EP2188402B1 - Martensitischer edelstahl, verfahren zur herstellung von teilen aus diesem stahl und daraus hergestellte teile - Google Patents

Martensitischer edelstahl, verfahren zur herstellung von teilen aus diesem stahl und daraus hergestellte teile Download PDF

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EP2188402B1
EP2188402B1 EP08830336A EP08830336A EP2188402B1 EP 2188402 B1 EP2188402 B1 EP 2188402B1 EP 08830336 A EP08830336 A EP 08830336A EP 08830336 A EP08830336 A EP 08830336A EP 2188402 B1 EP2188402 B1 EP 2188402B1
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Prior art keywords
steel
trace levels
traces
temperature
hardness
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French (fr)
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EP2188402A1 (de
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André GRELLIER
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Aubert and Duval SA
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Aubert and Duval SA
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    • 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
    • C21D1/18—Hardening; Quenching with or without subsequent tempering
    • C21D1/19—Hardening; Quenching with or without subsequent tempering by interrupted quenching
    • C21D1/22—Martempering
    • 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
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/002—Heat treatment of ferrous alloys containing Cr
    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • 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
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/24—Ferrous alloys, e.g. steel alloys containing chromium with vanadium
    • 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
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/008—Martensite

Definitions

  • the present invention relates to iron and steel, more specifically, martensitic stainless steels, intended for example for the manufacture of molds for the production of plastics by injection.
  • the industry uses stainless steels of the AISI 420 family with a chromium content of 12 to 15% (in percentages by weight, like all the contents indicated in the rest of the text). , a silicon content of less than 1%, a manganese content of less than 1%, a carbon content of 0.16 to 0.45%, and a nitrogen content which is the result naturally of the production and generally up to 0.03%.
  • the vanadium content does not exceed 0.1% and results from the simple melting of the raw materials.
  • the molybdenum content results from the melting of the raw materials and does not exceed 0.2%, unless 0.2 to 1.0% is added to improve the corrosion resistance.
  • the X40Cr14 nomenclature steel capable of exceeding a hardness of 50 HRC by virtue of its carbon content of 0.36-0.45%, offers an appreciable abrasion resistance.
  • JP10110248 relates to martensitic stainless steels, for example for the manufacture of molds for the production of plastics by injection and comprises, in percentages by weight, C: 0.15 - 0.04%, N 0.02 -0.15%, Cr: 11 - 15%, V, 0 - 0.25%, Mo + 1 ⁇ 2 W: 0 - 3%, Ni: 0.01 - 0.2%, Mn: 0 - 2%, Si: 0 - 2%, Cu 0.1 - 1%, Ti: 0 - 0.25%, Nb: 0 - 0.25%, Al: 0 - 0, 1%, S: 0 - 0.005%, B: 0 - 0.1%, Ca : 0 - 0.1%, Mg: 0 - 0.1%, Fe remain and a method of manufacturing a piece of this martensitic stainless steel.
  • the choice of the low temperatures allows only a partial release of the stresses, and if the composition of the steel and the quenching cycle left residual austenite, the income not decomposing it, the hardness target is not reached.
  • High temperature incomes break down austenite and relax residual stresses, but decrease toughness and corrosion resistance.
  • traces ⁇ Nb ⁇ 0.010%.
  • Said incomes may each be carried out at a temperature of 200 to 400 ° C., preferably 300 to 380 ° C. for a minimum of 2 hours, while maintaining the nominal temperature at least 1 hour at the core, so as to obtain a hardness from 49 to 55 HRC.
  • Said incomes can each be carried out at a temperature of 530 to 540 ° C for a minimum of 2 hours while maintaining a core temperature of the nominal temperature of at least 1 hour, so as to obtain a hardness between 42 and 50 HRC.
  • the invention also relates to a martensitic stainless steel part, characterized in that the element manufactured by the process is manufactured according to the preceding method.
  • It may be a mold element for the manufacture of plastic articles.
  • the invention is based on a steel composition whose carbon and chromium contents are simultaneously at the bottom of the ranges usually required, and sometimes even below for the chromium content, with the imposition of conditions. other elements present or to be limited or avoided.
  • a manufacturing method is associated with this composition.
  • the approach of the inventors has focused on the real consideration of the properties of the steel resulting from the manufacture, and in particular of the industrial treatment as described above, and not according to laboratory conditions.
  • the research was carried out with the aim of optimizing the action of the alloying elements to limit the quantity introduced.
