EP3885459A1 - Matériau métallique dur à base de carbure de tungstène exempt de cobalt - Google Patents

Matériau métallique dur à base de carbure de tungstène exempt de cobalt Download PDF

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Publication number
EP3885459A1
EP3885459A1 EP20165742.6A EP20165742A EP3885459A1 EP 3885459 A1 EP3885459 A1 EP 3885459A1 EP 20165742 A EP20165742 A EP 20165742A EP 3885459 A1 EP3885459 A1 EP 3885459A1
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EP
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Prior art keywords
weight
hard metal
metal material
tungsten carbide
content
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EP20165742.6A
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German (de)
English (en)
Inventor
Ralph USELDINGER
Claudio BERTALAN
Leonel Pereira Coelho
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Ceratizit Luxembourg SARL
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Ceratizit Luxembourg SARL
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Priority to EP20165742.6A priority Critical patent/EP3885459A1/fr
Priority to CN202180023942.XA priority patent/CN115349023B/zh
Priority to US17/913,626 priority patent/US20230151461A1/en
Priority to EP21711586.4A priority patent/EP4127258A1/fr
Priority to JP2022556637A priority patent/JP7490075B2/ja
Priority to PCT/EP2021/056762 priority patent/WO2021191009A1/fr
Publication of EP3885459A1 publication Critical patent/EP3885459A1/fr
Withdrawn legal-status Critical Current

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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
    • C22C29/06—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 carbides, but not containing other metal compounds
    • C22C29/08—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 carbides, but not containing other metal compounds based on tungsten carbide
    • 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
    • C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
    • 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
    • C22C29/06—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 carbides, but not containing other metal compounds
    • C22C29/067—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 carbides, but not containing other metal compounds comprising a particular metallic binder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/46—Ferrous alloys, e.g. steel alloys containing chromium with nickel with vanadium
    • 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

