EP1044287B1 - Verfahren zur herstellung nitridierter formteile - Google Patents

Verfahren zur herstellung nitridierter formteile Download PDF

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Publication number
EP1044287B1
EP1044287B1 EP99946245A EP99946245A EP1044287B1 EP 1044287 B1 EP1044287 B1 EP 1044287B1 EP 99946245 A EP99946245 A EP 99946245A EP 99946245 A EP99946245 A EP 99946245A EP 1044287 B1 EP1044287 B1 EP 1044287B1
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EP
European Patent Office
Prior art keywords
nitriding
temperature
steel
ingot
weight
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Expired - Lifetime
Application number
EP99946245A
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English (en)
French (fr)
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EP1044287A1 (de
Inventor
Philippe Dubois
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.)
Aubert and Duval SA
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Aubert and Duval SA
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    • 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
    • C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium 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
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • 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
    • C22C38/24—Ferrous alloys, e.g. steel alloys containing chromium with vanadium
    • 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
    • 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
    • C23C8/24—Nitriding
    • C23C8/26—Nitriding of ferrous surfaces

Definitions

  • the present invention relates to a method for manufacturing parts made of steel.
  • Nitriding is a thermochemical surface hardening treatment by introducing nitrogen into the steel. This method is used in all fields of mechanics and is used in particular to manufacture gears, splines, drive shafts, cam shafts, engine engine distribution parts, pump bodies, injector bodies , crankshafts, extrusion screws, hydraulic distributors, guide rails, rolling cages, control gauges and shaping tools.
  • Nitriding is generally carried out in a temperature range of about 450 to 600 ° C where the diffusion of nitrogen is relatively slow.
  • Conventional nitriding steels such as 40CrAlMo6.12, 25NiAlCr14.12, 30CrMo12 or 32CrMoV13 (the chemical compositions of which are given in Table 1 below), only make it possible to obtain only modest nitride layer thicknesses. on the order of about 0.7 mm maximum, the nitriding steps having excessively long periods of up to about 200 hours.
  • the sulfur is limited to 0.015% and the phosphorus to 0.020% by weight.
  • Elements such as calcium, cerium, titanium, zirconium, niobium which serve either to deoxidize the steel or to sharpen the grain size are preferably limited to 0.1% by weight each.
  • Carbon also contributes to the hardenability of the alloy as well as its resistance to tempering and its resistance to softening during the nitriding cycle.
  • Silicon must be limited because it leads, during nitriding, to the precipitation of carbonitrides which contribute little to hardening, but reduce the rate of diffusion of nitrogen. For these reasons, it is limited to a maximum of 0.5% by weight, and preferably to 0.35% by weight.
  • Chromium is one of the most important elements in obtaining the characteristics of the nitrided layer, but it leads to a significant precipitation of nitrogen in the form of carbonitrides, which reduces the rate of diffusion of the nitrogen in the nitrided layer. Chromium also has a beneficial influence on the hardenability of the undercoat. These considerations lead to limiting the chromium content to 0.8-2% by weight, preferably 1.1-1.8% by weight.
  • the quenching loss induced by the lowering of the chromium content is partly compensated by an increase in the manganese and nickel contents.
  • these two elements must not be added in excessively high content, since this leads respectively to segregations of chemical composition and embrittlement of the underlayer during nitriding.
  • the contents are limited to 1.5% by weight at the most for manganese and nickel. Tighter ranges are preferred: 0.2-1.1% by weight for manganese and 0.5-1.3% by weight for nickel.
  • the molybdenum and vanadium elements increase the resistance to the steel's yield and limit its softening during nitriding.
  • Their content must be limited because too much would lead to embrittlement of the steel underlay.
  • the contents are therefore limited to 0.6-2% by weight for molybdenum, to at most 0.5% by weight for vanadium, and 0.05% -0.4% by weight for aluminum. Tighter ranges are preferred: 0.8-1.5% by weight for the molybdenum, 0.1-0.4% by weight for vanadium and 0.1-0.3% by weight for aluminum.
  • the steel for the process according to the invention is obtained by production techniques according to claim 1
  • VIM reduced pressure
  • thermomechanical transformations aiming at conferring on the product made in this alloy a sufficient degree of wrought which one will prefer greater than or equal to 3 Lower wrought rates can be allowed for large parts.
  • thermomechanical transformations are based on conventional procedures, such as rolling, forging, stamping or spinning.
  • a normalization is carried out from a temperature above the critical point (AC 3 ), followed by an air cooling and a softening recovery at a temperature below the point critical (AC 1 ).
  • the temperature of the critical point (AC 1 ) is generally in the range of 700 ° C to 790 ° C, while the temperature of the critical point (AC 3 ) is generally in the range of 800 ° C at 890 ° C.
  • the products are then tempered and returned in the form of rolled bar, forged or stamped blank, pre-machined parts.
  • the quenching is carried out from a higher than critical point austenitization temperature (AC 3 ) in the range of 900 to 1000 ° C, for example.
  • the quenching fluid is conventionally adjusted according to the section of the products.
  • the income is then carried out at a temperature adjusted according to the desired mechanical characteristics for the core, in the range of about 550 ° C to about 750 ° C. Its choice must take into account the temperature at which the nitriding will take place. A higher tempering temperature of at least 30 ° C than the nitriding temperature is preferred. In some special cases, nitriding can take the place of income.
  • Nitriding, stage f of the process according to the invention is then carried out on a finished part or almost finished machining.
  • the time and temperature parameters are to be set according to the desired compromise in surface hardness, depth and microstructure for the layer. It is possible to implement a gaseous nitriding with ammonia, or an ion nitriding with nitrogen or even nitriding in a bath of salts capable of releasing nitrogen on the surface of the steel.
