrate body, a lowering of the inner Have experienced tensile stresses (either increasing the compressive stresses or minimizing the tensile stresses).
7. Schneideinsatz zum Zerspanen, bestehend aus einem Hartmetall-, Cermet-, oder Keramik-Substratkörper mit einer ein- oder mehrlagigen Beschichtung aus Carbiden, Nitriden, Car- bonitriden, Oxicarbonitriden und/oder Boriden der Elemente der IVa bis Vla-Gruppe des Periodensystems, borhaltigen Hartstoffverbindungen und/oder oxidischen Verbindungen des Aluminiums und/oder Zirkoniums, die mittels eines PCVD- oder CVD-Verfahrens aufgetragen worden sind, dadurch gekennzeichnet, daß die Druckeigenspannung in der äußeren bzw. äußersten Schicht > 4 GPa, vorzugsweise 4,5 bis7. Cutting insert for machining, consisting of a hard metal, cermet or ceramic substrate body with a single or multi-layer coating of carbides, nitrides, carbonitrides, oxicarbonitrides and / or borides of the elements of the IVa to Vla group of the periodic table , boron-containing hard material compounds and / or oxidic compounds of aluminum and / or zirconium, which have been applied by means of a PCVD or CVD process, characterized in that the residual compressive stress in the outer or outermost layer is> 4 GPa, preferably 4.5 to
10 GPa beträgt.Is 10 GPa.
8. Schneideinsatz nach Anspruch 7, dadurch gekennzeichnet, daß der Substratkörper aus einem Hartmetall mit einer sich zu seiner oberflächennahen Randzonen ändernden Hartstoffzusammensetzungen oder -gehalt (Hartstoffgradient) besteht.8. Cutting insert according to claim 7, characterized in that the substrate body consists of a hard metal with a hard material composition or content (hard material gradient) which changes to its edge zones near the surface.
9. Schneideinsatz nach Anspruch 7, dadurch gekennzeichnet, daß der Substratkörper einer Oxid- oder Nitridkeramik ist. 9. Cutting insert according to claim 7, characterized in that the substrate body is an oxide or nitride ceramic.
0. Schneideinsatz nach einem der Ansprüche 7 bis 9, dadurch gekennzeichnet, daß die Schichtdicke einer einzelnen Schicht mindestens 0,1 μm und maximal 10 μm und/oder bei einer mehrlagigen Beschichtung die Gesamtschichtdicke < 20 μm beträgt. 0. Cutting insert according to one of claims 7 to 9, characterized in that the layer thickness of a single layer is at least 0.1 μm and a maximum of 10 μm and / or in the case of a multi-layer coating the total layer thickness is <20 μm.
EP01991711A 2001-03-27 2001-12-22 Method for increasing compression stress or reducing internal tension stress of a cvd, pcvd or pvd layer and cutting insert for machining Withdrawn EP1311712A2 (en)

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US6884496B2 (en) 2005-04-26
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