  • the toughness mediocre for this family of steels, is, for a given hardness, the lower the chromium content is high. It could be improved by balancing the composition, especially with additions of nickel and manganese to maintain a residue of austenite quenching. This solution, which also has no effect if the revenues are achieved above 500 ° C, however, proves unstable and handicaps the achievement of hardness. It was not retained, especially since it was not compatible with the desired lowering of the content of alloying elements.
  • Table 1 groups the compositions of the samples studied.
  • the "Reference" sample corresponds to a standard X40Cr14 type steel.
  • the samples Exp.1 to Exp.7 are not in accordance with the invention but make it possible to identify the disadvantages of not respecting all the conditions required by the invention.
  • Samples Inv.1 and Inv.2 are in accordance with the invention.
  • the object of the invention is therefore to design an optimized steel intended to be treated according to the range of industrial quenching speeds, preferably with a subsequent double low temperature ( ⁇ 400 ° C.) for a hardness of 52 HRC with tenacity and a corrosion resistance equal to or greater than that of the reference steel AISI 420 or X40Cr14 in its usual implementation.
  • the invention has the objective of minimizing the addition of alloying elements, in particular metal elements, in order to reduce the cost of production, to prevent the presence of residual austenite after quenching, and to reduce the amplitude. interdendritic segregation is detrimental to the tenacity and quality of polish.
  • the nitrogen content must be between 0.05% and 0.15% and preferably between 0.08% and 0.12%. This element is therefore systematically present at a high content, because it is essential to form type V carbonings (C, N) capable of preventing grain growth after austenization once the dissolved chromium carbides. An excessive content would however be detrimental by exceeding the solubility limit in the solid state and would be a source of metallurgical defects. Nitrogen combines with carbon to impart hardness and contributes to corrosion resistance. The nitrogen content can be adjusted by blowing nitrogen gas during the preparation of the liquid steel.
  • Chrome gives steel its resistance to corrosion. Given the industrial quenching speeds practiced, and the income range chosen, and according to the mechanisms mentioned above, its content must be between 10 and 12.4% and preferably between 11.0 and 12.4% .
  • the vanadium must be present at a content of between 0.10% and 0.40% and preferably between 0.15% and 0.35%. Its presence is essential to form with carbon and nitrogen a sufficient density of micro- and nano-precipitates able to prevent the growth of the grain. Too high a content would be detrimental by the excessive fixation of the carbon which would be lacking for the hardening, and by the formation, during the solidification, of carbides isolated or in clusters unfavorable to the tenacity and the quality of the polish.
  • Molybdenum completes the action of chromium for corrosion resistance; it is present, by recycling or by voluntary addition, at percentages between 0.10 and 1.0%. A higher content would be detrimental by increasing the amplitude of interdendritic segregation, and by the risk of forming delta ferrite.
  • Nickel may be present at levels less than 1.0%, mainly because of the input by the raw materials. No favorable action of an addition within this limit for toughness was noted. On the other hand, a higher content would be likely to maintain residual austenite in the treated state.
  • Silicon is naturally present for the elaboration and deoxidation of steel. Its content must be limited to 1.0% and preferably 0.5%, since it acts on the solidification process and the delta-gamma transformation and can therefore cause the presence of delta ferrite or local segregations consecutive to the presence of this phase at the end of solidification before wrought.
  • Tungsten may be present at levels less than 1.0% without having a favorable or detrimental effect on the product. Nevertheless, by its individual action or by synergy with molybdenum, it can promote the presence of delta ferrite in the state of use, or local precipitation or segregation originating from the presence of delta ferrite at any stage of the process. thermomechanical. It will be preferred to meet the condition 0.10% ⁇ Mo + W / 2 ⁇ 1.20%.
  • Cobalt and copper have no identified beneficial effect but may be present at levels less than or equal to 1.0%; higher grades may favor the presence of residual austenite.
  • the total contents of Mn, Cu and Co is ⁇ 1.8%, so as to limit the risks of presence of residual austenite.
  • Titanium and niobium are very reactive elements that form very hard precipitates harmful to the quality of polishing. Their content must be kept as low as possible: at most 0.010%, preferably at most 0.003% for Ti, and at most 0.050%, preferably at most 0.010% for Nb.
  • the added aluminum for the deoxidation of the steel can remain present in oxide inclusions very harmful for the polishing.
  • the level of addition must be adapted to the processing methods used. A maximum level of 0.050% is tolerable, provided that it does not lead to the presence of inclusions of alumina or silico-aluminates in large quantities which would lead to an exceedance of the acceptable O content (0.0040% better, 0.0015%).
