WO2020098448A1 - 高强度不锈钢、热处理工艺及成形构件 - Google Patents

高强度不锈钢、热处理工艺及成形构件 Download PDF

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WO2020098448A1
WO2020098448A1 PCT/CN2019/111884 CN2019111884W WO2020098448A1 WO 2020098448 A1 WO2020098448 A1 WO 2020098448A1 CN 2019111884 W CN2019111884 W CN 2019111884W WO 2020098448 A1 WO2020098448 A1 WO 2020098448A1
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stainless steel
less
strength stainless
heat treatment
treatment process
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French (fr)
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易红亮
邓彪
王国栋
熊小川
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育材堂（苏州）材料科技有限公司
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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
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/005—Heat treatment of ferrous alloys containing Mn
    • 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
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/008—Heat treatment of ferrous alloys containing Si
    • 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
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • 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
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • 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
    • C22C38/26—Ferrous alloys, e.g. steel alloys containing chromium with niobium or tantalum
    • 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
    • C22C38/28—Ferrous alloys, e.g. steel alloys containing chromium with titanium or zirconium
    • 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
    • C22C38/34—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon
    • 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
    • C22C38/38—Ferrous alloys, e.g. steel alloys containing chromium 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
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/001—Austenite
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the invention relates to a high-strength stainless steel, a heat treatment process and a shaped member.
  • martensitic chromium stainless steels (Cr13, Cr13Mo, etc.) are widely used in knives, turbine blades, bearings, valves, structural parts and wear-resistant parts because of their good corrosion resistance and high strength.
  • the hardness of this type of stainless steel is still very high after tempering, and the toughness has improved. With the increase of carbon content, the hardness gradually increases, but the toughness and corrosion resistance gradually decrease.
  • the microstructure of commonly used high-strength stainless steel is basically a full martensite structure, austenite will reduce the hardness, so the austenite structure is often eliminated, but its effect of improving toughness is ignored.
  • the Quenching-Tempering Partitioning (Q & P) process utilizes the diffusion and enrichment of carbon atoms into residual austenite during tempering to stabilize austenite, which can significantly improve the strong plasticity of the material.
  • Q & P Quenching-Tempering Partitioning
  • a moderate amount of metastable austenite at room temperature plays a significant role in improving the shape and toughness of high strength stainless steel. It may be one of the effective ways to solve the poor strength-toughness matching of high-strength stainless steel.
  • an object of the present invention is to provide a high-strength and high-toughness stainless steel whose martensite transformation start temperature (Ms) is low, so that the quenching temperature can be reduced to room temperature during heat treatment,
  • Ms martensite transformation start temperature
  • Another object of the present invention is to provide a process for heat-treating the above-mentioned high-strength and high-toughness stainless steel, which has a large process window, simple and reliable temperature control, and can at the same time ensure the formation of ultra-high-strength and toughness shaped members.
  • Another object of the present invention is to provide a shaped member that can significantly improve plasticity and toughness while ensuring higher strength and hardness.
  • the first aspect of the present invention relates to a high-strength stainless steel comprising, by weight content, 0.2-0.35% C, 0.7-3.5% Mn, 0.6-2.0% Si, 11.0-17.0% Cr, 0.20% or less Nb, 0.20% or less Ti, and the balance Fe and impurities.
  • the martensite transformation start temperature (Ms) is lower than 250 ° C, so that after quenching to room temperature, tempering heat treatment can be performed at any time , Which makes the heat treatment process window larger.
  • Cr carbide is almost completely solutionized during solution treatment, and can retain an appropriate amount of residual austenite when quenched to room temperature.
  • the addition of Si suppresses the formation of cementite and the austenite does not decompose And, due to the diffusion and enrichment of carbon atoms, the retained austenite can be stable at room temperature, thereby increasing the plasticity and toughness of the shaped member.
  • the C content is 0.2 to 0.3%
  • the Cr content is 12.0 to 14%
  • the Nb content is 0.10% or less
  • the Ti content is 0.10% or less.
  • the Ms point can be further controlled within the range of 120 to 200 ° C, thereby obtaining a larger process window and making it easier to obtain a high-strength and toughened shaped member.
  • the above high-strength stainless steel may further include one or more of the group consisting of: 2.0% or less Mo; 1.0% or less W; 1.0% or less V; 3.0% or less Cu; 4.0% or less Ni ; Zr below 0.4%.
  • the second aspect of the present invention relates to a heat treatment process of high-strength stainless steel.