Definitions

  • the present invention relates to a cobalt-free tungsten carbide-based hard metal material.
  • Tungsten carbide-based hard metal materials are composite materials in which hard material particles formed at least predominantly by tungsten carbide form the predominant part of the composite material and spaces between the hard material particles are filled by a ductile metallic binder.
  • Such hard metal materials have been used for many years due to their advantageous material properties, such as in particular high hardness in connection with good fracture toughness in a wide variety of areas, such as metal cutting, in wear parts, in woodworking tools, in forming tools, etc.
  • the material requirements when using such hard metal materials in the various areas of application are very different.
  • a high hardness is primarily decisive, for other applications, for example, good fracture toughness K lc .
  • a high level of corrosion resistance and high flexural strength can also be important.
  • the ductile metallic binder is formed by cobalt or a cobalt-based alloy.
  • a basic alloy of an element is understood to mean that this element forms the largest component of the alloy.
  • REACH regulation mixtures and substances containing Co are classified in Category 1B with regard to carcinogenicity if their Co content is> 0.1%.
  • hard metal materials containing Co as well as hard metal powder and granules are also to be classified in cancer category 1B of substances that are likely to affect humans are carcinogenic.
  • the object of the present invention is to provide an improved cobalt-free tungsten carbide-based hard metal material which, in addition to high hardness, good fracture toughness K lc and relatively high flexural strength BBF, also has good corrosion resistance and high heat resistance and is also reliable in a conventional Can manufacture production plant for hard metal materials.
  • the ratio of the two main constituents of the binder Fe and Ni to one another is in the range 0.70 Fe / (Fe + Ni) 0.95, i.e. the binder contains significantly more Fe than Ni (70-95% by weight related on the total content of (Fe + Ni)), a good compromise is achieved with regard to the mechanical properties of hardness, fracture toughness and flexural strength. With an even higher proportion of Fe, the hard metal material would become too brittle. With a lower proportion of Fe, i.e. a higher relative proportion of Ni, neither a satisfactory hardness nor a satisfactory fracture toughness would be achieved.
  • the hard metal material would not have a satisfactory corrosion resistance and would have a pronounced plastic behavior at high temperatures, that is, a low creep resistance.
  • the proportion of Cr / (Fe + Ni + Cr) of Cr to the total proportion of Fe, Ni and Cr is at least 0.5% by weight. It has been found that only such a minimum amount of Cr in the metallic binder leads to satisfactory corrosion resistance and sufficient improvement in creep resistance.
  • the solubility of Cr in the metallic binder is limited. If Cr is added in excess of the solubility limit, Cr-containing precipitates occur in the form of mixed carbides, which have a very adverse effect on the mechanical properties of the hard metal material, in particular greatly reducing the flexural strength.
  • the solubility of Cr in the metallic binder is also dependent on the Fe content of the binder (or on the Fe / (Fe + Ni) ratio).
  • the higher the Fe content the lower the solubility of Cr in the metallic binder.
  • the hard material particles are at least predominantly formed by tungsten carbide.
  • the hard material particles can preferably consist at least approximately only of tungsten carbide. However, small amounts of other hard material particles are also possible in addition to the tungsten carbide.
  • the content of the metallic binder is 5-25% by weight.
  • the hardness, the fracture toughness and the flexural strength can be set in a range that is advantageous for many different applications.
  • the Mo content Mo / (Fe + Ni + Cr) can preferably be> 0% by weight.
  • V content V / (Fe + Ni + Cr) 1% by weight. Since no pronounced grain growth of the tungsten carbide grains occurs in the case of the metallic binder formed by an iron-nickel base alloy, no significant vanadium contents are required. Furthermore, undesired embrittlement can be avoided by keeping the vanadium content as low as possible.
  • a good improvement in the corrosion resistance and creep resistance is achieved by a relatively high proportion of chromium dissolved in the iron-nickel base alloy.
  • the mean grain size of the tungsten carbide is 0.05-12 ⁇ m.
  • the properties of the cobalt-free tungsten carbide-based hard metal material can be specifically adapted to the respective applications by adjusting the grain size. Since in the iron-nickel base alloy of the metallic binder, in contrast to cobalt-based binder systems, there is no strong grain growth of the tungsten carbide grains, even very small mean grain sizes can be set by selecting the tungsten carbide starting powder accordingly.
