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EP1664363A1 - Hard metal or cermet body and method for producing the same - Google Patents

Hard metal or cermet body and method for producing the same

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Publication number
EP1664363A1
EP1664363A1 EP04732930A EP04732930A EP1664363A1 EP 1664363 A1 EP1664363 A1 EP 1664363A1 EP 04732930 A EP04732930 A EP 04732930A EP 04732930 A EP04732930 A EP 04732930A EP 1664363 A1 EP1664363 A1 EP 1664363A1
Authority
EP
European Patent Office
Prior art keywords
mass
layer
volume
carbonitrides
nitrides
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.)
Granted
Application number
EP04732930A
Other languages
German (de)
French (fr)
Other versions
EP1664363B1 (en
Inventor
Walter Lengauer
Vera Ucakar
Klaus Dreyer
Dieter Kassel
Hans Werner Daub
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.)
Kennametal Widia Produktions GmbH and Co KG
Original Assignee
Kennametal Widia Produktions GmbH and Co KG
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
Application filed by Kennametal Widia Produktions GmbH and Co KG filed Critical Kennametal Widia Produktions GmbH and Co KG
Priority to PL04732930T priority Critical patent/PL1664363T3/en
Publication of EP1664363A1 publication Critical patent/EP1664363A1/en
Application granted granted Critical
Publication of EP1664363B1 publication Critical patent/EP1664363B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • B22F3/101—Changing atmosphere
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • 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
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/76—Adjusting the composition of the atmosphere
    • 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 hard metal or cermet body having a hard material phase of WC and at least one carbide, nitride, carbonitride or oxicarbonitride of at least one of the elements of the IVa or Va group of the periodic table and having a binder phase of Fe, Co and / or Ni whose Proportion is 3-25 mass%, with a single or multiple contiguous surfaces, with a 2-1 OO ⁇ m thick first layer below the single or at least one of the surfaces, having a binder metal content of 2-25 mass% and up to 25% by volume of nitrides or carbonitrides of one or more metals of the IVa group of the Periodic Table and / or up to 10% by volume of carbides and / or carbonitrides of V, Nb, Ta and / or Cr.
  • the invention further relates to a method for producing the aforementioned body, which after sintering or during sintering has undergone a first heat treatment to produce the aforesaid layer.
  • the nitrogen required for the nitroxide can be converted to the cemented carbide both by a nitrogen atmosphere used and in the form of nitrides or carbonitrides of one of the hard material carbides. be fed mixture approach.
  • the sintering is introduced under vacuum so that the gradient zone formation can occur.
  • the gradient zone can also be obtained by subjecting the cemented carbide, after sintering in the temperature range from about 1150 to at most 1300 ° C., to a nitrogen treatment under elevated pressure.
  • the sintering of the hard metal by dewaxing to 600 ° C, holding, heating to sintering temperature and subsequent vacuum sintering at 0.1 to 100 Pa and then pressure sintering done.
  • the sintered body is subjected to a pressure treatment with a nitrogen at 1 to 10 MPa and a subsequent vacuum treatment at 10 to 100 Pa.
  • DE 197 52 289 C1 states that a subsequent mechanical finish machining of the substrate body for producing a final contour is accompanied by an at least partial removal of the edge zones, so that the properties of the gradient zones which are assessed to be positive are completely or partially lost again.
  • DE 197 52 289 proposes to post-treat the substrate body in a vacuum at about 600-1300 ° C. for a period of up to 150 min after finish-machining.
  • a surface marginal zone is formed on the machined surfaces, enriched with binder metals and free of cubic mixed carbide.
  • the thickness of this view is 5-35 ⁇ m.
  • the wear resistance of such carbide or cermet body is to be improved, which are used as cutting tools.
  • the cemented carbide or cermet body has, beneath a 2 to 100 ⁇ m thick first layer with increased binder content and a reduced proportion of mixed carbides, a further 2 to 40 ⁇ m thick second layer which has a higher nitrogen content than the first layer and which consists essentially of nitrides and / or carbonitrides of the metals of the IVa group of the Periodic Table and phase proportions of up to 10% by volume of »carbides, nitrides, carbonitrides or oxycarbonitrides of the elements, Mo, V, Ta, Nb, Cr and / or dissolved in the hard material phase Amounts of up to 5 mass% V, Nb, Ta and up to 2 mass% Cr, Mo, W and contains up to 15 mass% binder.
  • this second layer is a transition zone having a thickness of 2 to 100 ⁇ m, in which the composition gradually changes to a homogeneous composition in the interior of the core of the cemented carbide or cermet body.
  • a relatively tough and abrasive resistant zone is given with high levels of WC
  • underlying layer is a diffusion-resistant, hard layer with high nitride or carbonitride proportions.
  • said first layer has only up to 2% by mass of carbides or carbonitrides of at least one of the metals V, Nb, Ta and / or Cr.
  • the first layer has a composition consisting of 4 to 15 mass% or 7 to 22 volume% binder metal (s), 80 to 96 mass% or 66 to 93 volume% WC and 0 to 5 mass% or 0 to 12 volume% TiCN and / or TiN.
  • the total amount of the aforementioned substances gives 100 mass% or 100 volume%.
  • the second layer preferably has 3 to 15 mass% or 2 to 15 volume%
  • the nitrogen content in said second layer is from 8 to 22 mass% when the nitrides in that layer are present exclusively as metal nitrides.
  • the nitride level decreases in the presence of metal carbonitrides as nitrogen is replaced by carbon.
  • the nitrogen content of the second layer is thus preferably minimized to half, ie to 4 to 22 mass%.
  • the object is also achieved by a body according to claim 6.
  • the binder metal enriched and mixed carbide depleted first layer has been abraded, etched away or removed by other methods on one or more surfaces so that the cemented carbide or cermet body beneath the surface in question has the layer structure of claim 3.
  • the hard metal or cermet body can additionally have a single-layer or multi-layer coating on at least one surface.
  • This coating may consist of carbides, nitrides, carbonitrides, oxides, oxynitrides of the elements of the IVa-Vla group of the Periodic Table, but also Al 2 O 3 , ZrO 2) HfO 2 , AlON or carbon, preferably as diamond or molybdenum or tungsten sulfides ,
  • the number of additional layers applied for example by means of PVD or CVD, and the choice of layer compositions depend on the intended use.
  • the process according to claim 8 is used to produce the above-described cemented carbide or cermet body.
  • the cemented carbide or cermet body produced by powder metallurgy is subjected to a first heat treatment to produce a binder metal-enriched 2-100 ⁇ m thick layer and then additionally subjected to this heat treatment of a nitrogen atmosphere under a nitrogen pressure of 50 mbar (5 ⁇ 10 3 Pa) to 1 OObar (10 7 Pa) below the eutectic, preferably treated at 1000 ° C to 1200 ° C.
  • the binder metal-enriched and mixed-carbide-depleted first layer remains in its composition in the Essentially unchanged.
  • the first near-surface layer thus has the effect of a membrane which allows nitrogen to pass in from the outside in, while at the same time inhibiting diffusion of nitrogen-affine metals to the outside.
  • this membrane-like effect occurs only in a temperature range below the eutectic, namely at 1000 to 1200 ° C.
  • titanium or other nitrogen-affine metals diffuse in the direction of the substrate body surface, where they form corresponding nitrides in the near-surface edge zones.
  • the nitrogen diffusion slows down, so that the desired effect of nitrogen enrichment in the second layer practically no longer occurs. Compliance with the temperature limits in the second heat treatment is thus crucial for the success of the method according to the invention.
  • the resulting layer below at least one surface by grinding, etching or other methods to remove before the body in a nitrogen atmosphere under a Nitrogen pressure 5 x 10 3 Pa to 10 7 Pa below the eutectic, preferably at temperatures between 1000 ° C and 1200 ° C is treated.
  • a nitrogen-enriched, 2 to 40 ⁇ m thick layer with a higher nitrogen content forms immediately below the surface.
  • This method can be used, in particular, for substrate bodies which serve as cutting tools, the layer sequences a) to c) described in claim 1 being present underneath the free surface while on the chip surface. surface or at least in the region near the cutting edge of the rake surface only a layer sequence according to b) and c) or claim 3 is present.
  • the life in continuous section measured by the wear mark width and the Kolktiefe could be increased by 8 to 10 times.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)
  • Powder Metallurgy (AREA)
  • Polishing Bodies And Polishing Tools (AREA)
  • Ceramic Products (AREA)
  • Adornments (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