  • the heat treatment process includes the following steps: Step a: heat the high-strength stainless steel of the first aspect to 1000 to 1200 ° C and keep it for 1 to 3600s; Step b: The high-strength stainless steel processed in the step a is cooled to below 100 ° C; and in the step c, the high-strength stainless steel processed in the step b is heated to 150-400 ° C and then kept for 10 to 10000s, and then Cool to room temperature by any cooling method.
  • the solution treatment temperature in step a is between 1000 and 1200 ° C, and the carbides of Cr are substantially completely dissolved, which improves the pitting corrosion resistance of the substrate; the martensite begins to have a low phase transition point, after solution treatment Quenching to room temperature in step b can retain an appropriate amount of retained austenite.
  • step b Due to its greater quenching martensite stress and poor residual austenite stability, its high hardness is high but its plastic toughness is extremely poor; Low temperature tempering treatment, eliminate the stress in the quenched martensite to obtain the tempered martensite structure to improve the toughness of the martensite itself, and at the same time, the carbon atoms are distributed from the supersaturated martensite to the residual austenite to stabilize the austenite. Metastable plate-like or film-like austenite with reasonable stability at room temperature. The residual austenite can greatly improve the plasticity and toughness of steel materials due to its TRIP effect. Therefore, compared with the quenched structure in step b, step c After the tempered structure is slightly reduced, the plastic toughness is significantly improved.
  • the macro-hardness of the high-strength stainless steel processed by the heat treatment process of the present invention reaches 48HRC-55HRC, the impact absorption work of the 2mm deep U-notch standard sample is between 30J-130J, the yield strength is 1100MPa-1300MPa, the tensile strength is 1600MPa-1900MPa, The elongation rate is 9.0% ⁇ 15%.
  • the pitting potential in the 3.5% NaCl solution reaches more than 270mV. High corrosion resistance, high strength and toughness and strong plasticity are achieved simultaneously.
  • step b the high-strength stainless steel is quenched to room temperature, so the process window is large, and temperature control is easier.
  • step a heat is maintained at 1000 to 1100 ° C for 60 to 3600s.
  • the holding time can be set to 60 to 900s.
  • the holding time can be set from 90 to 1200s.
  • step a it is heated rapidly at a heating rate of 10 ° C / s or more to 1050 to 1200 ° C, and then kept for 1 to 600s. More preferably, in the step a, it is rapidly heated to 1050 to 1200 ° C at a heating rate of 20 ° C / s or more, and then kept for 1 to 30s.
  • the solution treatment in step a includes long-term heat preservation and rapid austenitization.
  • the chromium carbides are almost completely solid solution, and the grains are easy to coarsen, so a lower heating temperature of 1000 ⁇ 1100 °C is used.
  • rapid austenitization can avoid grain growth and coarsening, reduce the grain size, and use a higher heating temperature of 1050 to 1200 ° C for rapid austenitization. Therefore, for step a, rapid heating at a heating rate of 10 ° C / s or more to 1050 to 1200 ° C for 1 to 600 s can significantly reduce the grain size.
  • By rapidly heating to a temperature of 1050 to 1200 ° C for 1 to 30 s at a heating rate of more than 20 ° C / s its grain size is further reduced.
  • step a and step b high-strength stainless steel can be hot stamped into the desired member shape.
  • the material is first treated with solution austenite and then hot stamped by the mold, and then quickly cooled to room temperature.
  • This process is similar to step a and step b of the heat treatment process of the present invention.
  • the workpiece can be hot stamped into the desired member shape after high-temperature austenitization in step a, and then step b Quick cooling, has little effect on material properties.
  • step b it is cooled to room temperature at an average cooling rate of 10 ° C / s or more.
  • the high-strength stainless steel of the present invention has better alloying properties and better hardenability.
  • step c when the thickness of the high-strength stainless steel is less than 4 mm, the holding time can be set to 1 to 30 min, and when the thickness of the high-strength stainless steel is greater than or equal to 4 mm, the holding time can be set to 4 to 60 min.
  • the third aspect of the present invention relates to a shaped member made of the high-strength stainless steel of the first aspect, the microstructure of the shaped member consists of 5% to 30% of retained austenite, 70% by area -95% martensite, less than 1% Nb, Ti carbides, and less than 2% Cr carbides.
  • the above-mentioned shaped member can be made by the heat treatment process of the second aspect, and after step b, a quenched structure of high-strength stainless steel is obtained, and its microstructure in terms of area is from 5% to 30% of retained austenite, 70% to 95% Martensite, less than 1% Nb, Ti carbides, and less than 2% Cr carbides, residual austenite exists in the form of laths or films, with an average thickness of less than 300 nm.
