WO2022131504A1 - Acier inoxydable austénitique doté d'une résistance au ramollissement à haute température améliorée - Google Patents

Acier inoxydable austénitique doté d'une résistance au ramollissement à haute température améliorée Download PDF

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WO2022131504A1
WO2022131504A1 PCT/KR2021/014158 KR2021014158W WO2022131504A1 WO 2022131504 A1 WO2022131504 A1 WO 2022131504A1 KR 2021014158 W KR2021014158 W KR 2021014158W WO 2022131504 A1 WO2022131504 A1 WO 2022131504A1
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stainless steel
austenitic stainless
high temperature
softening
rolling
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PCT/KR2021/014158
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English (en)
Korean (ko)
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이재화
이문수
조규진
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주식회사 포스코
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Publication of WO2022131504A1 publication Critical patent/WO2022131504A1/fr

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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
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
    • 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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • 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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/005—Modifying the physical properties by deformation combined with, or followed by, heat treatment of ferrous 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
    • C22C38/42—Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
    • 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
    • C21D2211/001—Austenite

Definitions

  • the present invention relates to austenitic stainless steel having improved resistance to softening at high temperatures, and more particularly, to austenitic stainless steel capable of preventing softening even at a high temperature of 500 to 600° C., which is mainly used for gaskets.
  • a cylinder head gasket or an exhaust manifold gasket of an automobile or motorcycle engine is a part exposed to repeated pressure fluctuations under high temperature, high pressure, and high vibration characteristic of an engine.
  • a high pressure is applied during compression to the automobile engine cylinder gasket, it must be in contact with both contacting counterparts with a high surface pressure in order to maintain the sealability of the combustion gas.
  • austenitic stainless steel is deformed by transformation from an unstable austenite phase to a martensite phase at room temperature during cold working, that is, transformation induced plasticity.
  • transformation induced plasticity the strength of the material also increases. Therefore, in order to secure the strength of the material, it is necessary to increase the cold rolling reduction ratio.
  • the yield stress (0.2% yield strength) continuously increases, resulting in a rough surface during gasket molding, local stress concentration in the material, and necking in the bent portion. do.
  • the above-mentioned surface and processing shape defects are factors that significantly deteriorate the gas sealing properties. That is, an increase in the cold rolling reduction rate acts as a factor that deteriorates toughness, fatigue resistance, and workability.
  • the material is softened (strength decreased) as the above-described processed martensite phase is decomposed, and the stability is poor.
  • Embodiments of the present invention are intended to provide an austenitic stainless steel capable of securing softening resistance at a temperature of 500° C. or higher by refining crystal grains.
  • the austenitic stainless steel having improved resistance to high temperature softening according to an embodiment of the present invention is, by weight, C: 0.02 to 0.15%, N: 0.1 to 0.3%, Si: 0.2 to 0.7, Mn: 2.0 to 5.0% , Cr: 17.0 to 19.0%, Ni: 2.5 to 5.0%, Cu: 1.0 to 3.0%, the remaining Fe and unavoidable impurities, and satisfies the following formula (1).
  • C, N, Si, Mn, Cr, Ni, and Cu mean weight % of each element.
  • the average grain diameter may be 10 ⁇ m or less.
  • Ca: 0.001 to 0.003%, B: 0.001 to 0.005%, P: 0.1% or less (excluding 0) and S: 0.01% or less (excluding 0) at least one of may further include.
  • the yield strength may be 450 MPa or more.
  • the hardness may be 450 Hv or more.
  • the elongation may be 35% or more.
  • a method of manufacturing austenitic stainless steel having improved resistance to high temperature softening according to another embodiment of the present invention, in weight %, C: 0.02 to 0.15%, N: 0.1 to 0.3%, Si: 0.2 to 0.7, Mn: 2.0 to 5.0%, Cr: 17.0 to 19.0%, Ni: 2.5 to 5.0%, Cu: 1.0 to 3.0%, including the remaining Fe and unavoidable impurities, hot rolling and hot annealing of a slab satisfying the following formula (1) step; cold-rolling the hot-rolled annealing material to a total reduction ratio of 50% or more; and heat-treating the cold-rolled material at 900°C to 1000°C.
  • C, N, Si, Mn, Cr, Ni, and Cu mean weight % of each element.
  • the total reduction ratio may be 70% or more.
  • the hot rolling may be performed at 1,050 to 1,300 °C.
  • the step of solution heat treatment at 1050 to 1200 °C may be further included.