  • the sulfur is preferentially limited to a content of less than 0.003% to prevent the formation of sulphide inclusions.
  • it may be chosen to make a voluntary addition in the range 0.003 to 0.020% preferably associated with another element (SE up to 0.010%, Ca up to 0.020%, La up to 0.040%). %, Ce up to 0.040%) promoting the formation of globular sulphides to improve machinability, to the detriment to a certain extent of the quality of the polish.
  • the maximum oxygen content is 0.0040%, preferably 0.0015%.
  • the phosphorus content is limited to 0.03% which is a common content in this class of steels. There was no adverse effect of P in this range.
  • Boron may be added to improve quenchability at a level not exceeding 0.0050%.
  • the products shall be manufactured in accordance with the state of the art for high-grade special steels for plastics molding applications, with the objective of limiting the inclusion content and segregation for obtaining a quality polish.
  • the preparation must include, after melting, a phase of deoxidation and elimination of inclusions in a metallurgical reactor.
  • a phase of deoxidation and elimination of inclusions in a metallurgical reactor.
  • it will be practiced remelting by consumable electrode slag to improve the inclusion cleanliness and distribute the alloy elements, and above all the nitrogen, homogeneously throughout the mass.
  • thermomechanical transformation by forging or rolling completed by annealing must follow to complete the homogeneity and compactness of the microstructure.
  • the products After machining the workpiece to the final shape and before putting into operation, the products must, according to the preferred procedure, undergo a heat treatment comprising austenization at about 1020 ° C (from 990 to 1040 ° C, preferably 1000- 1030 ° C), a controlled quenching, for example under a neutral gas pressure, at a speed of between 10 and 40 ° C / min adapted to the size of the workpiece, then two returns at a temperature of 200 to 400 ° C, preferably between 300 and 380 ° C to obtain a hardness close to 52 HRC ⁇ 2 HRC, and generally between 49 and 55 HRC.
  • a heat treatment comprising austenization at about 1020 ° C (from 990 to 1040 ° C, preferably 1000- 1030 ° C)
  • a controlled quenching for example under a neutral gas pressure
  • the steel defined by the invention may be treated with a double feed from 530 ° C. to 560 ° C. for hardnesses less than or equal to 50 HRC and greater than or equal to at 42 HRC, conditions in which corrosion resistance is sufficient.
  • the chromium carbides (M 23 C 6 ) existing in the delivery state are redissolved during the austenization that precedes quenching, and the temperature of the maintenance is limited to 1020/1030 ° C to prevent grain growth.
  • the temperature of the maintenance is limited to 1020/1030 ° C to prevent grain growth.
  • this dissolution temperature there remains a significant amount of carbides distributed heterogeneously.
  • the effective density of micrometric carbides observed on industrial products and illustrated on the Figure 1 effectively decreases significantly between the reference composition and the compositions of the invention, which constitutes a favorable factor for the quality of the polished state.
  • the corrosion resistance capacity is, theoretically according to the basic knowledge, primarily related to the chromium content available in the matrix; thermodynamic calculations show that carbons undissolved in austenization set about 0.9% chromium. This amount of chromium unavailable for corrosion resistance becomes less than 0.1% for vanadium and nitrogen alloyed experimental grades. According to the following formula:
  • the electrochemical method performed according to the ASTM G 108 standard consists, in a 1% by weight aqueous H 2 SO 4 solution, of polarizing the sample for 15 minutes at a potential of -550mV / ECS and then carrying out a forward scan. and back to 60mV / min from -550mV to + 500mV.
  • the intensity-potential curves at the return can have two peaks, one (Pic1) due to the dissolution of the matrix, the second (Pic 2), at a higher potential, connected to the dissolution at the right of carbide precipitates of chromium. Steel is all the more sensitive to corrosion as the dissolution current is intense. Characteristic curves are presented in figures 2 and 3 .
  • the figure 2 demonstrates for the casting INV1 that the steel is strongly sensitized with respect to corrosion for incomes made in the hardening zone around 500 ° C. If corrosion resistance is a characteristic that should be favored for the applications envisaged, we will favor low-temperature incomes (200-380 ° C).
  • a quenching speed compatible with the know-how of the heat treatment and between 10 and 40 ° C./min in the temperature range 800 to 400 ° C. will be chosen.
  • compositions of the invention make it possible to obtain the hardness of 52 HRC or more after quenching under industrial conditions and double-tempered at 380 ° C., despite the softening experienced in this field for this family of steel from crude. quenching, as shown in figure 5 .