  • a quenched structure of high-strength stainless steel is obtained, the microstructure of which is from 5% to 20% of retained austenite, less than 0.3% of Nb and Ti carbides, and less than 0.5 % Of the carbide of Cr, the rest is composed of martensite, the residual austenite exists in the form of laths or films, and the thickness is less than 300 nm.
  • step c the tempered structure is obtained.
  • the internal stress of quenched martensite is greatly reduced, and the toughness is significantly improved.
  • Si element and high Cr element the precipitation of cementite is suppressed, and the carbon atoms Diffusion and distribution from supersaturated martensite to residual austenite makes residual austenite more stable, and a large amount of residual austenite still exists after tempering.
  • the microstructure of high-strength stainless steel is still composed of 5% -30% residual austenite, 70% -95% martensite, less than 1% Nb, Ti carbide, and less than 2% Cr
  • the carbide is composed of residual austenite in the form of laths or films, with an average thickness of less than 300 nanometers.
  • a tempered structure of high-strength stainless steel is obtained, and its microstructure is still from 5% to 20% of residual austenite, less than 0.3% of Nb and Ti carbide, and less than 0.5% Cr carbides, the rest is composed of martensite, the residual austenite exists in the form of laths or films, and the thickness is less than 300 nm.
  • the macro hardness of the shaped member according to the present invention is between 48HRC and 55HRC, the impact absorption work of the 2mm deep U-notch standard sample is between 30J and 130J, and the toughness is significantly improved compared to stainless steel with the same hardness;
  • the pitting potential is above 270mV;
  • the yield strength is 1100MPa-1300MPa, the tensile strength is 1600MPa-1900MPa, and the elongation is 9.0% -15%.
  • Its strong plasticity is superior to the existing Cr13 martensitic stainless steel products, and can be used for traditional high-strength stainless steel products such as medical equipment, springs, valves and general engineering components in the steam environment. Stamping production line, used in automobile crash safety structural parts.
  • the production cost is not much different from the traditional Cr13 martensitic stainless steel, but its strength, toughness and corrosion resistance are significantly improved.
  • the heat treatment process of the present invention is the same as the conventional stainless steel quenching and tempering process, without changing the original stainless steel production line, but the structure regulation and tempering treatment are significantly different.
  • the composition of austenite is not precipitated by cementite, so under the premise of high hardness, the plastic toughness is significantly improved.
  • FIG. 1 is a photomicrograph of samples 3 to 7 according to the present invention, where the broken line is the grain boundary line.
  • the high-strength stainless steel of the present invention includes, by weight content: 0.2-0.35% C, 0.7-3.50% Mn, 0.6-2.0% Si, 11.0-17.0% Cr, 0.20% or less Nb, 0.20 or less % Ti.
  • the C content is preferably 0.2 to 0.3%
  • the Cr content is preferably 12.0 to 14%
  • the Nb content is preferably 0.10% or less
  • the Ti content is preferably 0.10% or less. It may also include one or more of the group consisting of: 2.0% or less Mo; 1.0% or less W; 1.0% or less V; 3.0% or less Cu; 4.0% or less Ni; 0.4% or less Zr.
  • the balance is Fe and impurities.
  • carbon is the most important strengthening element, and its strength is improved by means of solid solution strengthening and dispersion precipitation strengthening.
  • carbon is also an austenite stabilizing element.
  • the carbon atoms are small and the diffusion rate is large. During the low temperature tempering process, they can quickly diffuse from carbon supersaturated martensite to residual austenite, and enrich in the residual austenite, increasing the residual austenite.
  • Body stability When the carbon content is lower than 0.20%, its strength is lower; when the carbon content is higher than 0.35%, the temperature at which the carbide completely dissolves in the matrix is too high, the original austenite grains are coarse, and the toughness is extremely poor.
  • the carbon content is controlled at 0.20 to 0.35%. In this range, carbon element can meet the requirements of stabilizing retained austenite and increase the toughness of the material.
  • the main function of chromium is to improve the corrosion resistance, which can react with oxygen to form a dense passivation film and suppress further corrosion of the substrate.
  • Chromium is also a strong carbide-forming element. It easily forms carbides such as Cr 23 C 6 with carbon and precipitates at the grain boundaries, which can effectively suppress the growth of grains and also reduce the chromium content at the grain boundaries. Corrosion resistance decreased. Properly increasing the solution treatment temperature can make the chromium carbide completely solution and increase the resistance to intergranular corrosion, but on the other hand, it will lead to abnormally large austenite grains.
  • the 17.0% chromium content has met the corrosion resistance requirements.
  • the upper limit of chromium content is 17.0%.
  • the chromium content is less than 11.0%, a dense passivation film cannot be formed, and the corrosion resistance drops sharply. Therefore, the lower limit of the chromium content is 11.0%.
