EP0996757B1 - Alliage de carbonitrure a base de titane, comportant une zone superficielle nitruree - Google Patents

Alliage de carbonitrure a base de titane, comportant une zone superficielle nitruree Download PDF

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Publication number
EP0996757B1
EP0996757B1 EP98923278A EP98923278A EP0996757B1 EP 0996757 B1 EP0996757 B1 EP 0996757B1 EP 98923278 A EP98923278 A EP 98923278A EP 98923278 A EP98923278 A EP 98923278A EP 0996757 B1 EP0996757 B1 EP 0996757B1
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EP
European Patent Office
Prior art keywords
atomic
binder phase
titanium
phase
cutting tool
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.)
Expired - Lifetime
Application number
EP98923278A
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German (de)
English (en)
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EP0996757A1 (fr
Inventor
Gerold Weinl
Ulf Rolander
Per Lindahl
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Sandvik AB
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Sandvik AB
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/04—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbonitrides
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/20—Carburising
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the present invention relates to a liquid phase sintered body of a carbonitride alloy with titanium as main component which has improved properties particularly when used as cutting tool material in cutting operations requiring sharp edges in combination with high wear resistance and plastic deformation resistance. This has been achieved by heat treating the material in a nitrogen atmosphere.
  • Titanium based carbonitride alloys so called cermets
  • cermets are today well established as insert material in the metal cutting industry and are especially used for finishing. They consist of carbonitride hard constituents embedded in a metallic binder phase.
  • the hard constituent grains generally have a complex structure with a core surrounded by a rim of other composition.
  • group VIa elements In addition to titanium, group VIa elements, normally both molybdenum and tungsten and sometimes chromium, are added to facilitate wetting between binder and hard constituents and to strengthen the binder by means of solution hardening.
  • Group IVa and/or Va elements i.e. Zr, Hf, V, Nb and Ta, are also added in all commercial alloys available today. All these additional elements are usually added as carbides, nitrides and/or carbonitrides.
  • the grain size of the hard constituents is usually ⁇ 2 ⁇ m.
  • the binder phase is normally a solid solution of mainly both cobalt and nickel.
  • the amount of binder phase is generally 3 - 25 wt%.
  • Other elements are sometimes added as well, e.g. aluminium, which are said to harden the binder phase and/or improve the wetting between hard constituents and binder phase.
  • cermets compared to WC-Co based material are relatively high wear resistance and chemical inertness can be obtained without applying surface coatings. This property is utilized mainly in extreme finishing operations requiring sharp edges and chemical inertness to cut at low feed and high speed. However, these desirable properties are generally obtained at the expense of toughness and edge security as well as ease of production.
  • the most successful materials have large nitrogen content (N/(C+N) often exceeding 50%) which makes sintering in conventional processes difficult due to porosity caused by denitrification. High nitrogen content also makes the material difficult to grind. Grinding may be necessary to obtain sharp defect free edges and close tolerances.
  • US 4,447,263 discloses inserts of a titanium based carbonitride alloy provided with a wear resistant surface layer of carbonitride or oxycarbonitride alone or in combination where the surface layer is completely free from binder phase.
  • the layer is obtained by a heat treatment at 1100 - 1350°C in an atmosphere of N 2 , CO and/or CO 2 at subpressure.
  • US 5,336,292 where the surface layer contains a low amount of binder phase but is separated from the interior of the material by a sharp interface to a binder phase enriched zone.
  • the layer is obtained by heat treatment in an atmosphere of N 2 and/or NH 3 possibly in combination with at least one of CH 4 , CO and CO 2 at 1100 - 1350°C for 1-25 hours at atmospheric pressure or higher.
  • the heat treatment is performed as a process step included in the cooling part of the sintering cycle or as a separate process e.g. as last production step, after any optional grinding operation has been performed.
  • Fig 1 is a photomicrograph in 2000X showing a portion of an insert of the present invention.
  • Fig 2 is an EMPA (electron Microprobe Analysis) line scan of Co, N, W, Ti and C in a portion of an insert of the present invention.
  • Fig 3 is an X-ray diffractogram of the heat treated surface of an insert of the present invention.
