WO2009126978A1 - Procédé de fabrication de couches de revêtement en ti (c, n, o) - Google Patents

Procédé de fabrication de couches de revêtement en ti (c, n, o) Download PDF

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Publication number
WO2009126978A1
WO2009126978A1 PCT/AT2009/000048 AT2009000048W WO2009126978A1 WO 2009126978 A1 WO2009126978 A1 WO 2009126978A1 AT 2009000048 W AT2009000048 W AT 2009000048W WO 2009126978 A1 WO2009126978 A1 WO 2009126978A1
Authority
WO
WIPO (PCT)
Prior art keywords
coating layer
tool
titanium
nitrogen
substrate
Prior art date
Application number
PCT/AT2009/000048
Other languages
German (de)
English (en)
Inventor
Reinhard Pitonak
Arno KÖPF
Ronald Weissenbacher
Original Assignee
Boehlerit Gmbh & 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 Boehlerit Gmbh & Co. Kg. filed Critical Boehlerit Gmbh & Co. Kg.
Publication of WO2009126978A1 publication Critical patent/WO2009126978A1/fr

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
    • 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
    • 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
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
    • C23C16/029—Graded interfaces
    • 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
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/36—Carbonitrides

Definitions

  • the invention relates to a method for producing a coating, wherein a coating layer contains titanium, carbon, nitrogen and oxygen or consists of these elements.
  • the invention relates to a tool or a tool insert, in particular a cutting tool insert such as an indexable insert, with a substrate of a hard metal, which is provided with a coating of one or more coating layers, wherein a coating layer of the elements titanium, carbon, nitrogen and oxygen and optionally further metallic elements is formed.
  • Machining tools or tool inserts such as indexable inserts
  • indexable inserts on the one hand be wear-resistant and highly durable and on the other hand be designed so that a friction occurring in use, which is given in a relative movement of the workpieces to be machined and the employed tools or tool inserts, for example in a Turning a steel is minimized.
  • cutting tools or tool inserts are generally provided with multi-layer coatings, starting from the substrate first several a wear resistance of a tool or tool insert increasing coating layers and then or workpiece side lubricating having outermost coating layer are provided.
  • EP 1 118 688 A1 has disclosed coating layers of Ti (C 1 N 1 O) by means of Medium Temperature Chemical Vapor Deposition (MTCVD) by precipitation from a reaction gas containing H 2 , N 2 , CH 3 CN, TiCl 4 and CO 2 and / or produce CO at a temperature of 700 0 C to 900 0 C.
  • MTCVD Medium Temperature Chemical Vapor Deposition
  • the invention has for its object to provide a method of the type mentioned above, wherein the coating layer with titanium, carbon, nitrogen and oxygen adheres well to the substrate or an underlying coating layer, is substantially dense and can serve as a sliding layer and wherein this coating layer has a structure that gives this at the same time a high stability.
  • a method of the aforementioned type which comprises the following steps: a) providing a substrate; b) optionally depositing one or more coating layers on the substrate; c) then commencing the deposition of a coating layer of titanium carbonitride which has substantially homogeneously distributed regions of higher carbon content and lower nitrogen content or vice versa; d) simultaneous oxidation of the coating layer further developing in step c) or subsequent oxidation of the coating layer obtained after completion of step c); e) then optionally depositing a coating layer of a titanium oxide.
  • the advantages achieved by the invention can be seen in particular in that a favorable microstructure formation for the subsequent oxidation is created by the titanium carbonitride coating layer, which in some cases contains more carbon than nitrogen and some nitrogen than carbon in some cases in step c) in the oxidation, primarily the higher carbon content regions are oxidized while the higher nitrogen content regions show less tendency to oxidize. It can therefore be a favorable when oxidizing Structure in which the more oxidized areas with pre-oxidation higher carbon content are important for the lubricating effect, whereas the less heavily oxidized areas with pre-oxidation higher nitrogen content of the coating layer provide stability. Since the oxidation is only started and carried out when at least part of the coating layer has been deposited, good bonding to the substrate or an underlying coating layer is achieved. In addition, the coating layer is also dense. Moreover, the coating layer produced in this way is also excellently suited for depositing titanium oxide coating layers which can be readily adhered and densely sealed by means of a CVD process, so that the sliding properties can additionally be optimized.