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Claims (16)

  1. Martensitischer Edelstahl, dadurch gekennzeichnet, dass er in Gewichtsprozenten:
    - 0,22 ≤ C ≤ 0,32%
    - 0,05 ≤ N ≤ N 0,15%, mit 0,33% ≤ C+N ≤ 0,43%
    - 10% ≤ Cr ≤ 12,4 %
    - 0,10% ≤ V ≤ 0,40%
    - 0,10% ≤ Mo ≤ 1,0%
    - Spuren ≤ Ni ≤ 1,0%
    - Spuren ≤ Mn ≤ 1,0%
    - Spuren ≤ Si ≤ 1,0%
    - Spuren ≤ W ≤ 1,0%
    - Spuren ≤ Co ≤ 1,0%
    - Spuren ≤ Cu ≤ 1,0%
    - Spuren ≤ Ti ≤ 0,010%
    - Spulen ≤ Nb ≤ 0.050%
    - Spuren ≤ Al ≤ 0,050%
    - Spuren ≤ S ≤ 0,020%
    - Spuren ≤ O ≤ 0,0040%
    - Spuren ≤ P ≤ 0,03%
    - Spuren ≤ B ≤ 0,0050%
    - Spuren ≤ Ca ≤ 0,020%
    - Spuren ≤ Se ≤ 0,010%
    - Spuren ≤ La ≤ 0,040%
    - Spuren ≤ Ce ≤ 0,040%
    umfasst, wobei der Rest Eisen und Verunreinigungen, die aus der Bearbeitung resultieren, ist.
  2. Stahl gemäß Anspruch 1, dadurch gekennzeichnet, dass 0,08% ≤ N ≤ 0,12% ist.
  3. Stahl gemäß Anspruch 1 oder 2, dadurch gekennzeichnet, dass 11,0% ≤ Cr ≤ 12.4% ist.
  4. Stahl gemäß einem der Ansprüche 1 bis 3, durch gekennzeichnet, dass 0,15% ≤ V ≤ 0,35% ist.
  5. Stahl gemäß einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass Spuren ≤ Si ≤ 0.5% ist,
  6. Stahl gemäß einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass 0.10% ≤ Mo + W/2 ≤ 1,20% ist.
  7. Stahl gemäß einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, dass Spuren ≤ Ti ≤ 0,003% ist.
  8. Stahl gemäß einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, dass Spuren ≤ Nb ≤ 0,010% ist.
  9. Stahl gemäß einem der Ansprüche 1 bis 8, dadurch gekennzeichnet, dass Spuren ≤ O ≤ 0.0015% ist.
  10. Stahl gemäß einem der Ansprüche 1 bis 9, dadurch gekennzeichnet, dass Spuren ≤ S ≤ 0,003% ist.
  11. Stahl gemäß einem der Ansprüche 1 bis 10, dadurch gekennzeichnet, dass Spuren ≤ Mn + Cu + Co ≤ 1,8%, ist.
  12. Verfahren zur Herstellung eines martensitischen Edelstahlteils, dadurch gekennzeichnet, dass:
    - ein Stahl gemäß einem der Ansprüche 1 bis 11 erzeugt, gegossen, geschmiedet oder gewalzt und geglüht wird;
    - der Stahl so verarbeitet wird, dass ihm die Form des Teiles gegeben wird;
    - der verarbeitet Stahl, bei einer Temperatur von 990-1040 °C, bevorzugt 1000∼1030°C austenitisiert wird,
    - der austenitisierte Stahl mit einer Geschwindigkeit im Temperaturintervall von 800 bis 400 °C zwischen 10 und 40 °C/min abgeschreckt wird;
    - der abgeschreckte Stahl zwei Mal getempert wird, um ihm seine endgültige Härte zu verleihen.
  13. Verfahren gemäß Anspruch 12, dadurch gekennzeichnet, dass beide Tempern bei einer Temperatur von 200 bis 400 °C, bevorzugt 300 bis 380 °C während mindestens 2 h, um die Aufrechterhaltung der nominalen Temperatur im Kern für mindestens 1 h zu gewährleisten, so vorgenommen werden, dass eine Härte von 49 bis 55 HRC erhalten wird.
  14. Verfahren gemäß Anspruch 12, dadurch gekennzeichnet, dass beide Tempern bei einer Temperatur von 530 bis 560 °C während mindestens 2 h, um die Aufrechterhaltung der nominalen Temperatur im Kern für mindestens 1 h zu gewährleisten, so vorgenommen wird, dass eine Härte von 42 bis 50 HRC erhalten wird.
  15. Martensitisches Edelstahlteil, dadurch gekennzeichnet, dass das Formelement, welches durch das Verfahren hergestellt wird, hergestellt wird gemäß einem der Ansprüche 12 bis 14,
  16. Teil gemäß Anspruch 15, dadurch gekennzeichnet, dass es sich um ein Gussformelement handelt, dass zur Herstellung von Plastikartikeln bestimmt ist.
EP08830336A 2007-09-10 2008-08-25 Martensitischer edelstahl, verfahren zur herstellung von teilen aus diesem stahl und daraus hergestellte teile Revoked EP2188402B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0757451A FR2920784B1 (fr) 2007-09-10 2007-09-10 Acier inoxydable martensitique, procede de fabrication de pieces realisees en cet acier et pieces ainsi realisees
PCT/FR2008/051525 WO2009034282A1 (fr) 2007-09-10 2008-08-25 Acier inoxydable martensitique, procédé de fabrication de pièces réalisées en cet acier et pièces ainsi réalisées.