  • the process used little influence on the hardness gradient of the nitrided layer, which depends mainly on the chemical composition of the steel.
  • the standard steel chosen as a comparator is 32CrMoV13 steel, which was developed in the past to optimize the characteristic compromise at core / surface hardness / kinetics of nitriding and which remains to this day one of the best nitriding steels available. .
  • the nitriding step it was systematically performed with the gaseous nitriding method using ammonia.
  • This ingot was developed by arc melting, it was then homogenized at high temperature (1100 ° C) to obtain a uniform structure, then it was forged.
  • the forged products were slowly cooled in the oven. They have been standardized in order to dissolve the carbides, to homogenize the austenitic structure and to refine the grain.
  • Bars from this ingot were austenitized at 940 ° C, quenched with oil, and then returned to a temperature of 650 ° C.
  • This profile shows that the steel has, for the same nitriding cycle, a superficial hardness equivalent to that of 32CrMoV13 steel and a much higher nitride depth.
  • This ingot was developed by arc melting, it was then homogenized at high temperature (1100 ° C) to obtain a uniform structure, then it was forged.
  • the forged products were slowly cooled in the oven. They have been standardized in order to dissolve the carbides, to homogenize the austenitic structure and to refine the grain.
  • Bars from this ingot were austenitized at 940 ° C, quenched with oil, and then returned to a temperature of 650 ° C.
  • This profile shows that the steel has, for the same nitriding cycle, a superficial hardness equivalent to that of 32CrMoV13 steel and a much higher nitride depth.
  • This ingot was developed by arc melting, it was then homogenized at high temperature (1100 ° C) to obtain a uniform structure, then it was forged. Forged products have been slowly cooled in the oven. They have been standardized in order to dissolve the carbides, to homogenize the austenitic structure and to refine the grain.
  • Bars from this ingot were austenitized at 940 ° C, quenched with oil, and then returned to a temperature of 650 ° C.
  • This profile shows that the steel has, for the same nitriding cycle, a superficial hardness equivalent to that of 32CrMoV13 steel and a much higher nitride depth.
  • This ingot was developed by arc melting, it was then homogenized at high temperature (1100 ° C) to obtain a uniform structure, then it was forged.
  • the forged products were slowly cooled in the oven. They have been standardized in order to dissolve the carbides, to homogenize the austenitic structure and to refine the grain.
  • Bars from this ingot were austenitized at 940 ° C, quenched with oil, and then returned to a temperature of 650 ° C.
  • This profile shows that the steel has, for the same nitriding cycle, a superficial hardness equivalent to that of 32CrMoV13 steel and a much higher nitride depth.
  • This ingot was developed by arc melting, it was then homogenized at high temperature (1100 ° C) to obtain a uniform structure, then it was forged.
  • the forged products were slowly cooled in the oven. They have been standardized in order to dissolve the carbides, to homogenize the austenitic structure and to refine the grain.
  • Bars from this ingot were austenitized at 940 ° C, quenched with oil, and then returned to a temperature of 650 ° C.
  • This profile shows that the steel has, for the same nitriding cycle, a surface hardness equivalent to that of 32CrMoV13 steel and a much higher nitride depth.
  • This ingot was developed by arc melting, it was then homogenized at high temperature (1100 ° C) to obtain a uniform structure, then it was forged.
  • the forged products were slowly cooled in the oven. They have been standardized in order to dissolve the carbides, to homogenize the austenitic structure and to refine the grain.
  • Bars from this ingot were austenitized at 940 ° C, quenched with oil, and then returned to a temperature of 650 ° C.
  • This profile shows that the steel has, for the same nitriding cycle, a superficial hardness equivalent to that of 32CrMoV13 steel and a much higher nitride depth.
  • This ingot was developed by arc melting, it was then homogenized at high temperature (1100 ° C) to obtain a uniform structure, then it was forged.
  • the forged products were slowly cooled in the oven. They have been standardized in order to dissolve the carbides, to homogenize the austenitic structure and to refine the grain.
  • Bars from this ingot were austenitized at 940 ° C, quenched with oil, and then returned to a temperature of 650 ° C.
  • This profile shows that the steel has, for the same nitriding cycle, a superficial hardness equivalent to that of 32CrMoV13 steel and a much higher nitride depth.
  • This ingot was developed by arc melting, it was then homogenized at high temperature (1100 ° C) to obtain a uniform structure, then it was forged. Forged products have been slowly cooled in the oven. They have been standardized in order to dissolve the carbides, to homogenize the austenitic structure and to refine the grain.
  • Bars from this ingot were austenitized at 940 ° C, quenched with oil, and then returned to a temperature of 650 ° C.
  • This profile shows that the steel has, for the same nitriding cycle, a superficial hardness equivalent to that of 32CrMoV13 steel and a much higher nitride depth.
  • This ingot was obtained by vacuum melting then remelting by consumable electrode, it was then warmed at high temperature (1100 ° C) to homogenize the structure and then it was rolled to result in cylindrical bars of 100 mm diameter. These bars have undergone a standardization treatment in order to dissolve the carbides, homogenize the austenitic structure and refine the grain size.
  • the figure 9 Moreover, it is possible to compare the hardness profiles obtained after nitriding with this steel and with a 32CrMoV13 steel.
  • the depth of the hardness gradient makes it possible to measure the performance of a steel according to the invention in terms of nitriding kinetics. This depth is conventionally defined in Europe by measuring the depth at which the hardness is equal to that of the heart + 100 HV (Vickers hardness).
  • a part manufactured according to the invention has an excellent compromise between mechanical tensile strength, resilience and toughness of the underlayer.
  • it has an excellent compromise between the surface hardness, the depth of nitriding and the duration of the nitriding cycle.
  • the parts manufactured according to the invention can be, in particular, bars, sheets, blanks forged or stamped, tubes or son.