The invention relates to a hard metal or cermet body comprising a single or several adjoining surfaces. A first layer with a thickness of between 2-100 νm is located beneath the single surface or at least one of the surfaces, said layer comprising an auxiliary metal fraction of between 2 and 25 mass % and up to 25 volume % nitrides or carbonitrides of one or more metals of the IVa group of the periodic table and/or up to 10 volume % carbides and/or carbonitrides of the elements V, Nb, Ta and/or Cr, with WC making up the residual amount. A second layer with a thickness of between 2 and 40 νm is located beneath the first layer, said second layer having a higher nitrogen fraction than the first layer and consisting essentially of nitrides and/or carbonitrides of metals of the IVa group of the periodic table, in addition to containing phase fractions of up to 10 volume % of carbides, nitrides, carbonitrides or oxycarbonitrides of the elements W, Mo, V, Ta, Nb, Cr and/or fractions that are dissolved in the hard substance phase amounting to up to 5 mass % V, NB, TA and up to 2 mass % CR, Mo, W and also containing up to 15 mass % binding agents. A transition zone with a thickness of between 2 and 100 νm is located beneath the second layer, the composition changing gradually to a homogeneous composition in the interior core of the hard metal or cermet body in said zone. To produce said sequence of layers, after being subjected to thermal treatment to produce a layer rich in an auxiliary metal, the body is treated in a nitrogen atmosphere under a nitrogen pressure of 5x103Pa to 107Pa below the eutectic.

Description

Hartmetall- oder Cermetkörper und Verfahren zu seiner HerstellungCarbide or cermet body and process for its preparation

Die Erfindung betrifft einen Hartmetall- oder Cermetkörper mit einer Hartstoffphase aus WC und mindestens einem Carbid, Nitrid, Carbonitrid oder Oxicarbonitrid mindestens eines der Elemente der IVa- oder Va-Gruppe des Periodensystems und mit einer Binderphase aus Fe, Co und/oder Ni, deren Anteil 3-25 Massen% beträgt, mit einer einzigen oder mit mehreren aneinander grenzender Oberflächen, wobei unterhalb der einzigen oder zumindest einer der Oberflächen eine 2-1 OOμm dicke erste Schicht angeordnet ist, die einen Bindemetallanteil von 2-25 Massen% und bis zu 25 Volumen% Nitride oder Carbonitride eines oder mehrerer Metalle der IVa-Gruppe des Periodensystems und/oder bis zu 10 Volumen% Carbide und/oder Carbonitride des V, Nb, Ta und/oder Cr aufweist.The invention relates to a hard metal or cermet body having a hard material phase of WC and at least one carbide, nitride, carbonitride or oxicarbonitride of at least one of the elements of the IVa or Va group of the periodic table and having a binder phase of Fe, Co and / or Ni whose Proportion is 3-25 mass%, with a single or multiple contiguous surfaces, with a 2-1 OOμm thick first layer below the single or at least one of the surfaces, having a binder metal content of 2-25 mass% and up to 25% by volume of nitrides or carbonitrides of one or more metals of the IVa group of the Periodic Table and / or up to 10% by volume of carbides and / or carbonitrides of V, Nb, Ta and / or Cr.