  • Silicon is an important element of the steel of the present invention.
  • silicon can suppress the precipitation of cementite during low-temperature tempering, and promote the diffusion of carbon into residual austenite in a free state.
  • the silicon content is less than 0.6%, the precipitation of cementite cannot be effectively suppressed; on the other hand, when the silicon content is too high, the toughness and plasticity of the steel can be significantly reduced. Therefore, the silicon content is controlled at 0.6 to 2.0%.
  • Manganese is another important element in the steel of the present invention. Manganese can improve the hardenability. At the same time, manganese is also an austenite stabilizing element, which can reduce the starting temperature (Ms) of austenite to martensite. Under the premise of determining the composition of other alloys that affect the Ms point, the Ms point can only be adjusted by controlling the manganese content, thereby controlling the residual austenite content when quenched to room temperature.
  • the shaped member of the present invention contains 5.0% to 30.0% of retained austenite by area, which is mainly unconverted austenite when quenched to room temperature.
  • the manganese content is limited by the content of carbon, chromium and silicon. In order to obtain an appropriate amount of residual austenite at room temperature, the manganese content is controlled at 0.7 to 3.50%.
  • Nb, Ti ⁇ 0.20%, preferably ⁇ 0.10%
  • niobium and titanium are strong carbide-forming elements. Compared with chromium carbides, their carbide solid solution deposits are smaller. In the steel material of the present invention, chromium carbides are completely in solution during high-temperature solution treatment, while niobium and titanium carbides still exist, suppressing the growth of crystal grains. When niobium and titanium are not present, the growth of austenite grains during solution treatment is not inhibited, the grains are coarse, and the strength and toughness are reduced. On the other hand, when the content of niobium and titanium is too high, more large-size niobium and titanium carbon oxides are easily precipitated during solidification, which affects the toughness of the material. Therefore, the content of niobium and titanium should be controlled below 0.20%.
  • Mo 2.0% or less; W: 1.0% or less; V: 1.0% or less; Zr: 0.4% or less
  • Molybdenum, tungsten, vanadium and zirconium are all carbide-forming elements that can refine grains and increase strength.
  • these elements mainly play the role of solid solution strengthening and precipitation strengthening, and the increase in the content is not obvious for the improvement of these effects.
  • Nickel can improve the processing performance and corrosion resistance of steel, and nickel is also an austenitic stable element. In the steel of the present invention, too much nickel will affect the residual austenite content and increase unnecessary cost.
  • Copper can improve the strength and corrosion resistance, but when the copper content exceeds 3.0%, it will lead to deterioration in processability and increase unnecessary cost.
  • Table 1 below shows the composition of some steel materials according to the present invention, the balance being iron and impurities, and the following components are all calculated by weight percentage.
  • a plurality of samples were prepared for 1, 2, 3, and 4 in Table 1, and each was heat-treated.
  • the heat treatment process includes the following steps:
  • Solution treatment heating to 1000 ⁇ 1200 °C, preferably 1000 ⁇ 1100 °C, holding for 1 ⁇ 3600s;
  • Tempering heat treatment heating to 150 ⁇ 400 °C for 10 ⁇ 10000s and then cooling to room temperature by any cooling method.
  • the pitting potential of the steel material of the present invention reaches 270 mV.
  • the electrolyte solution used is 3.5% NaCl physiological saline
  • the reference electrode is a KCl saturated calomel electrode
  • the counter electrode is a platinum electrode.
  • the shaped member obtained by the steel material of the present invention after the heat treatment method of the present invention has high hardness, high toughness and high intergranular corrosion resistance, and its production cost has not been significantly increased, and has high industrial value. .