  • the coating layer prepared in step c) can be subsequently oxidized, it is more favorable for a homogeneous microstructure in the coating layer if the oxidation is started even after formation of a thin bonding region and continued during a further growth of the coating layer growing in step c). It has proven to be particularly favorable when in step c) with respect to nitrogen and carbon, a gradient layer is formed, in such a way that towards the end of the construction of the coating layer, a nitrogen concentration is zero. As a result, a particularly dense outer surface of the coating layer can be achieved, which consists predominantly of a titanium oxide and can serve both as a working layer and as a bonding layer for further coating layers.
  • the individual coating layers are preferably deposited by a CVD method. It is advisable for the longest possible service life of the coating layer in use that the in step c) or step d) building or in step c) obtained coating layer with a thickness of more than 10 .mu.m, in particular more than 15 microns created becomes. This is particularly recommended if this coating layer is used as a working coating layer in the tool.
  • the coating layer which is built up in step c) or step d) or obtained in step c) is oxidized only in the region of a surface zone facing away from the substrate.
  • the coating layer comprises then on the substrate side a hard and wear-resistant zone of titanium carbonitride and a workpiece-side zone made of Ti (C 1 N 1 O), which brings the desired sliding properties in use with it. It has proven to be expedient if the surface zone in a range of less than 5 microns, measured from the freely accessible surface, is oxidized.
  • the oxidation may in itself be carried out with any gases which allow the desired oxidation of at least the higher carbon content regions.
  • the coating layer that builds up in step c) or step d) or obtained in step c) can be oxidized with oxygen.
  • the coating layer building up in step c) or step d) or obtained in step c) is oxidized by the addition of CO 2 , since a more mild oxidation than with oxygen can be achieved with CO 2 .
  • CO can be used in addition to CO 2 : At average reaction temperatures of about 1000 0 C, CO 2 is in equilibrium with CO and C (Boudouard equilibrium). The amounts of CO 2 and CO introduced can be used to precisely control the equilibrium and therefore the oxidation.
  • the coating layer in step c) is prepared first without supply of oxidizing gases directly on the substrate or a coating layer deposited in step b) and then, with further construction of the coating layer, an oxidizing gas with the already partially deposited coating layer Contact is brought.
  • the partial construction of a titanium carbonitride coating layer first results in a good bond to the substrate or an already deposited coating layer.
  • the portion of the coating layer beyond this connection region is then oxidized in order to ensure the desired lubricating effect.
  • the layer is in step c) or step d) building up or step c) obtained by depositing a reaction gas containing TiCl 4, CH 4 , N 2 , radical H 2 at a reaction temperature of 900 0 C to 1100 0 C 1 preferably 930 0 C to 1070 0 C 1 is created.
  • the reaction temperature is initially maintained at about 950 ° C., for example for about 30 minutes, after which the reaction temperature is raised to about 1020 ° C.
  • the coating layer is formed with titanium carbonitride crystallites having a core-shell structure wherein the core contains more nitrogen than carbon and the shell contains more carbon than nitrogen. If the oxidation is carried out, the cladding is primarily oxidized, which on the one hand is more easily accessible and on the other hand has more carbon and therefore oxidizes more easily.
  • the method according to the invention is fundamentally applicable to all types of substrates, it is preferably used in situations in which the substrate is a hard metal.
  • the method according to the invention is suitable for coating cutting tool inserts, in particular indexable inserts for machining steel.
  • a further object of the invention is to provide a tool or a tool insert, which is provided with a favorable for a machining of steel coating.
  • a tool or a tool insert in particular a cutting tool insert such as an indexable insert, with a substrate of a hard metal, which is provided with a coating of one or more coating layers, wherein a coating layer of the elements titanium, carbon, nitrogen and oxygen and optionally further metallic elements homogeneously distributed regions having higher carbon content and lower nitrogen content or vice versa, wherein at least the regions of higher carbon content are at least partially oxidized and wherein said coating layer of the substrate Considering an outermost coating layer or wearing a coating layer of titanium oxide, which is the outermost coating layer reached.