Die Erfindung betrifft ferner ein Verfahren zur Herstellung des vorgenannten Körpers, der nach dem Sintern oder während des Sinterns einer ersten Wärmebehandlung zur Erzeugung der vorgenannten Schicht unterzogen worden ist.The invention further relates to a method for producing the aforementioned body, which after sintering or during sintering has undergone a first heat treatment to produce the aforesaid layer.

In der DE 197 52 289 C1 wird unter Hinweis auf diverse Literaturstellen ausgeführt, dass eine oberflächennahe, binderreiche und mischcarbϊdarme Zone einen großen Einfluss auf die Zähigkeit des Substratkörpers und auf die Haftung einer etwa auf diesem Substratkörper aufgetragenen Beschichtung hat. Der Abtransport der kubischen Mischcarbidphase verläuft über einen Aufstickung sprozess durch Zugabe von Stickstoff, der in einer nachfolgenden Vakuumbehandlung wieder rückgängig gemacht werden kann und zu einer bevorzugten Auflösung und dem Diffusionstrans- port der Mischcarbidphase im Bindemetall führt. Für die Herstellung der Randzonen bzw. Gradientenstrukturen solcher Substratkörper werden verschiedene Verfahren angegeben: Beispielsweise kann eine Nitrierbehandlung des Hartmetalls unterhalb der Schmelztemperatur der Binderphase durchgeführt werden, wobei anschließend unter Vakuum bis zur Sintertemperatur aufgeheizt wird. Der für die Aufstickung erforderliche Stickstoff kann sowohl durch eine verwendete Stickstoffatmosphäre als auch in Form von Nitriden oder Carbonitriden eines der Hartstoffcarbide zum Hartmetall- mischungsansatz zugeführt werden. Die Sinterung wird unter Vakuum eingeleitet, damit die Gradientenzonenbildung eintreten kann. Die Gradientenzone kann auch dadurch erhalten werden, dass das Hartmetall im Anschluss an die Sinterung im Temperaturbereich von ca. 1150 bis maximal 1300°C einer Stickstoffbehandlung unter erhöhtem Druck ausgesetzt wird. Alternativ hierzu kann die Sinterung des Hartmetalls durch Entwachsen bis 600°C, Halten, Aufheizen auf Sintertemperatur und anschließendes Vakuumsintern bei 0,1 bis 100 Pa und anschließendem Drucksintern erfolgen. Nach Abkühlung des Hartmetall-Formkörpers auf unter 1280°C wird der Sinterkörper einer Druckbehandlung mit einem Stickstoff bei 1 bis 10 MPa und einer anschließenden Vakuumbehandlung bei 10 bis 100 Pa unterzogen.In DE 197 52 289 C1, it is stated with reference to various references that a near-surface, binder-rich and mixed carbondial zone has a great influence on the toughness of the substrate body and on the adhesion of a coating applied approximately to this substrate body. The transport of the cubic mixed carbide phase proceeds via a nitroprocess by addition of nitrogen, which can be reversed in a subsequent vacuum treatment and leads to a preferred dissolution and the diffusion transport of the mixed carbide phase in the binder metal. Various methods are given for the production of the edge zones or gradient structures of such substrate bodies: For example, a nitriding treatment of the cemented carbide below the melting temperature of the binder phase can be carried out, the mixture then being heated up to the sintering temperature under vacuum. The nitrogen required for the nitroxide can be converted to the cemented carbide both by a nitrogen atmosphere used and in the form of nitrides or carbonitrides of one of the hard material carbides. be fed mixture approach. The sintering is introduced under vacuum so that the gradient zone formation can occur. The gradient zone can also be obtained by subjecting the cemented carbide, after sintering in the temperature range from about 1150 to at most 1300 ° C., to a nitrogen treatment under elevated pressure. Alternatively, the sintering of the hard metal by dewaxing to 600 ° C, holding, heating to sintering temperature and subsequent vacuum sintering at 0.1 to 100 Pa and then pressure sintering done. After cooling the hard metal shaped body to below 1280 ° C, the sintered body is subjected to a pressure treatment with a nitrogen at 1 to 10 MPa and a subsequent vacuum treatment at 10 to 100 Pa.

Als nachteilig wird in der DE 197 52 289 C1 angegeben, dass eine anschließende mechanische Finish-Bearbeitung des Substratkörpers zur Herstellung einer Endkontur mit einem zumindest teilweisen Abtrag der Randzonen einhergeht, so dass die als positiv bewerteten Eigenschaften der Gradientenzonen ganz oder teilweise wieder verloren gehen. Um diesen Nachteil zu beheben, wird in der DE 197 52 289 vorgeschlagen, den Substratkörper nach der Finish-Bearbeitung im Vakuum bei etwa 600-1300°C über einen Zeitraum von bis zu 150 Min nachzubehandeln. An den mechanisch bearbeiteten Oberflächen bilde sich hierdurch erneut eine Oberflächen- randzone aus, die mit Bindemetallen angereichert und frei von kubischem Mischcar- bid ist. Die Dicke dieser Sicht beträgt 5-35μm.DE 197 52 289 C1 states that a subsequent mechanical finish machining of the substrate body for producing a final contour is accompanied by an at least partial removal of the edge zones, so that the properties of the gradient zones which are assessed to be positive are completely or partially lost again. To remedy this disadvantage, DE 197 52 289 proposes to post-treat the substrate body in a vacuum at about 600-1300 ° C. for a period of up to 150 min after finish-machining. As a result, once again a surface marginal zone is formed on the machined surfaces, enriched with binder metals and free of cubic mixed carbide. The thickness of this view is 5-35μm.