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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)
  • Heat Treatment Of Articles (AREA)
  • Heat Treatment Of Steel (AREA)
  • Ceramic Products (AREA)
  • Saccharide Compounds (AREA)
  • Catalysts (AREA)
  • Treatment Of Steel In Its Molten State (AREA)

Claims (5)

  1. Verfahren zur Herstellung von bearbeiteten und nitrierten Teilen mit folgenden Schritten
    a) Herstellung einer Charge bestimmt dafür, eine bestimmte chemische Zusammensetzung zu erhalten mit, ausgedrückt in Gew.-%, 0,25 bis 0,37% C; 1,1 bis 1,8% Cr, 0,8 bis 1,5% Mo; 0,1 bis 0,3% Al; 0,2 bis 1,1% Mn; 0,5 bis 1,3% Ni; 0,1 bis 0,4 V, mehr als 0,35% Si, mehr als 0,015% S und mehr als 0,020% P, wobei der Rest durch Eisen und restliche Verunreinigungen gebildet ist, wobei die Gehalte dieser Zusammensetzung an Cr, Mo, V und Al, ausgedrückt in Gew.-%, folgende Beziehung erfüllen: 4 ≤ 3Cr + Mo + V + 2Al ≤ 8,
    b) Erschmelzen der genannten Charge in einem Lichtbogenofen oder einem Vakuuminduktionsschmelzofen durch Elektroschlackeumschmelzen oder Lichtbogenschmelzen, eventuell gefolgt von einem umschmelzen mit selbstverzehrender Elektrode,
    c) Erwärmung und Warmumformung des Blocks,
    d) Diffusionsglühen der Struktur und Kornfeinen umfassend ein Normalglühen bei einer Temperatur oberhalb derjenigen des kritischen Punktes AC3, eine Luftkühlung und ein Anlassen zum Weichmachen bei einer Temperatur unterhalb derjenigen des kritischen Punktes AC1,
    e) Gebrauchsvergütung umfassend ein Abschrecken ausgehend von einer Austenitisierungstemperatur im Bereich von 900 bis 1000°C, gefolgt von einem Anlassen bei einer Temperatur von 550 bis 750°C und
    f) Nitrieren.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass das Erschmelzen in einem Lichtbogenofen des Schrittes b) bei reduziertem Druck ausgeführt wird.
  3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die Anlasstemperatur im Schritt e) mindestens 30° höher ist als die Temperatur der Nitrierung.
  4. Verfahren nach einem beliebigen der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass die chemische Zusammensetzung des Schrittes a) zusätzlich mehr als 0,1 Gew.-% jedes der Elemente Ca, Ce, Nb, Ti, Zr umfasst.
  5. Verfahren nach einem beliebigen der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass die genannte chemische Zusammensetzung ausgedrückt in Gew.% gebildet ist durch C 0,32%, Si 0,03%, Mn 0,86%, Cr 1,35%, Ni 0,78%, Mo 1,15%, V 0,28% und Al 0,19%, wobei der Rest durch Eisen und restliche Verunreinigungen gebildet ist.
EP99946245A 1998-09-30 1999-09-28 Verfahren zur herstellung nitridierter formteile Expired - Lifetime EP1044287B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR9812209A FR2783840B1 (fr) 1998-09-30 1998-09-30 Acier permettant des cinetiques de nitruration elevees, procede pour son obtention et pieces formees avec cet acier
FR9812209 1998-09-30
PCT/FR1999/002297 WO2000018975A1 (fr) 1998-09-30 1999-09-28 Acier de nitruration, procede pour son obtention et pieces formees avec cet acier