  • the sintered titanium-based carbonitride alloy of teh present invention contains 2-15 atomic %, preferably 2-6 atomic %, tungsten and/or molybdenum. Apart from titanium, the alloy contains 0-15 atomic % of group IVa and/or group Va elements, preferably 0-5 atomic % tantalum and/or niobium. As binder phase forming element 5-25 atomic %, preferably 9-16 atomic %, cobalt is added. The alloy has a N/(C+N) ratio in the range 10-60 atomic %, preferably 10-40 atomic %. Most preferably no elements apart from C, N, Ti, W, Ta and Co are intentionally added.
  • the nitrogen content increases towards the surface.
  • This enrichment is mainly due to the presence of TiN grains formed during heat treatment and can be identified by X-ray diffraction. These TiN grains may grow separately but can also grow epitaxially, forming an outer shell at least partly surrounding carbonitride grains.
  • the nitrogen enriched zone has a binder phase content being approximately the same as in the bulk and being distributed all the way out to the surface.
  • the Co content at the surface is 50-150 %, preferably 75-130%, most preferably 90-125%, of the bulk value depending on whether any Co gradient towards the surface was present in the material prior to heat treatment.
  • the enriched zone is not a coating and not an essentially binder phase free hard phase layer.
  • the Co-content in the surface zone is essentially the same as in the inner part of the body.
  • Ti containing hard phase is seen as two distinct peaks, one peak originating from TiN, the other peak originating from mixed cubic carbonitride phase.
  • the intensity ratio TiN(200)/TiCN(200) shall be >0.5, preferably >1, most preferably >1.5.
  • a distinct peak originating from Co based binder phase is also seen.
  • the alloy must not contain nickel and/or iron apart from inevitable impurities. For higher levels of these binder forming elements the desired microstructure cannot be produced. Instead an essentially binder phase free hard phase surface layer is formed. Such layers have been presented by previous inventors as an alternative to expensive coating operations but have inferior properties compared to CVD- and PVD coatings.
  • the sintered carbonitride alloys according to the present invention are made by a method in which powders of carbides, carbonitrides and/or nitrides are mixed with Co to a prescribed composition and pressed into green bodies of desired shape.
  • the green bodies are liquid phase sintered in vacuum or a controlled gas atmosphere at a temperature in the range 1370-1500 °C, preferably using the technique described in Swedish patent application 9701858-4.
  • the inserts are heat treated at a temperature of 1150-1250 °C in an atmosphere comprising 500-1500 mbar, preferably 1000-1500 mbar, nitrogen gas for 1-40 hours, preferably 10-25 hours.
  • nitrification can be used to enhance chemical inertness, wear resistance and plastic deformation resistance of cermets without obtaining a hard phase surface layer.
  • the reason for this has turned out to be that in a Co based binder phase and at relatively high nitrogen pressures in the furnace, nitrogen diffusion from the surface is distinctly faster than titanium diffusion.
  • TiN is nucleated inside the material rather than at the surface. The rate of TiN formation at a given depth from the surface is determined by the nitrogen activity at that depth. Ti is most probably taken predominantly from the rims of the hard phase grains. Thus, the rims are dissolved at least to some extent, leading to decreased grain size.
  • a powder mixture with a chemical composition of (at%) 40.7% Ti, 3.6% W, 30.4% C 13.9% N and 11.4% Co was manufactured from Ti(C,N), WC and Co raw material powders.
  • the mean grain size of the Ti(C,N) and WC powders were 1.4 ⁇ m.
  • the powder mixture was wet milled, dried and pressed into green bodies of the insert type TNMG 160408-PF. The bodies were liquid phase sintered at 1430 °C for 90 minutes in a 10 mbar Ar atmosphere.
  • Fig 1 shows polished cross sections of the inserts prepared by standard metallographic techniques and characterised using optical microscopy and electron microprobe analysis (EMPA). Optical microscopy showed that the inserts had a golden to bronze coloured approximately 40 ⁇ m thick surface zone, Fig 1.
  • Fig 2 shows an EMPA line scan analysis of Co, N, W, Ti and C ranging from the surface and 500 ⁇ m into the material.
  • Fig 3 shows an X-ray diffractogram of the heat treated surface.
  • the Ti-based hard phase gives rise to two distinct series of peaks, one originating from TiN with an intensity being approximately twice that of the other, which originates from a carbonitride phase. Co peaks are also present in the diffractogram.
  • TNMG160408-PF inserts were manufactured of a powder mixture consisting of (in atomic-%) Co 8.3, Ni 4.2, Ti 34.8, Ta 2.5, Nb 0.8, W 4.2, Mo 2, C 26.6 and N 16.6 and liquid phase sintered in a conventional process. These inserts were coated with an about 4 ⁇ m thick Ti(C,N)-layer and a less than 1 ⁇ m thick TiN-layer using the physical vapour deposition technique (PVD). This is a well established PVD-coated cermet grade within the P25-range for turning.
  • PVD physical vapour deposition technique