Es ist Aufgabe der vorliegenden Erfindung, den eingangs genannten Hartmetall- oder Cermetkörper im Hinblick auf seine Verschleißeigenschaften zu verbessern. Insbesondere soll die Verschleißfestigkeit solcher Hartmetall- oder Cermetkörper verbessert werden, die als Zerspanungswerkzeuge eingesetzt werden.It is an object of the present invention to improve the aforementioned hard metal or cermet body with regard to its wear properties. In particular, the wear resistance of such carbide or cermet body is to be improved, which are used as cutting tools.

Diese Aufgabe wird durch einen Hartmetall- oder Cermetkörper nach Anspruch 1 gelöst. Erfindungsgemäß besitzt der Hartmetall- oder Cermetkörper unterhalb einer 2 bis 100 μm dicken ersten Schicht mit erhöhtem Binderanteil und einem verringerten Anteil an Mischcarbiden eine weitere 2 bis 40 μm dicke zweite Schicht, die einen höheren Stickstoffanteil als die erste Schicht besitzt und die im wesentlichen aus Nitriden und/oder Carbonitriden der Metalle der IVa-Gruppe des Periodensystems besteht und Phasenanteile von bis zu 10 Volumen%» an Carbiden, Nitriden, Carbonitriden oder Oxycarbonitriden der Elemente , Mo, V, Ta, Nb, Cr und/oder an in der Hartstoffphase gelösten Anteilen von bis zu 5 Masse% V, Nb, Ta und bis zu 2 Masse% Cr, Mo, W besitzt und bis zu 15 Massen% Binder enthält. Unterhalb dieser zweiten Schicht befindet sich eine Übergangszone mit einer Dicke von 2 bis 100 μm, in der sich die Zusammensetzung graduell zu einer homogenen Zusammensetzung im Kerninneren des Hartmetall- oder Cermetkörpers ändert. In der ersten Schicht ist somit eine relativ zähe und abrasiv beständige Zone mit hohen WC-Anteilen gegeben, während in der zweiten, darunterliegenden Schicht eine diffusionsbeständige, harte Schicht mit hohen Nitrid- oder Carbonitrid-Anteilen liegt.This object is achieved by a cemented carbide or cermet body according to claim 1. According to the invention, the cemented carbide or cermet body has, beneath a 2 to 100 μm thick first layer with increased binder content and a reduced proportion of mixed carbides, a further 2 to 40 μm thick second layer which has a higher nitrogen content than the first layer and which consists essentially of nitrides and / or carbonitrides of the metals of the IVa group of the Periodic Table and phase proportions of up to 10% by volume of »carbides, nitrides, carbonitrides or oxycarbonitrides of the elements, Mo, V, Ta, Nb, Cr and / or dissolved in the hard material phase Amounts of up to 5 mass% V, Nb, Ta and up to 2 mass% Cr, Mo, W and contains up to 15 mass% binder. Below this second layer is a transition zone having a thickness of 2 to 100 μm, in which the composition gradually changes to a homogeneous composition in the interior of the core of the cemented carbide or cermet body. In the first layer thus a relatively tough and abrasive resistant zone is given with high levels of WC, while in the second, underlying layer is a diffusion-resistant, hard layer with high nitride or carbonitride proportions.

Nach einer Weiterbildung der Erfindung besitzt die genannte erste Schicht nur bis zu 2 Massen% Carbide oder Carbonitride mindestens eines der Metalle V, Nb, Ta und/oder Cr.According to a development of the invention, said first layer has only up to 2% by mass of carbides or carbonitrides of at least one of the metals V, Nb, Ta and / or Cr.

Vorzugsweise besitzt die erste Schicht eine Zusammensetzung, bestehend aus 4 bis 15 Massen% oder 7 bis 22 Volumen% Bindemetall(e), 80 bis 96 Massen% oder 66 bis 93 Volumen% WC und 0 bis 5 Massen% oder 0 bis 12 Volumen% TiCN und/oder TiN. Die Gesamtmenge der vorgenannten Stoffe ergibt 100 Massen% oder 100 Volumen%.Preferably, the first layer has a composition consisting of 4 to 15 mass% or 7 to 22 volume% binder metal (s), 80 to 96 mass% or 66 to 93 volume% WC and 0 to 5 mass% or 0 to 12 volume% TiCN and / or TiN. The total amount of the aforementioned substances gives 100 mass% or 100 volume%.