Abstract

本发明涉及一种高强度不锈钢、热处理工艺及成形构件。该高强度不锈钢以重量含量计包括0.2-0.35％的C、0.7-3.50％的Mn、0.6-2.0％的Si、11-17％的Cr、小于等于0.20％的Nb、小于等于0.20％的Ti，余量为Fe和杂质。热处理工艺包括以下步骤：步骤a：将所述高强度不锈钢加热至1000～1200℃后保温1～3600s；步骤b：将经过步骤a处理后的高强度不锈钢冷却至100℃以下；以及步骤c，将经过步骤b处理后的高强度不锈钢加热至150～400℃后保温10～10000s，然后以任意冷却方式冷却到室温。成形构件由所述高强度不锈钢制成，成形构件的微观组织以面积计由5％-30％的残余奥氏体，70％-95％的马氏体，低于1％的Nb、Ti碳化物，以及低于2％的Cr的碳化物构成。

Description

高强度不锈钢、热处理工艺及成形构件 技术领域
本发明涉及一种高强度不锈钢、热处理工艺及成形构件。
背景技术
常用马氏体铬不锈钢(Cr13、Cr13Mo等)因为其良好的耐蚀性以及较高的强度而被广泛应用于刀具、汽轮机叶片、轴承、阀门、结构件和耐磨件等。这类不锈钢经调质处理后硬度仍然很高，韧性有所改善，且随着碳含量的提高硬度逐渐增加，韧性和耐蚀性却逐渐降低。
高强度不锈钢最常用和最廉价的方式是通过提高成分中碳含量，来显著提高硬度，但同时韧性也急剧降低，而且在高温固溶处理时铬碳化物很难完全溶解，导致晶界处贫铬耐点蚀性能下降，这些是目前高强度不锈钢发展面临的难题。
常用高强度不锈钢的显微组织基本为全马氏体结构，奥氏体会降低硬度，故往往消除了奥氏体组织，却忽略了其提高韧性的作用。淬火～回火配分(Q&P)工艺利用回火过程中碳原子向残余奥氏体中的扩散富集稳定了奥氏体，从而能显著提高材料的强塑性。近些年，很多关于利用淬火～配分工艺提高马氏体不锈钢强塑性的研究也相继被发表，室温下适量亚稳定的奥氏体在提高高强度不锈钢的塑形和韧性方面作用明显，此方法可能是解决高强度不锈钢强韧性匹配性差的有效途径之一。
例如，2013年中国知网收录的学位论文《3Cr13马氏体不锈钢的组织与性能研究》(东北大学，张盛攀)以3Cr13马氏体不锈钢为研究对象，针对Q&P工艺中淬火温度、配分温度和配分时间3种参数设计了多种不同的Q&P热处理工艺，通过观察试样的显微组织，对比其力学性能，分析了Q&P热处理工艺对3Cr13钢组织转变、力学性能影响的规律，评估了Q&P热处理工艺在传统马氏体不锈钢中应用的可能性，其最佳抗拉强度达到1700MPa，延伸率达到18％(圆棒试样)。
但是，该论文仅仅是将Q&P工艺尝试性应用于3Cr13钢，并没有意识到高温固溶处理时铬碳化物大量未固溶导致的耐蚀性下降问题以及其性能的稳定性问题，同时其淬火温度对性能影响较大，工艺窗口 窄，难以工业应用。
发明内容
针对上述现有技术存在的问题，本发明的一个目的在于提供一种高强度高韧性不锈钢，其马氏体相变开始温度(Ms)较低，从而能够在热处理时将淬火温度降低至室温，使得热处理工艺窗口大，同时能确保获得具有超高强韧性的成形构件。
本发明的另一目的在于提供一种对上述高强度高韧性不锈钢进行热处理的工艺，其工艺窗口大，温度控制简单可靠，同时能确保获得超高强韧性的成形构件。
本发明的又一目的在于提供一种成形构件，其能够在确保较高强度和硬度的前提下，显著提高塑性和韧性。
本发明的第一方面涉及一种高强度不锈钢，以重量含量计，所述高强度不锈钢包括0.2～0.35％的C、0.7～3.5％的Mn、0.6～2.0％的Si、11.0～17.0％的Cr、小于等于0.20％的Nb、小于等于0.20％的Ti，余量为Fe和杂质。根据本发明，通过调整Si、Mn的含量与C、Cr的配比，使得马氏体相变开始温度(Ms)低于250℃，从而能够在淬火至室温之后，任意时间后进行回火热处理，这使得热处理工艺窗口变大。同时，固溶处理时Cr碳化物基本完全固溶，淬火到室温时能够保留适量残余奥氏体，在随后的回火过程中，Si的添加抑制了渗碳体的形成，奥氏体没有分解，并且由于碳原子的扩散富集，残余奥氏体能够稳定存在于室温条件下，从而增加了成形构件的塑性和韧性。