  • an austenitic stainless steel applicable as a gasket material because it is possible to secure softening resistance at a temperature of 500° C. or higher while ensuring strength and workability.
  • an austenitic stainless steel having a reduced nickel content while ensuring elongation and corrosion resistance comparable to the existing 301 stainless steel.
  • Example 1 is a microstructure photograph taken with an optical microscope (Optical Microscope, OM) of Comparative Example 1 and Example 1 steel.
  • the austenitic stainless steel having improved resistance to high temperature softening according to an embodiment of the present invention is, by weight, C: 0.02 to 0.15%, N: 0.1 to 0.3%, Si: 0.2 to 0.7, Mn: 2.0 to 5.0% , Cr: 17.0 to 19.0%, Ni: 2.5 to 5.0%, Cu: 1.0 to 3.0%, the remaining Fe and unavoidable impurities, and satisfies the following formula (1).
  • C, N, Si, Mn, Cr, Ni, and Cu mean weight % of each element.
  • Methods for improving the strength of a material include solid solution strengthening, precipitation strengthening, dispersion strengthening, generation of martensite phase, crystal grain refinement, and the like.
  • the method of refining the crystal grains of the material can not only expect an improvement in superior strength compared to the strength obtained through a conventional level of heat treatment, but also improve the strength and toughness, thereby improving the mechanical properties of the material. It is used as a useful tool to improve.
  • the method of refining the crystal grains of the material is attracting attention in various alloy fields because it can reduce defects inside the material, obtain a uniform material, and does not require the addition of additional alloying elements.
  • thermomechanical control process a process induced transformation process (SIMRT, Strain-Induced Martensite and its Reverse Transformation) is widely used.
  • the processing induced transformation process is a method using the characteristic of reverse transformation of the martensite phase introduced during cold working to an austenite phase by cold working a material having a metastable austenite structure at room temperature and heating it to a temperature of 600° C. or higher.
  • the reverse transformation austenite phase Compared to untransformed austenite, the reverse transformation austenite phase has a higher dislocation density and fine grains, so the strength of the material can be improved, and the elongation rate is greater than that of the austenite phase before reverse transformation.
  • the present inventors derived the stability range of the austenite phase considering both the amount of martensite produced during cold working and the reverse transformation temperature related to the grain size of the austenitic stainless steel.
  • the austenitic stainless steel having improved resistance to high temperature softening according to an aspect of the present invention is, by weight, C: 0.02 to 0.15%, N: 0.1 to 0.3%, Si: 0.2 to 0.7%, Mn: 2.0 to 5.0% , Cr: 17.0 to 19.0%, Ni: 2.5 to 5.0%, Cu: 1.0 to 3.0%, remaining Fe and unavoidable impurities.
  • the unit is % by weight.
  • the content of C is 0.02 to 0.15%.
  • Carbon (C) is an effective element for stabilizing the austenite phase, and in the present invention, 0.02% or more may be added to secure the strength of the material.
  • the content when the content is excessive, it not only reduces cold workability due to solid solution strengthening, but also induces grain boundary precipitation of Cr carbides by combining with Cr, thereby reducing ductility, toughness and corrosion resistance, and martensite transformation start temperature (Martensite Start temperature). , Ms) is lowered, so there is a problem that strength cannot be secured because the generation of stress-induced martensite is not smooth during cold working, and the upper limit can be limited to 0.15%.
  • the content of N is 0.1 to 0.3%.
  • the content of Si is 0.2 to 0.7%.
  • Silicon (Si) is an element that acts as a deoxidizer during the steelmaking process, and may be added in an amount of 0.2% or more to secure corrosion resistance.
  • the content of silicon, which is a ferrite phase stabilizing element is excessive, delta ( ⁇ )-ferrite is formed in the cast slab to reduce hot workability, and there is a problem in that the ductility and toughness of the steel are lowered in the solid solution strengthening effect.
  • the upper limit may be limited to 0.7%.
  • the content of Mn is 2.0 to 5.0%.
  • Manganese (Mn) is an austenite phase stabilizing element added instead of nickel (Ni) in the present invention. It is effective in improving cold rolling properties by suppressing processing-induced martensite formation, and increasing the solubility of nitrogen (N) during the steelmaking process. 2.0% or more can be added as an element to However, if the content is excessive, the martensite transformation initiation temperature (Ms) is lowered, so that the generation of stress-induced martensite during cold working is not smooth, and the surface quality is reduced due to surface oxidation during hot rolling and reverse transformation heat treatment. , since the increase in S-based inclusions (MnS) may reduce the ductility, toughness and corrosion resistance of the steel, the upper limit thereof may be limited to 5.0%.