Die zweite Schicht besitzt vorzugsweise 3 bis 15 Massen% oder 2 bis 15 Volumen%The second layer preferably has 3 to 15 mass% or 2 to 15 volume%

Bindemetall(e), 0 bis 50 Massen% oder 0 bis 30 Vol umen% WC und 35 bisBinding metal (s), 0 to 50 mass% or 0 to 30 vol% WC and 35 to

98 Massen% oder 55 bis 98 Volumen% TiCN oder TiN, wobei die Gesamtmenge aus98 mass% or 55 to 98 volume% TiCN or TiN, the total amount being

Bindemetall, WC und TiCN und/oder TiN 100 Massen% oder 100 Volumen% ergeben. Vorzugsweise beträgt der Stickstoffgehalt in der genannten zweiten Schicht 8 bis 22 Massen%, wenn die Nitride in dieser Schicht ausschließlich als Metallnitride vorliegen. Der Nitridanteil sinkt bei der Anwesenheit von Metallcarbonitriden in dem Maß, in dem Stickstoff durch Kohlenstoff ersetzt wird. Bei jeweils hälftig (zu 50 Atom%) vorliegendem TiCN minimiert sich der Stickstoffgehalt der zweiten Schicht somit vorzugsweise auf die Hälfte, d.h. auf 4 bis 22 Massen%.Binder metal, WC and TiCN and / or TiN 100% by mass or 100% by volume. Preferably, the nitrogen content in said second layer is from 8 to 22 mass% when the nitrides in that layer are present exclusively as metal nitrides. The nitride level decreases in the presence of metal carbonitrides as nitrogen is replaced by carbon. With in each case halved (to 50 atomic%) present TiCN, the nitrogen content of the second layer is thus preferably minimized to half, ie to 4 to 22 mass%.

Alternativ wird die Aufgabe auch durch einen Körper gemäß Anspruch 6 gelöst. Bei diesem Körper ist die bindermetallangereicherte und mischcarbidverarmte erste Schicht an einer oder mehreren Oberflächer abgeschliffen, weggeätzt oder durch andere Verfahren entfernt worden, so dass der Hartmetall- oder Cermetkörper unterhalb der betreffenden Oberfläche das Schichtgefüge gemäß Anspruch 3 besitzt.Alternatively, the object is also achieved by a body according to claim 6. In this body, the binder metal enriched and mixed carbide depleted first layer has been abraded, etched away or removed by other methods on one or more surfaces so that the cemented carbide or cermet body beneath the surface in question has the layer structure of claim 3.

Nach einer weiteren Ausgestaltung der Erfindung kann der Hartmetall- oder Cermetkörper zusätzlich auf mindestens einer Oberfläche eine ein- oder mehrlagige Beschichtung aufweisen. Diese Beschichtung kann aus Carbiden, Nitriden, Carbonitriden, Oxiden, Oxinitriden der Elemente der IVa-Vla-Gruppe des Periodensystems, aber auch AI2O3, ZrO2) HfO2, AlON oder Kohlenstoff, vorzugsweise als Diamant oder Molybdän- oder Wolframsulfiden bestehen. Die Zahl der zusätzlichen, beispielsweise mittels PVD oder CVD aufgetragenen Schichten und die Auswahl der Schichtzusammensetzungen richten sich nach den Anwendungszwecken.According to a further embodiment of the invention, the hard metal or cermet body can additionally have a single-layer or multi-layer coating on at least one surface. This coating may consist of carbides, nitrides, carbonitrides, oxides, oxynitrides of the elements of the IVa-Vla group of the Periodic Table, but also Al 2 O 3 , ZrO 2) HfO 2 , AlON or carbon, preferably as diamond or molybdenum or tungsten sulfides , The number of additional layers applied, for example by means of PVD or CVD, and the choice of layer compositions depend on the intended use.

Zur Herstellung des vorbeschriebenen Hartmetall- oder Cermetkörpers wird das Verfahren nach Anspruch 8 verwendet. Der auf pulvermetallurgischem Wege hergestellte Hartmetall- oder Cermetkörper wird nach dem Sintern oder während des Sinterns einer ersten Wärmebehandlung zur Erzeugung einer bindemetallangereicher- ten 2-100μm dicken Schicht einer Wärmebehandlung unterzogen und anschließend zusätzlich an diese Wärmebehandlung einer Stickstoffatmosphäre unter einem Stickstoffdruck von 50mbar (5x103Pa) bis 1 OObar (107Pa) unterhalb des Eutektikums, vorzugsweise bei 1.000°C bis 1.200°C behandelt. Hierbei bleibt die bindemetallange- reicherte und mischcarbidverarmte erste Schicht in ihrer Zusammensetzung im Wesentlichen unverändert. Während der Wärmebehandlung unter Stickstoff wird Stickstoff ins Körperinnere transportiert, wobei gleichzeitig die äußere erste Schicht von 2 bis 100 μm Dicke als Diffusionsbarriere für Titan und andere gegebenenfalls im Körper vorhandene stickstoffaffine Metalle wirkt, die nicht nach außen wandern können. Die erste oberflächennahe Schicht hat demnach die Wirkung einer Membran, die Stickstoff von außen nach innen durchlässt, gleichzeitig eine Diffusion von stickstoffaffinen Metallen nach außen hemmt. Diese membranartige Wirkung tritt jedoch nur in einem Temperaturbereich unterhalb des Eutektikums, nämlich bei 1000 bis 1200°C auf. Bei höheren Temperaturen diffundieren Titan oder andere stickstoffaffine Metalle in Richtung der Substratkörperoberfäche und bilden dort entsprechende Nitride in den oberflächennahen Randzonen. Bei niedrigeren Temperaturen als 1000°C verlangsamt sich die Stickstoffdiffusion derart, so dass der gewünschte Effekt der Stickstoffanreicherung in der zweiten Schicht praktisch nicht mehr eintritt. Die Einhaltung der Temperaturgrenzen bei der zweiten Wärmebehandlung ist somit für den Erfolg des erfindungsgemäßen Verfahrens entscheidend.The process according to claim 8 is used to produce the above-described cemented carbide or cermet body. After sintering or during sintering, the cemented carbide or cermet body produced by powder metallurgy is subjected to a first heat treatment to produce a binder metal-enriched 2-100 μm thick layer and then additionally subjected to this heat treatment of a nitrogen atmosphere under a nitrogen pressure of 50 mbar (5 × 10 3 Pa) to 1 OObar (10 7 Pa) below the eutectic, preferably treated at 1000 ° C to 1200 ° C. Here, the binder metal-enriched and mixed-carbide-depleted first layer remains in its composition in the Essentially unchanged. During the heat treatment under nitrogen, nitrogen is transported inside the body, at the same time the outer first layer of 2 to 100 microns thick diffusion barrier for titanium and other possibly present in the body nitrogen-affine metals that can not migrate to the outside. The first near-surface layer thus has the effect of a membrane which allows nitrogen to pass in from the outside in, while at the same time inhibiting diffusion of nitrogen-affine metals to the outside. However, this membrane-like effect occurs only in a temperature range below the eutectic, namely at 1000 to 1200 ° C. At higher temperatures, titanium or other nitrogen-affine metals diffuse in the direction of the substrate body surface, where they form corresponding nitrides in the near-surface edge zones. At temperatures lower than 1000 ° C, the nitrogen diffusion slows down, so that the desired effect of nitrogen enrichment in the second layer practically no longer occurs. Compliance with the temperature limits in the second heat treatment is thus crucial for the success of the method according to the invention.