优选的是，C含量为0.2～0.3％，Cr含量为12.0～14％，Nb含量小于等于0.10％，Ti含量小于等于0.10％。
这种情况下，能够将Ms点进一步控制在120～200℃的范围内，从而获得更大的工艺窗口，更容易获得高强韧性的成形构件。
上述高强度不锈钢还可以包括由以下元素组成的组中的一种或多种：2.0％以下的Mo；1.0％以下的W；1.0％以下的V；3.0％以下的Cu；4.0％以下的Ni；0.4％以下的Zr。
本发明的第二方面涉及一种高强度不锈钢的热处理工艺，该热处理工艺包括以下步骤：步骤a：将第一方面的高强度不锈钢加热至1000～1200℃后保温1～3600s；步骤b：将经过所述步骤a处理后的所 述高强度不锈钢冷却至100℃以下；以及步骤c，将经过所述步骤b处理后的所述高强度不锈钢加热至150～400℃后保温10～10000s，然后以任意冷却方式冷却到室温。
根据本发明，步骤a中的固溶处理温度在1000～1200℃之间，Cr的碳化物基本完全固溶，提高基体耐点蚀性能；马氏体开始相变点较低，固溶处理后在步骤b中淬火到室温能够保留适量残余奥氏体，由于其淬火马氏体内应力较大而且残余奥氏体稳定性差，因此其强硬度虽然较高但塑韧性极差；然后经过步骤c的低温回火处理，消除淬火马氏体内应力得到回火马氏体组织从而改善马氏体本身的韧性，同时碳原子从过饱和的马氏体配分到残余奥氏体中稳定奥氏体，得到室温下稳定性合理的亚稳态板状或薄膜状奥氏体，该残余奥氏体因其TRIP效应可大幅提高钢铁材料的塑性和韧性，因此相对步骤b中的淬火态组织，经步骤c后的回火态组织在强硬度少量下降的前提下，塑韧性显著提高。
经过本发明的热处理工艺处理后的高强度不锈钢宏观硬度达到48HRC～55HRC，2mm深U型缺口标准试样冲击吸收功在30J～130J之间，屈服强度1100MPa～1300MPa，抗拉强度1600MPa～1900MPa，延伸率9.0％～15％，同时在质量分数为3.5％NaCl溶液中点蚀电位达到270mV以上，高耐蚀性、高强韧性及强塑性同时实现。而且，根据本发明，在步骤b中将高强度不锈钢淬火至室温，因此工艺窗口大，温度控制更易进行。
优选的是，在步骤a中，加热至1000～1100℃后保温60～3600s，当高强度不锈钢的厚度小于4mm时，保温时间可设定为60～900s，当高强度不锈钢的厚度大于等于4mm时，保温时间可设定为90～1200s。
或者优选的是，在所述步骤a中，以10℃/s以上的加热速率快速加热至1050～1200℃后保温1～600s。更加优选的是，在所述步骤a中，以20℃/s以上的加热速率快速加热至1050～1200℃后保温1～30s。
在本发明中，步骤a的固溶处理包括长时间保温和快速奥氏体化。长时间保温时，由于固溶温度较高，铬碳化物基本完全固溶，晶粒容易粗化，因此采用较低加热温度1000～1100℃。另一方面，由于晶粒的长大需要时间，所以快速奥氏体化可以避免晶粒长大粗化，降低晶粒尺寸，为快速实现奥氏体化采用较高加热温度1050～1200℃。因此对于 步骤a，以10℃/s以上的加热速率快速加热至1050～1200℃保温1～600s，能显著降低晶粒尺寸。通过以20℃/s以上的加热速率快速加热至1050～1200℃保温1～30s，其晶粒尺寸进一步降低。
在步骤a与步骤b之间，可以将高强度不锈钢热冲压成形为所需构件形状。
在热冲压生产线中，材料先被固溶奥氏体处理后再经模具热冲压，然后快速冷却至室温。此过程与本发明的热处理工艺的步骤a及步骤b相似，在步骤a与步骤b之间，工件经步骤a高温奥氏体化后可被热冲压成形为所需构件形状，然后经步骤b快速冷却，对材料性能影响不大。
优选的是，在步骤b中，以10℃/s以上的平均冷速冷却至室温。
本发明的高强度不锈钢由于添加合金元素较多，淬透性较好，但为了避免Cr碳化物析出，在b步骤中，优选以10℃/s以上的平均冷速冷却至室温。
在步骤c中，当高强度不锈钢的厚度小于4mm时，保温时间可设定为1～30min，当高强度不锈钢的厚度大于等于4mm时，保温时间可设定为4～60min。
本发明的第三方面涉及一种成形构件，该成形构件由第一方面的高强度不锈钢制成，所述成形构件的微观组织以面积计由5％～30％的残余奥氏体，70％～95％的马氏体，低于1％的Nb、Ti碳化物，以及低于2％的Cr的碳化物构成。