  • the content of Cr is 17.0 to 19.0%.
  • Chromium (Cr) is a basic element that stabilizes ferrite and contains the most among elements for improving corrosion resistance of stainless steel. In the present invention, 17.0% or more may be added to suppress the formation of martensite phase.
  • chromium which is a ferrite phase stabilizing element
  • delta ( ⁇ )-ferrite is formed in the cast slab to reduce hot workability, and stress-induced martensite is not smoothly generated during cold working, and martensite is formed.
  • the content of Ni is 2.5 to 5.0%.
  • Nickel (Ni) is the most powerful austenite phase stabilizing element, and as its content increases, the austenite phase is stabilized to soften the material.
  • Ni is added by 2.5% or more. It is essential However, if the content is excessive, as Ni is an expensive element, it causes an increase in raw material cost, and the martensite transformation initiation temperature (Ms) is lowered, so that the generation of stress-induced martensite is not smooth during cold working, so strength is secured. Since there is a problem that it cannot be done, the upper limit can be limited to 5.0%.
  • the content of Cu is 1.0 to 3.0%%.
  • Copper (Cu) is an austenite phase stabilizing element, and in the present invention, it is added by 1.0% or more in order to soften the material by reducing Stacking Fault Energy (SFE).
  • SFE Stacking Fault Energy
  • Ms martensite transformation initiation temperature
  • Ca: 0.001 to 0.003%, B: 0.001 to 0.005%, P: 0.1% or less (excluding 0) and S: 0.01% or less (excluding 0) at least one of may further include.
  • the content of Ca is 0.001 to 0.003%.
  • Calcium (Ca) is an element that suppresses the formation of MnS steel-making inclusions generated at grain boundaries when Mn is contained in a large amount. In the present invention, 0.001% or more may be added to improve the cleanliness of the material. However, when the content is excessive, there is a problem that Ca-based inclusions are generated to deteriorate the hot workability and surface quality of the material, so the upper limit can be limited to 0.003%.
  • the content of B is 0.001 to 0.005%.
  • Boron (B) is an effective element for suppressing crack generation during casting and securing good surface quality, and may be added in an amount of 0.001% or more. However, if the content is excessive, there is a problem that nitride (BN) is formed on the surface of the product during the annealing/pickling process to deteriorate the surface quality, so the upper limit may be limited to 0.005%.
  • the content of P is 0.1% or less (excluding 0).
  • Phosphorus (P) is an impurity that is unavoidably contained in steel and is an element that causes intergranular corrosion or inhibits hot workability.
  • the upper limit of the P content is managed as 0.1%.
  • the content of S is 0.01% or less (excluding 0).
  • S is an impurity that is unavoidably contained in steel, and is an element that segregates at grain boundaries and is a major cause of inhibiting hot workability, so it is desirable to control its content as low as possible.
  • the upper limit of the S content is managed as 0.015%.
  • the remaining component of the present invention is iron (Fe).
  • Fe iron
  • martensitic transformation occurs by plastic (cold) working at a temperature higher than or equal to the martensitic transformation initiation temperature (Ms).
  • the above-mentioned martensitic phase fraction depends on the austenite phase stability.
  • the upper limit temperature at which the phase transformation occurs by such plastic working is expressed by the Md value, and is a measure of the degree of phase transformation occurring by the processing.
  • the temperature (°C) at which 50% of the phase transformation to martensite occurs is defined as Md 30 .
  • Md 30 value is used as an index for determining the degree of austenite stabilization of conventional austenitic stainless steels, and can be expressed by the component relational expression of Equation (1) below.
  • Equation (1) the higher the value of Equation (1), the more active the transformation from the austenite phase to the martensite phase occurred due to external stress, but surface defects occurred and the workability decreased. It was tried to control the transformation amount of processing-induced martensite through the value.
  • the Md 30 value expressed by Equation (1) satisfies the range of -30°C to 30°C.
  • Equation (1) When the value of Equation (1) is less than -30°C, the processing-induced martensite phase acting as a nucleation site cannot be secured, and the average grain size cannot be derived to 10 ⁇ m or less. On the other hand, when the value of Equation (1) is too high, the austenitic stainless steel of the above-mentioned alloy composition is accompanied by a sharp work-induced martensitic transformation behavior due to external deformation. Accordingly, there is a problem that surface defects of the austenitic stainless steel occur and workability is reduced, so that the upper limit of Equation (1) is limited to 30°C.