Alternativ ist es auch möglich, nach dem ersten Behandlungsschritt, der zu einer Ausbildung einer Mischcarbidverarmung und Bindemetallanreicherung in einer ersten Schicht erfolgt, die entstandene Schicht unterhalb mindestens einer Oberfläche durch Schleifen, Ätzen oder andere Methoden zu entfernen, bevor der Körper in einer Stickstoffatmosphäre unter einem Stickstoffdruck 5 x 103 Pa bis 107 Pa unterhalb des Eutektikums, vorzugsweise bei Temperaturen zwischen 1000°C und 1200°C behandelt wird. An den Orten, an denen zuvor die durch die erste Wärmebehandlung entstandene Schicht entfernt worden ist, bildet sich unmittelbar unter der Oberfläche eine stickstoffangereicherte, 2 bis 40 μm dicke Schicht mit einem höheren Stickstoffanteil aus.Alternatively, it is also possible after the first treatment step, which leads to a formation of a mixed carbide depletion and binder metal enrichment in a first layer, the resulting layer below at least one surface by grinding, etching or other methods to remove before the body in a nitrogen atmosphere under a Nitrogen pressure 5 x 10 3 Pa to 10 7 Pa below the eutectic, preferably at temperatures between 1000 ° C and 1200 ° C is treated. At the locations where previously the layer formed by the first heat treatment has been removed, a nitrogen-enriched, 2 to 40 μm thick layer with a higher nitrogen content forms immediately below the surface.

Dieses Verfahren kann insbesondere bei solchen Substratkörpern angewendet werden, die als Zerspanungswerkzeuge dienen, wobei unterhalb der Freifläche die im Anspruch 1 beschriebenen Schichtfolgen a) bis c) vorliegen, während auf der Span- fläche oder zumindest in dem schneidkantennahen Bereich der Spanfläche lediglich eine Schichtfolge gemäß b) und c) bzw. Anspruch 3 vorliegt.This method can be used, in particular, for substrate bodies which serve as cutting tools, the layer sequences a) to c) described in claim 1 being present underneath the free surface while on the chip surface. surface or at least in the region near the cutting edge of the rake surface only a layer sequence according to b) and c) or claim 3 is present.

Gegenüber solchen Werkzeugen aus Substratkörpern, die lediglich dem nach dem Stand der Technik bekannten Wärmebehandlungsverfahren unterzogen worden sind, konnten die Standzeiten im kontinuierlichen Schnitt, gemessen an der Verschleißmarkenbreite und der Kolktiefe um das 8- bis 10-fache gesteigert werden. Compared to such tools made of substrate bodies, which have been subjected only to the known in the prior art heat treatment process, the life in continuous section, measured by the wear mark width and the Kolktiefe could be increased by 8 to 10 times.