上述成形构件可由第二方面的热处理工艺制成，经步骤b之后得到高强度不锈钢的淬火态组织，其微观组织以面积计由5％～30％的残余奥氏体、70％～95％的马氏体、低于1％的Nb、Ti碳化物、以及低于2％的Cr的碳化物构成，残余奥氏体以板条或薄膜状存在，平均厚度小于300纳米。
优选的是，经步骤b之后得到高强度不锈钢的淬火态组织，其微观组织以面积计由5％～20％的残余奥氏体，低于0.3％的Nb、Ti碳化物，以及低于0.5％的Cr的碳化物，其余为马氏体构成，残余奥氏体以板条或薄膜状存在，厚度小于300纳米。
经步骤c之后得到回火组织，淬火态马氏体经回火处理后内应力大幅度降低，韧性显著提高，同时，由于Si元素的添加和高Cr元素抑 制了渗碳体的析出，碳原子从过饱和的马氏体中扩散配分到残余奥氏体中，使得残余奥氏体更加稳定，回火之后残余奥氏体仍然大量存在。高强度不锈钢的微观组织以面积计仍由5％～30％的残余奥氏体，70％～95％的马氏体，低于1％的Nb、Ti碳化物，以及低于2％的Cr的碳化物构成，残余奥氏体以板条或薄膜状存在，平均厚度小于300纳米。
优选的是，经步骤c之后得到高强度不锈钢的回火组织，其微观组织仍以面积计由5％～20％的残余奥氏体，低于0.3％的Nb、Ti碳化物，以及低于0.5％的Cr的碳化物，其余为马氏体构成，残余奥氏体以板条或薄膜状存在，厚度小于300纳米。
根据本发明的成形构件宏观硬度在48HRC～55HRC之间，2mm深U型缺口标准试样冲击吸收功在30J～130J之间，韧性相对同等硬度不锈钢显著提高；在质量分数为3.5％NaCl溶液中点蚀电位达到270mV以上；屈服强度1100MPa～1300MPa，抗拉强度1600MPa～1900MPa，延伸率9.0％～15％。其强塑性优于现有的Cr13马氏体不锈钢产品，可用于医疗器械、弹簧、阀门及蒸汽环境通用工程部件等传统高强度不锈钢产品，同时本发明满足汽车碰撞安全结构件要求，可用于热冲压生产线，应用于汽车碰撞安全结构件。
采用本发明的技术方案，在生产成本上与传统Cr13马氏体不锈钢差异不大，但其强韧性、耐蚀性却显著提高。这是因为，本发明的热处理工艺与传统不锈钢的调质处理工艺相同，不用改变原不锈钢的生产线，但是组织调控与调质处理显著不同，显微组织主要由回火马氏体和亚稳定奥氏体组成，没有渗碳体析出，因此在强硬度较高的前提下，塑韧性显著提高。
附图说明
图1是根据本发明的试样3～7的显微组织照片，其中虚线为晶界线。
图2是根据本发明的试样3～7的电化学腐蚀极化曲线图。
具体实施方式
本发明的高强度不锈钢以重量含量计包括：0.2～0.35％的C、 0.7～3.50％的Mn、0.6～2.0％的Si、11.0～17.0％的Cr、小于等于0.20％的Nb、小于等于0.20％的Ti。其中，C含量优选为0.2～0.3％，Cr含量优选为12.0～14％，Nb含量优选小于等于0.10％，Ti含量优选小于等于0.10％。还可包括由以下元素组成的组中的一种或多种：2.0％以下的Mo；1.0％以下的W；1.0％以下的V；3.0％以下的Cu；4.0％以下的Ni；0.4％以下的Zr。余量为Fe和杂质。
下面对各化学成分的含量范围分别进行说明。
C：0.20～0.35％，优选为0.2～0.3％
在本发明钢材中，碳是最主要的强化元素，其通过固溶强化以及弥散析出强化的方式来提高强度。碳除了作为强化元素，同时也是奥氏体稳定元素。碳原子较小，扩散速率大，在低温回火过程中能够很快从碳过饱和的马氏体中扩散到残余奥氏体中，并在残余奥氏体中富集，增加了残余奥氏体的稳定性。当碳含量低于0.20％时，其强度较低；当碳含量高于0.35％时，碳化物完全固溶于基体的温度过高，原奥氏体晶粒粗大，并且韧性极差。为了综合良好的强度和韧性，将碳含量控制在0.20～0.35％。在这一范围中，碳元素能够满足稳定残余奥氏体的要求，增加材料的韧性。
Cr：11.0～17.0％，优选为12.0～14％