  • a tool or tool insert according to the invention comprises a highly adhering, stable and at the same time good machining properties during the machining of a steel extreme coating layer.
  • further coating layers may be provided between the substrate and the outermost coating layer (s), which increase the wear resistance of the coating.
  • the coating layer of the elements titanium, carbon, nitrogen and oxygen and optionally further metallic elements has areas with a core-shell structure, wherein, based on a composition in atomic percent, the core more nitrogen than in total carbon and Oxygen and the mantle in total more carbon and oxygen than nitrogen.
  • An average crystallite size in the coating layer of the elements titanium, carbon, nitrogen and oxygen and optionally further metallic elements is preferably less than 0.3 ⁇ m, preferably less than 0.2 ⁇ m, in particular less than 0.1 ⁇ m.
  • the next optional titanium metallic elements such as chromium, should have a maximum of 30 atomic percent, based on the content of all metallic elements in the coating layer, in order to achieve in the production of the advantageous structural formation.
  • the outermost coating layer may be formed as a gradient layer in which a substrate-side zone of the elements titanium, carbon, nitrogen and oxygen merges into a zone consisting essentially of a titanium oxide.
  • Essentially consisting of titanium oxide zone preferably has a thickness of less than 5 .mu.m, in particular less than 3 microns, on.
  • Fig. 1 is a micrograph of a portion of a coating
  • FIG. 2 shows an enlarged detail of a microsection of a coating
  • Fig. 3 is a schematic representation of a part of the structure of an inventive
  • Fig. 4 is a diagram concerning results of wear tests.
  • a multi-layer coating was deposited by CVD.
  • a titanium nitride coating layer with a layer thickness of about 0.5 microns, then at a temperature of about 800 0 C, a coating layer of titanium carbonitride (MTCVD-TiCN) with a layer thickness of about 3 microns , Then another coating layer of titanium carbonitride, prepared according to WO 2007/056785 A1, deposited with a layer thickness of about 5 microns and finally a coating layer of Al 2 O 3 with a layer thickness of about 3 microns.
  • MTCVD-TiCN titanium carbonitride
  • a reaction gas containing about 5 percent by volume TiCl 4 and CH 4 , N 2 and H 2 in a molar ratio of 1:10:25 first at a substrate temperature of about 950 0 C for supplied for about 30 minutes and started the deposition of a coating layer.
  • the substrate or reaction temperature was increased to about 1020 0 C and the reaction continued for about 90 minutes, forming a Ti (C, N) coating layer with crystallites having an average crystallite size of less than 50 nanometers ,
  • the crystallites in turn formed areas with nitrogen-rich cores and carbon-rich coats, so uneven distribution of elements.
  • a coating layer produced as described above has a structure with regions of a core-shell structure below the region consisting of pure titanium oxide, wherein the jacket regions are at least partially oxidized and appear dark. It is believed that this structure is responsible for the excellent bonding and dense formation of the titanium oxide zone.
  • indexable insert coated as described above was evaluated for its life in turning a tempered steel shaft.
  • indexable insert used, in which the coating provided there was basically the same structure, but instead of the final
  • Coating layer of Ti (C 1 N 7 O) or titanium oxide was formed with an Al 2 O 3 coating layer.
  • the cutting parameters were as follows:
  • Feed f 0.30 rpm; Setting angle K: 95 °;
  • the wear was measured as a function of the machining time.
  • the wear measurement was carried out according to ⁇ NORM A 2750, series 10.
  • outermost coating layers produced according to the invention also adhered particularly well to underlying coating layers and could not be removed by irradiation with a mixture of water and corundum even at a pressure of 3 bar.
  • the time being to completely form the titanium carbonitride coating layer and then to oxidize it, for example, with pure CO 2 .
  • the coating layer is formed identically over its entire thickness or thickness, ie without transition into a surface zone of titanium oxide, which may be favorable for special applications. If required, however, a coating layer of titanium oxide may additionally be deposited separately on this coating layer, in particular by means of a CVD method.