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EP2188402A1 EP2188402A1 (de) 2010-05-26
EP2188402B1 true EP2188402B1 (de) 2012-05-23

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EP08830336A Revoked EP2188402B1 (de) 2007-09-10 2008-08-25 Martensitischer edelstahl, verfahren zur herstellung von teilen aus diesem stahl und daraus hergestellte teile

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US (1) US20100276038A1 (de)
EP (1) EP2188402B1 (de)
JP (1) JP2010539325A (de)
KR (1) KR20100059965A (de)
CN (1) CN101861407A (de)
CA (1) CA2698889A1 (de)
FR (1) FR2920784B1 (de)
RU (1) RU2010114173A (de)
WO (1) WO2009034282A1 (de)

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CN110656293A (zh) * 2019-11-01 2020-01-07 育材堂（苏州）材料科技有限公司 含Mo高硬度不锈钢、热处理工艺及成形构件
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CN111440995B (zh) * 2020-05-25 2021-02-05 江苏丰尚智能科技有限公司 一种小孔径环模的制造方法

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CA2698889A1 (fr) 2009-03-19
FR2920784A1 (fr) 2009-03-13
RU2010114173A (ru) 2011-10-20
US20100276038A1 (en) 2010-11-04
CN101861407A (zh) 2010-10-13
EP2188402A1 (de) 2010-05-26
JP2010539325A (ja) 2010-12-16
FR2920784B1 (fr) 2010-12-10
WO2009034282A1 (fr) 2009-03-19

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