  • a method of manufacturing austenitic stainless steel having improved resistance to high temperature softening according to an embodiment of the present invention, in weight%, in weight%, C: 0.02 to 0.15%, N: 0.1 to 0.3%, Si: 0.2 to 0.7, Mn : 2.0 to 5.0%, Cr: 17.0 to 19.0%, Ni: 2.5 to 5.0%, Cu: 1.0 to 3.0%, including the remaining Fe and unavoidable impurities, hot rolling and hot rolling a slab satisfying the following formula (1) annealing; cold-rolling the hot-rolled annealing material to a total reduction ratio of 50% or more; and cold-rolling and annealing the cold-rolled material at 900°C to 1000°C.
  • C, N, Si, Mn, Cr, Ni, and Cu mean weight % of each element.
  • a slab having the above composition may be subjected to conventional casting, hot rolling, solution heat treatment and pickling to manufacture a hot-rolled annealed material.
  • the slab can be hot rolled at a temperature of 1,050 to 1,300 ° C, which is a normal rolling temperature, and solution heat treatment is performed in a temperature range of 1,050 to 1,200 ° C to remove surface defects of the hot-rolled steel sheet and dissolve precipitates. can be performed.
  • the solution heat treatment may be performed for 60 to 120 seconds.
  • the hot-rolled steel sheet may be pickled to remove surface scale, and then cold-rolled to manufacture a thin film.
  • the austenite phase of the hot-rolled annealed steel sheet is transformed into a processing-induced martensitic phase by processing, and as the rolling reduction increases, the fraction of the martensite phase increases, thereby increasing the yield strength of the material.
  • a relatively high reduction ratio of 50% or more is applied to promote the production of processed induced martensite to secure a yield strength of 500Mpa or more.
  • the total reduction ratio can be controlled to 70% or more.
  • the heat treatment for forming the reverse transformation austenite phase may be performed in the range of the austenite reverse transformation completion temperature (Austenite finish temperature, hereinafter AF) to AF+50°C.
  • austenite reverse transformation completion temperature Austenite finish temperature, hereinafter AF
  • the reverse transformation heat treatment temperature is preferably controlled to be low in the vicinity of the austenite reverse transformation completion temperature AF.
  • reverse transformation heat treatment may be performed at 900°C to 1000°C for 10 seconds to 10 minutes.
  • the cold-rolled material thus manufactured has an average grain size of 10 ⁇ m or less.
  • the manufactured cold rolled material has a yield strength of 450 MPa or more.
  • the manufactured cold-rolled material can secure a hardness of 450 Hv or more even at a temperature of 500 ° C. or more.
  • a slab was prepared through ingot melting, heated at 1,230 ° C. for 2 hours, and then hot rolled to a thickness of 3 mm was performed. After hot rolling, 1,050 Solution heat treatment was performed at °C. Next, the hot-rolled coil was subjected to cold rolling at a reduction ratio of 50%, and heat treatment was performed at 900° C. for 1 minute.
  • Example 1 0.11 0.210 0.45 3.9 18.0 3.5 1.5 0.04 0.004 -24.17
  • Example 2 0.05 0.180 0.3 3.6 17.7 3.7 2.0 0.04 0.004 5.03
  • Comparative Example 1 0.06 0.22 0.55 4.3 18.7 4.2 1.4 0.04 0.004 -36.84
  • Comparative Example 2 0.08 0.16 0.4 3.2 17.3 3.2 1.3 0.04 0.004 43.01
  • a tensile test was performed at a speed of 20 mm/min using a test piece processed according to the JIS 13B standard, and yield strength (MPa) was measured.
  • the average grain size was measured by photographing with an optical microscope (Optical Microscope, OM) after performing nitric acid electrolytic pickling on the cold-rolled steel sheet. Through an image analyzer of the obtained microstructure photograph, arbitrary 3 points of the steel plate were measured, and then the average value was expressed.
  • optical microscope Optical Microscope, OM
  • temper rolling was performed with a work roll having an average roughness of #600 or more, and the hardness and formability of the temper rolling material were evaluated.
  • the hardness of the temper rolling material was shown in Table 2 below by measuring the hardness value of the surface portion under the condition of Vickers hardness (1 kg/f).
  • the hardness value of the surface part was measured under the condition of Vickers hardness (1 kg/f), and it is shown in Table 2 below.
  • Example 1 is a microstructure photograph taken with an optical microscope (Optical Microscope, OM) of Comparative Example 1 and Example 1 steel.
  • Example 3 in Comparative Example 3 to which general heat treatment conditions were applied, the average grain size was 32 ⁇ m and exceeded 10 ⁇ m, whereas Example 3 was heat treated at a temperature near the austenite reverse transformation completion temperature (AF). In the case of , the average grain size was as fine as 8 ⁇ m.
  • AF austenite reverse transformation completion temperature
  • the alloy component and the relational expression to derive the grain size to 10 ⁇ m or less, excellent elongation and surface quality of 35% or more can be secured during temper rolling, and the gasket application temperature is 500 to It is possible to manufacture austenitic stainless steel that can prevent softening in the temperature range of 600 °C.
  • the present invention while ensuring strength and workability, it is possible to secure softening resistance at a temperature of 500° C. or higher, so that it can be applied as a gasket material.