  • the mean grain size of the tungsten carbide is preferably 0.1-6 ⁇ m.
  • the hard metal material has a specific composition, which is described in more detail below.
  • the hard metal material consists predominantly of 70-97% by weight of hard material particles which are at least predominantly formed by tungsten carbide.
  • the hard material particles can consist of tungsten carbide.
  • the hard metal material also has 3-30% by weight of a metallic binder.
  • the proportion of the metallic binder can preferably be 5 to 25% by weight of the hard metal material.
  • the metallic binder is an iron-nickel base alloy, so it has iron and nickel as the main components. In addition to iron and nickel, the metallic binder has at least chromium.
  • the hard metal material is cobalt-free, i.e. it has no cobalt or at most traces of cobalt as unavoidable impurities.
  • the hard metal material can optionally also contain up to 10% by weight of molybdenum in relation to the total content of iron, nickel and chromium, ie Mo / (Fe + Ni + Cr) ⁇ 10% by weight, up to a maximum of 2% by weight Vanadium in relation to the total iron, nickel and chromium content, ie V / (Fe + Ni + Cr) ⁇ 2% by weight, as well as up to a total of 1% by weight of the hard metal material unavoidable impurities.
  • the following preferably applies to the Mo content: Mo / (Fe + Ni + Cr) 6% by weight.
  • the iron-nickel base alloy of the metallic binder has a higher proportion of iron than nickel.
  • the iron content is 70-95% by weight of the total iron and nickel content (Fe + Ni).
  • the iron content is preferably 75-90% by weight of the total iron and nickel content.
  • the chromium content of the hard metal material is at least 0.5% by weight of the total content (Fe + Ni + Cr) of iron, nickel and chromium.
  • the chromium content can preferably be at least 1.5% by weight of the total iron, nickel and chromium content, more preferably at least 2.0% by weight.
  • an iron-nickel ratio in the range 0.7 ⁇ Fe / (Fe + Ni) ⁇ 0.83, the chromium content in relation to the total content (Fe + Ni + Cr) is at most (- 0.625 * (Fe / (Fe + Ni)) + 3.2688) wt%.
  • the chromium content in relation to the total content (Fe + Ni + Cr) is at most (- 27.5 * (Fe / (Fe + Ni)) + 25.575) wt%. With an even higher iron content, the chromium content in relation to the total content (Fe + Ni + Cr) is at most 2.2% by weight.
  • phase diagrams of FIGS. 1 to 3 exemplified in more detail the problems that arise for the industrial production of cobalt-free tungsten carbide-based hard metal material with a metallic binder formed by an iron-nickel-based alloy when chromium is added.
  • the carbon content in% by weight is plotted on the horizontal axis.
  • phase diagram Fig. 1 (ie for a chromium content of Cr / (Fe + Ni + Cr) of 2.2% by weight) at 1000 ° C. between carbon contents of 5.565 to 5.64% by weight, the range 10 ("fcc + WC "), which is aimed at in the production of the cobalt-free tungsten carbide-based hard metal material, namely an area in which tungsten carbide grains and metallic binders are present without the formation of an ⁇ phase (as in the case of a lower carbon content, see area" fcc + WC + ⁇ ") and without the formation of mixed carbide precipitates (as with a higher carbon content, see section" fcc + WC + M 7 C 3 ").
  • phase diagram for a chromium content of Cr / (Fe + Ni + Cr) 2.6 wt .-%
  • the width of the desired range 10 increases with increasing
  • the chromium content drops sharply.
  • the width of the region 10 is only very narrow with a chromium content of Cr / (Fe + Ni + Cr) of 3.0% by weight.
  • the phase diagram in Fig. 3 At 1000 ° C. it only extends between carbon contents of approx. 5.565% by weight to approx. 5.605% by weight.
  • the risk of undesired mixed carbide or ⁇ -phase precipitations increases rapidly if the process atmosphere and thus the carbon balance cannot be kept within narrow tolerances.
  • the cobalt-free tungsten carbide-based hard metal material can - depending on the intended area of application - have an average grain size of the tungsten carbide of 0.05-12 ⁇ m, preferably 0.1-6 ⁇ m.
  • the mean grain size of the tungsten carbide grains in the hard metal material can be determined using the "equivalent circle diameter (ECD)” method from EBSD (electron backscatter diffraction) recordings. This method is for example in " Development of a quantitative method for grain size measurement using EBSD "; Master of Science Thesis, Sweden 2012, by Frederik Josefsson described.
  • the cobalt-free tungsten carbide-based hard metal material according to the embodiment was produced by powder metallurgy using WC powder with a particle size (FSSS, Fisher sieve sizes) of 0.6 ⁇ m or 1.2 ⁇ m or 1.95 ⁇ m for the hard metal materials with the different grain sizes; Fe powder with an FSSS particle size of 2.3 ⁇ m, Ni powder with an FSSS particle size of 2.5 ⁇ m, Cr 3 C 2 powder with an FSSS particle size of 1.5 ⁇ m, Mo 2 C powder with an FSSS particle size of 1.35 ⁇ m and VC powder with an FSSS particle size of 1 ⁇ m. In the comparative examples, Co powder with an FSSS particle size 0.9 ⁇ m was also used.