Publications (2)

Publication Number Publication Date
EP1044287A1 EP1044287A1 (de) 2000-10-18
EP1044287B1 true EP1044287B1 (de) 2011-11-02

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EP99946245A Expired - Lifetime EP1044287B1 (de) 1998-09-30 1999-09-28 Verfahren zur herstellung nitridierter formteile

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EP (1) EP1044287B1 (de)
AT (1) ATE531832T1 (de)
CA (1) CA2312034C (de)
DK (1) DK1044287T3 (de)
ES (1) ES2374261T3 (de)
FR (1) FR2783840B1 (de)
WO (1) WO2000018975A1 (de)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4142853B2 (ja) * 2001-03-22 2008-09-03 新日本製鐵株式会社 耐遅れ破壊特性に優れた高力ボルト
FR2884879B1 (fr) 2005-04-22 2007-08-03 Stephanois Rech Mec Couple d'organes de guidage dont l'un est en acier particulier conduisant a des performances ameliorees.
DE102006025008B4 (de) 2006-05-30 2022-09-15 Schaeffler Technologies AG & Co. KG Verfahren zum Härten von Laufflächen von Wälzlagerkomponenten
DE102011088234A1 (de) * 2011-12-12 2013-06-13 Aktiebolaget Skf Bauteil

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0756043B2 (ja) * 1988-09-27 1995-06-14 マツダ株式会社 鋼部材の製造方法
JPH0445244A (ja) * 1990-06-09 1992-02-14 Aichi Steel Works Ltd 疲労強度の優れた迅速窒化用鋼
JPH073392A (ja) * 1993-06-18 1995-01-06 Nkk Corp 窒化用鋼
JP2885061B2 (ja) * 1994-04-20 1999-04-19 日本鋼管株式会社 疲労特性に優れた窒化鋼部材の製造方法
JPH0849058A (ja) * 1994-08-03 1996-02-20 Nkk Corp 熱処理歪みの少ない耐摩耗窒化鋼部材の製造方法
JPH08176732A (ja) * 1994-12-27 1996-07-09 Nkk Corp 被削性の優れた窒化用鋼
JP3069256B2 (ja) * 1995-01-12 2000-07-24 住友金属工業株式会社 靭性に優れた窒化用鋼
US5938865A (en) * 1995-05-15 1999-08-17 Sumitomo Metal Industries, Ltc. Process for producing high-strength seamless steel pipe having excellent sulfide stress cracking resistance

Also Published As

Publication number Publication date
CA2312034C (fr) 2010-06-01
FR2783840B1 (fr) 2000-11-10
DK1044287T3 (da) 2011-12-12
ES2374261T3 (es) 2012-02-15
ATE531832T1 (de) 2011-11-15
WO2000018975A1 (fr) 2000-04-06
FR2783840A1 (fr) 2000-03-31
CA2312034A1 (fr) 2000-04-06
EP1044287A1 (de) 2000-10-18

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