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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)
  • Inorganic Chemistry (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

L'invention concerne un procédé de fabrication d'un revêtement selon lequel une couche de revêtement contient du titane, du carbone, de l'azote et de l'oxygène ou est constituée de ces éléments. Pour doter des outils ou des garnitures d'outils d'une couche de revêtement d'une structure avantageuse, qui est stable et présente en utilisation un effet de lubrification, l'invention propose un procédé qui présente les étapes suivantes : a) prendre un substrat, b) facultativement, déposer une ou plusieurs couches de revêtement sur le substrat, c) puis commencer le dépôt d'une couche de revêtement en carbonitrure de titane qui présente des zones à forte teneur en carbone et à faible teneur en azote ou inversement, et de répartition essentiellement uniforme, d) en même temps, oxyder la couche de revêtement qui continue à se former selon l'étape c) ou oxyder ultérieurement la couche de revêtement obtenue une fois l'étape c) terminée et e) ensuite, déposer facultativement une couche de revêtement en oxyde de titane. L'invention concerne en outre un outil ou une garniture d'outil, en particulier une garniture d'outil de coupe, par exemple une plaquette réversible, qui présente un substrat en métal dur doté d'un revêtement ainsi réalisé.
PCT/AT2009/000048 2008-04-17 2009-02-10 Procédé de fabrication de couches de revêtement en ti (c, n, o) WO2009126978A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ATA607/2008 2008-04-17
AT6072008A AT505908B1 (de) 2008-04-17 2008-04-17 Verfahren zum herstellen einer ti(c,n,o)-beschichtungslage

Publications (1)

Publication Number Publication Date
WO2009126978A1 true WO2009126978A1 (fr) 2009-10-22

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PCT/AT2009/000048 WO2009126978A1 (fr) 2008-04-17 2009-02-10 Procédé de fabrication de couches de revêtement en ti (c, n, o)

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AT (1) AT505908B1 (fr)
WO (1) WO2009126978A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102013115005B4 (de) 2013-12-31 2022-01-05 Gottfried Wilhelm Leibniz Universität Hannover Verfahren zum Erzeugen einer oxidierten Oberfläche einer Metalllegierung, insbesondere bei Bauteilen, solche Bauteile und Werkzeuge, sowie der Verwendung

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0031805A1 (fr) * 1979-12-28 1981-07-08 Vereinigte Edelstahlwerke Aktiengesellschaft (Vew) Corps dur, notamment pièce d'usure en métal dur, et procédé pour sa fabrication
EP0643152A2 (fr) * 1993-09-09 1995-03-15 Plansee Tizit Gesellschaft M.B.H. Outil de coupe
JPH08269719A (ja) * 1995-03-29 1996-10-15 Mitsubishi Materials Corp チタンの炭窒酸化物層表面被覆切削工具の製造方法
US20020086147A1 (en) * 2000-05-31 2002-07-04 Mitsubishi Materials Corporation Coated cemented carbide cutting tool member and process for producing the same
WO2007056779A1 (fr) * 2005-11-17 2007-05-24 Boehlerit Gmbh & Co. Kg. Corps en metal dur enduit
WO2007056785A1 (fr) * 2005-11-17 2007-05-24 Boehlerit Gmbh & Co. Kg. Couche de carbonitrure metallique et procede de production d'une couche de carbonitrure metallique

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES494779A0 (es) * 1979-08-09 1981-03-16 Mitsubishi Metal Corp Procedimiento para la fabricacion de cuchillas dotadas de recubrimiento,para herramientas de corte
US6733874B2 (en) * 2001-08-31 2004-05-11 Mitsubishi Materials Corporation Surface-coated carbide alloy cutting tool
DE102004063816B3 (de) * 2004-12-30 2006-05-18 Walter Ag Al2O3-Multilagenplatte
JP2008055583A (ja) * 2006-09-01 2008-03-13 Mitsubishi Materials Corp 硬質被覆層がすぐれた耐摩耗性を発揮する表面被覆切削工具

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0031805A1 (fr) * 1979-12-28 1981-07-08 Vereinigte Edelstahlwerke Aktiengesellschaft (Vew) Corps dur, notamment pièce d'usure en métal dur, et procédé pour sa fabrication
EP0643152A2 (fr) * 1993-09-09 1995-03-15 Plansee Tizit Gesellschaft M.B.H. Outil de coupe
JPH08269719A (ja) * 1995-03-29 1996-10-15 Mitsubishi Materials Corp チタンの炭窒酸化物層表面被覆切削工具の製造方法
US20020086147A1 (en) * 2000-05-31 2002-07-04 Mitsubishi Materials Corporation Coated cemented carbide cutting tool member and process for producing the same
WO2007056779A1 (fr) * 2005-11-17 2007-05-24 Boehlerit Gmbh & Co. Kg. Corps en metal dur enduit
WO2007056785A1 (fr) * 2005-11-17 2007-05-24 Boehlerit Gmbh & Co. Kg. Couche de carbonitrure metallique et procede de production d'une couche de carbonitrure metallique

Also Published As

Publication number Publication date
AT505908A4 (de) 2009-05-15
AT505908B1 (de) 2009-05-15

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