Claims

Ansprücheclaims Hartmetall- oder Cermetkörper mit einer Hartstoffphase aus WC und mindestens einem Carbid, Nitrid, Carbonitrid oder Oxicabonitrid mindestens eines der Elemente der IVa- oder Va-Gruppe des Periodensystems und mit einer Binderphase aus Fe, Co und/oder Ni, deren Anteil 3-25 Massen% beträgt, mit einer einzigen oder mit mehreren aneinander grenzenden Oberflächen, wobei unterhalb der einzigen oder zumindest einer der Oberflächen a) eine 2-100μm dicke erste Schicht angeordnet ist, die einen Bindemetallanteil von 2-25 Massen% und bis zu 25 Volumen% Nitride o er Carbonitride eines oder mehrerer Metalle der IVa-Gruppe des Periodensystems und/oder bis zu 10 Volumen% Carbide und/oder Carbonitride des V, Nb, Ta und/oder Cr, Rest WC, aufweist, wobei die Menge der Nitride, Carbonitride oder Carbide der vorgenannten Metalle mindestens 0,01 VoIumen% beträgt, d a d u r c h g e k e n n z e i c h n e t, d a s s b) unter der ersten Schicht eine 2 bis 40 μm dicke zweite Schicht mit einem höheren Stickstoffanteil als in der ersten Schicht angeordnet ist, die im Wesentlichen aus Nitriden und/oder Carbonitriden der Metalle der IVa-Gruppe des Periodensystems besteht und die Phasenanteile von bis zu 10 VoIumen% an Carbiden, Nitriden, Carbonitriden oder Oxycarbonitriden der Elemente W, Mo, V, Ta, Nb, Cr und/oder an in der Hartstoffphase gelösten Anteilen von bis zu 5 Massen% V, Nb, Ta und bis zu 2 Massen% Cr, Mo, W besitzt und bis zu 1 5 Massen% Binder enthält, wobei die Menge der vorgenannten Phasenanteile mindestens 0,O1 Volumen% und/oder die Menge der in der Hartstoffphase gelösten vorgenannten Anteile mindestens 0,01 Massen% beträgt. c) dass unter der zweiten Schicht eine Übergangszone mit einer Dicke von 2 bis 100 μm angeordnet ist, in der sich die Zusammensetzung graduell auf eine homogene Zusammensetzung i m Kerninneren des Hartmetall- oder Cermetkörpers ändert. Cemented carbide or cermet body with a hard material phase of WC and at least one carbide, nitride, carbonitride or oxicabonitride at least one of the elements of the IVa or Va group of the Periodic Table and with a binder phase of Fe, Co and / or Ni, their proportion 3-25 Mass% is, with a single or with several adjoining surfaces, wherein below the single or at least one of the surfaces a) a 2-100μm thick first layer is arranged, which has a binding metal content of 2-25 mass% and up to 25 volume% Nitrides o er carbonitrides of one or more metals of the IVa group of the Periodic Table and / or up to 10% by volume of carbides and / or carbonitrides of V, Nb, Ta and / or Cr, balance WC, wherein the amount of nitrides, carbonitrides or carbide of the aforementioned metals is at least 0.01% by volume, characterized in thatb) under the first layer, a 2 to 40 μm thick second layer having a higher nitrogen content than in the the first layer is essentially composed of nitrides and / or carbonitrides of the metals of the IVa group of the periodic table and the phase fractions of up to 10% by volume of carbides, nitrides, carbonitrides or oxycarbonitrides of the elements W, Mo, V, Ta, Nb, Cr and / or in dissolved in the hard phase portions of up to 5 mass% V, Nb, Ta and up to 2 mass% Cr, Mo, W and contains up to 1 5 mass% binder, wherein the amount of the aforementioned Phase proportions at least 0, O1 volume% and / or the amount of the above-mentioned amounts dissolved in the hard material phase is at least 0.01 mass%. c) that under the second layer a transition zone with a thickness of 2 to 100 microns is arranged, in which the composition changes gradually to a homogeneous composition in the interior of the core of the hard metal or cermet body. 2. Hartmetall- oder Cermetkörper nach Anspruch 1, dadurch gekennzeichnet, dass die erste Schicht gemäß a) bis zu 2 Massen % an Carbiden oder Carbonitriden eines der Metalle V, Nb, Ta und/oder Cr aufweist.2. hard metal or cermet body according to claim 1, characterized in that the first layer according to a) up to 2% by mass of carbides or carbonitrides of one of the metals V, Nb, Ta and / or Cr. 3. Hartmetall- oder Cermetkörper nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die erste Schicht gemäß a) 4 bis 15 Massen% oder 7 bis 22 Volumen% Bindemetall(e), 80 bis 96 Massen% oder 66 bis 93 Volumen% WC und 0 bis 5 Massen% oder 0 bis 12 Volumen% TiCN und/oder TiN aufweist, wobei die Gesamtmengen an Bindemetalle, WC und TiCN und/oder TiN 100 Massen% bzw. 100 Volumen% ergeben.3. hard metal or cermet body according to claim 1 or 2, characterized in that the first layer according to a) 4 to 15 mass% or 7 to 22 volume% binder metal (s), 80 to 96 mass% or 66 to 93 volume% WC and 0 to 5 mass% or 0 to 12 volume% TiCN and / or TiN, the total amounts of binder metals, WC and TiCN and / or TiN being 100 mass% and 100 volume%, respectively. 4. Hartmetall- oder Cermetkörper nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass die zweite Schicht gemäß b) 3 bis 15 Massen% oder 2 bis 15 Volumen% Bindemetall(e), 0 bis 50 Massen% oder 0 bis 30 Volumen% WC und 35 bis 98 Massen% oder 55 bis 98 Volumen% TiCN und/oder TiN enthält, wobei die Gesamtmengen Bindemetall, WC und TiCN und/oder TiN 100 Massen% oder 100 Volumen% ergeben.4. hard metal or cermet body according to one of claims 1 to 3, characterized in that the second layer according to b) 3 to 15 mass% or 2 to 15 volume% binder metal (s), 0 to 50 mass% or 0 to 30 volume % WC and 35 to 98% by mass or 55 to 98% by volume of TiCN and / or TiN, the total amounts of binder metal, WC and TiCN and / or TiN giving 100 mass% or 100 volume%. 