  • FSSS particle size
  • the preparation was carried out by mixing the respective starting powder with a solvent in a ball mill or an attritor and then spray drying in the usual way.
  • the resulting granules were pressed and formed into the desired shape and were then sintered in a conventional manner to obtain the hard metal material.
  • Chromium can be used in powder metallurgy Production of the hard metal material, for example, as pure metal or in the form of Cr 3 C 2 - or Cr 2 N powder.
  • Mo can preferably be added in the form of Mo 2 C powder, but it is also possible, for example, to add it as pure metal or as, for example, (W, Mo) C mixed carbide.
  • Fe, Ni, Cr can be added individually or in pre-alloyed form.
  • Cobalt-free tungsten carbide-based hard metal materials and comparative examples according to the invention were produced by the method described above.
  • composition of the hard metal materials produced is summarized in Table 1 below.
  • Table 1 variety WC grain size [ ⁇ m] WC [wt.%] Co [wt.%] Fe [wt.%] Ni [wt.%] Fe / (Fe + Ni) [wt.%]
  • Additives Cr [wt.%] V [wt.%] Mo [wt.%] A. 0.5-0.8 rest 10 0 0 - 0.50 0.20 0.0 B. 0.5-0.8 rest 0 6.88 2.29 0.75 0 0 0 C. 0.5-0.8 rest 0 7.30 1.83 0.80 0 0 0 D. 0.5-0.8 rest 0 7.72 1.36 0.85 0 0 0 E.
  • the hard metal materials produced in the examples and comparative examples were each examined with regard to the mean grain size. Furthermore, the Vickers hardness HV10, the fracture toughness K IC and the bending strength BBF were determined on the hard metal materials produced.
  • the Vickers hardness HV10 was determined in accordance with ISO 3878: 1991 ("Hardmetals - Vickers hardness test”).
  • the fracture toughness K IC in MPa • m 1/2 was determined according to ISO 28079: 2009 with an indentation load of 10 kgf (corresponding to 98.0665 N).
  • the bending strength BBF was determined according to the ISO 3327: 2009 standard using a test object with a cylindrical cross-section (shape C).
  • 0.5-0.8 1650 9.5 3450 bad means bad means J 0.5-0.8 1600 10.5 3800 middle middle K 0.5-0.8 1610 10.4 2800 middle middle L. 0.8 - 1.3 1070 18.0 3400 bad bad M. 0.8 - 1.3 1120 17.8 3300 middle middle N 0.2-0.5 2030 7.2 3800 Well Well O 0.2-0.5 1880 7.5 4300 Well Well P. 0.2-0.5 1910 8.2 4000 middle middle Q 0.2-0.5 1970 7.6 3700 middle middle middle middle middle middle middle
  • the conventional cobalt-containing hard metal materials of the types N and O which also contain chromium and vanadium in addition to cobalt, also show both good corrosion resistance and good creep resistance. Due to their smaller mean grain size and their lower proportion of metallic binder, these grades N and O show a higher hardness and higher flexural strength, but on the other hand also a significantly reduced fracture toughness compared to grade A.
  • the L grade which is also used as a comparative example, of a cobalt-containing tungsten carbide-based hard metal material, which has neither chromium nor vanadium in addition to cobalt, has very high fracture toughness due to its higher content of metallic binder, but the corrosion resistance and creep resistance are both poor.
  • the comparative examples of types B, C, D and E are each cobalt-free tungsten carbide-based hard metal materials in which the metallic binder is an iron-nickel-based alloy that has no chromium.
  • the types B, C, D and E differ in the iron-nickel ratio of the metallic binder.
  • the total iron and nickel content (Fe + Ni) was adjusted so that the resulting volume of the binder essentially corresponds to that of a conventional cobalt-containing tungsten carbide-based hard metal material with 10% by weight of cobalt binder.
  • the examples of cobalt-free tungsten carbide-based hard metal materials of grades F, G, H and I differ from the comparative examples of grades B, C, D and E essentially in the addition of small amounts of chromium.
  • Table 3 the addition of chromium tends to slightly increase the hardness HV10 and the fracture toughness K IC tends to decrease slightly.
  • the addition of chromium has a positive effect on the bending strength BBF.
  • the addition of chromium significantly improves the corrosion resistance as well as the creep resistance. Overall, good values are achieved for the hardness HV10, the fracture toughness K IC and the flexural strength BBF.
  • a comparison of the example of the type M with the comparative example of the cobalt-containing type L shows that acceptable physical properties can be achieved compared to conventional cobalt-containing hard metal materials even with higher proportions of the metallic binder in the hard metal material.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)
EP20165742.6A 2020-03-26 2020-03-26 Matériau métallique dur à base de carbure de tungstène exempt de cobalt Withdrawn EP3885459A1 (fr)