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Abstract

La présente divulgation concerne un acier inoxydable austénitique doté d'une résistance au ramollissement à haute température améliorée. Selon la présente invention, l'acier inoxydable comprend, en % en poids, C : 0,02-0,15 %, N : 0,1-0,3 %, Si : 0,2-0,7 %, Mn : 2,0-5,0 %, Cr : 17,0-19,0 %, Ni : 2,5-5,0 %, Cu : 1,0-3,0 %, le reste étant du Fe et des impuretés inévitables, et répond à la formule (1). Formule (1) : -30 ≤ 551 - 462 x (C + N) - 9,2 x Si - 8,1 x Mn - 13,7 x Cr - 29 x (Ni + Cu) ≤ 30, où C, N, Si, Mn, Cr, Ni et Cu indiquent la teneur (% en poids) des éléments respectifs.
PCT/KR2021/014158 2020-12-14 2021-10-14 Acier inoxydable austénitique doté d'une résistance au ramollissement à haute température améliorée WO2022131504A1 (fr)

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KR1020200174138A KR102537950B1 (ko) 2020-12-14 2020-12-14 고온 연화저항성이 향상된 오스테나이트계 스테인리스강
KR10-2020-0174138 2020-12-14

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JP2017145460A (ja) * 2016-02-17 2017-08-24 新日鐵住金ステンレス株式会社 低温での耐破壊性に優れた構造部材用フェライト・オーステナイト系ステンレス鋼板及びその製造方法

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