5. Hartmetall- oder Cermetkörper nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass der Stickstoffgehalt in der zweiten Schicht gemäß b) 8 bis 22 Massen% beträgt, wenn gebundene Nitride in dieser Schicht ausschließlich als Metallnitrid vorliegen und der Stickstoffgehalt entsprechend dem Anteil, zu dem N-Atome in Metallcarbonitriden ersetzt werden, entsprechend proportional geringer wird.5. carbide or cermet body according to one of claims 1 to 4, characterized in that the nitrogen content in the second layer according to b) is 8 to 22 mass%, when bound nitrides are present in this layer exclusively as metal nitride and the nitrogen content corresponding to the proportion to which N atoms in metal carbonitrides are replaced, correspondingly proportionally smaller. 6. Hartmetall- oder Cermetkörper mit einer Hartstoffphase aus WC und mindestens einem Carbid, Nitrid, Carbonitrid oder Oxicarbonitrid mindestens eines der Elemente der IVa- oder Va-Gruppe des Periodensystems und mit einer Binderphase aus Fe, Co und/oder Ni, deren Anteil 3 bis 25 Massen% beträgt, dadurch gekennzeichnet, dass unterhalb der einzigen oder mindestens einer Oberfläche eine 2 bis 40 μm dicke Schicht angeordnet ist, die im Wesentlichen aus Nitriden und/oder Carbonitriden der Metalle der IVa-Gruppe des Periodensystems besteht und die Phasenanteile von bis zu 10 Volumen% an Carbiden, Nitriden, Carbonitriden oder Oxycarbonitriden der Elemente W, Mo, V, Ta, Nb, Cr und/oder an in der Hartstoffphase gelösten Anteilen von bis zu 5 Masse% V, Nb, Ta und bis zu 2 Masse% Cr, Mo, W besitzt und bis zu 15 Massen% Binder enthält und dass unter der zweiten Schicht eine Übergangszone mit einer Dicke von 2 bis 100 μm angeordnet ist, in der sich die Zusammensetzung graduell auf eine homogene Zusammensetzung im Kerninneren des Hartmetall- oder Cermetkörpers ändert.6. hard metal or cermet body with a hard material phase of WC and at least one carbide, nitride, carbonitride or oxicarbonitride at least one of the elements of the IVa or Va group of the Periodic Table and with a binder phase of Fe, Co and / or Ni, the proportion of 3 up to 25 mass%, characterized in that below the single or at least one surface a 2 to 40 micron thick layer is arranged, which consists essentially of nitrides and / or carbonitrides of the metals of the IVa group of the periodic table and the phase proportions of up to 10% by volume of carbides , Nitrides, carbonitrides or oxycarbonitrides of the elements W, Mo, V, Ta, Nb, Cr and / or dissolved in the hard phase portions of up to 5 mass% V, Nb, Ta and up to 2 mass% Cr, Mo, W and containing up to 15 mass% of binder and that under the second layer a transition zone with a thickness of 2 to 100 microns is arranged, in which the composition gradually changes to a homogeneous composition in the interior of the core of the cemented carbide or cermet body. 7. Hartmetall- oder Cermetkörper nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, dass mindestens eine Oberfläche eine ein- oder mehrlagige Beschichtung, bestehend aus Carbiden, Nitriden, Carbonitriden oder Oxinitri- den der Elemente der IVa- bis Vla-Gruppe des Periodensystems, Al203, Zr02, Hf02, AlON oder Kohlenstoff, vorzugsweise Diamant oder Mo oder W-Sulfiden aufweist.7. carbide or cermet body according to one of claims 1 to 6, characterized in that at least one surface of a single or multilayer coating consisting of carbides, nitrides, carbonitrides or Oxinitri- the elements of the IVa to Vla group of the Periodic Table , Al 2 O 3 , ZrO 2 , HfO 2 , AlON or carbon, preferably diamond or Mo or W sulfides. 8. Verfahren zur Herstellung eines Hartmetall- oder Cermetkörpers nach einem der Ansprüche 1 bis 5, der nach dem Sintern oder während des Sinters einer ersten Wärmebehandlung zur Erzeugung einer Schicht gemäß a) unterzogen worden ist, dadurch gekennzeichnet, dass im Anschluss an diese Wärmebehandlung der Körper einer Stickstoffatmosphäre unter einem N2-Druck von 5 x 103 Pa bis 107 Pa unterhalb des Eutektikums, vorzugsweise bei 1000°C bis 1200°C behandelt wird.8. A method for producing a hard metal or cermet body according to any one of claims 1 to 5, which has been subjected after sintering or during the sintering of a first heat treatment to produce a layer according to a), characterized in that following this heat treatment of the Body of a nitrogen atmosphere under an N 2 pressure of 5 x 10 3 Pa to 10 7 Pa below the eutectic, preferably at 1000 ° C to 1200 ° C is treated. 9. Verfahren zur Herstellung eines Hartmetall- oder Cermetkörpers nach Anspruch 6, der nach dem Sintern oder während des Sinters einer ersten Wärmebehandlung zur Erzeugung einer Schicht gemäß a) unterzogen worden ist, dadurch gekennzeichnet, dass zu indest teilweise oder vollständig die erste 2 bis 100 μm dicke Schicht mit der Zusammensetzung a) entfernt wird und im Anschluss daran der Körper einer Stickstoffatmosphäre unter einem N2-Druck von 5 x 103 Pa bis 107 Pa unterhalb des Eutektikums, vorzugsweise bei 1000°C bis 1200°C behandelt wird.9. A method for producing a hard metal or cermet body according to claim 6, which has been subjected after sintering or during the sintering of a first heat treatment to produce a layer according to a), characterized in that partially or completely to first 2 to 100 microns thick layer with the composition a) is removed and then the body of a nitrogen atmosphere under an N 2 pressure of 5 x 10 3 Pa to 10 7 Pa below the eutectic, preferably at 1000 ° C to 1200 ° C is treated. 10. Verfahren zur Herstellung eines Hartmetall- oder Cermetkörpers nach Anspruch 8 oder 9, dadurch gekennzeichnet, dass der Substratkörper anschließend mittels CVD oder PVD ein- oder mehrlagig beschichtet wird. 10. A method for producing a hard metal or cermet body according to claim 8 or 9, characterized in that the substrate body is then coated one or more layers by means of CVD or PVD.
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PL1664363T3 (en) 2011-02-28
WO2005026400A1 (en) 2005-03-24
CN1820089A (en) 2006-08-16
CN100439535C (en) 2008-12-03

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