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Powder Metallurgy (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)
  • Ceramic Products (AREA)
  • Carbon And Carbon Compounds (AREA)

Claims (3)

  1. Plaquette pour outil de coupe d'alliage de carbonitrure à base de titane fritté contenant des constituants durs à base de Ti, Zr, Hf, V, Nb, Ta, Cr, Mo et/ou W dans une phase liante de cobalt, ledit alliage ne contenant ni Ni, ni Fe, et ledit alliage ayant une zone superficielle enrichie d'azote d'une épaisseur de 5 à 60 µm, de préférence de 15 à 50 µm, de façon tout particulièrement préférée de 20 à 40 µm, avec une teneur en phase liante étant approximativement la même que dans la masse et étant distribuée sur toute la surface, et une teneur en Co à la surface dans la gamme de 50 à 150%, de préférence de 75 à 130%, de façon tout particulièrement préférée de 90 à 125% de la valeur de la masse.
  2. Plaquette pour outil de coupe selon la revendication 1, caractérisée en ce qu'un diffractogramme des rayons X de la surface contient 2 groupes de maxima ayant pour origine une phase dure à base de Ti et un groupe de maxima ayant pour origine une phase liante à base de Co, le rapport d'intensité TiN(200)/TiCN(200) étant supérieur à 0,5, de préférence supérieur à 1, de façon tout particulièrement préférée supérieur à 1,5.
  3. Plaquette pour outil de coupe selon l'une quelconque des revendications précédentes, caractérisée en ce qu'elle contient, outre les impuretés inévitables en plus du titane, 2 à 15, de préférence 2 à 7% atomique de tungstène et/ou de molybdène, 0 à 15% atomique d'éléments du groupe IVa et/ou du groupe Va, à part le titane, le tungstène et le molybdène, de préférence 0 à 5% atomique de tantale et/ou de niobium, 5 à 25, de préférence 9 à 16% atomique de cobalt et avec un rapport N/(C+N) moyen dans la gamme de 10 à 60, de préférence 10 à 40% atomique.
EP98923278A 1997-05-15 1998-05-15 Alliage de carbonitrure a base de titane, comportant une zone superficielle nitruree Expired - Lifetime EP0996757B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
SE9701859 1997-05-15
SE9701859A SE9701859D0 (sv) 1997-05-15 1997-05-15 Titanium based carbonitride alloy with nitrogen enriched surface zone
PCT/SE1998/000910 WO1998051831A1 (fr) 1997-05-15 1998-05-15 Alliage de carbonitrure a base de titane, comportant une zone superficielle nitruree

Publications (2)

Publication Number Publication Date
EP0996757A1 EP0996757A1 (fr) 2000-05-03
EP0996757B1 true EP0996757B1 (fr) 2002-11-20

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EP98923278A Expired - Lifetime EP0996757B1 (fr) 1997-05-15 1998-05-15 Alliage de carbonitrure a base de titane, comportant une zone superficielle nitruree

Country Status (7)

Country Link
EP (1) EP0996757B1 (fr)
JP (1) JP4170402B2 (fr)
AT (1) ATE228175T1 (fr)
DE (1) DE69809555T2 (fr)
IL (1) IL132346A (fr)
SE (1) SE9701859D0 (fr)
WO (1) WO1998051831A1 (fr)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE519830C2 (sv) * 1999-05-03 2003-04-15 Sandvik Ab Titanbaserad karbonitridlegering med bindefas av kobolt för finbearbetning
SE519832C2 (sv) * 1999-05-03 2003-04-15 Sandvik Ab Titanbaserad karbonitridlegering med bindefas av kobolt för lätt finbearbetning
SE519834C2 (sv) * 1999-05-03 2003-04-15 Sandvik Ab Titanbaserad karbonitridlegering med bindefas av kobolt för seghetskrävande finbearbetning
SE0103970L (sv) * 2001-11-27 2003-05-28 Seco Tools Ab Hårdmetall med bindefasanrikad ytzon
US7316724B2 (en) * 2003-05-20 2008-01-08 Exxonmobil Research And Engineering Company Multi-scale cermets for high temperature erosion-corrosion service
US7175687B2 (en) * 2003-05-20 2007-02-13 Exxonmobil Research And Engineering Company Advanced erosion-corrosion resistant boride cermets
JP4703122B2 (ja) * 2004-03-23 2011-06-15 京セラ株式会社 ＴｉＣＮ基サーメットの製造方法
JP4703123B2 (ja) * 2004-03-23 2011-06-15 京セラ株式会社 表面被覆ＴｉＣＮ基サーメットの製造方法
WO2008026700A1 (fr) * 2006-08-31 2008-03-06 Kyocera Corporation Outil de coupe, procédé pour sa fabrication et procédé de coupe

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4447263A (en) * 1981-12-22 1984-05-08 Mitsubishi Kinzoku Kabushiki Kaisha Blade member of cermet having surface reaction layer and process for producing same
SE9101865D0 (sv) * 1991-06-17 1991-06-17 Sandvik Ab Titanbaserad karbonitridlegering med slitstarkt ytskikt
WO1995030030A1 (fr) * 1994-05-03 1995-11-09 Widia Gmbh Cermet et son procede de production

Also Published As

Publication number Publication date
SE9701859D0 (sv) 1997-05-15
DE69809555T2 (de) 2003-03-27
JP2001524886A (ja) 2001-12-04
WO1998051831A1 (fr) 1998-11-19
EP0996757A1 (fr) 2000-05-03
JP4170402B2 (ja) 2008-10-22
IL132346A0 (en) 2001-03-19
ATE228175T1 (de) 2002-12-15
IL132346A (en) 2003-04-10
DE69809555D1 (de) 2003-01-02

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