Priority Applications (6)

Application Number Priority Date Filing Date Title
EP20165742.6A EP3885459A1 (fr) 2020-03-26 2020-03-26 Matériau métallique dur à base de carbure de tungstène exempt de cobalt
CN202180023942.XA CN115349023B (zh) 2020-03-26 2021-03-17 无钴、碳化钨基硬质合金材料
US17/913,626 US20230151461A1 (en) 2020-03-26 2021-03-17 Cobalt-free tungsten carbide-based hard-metal material
EP21711586.4A EP4127258A1 (fr) 2020-03-26 2021-03-17 Matériau de métal dur à base de carbure de tungstène exempt de cobalt
JP2022556637A JP7490075B2 (ja) 2020-03-26 2021-03-17 コバルトを含有しない炭化タングステン系超硬合金材料
PCT/EP2021/056762 WO2021191009A1 (fr) 2020-03-26 2021-03-17 Matériau de métal dur à base de carbure de tungstène exempt de cobalt

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Application Number Priority Date Filing Date Title
EP20165742.6A EP3885459A1 (fr) 2020-03-26 2020-03-26 Matériau métallique dur à base de carbure de tungstène exempt de cobalt

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EP21711586.4A Pending EP4127258A1 (fr) 2020-03-26 2021-03-17 Matériau de métal dur à base de carbure de tungstène exempt de cobalt

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EP (2) EP3885459A1 (fr)
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CN (1) CN115349023B (fr)
WO (1) WO2021191009A1 (fr)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102023135181A1 (de) 2022-12-15 2024-06-20 Hochschule Aalen, Körperschaft des öffentlichen Rechts Hartmetall
EP4389923A1 (fr) * 2022-12-20 2024-06-26 AB Sandvik Coromant Outil de coupe en carbure cémenté

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GB202204522D0 (en) * 2022-03-30 2022-05-11 Element Six Gmbh Cemented carbide material

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US20190194783A1 (en) * 2016-08-01 2019-06-27 Hitachi Metals, Ltd. Cemented carbide and its production method, and rolling roll

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CN101560623B (zh) * 2009-05-22 2011-07-20 华南理工大学 一种WC-增韧增强Ni3Al硬质合金及其制备方法
US20200024702A1 (en) * 2017-11-09 2020-01-23 U.S. Army Research Laboratory Attn: Rdrl-Loc-I Cemented carbide containing tungsten carbide and iron alloy binder

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US20190194783A1 (en) * 2016-08-01 2019-06-27 Hitachi Metals, Ltd. Cemented carbide and its production method, and rolling roll
US20180142331A1 (en) * 2016-11-10 2018-05-24 U.S. Army Research Laboratory Attn: Rdrl-Loc-I Cemented carbide containing tungsten carbide and finegrained iron alloy binder

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GRIES AND PRAKASH: "Cobalt free binder alloys for hard metals: consolidation of ready-to-press powder and sintered properties", TUNGSTEN, REFRACTORY & HARDMATERIALS VII : PROCEEDINGS OF THE SEVENTH INTERNATIONAL CONFERENCE ON TUNGSTEN, REFRACTORY AND HARDMATERIALS ... JUNE 8 - 12, 2008, [WASHINGTON, D.C.], METAL POWDER INDUSTRIES FEDERATION, 8 June 2008 (2008-06-08), pages 3 - 56, XP009153527, ISBN: 978-0-9783488-8-5 *
MURDOCH HEATHER A ET AL: "Metric mapping: A color coded atlas for guiding rapid development of novel cermets and its application to "green" WC binder", MATERIALS AND DESIGN, ELSEVIER, AMSTERDAM, NL, vol. 150, 9 April 2018 (2018-04-09), pages 64 - 74, XP085392468, ISSN: 0264-1275, DOI: 10.1016/J.MATDES.2018.04.008 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102023135181A1 (de) 2022-12-15 2024-06-20 Hochschule Aalen, Körperschaft des öffentlichen Rechts Hartmetall
EP4389923A1 (fr) * 2022-12-20 2024-06-26 AB Sandvik Coromant Outil de coupe en carbure cémenté

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JP2023518477A (ja) 2023-05-01
JP7490075B2 (ja) 2024-05-24
EP4127258A1 (fr) 2023-02-08
CN115349023A (zh) 2022-11-15
CN115349023B (zh) 2024-06-04
US20230151461A1 (en) 2023-05-18
WO2021191009A1 (fr) 2021-09-30

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