在本发明钢材中，铬主要的作用是提高耐蚀性，其能够与氧反应形成致密的钝化膜，抑制基体被进一步腐蚀。铬也是一种强碳化物形成元素，其极易与碳形成Cr 23C 6等碳化物并在晶界处析出，可以有效抑制晶粒的长大，同时也会导致晶界处铬含量降低，耐腐蚀能力下降。适当提高固溶处理温度可以使得铬碳化物完全固溶，耐晶间腐蚀能力上升，但另一方面会导致奥氏体晶粒异常粗大。由于本发明产品组织中的铬碳化物完全固溶于基体，17.0％铬含量已经满足耐蚀性要求，当铬含量过高时会导致铬碳化物完全固溶温度提高，并导致晶粒过大，因此，铬含量上限为17.0％。另一方面，当铬含量低于11.0％时，不能形成致密的钝化膜，耐蚀性急剧下降，因此，铬含量下限是11.0％。
Si：0.6～2.0％
硅是本发明钢材的重要元素。在本发明的钢材中，硅能够抑制低温回火过程中渗碳体的析出，促使碳以游离态扩散到残余奥氏体中。当硅含量低于0.6％时，不能有效抑制渗碳体的析出；另一方面，当硅 含量过高时，会够显著降低钢材的韧性和塑性。因此，硅含量控制在0.6～2.0％。
Mn：0.7～3.50％
锰是本发明钢材中的另一种重要元素。锰能够提高淬透性，同时锰还是奥氏体稳定元素，能够降低奥氏体转变为马氏体的开始温度(Ms)。在其它影响Ms点的合金成分确定的前提下，只能通过控制锰含量来调整Ms点，进而控制淬火到室温时的残余奥氏体含量。本发明的成形构件中含有以面积计5.0％～30.0％的残余奥氏体，其主要是淬火到室温时未转变的奥氏体。锰含量受限于碳、铬和硅的含量，为了得到室温下适量的残余奥氏体，将锰含量控制在0.7～3.50％。
Nb、Ti：≤0.20％，优选≤0.10％
铌、钛都是强碳化物形成元素，与铬碳化物相比，其碳化物固溶积小。本发明钢材中，高温固溶处理时，铬碳化物完全固溶，而铌、钛碳化物仍存在，抑制晶粒长大。当不存在铌、钛时，固溶处理时奥氏体晶粒长大不受抑制作用，晶粒粗大，强韧性降低。另一方面，当铌、钛含量过高时，凝固过程中容易析出较多大尺寸的铌、钛碳氧化物，影响材料韧性。因此，将铌、钛含量控制在0.20％以下。
Mo：2.0％以下；W：1.0％以下；V：1.0％以下；Zr：0.4％以下
钼、钨、钒和锆都是碳化物形成元素，能够细化晶粒并提高强度。在本发明钢材中，这些元素主要起到固溶强化以及析出强化作用，含量增加对于这些作用的提升并不明显。
Ni：4.0％以下
镍可以改善钢的加工性能并提高耐蚀性，同时镍也是一种奥氏体稳定元素。在本发明钢材中，过多的镍会影响残余奥氏体含量，并且增加不必要的成本。
Cu：3.0％以下
铜能够提高强度和耐蚀性，但是，铜含量超过3.0％时会导致加工性能劣化，并且增加不必要的成本。
必须说明的是，对于本发明的钢材而言，上述的钼、钨、钒、锆、镍和铜并不是必须的元素。
下述表1显示了根据本发明的一些钢材的成分，余量为铁和杂质，以下成分均按重量百分比计。
表1实施例材料化学成分(wt％)
试样 C Mn Si Cr Nb Ti
1 0.21 3.1 1.55 11.4 - -
2 0.30 2.1 1.55 11.7 - -
3 0.23 2.3 1.55 12.5 0.05 0.035
4 0.27 1.9 0.99 14.0 0.05 0.041
其中，“-”表示基本不含有该元素。
对表1中的1、2、3和4分别准备多个试样，并分别进行热处理。
具体而言，热处理工艺包括以下步骤：
a)进行固溶处理：加热至1000～1200℃，优选1000～1100℃，保温1～3600s；
b)冷却至100℃以下；
c)回火热处理：加热至150～400℃保温10～10000s然后以任意冷却方式冷却到室温。
各试样的热处理工艺参数以及热处理后的试样力学性能如表2、表3和表4所示，其中拉伸、冲击及三点弯试验的温度均为室温。
表2热处理工艺、组织及强韧性(冲击试样缺口2mm深U型缺口)
Figure PCTCN2019111884-appb-000001
Figure PCTCN2019111884-appb-000002
表3强塑性(拉伸试样标距50mm，厚度2mm)
试样 屈服强度/MPa 抗拉强度/MPa 延伸率/％
1-1 1100 1621 13.5
1-2 1109 1609 14.9
2-1 1356 1787 4.4(脆断)
2-2 1268 1626 4.1(脆断)
3-1 1250 1682 10.2
3-2 1258 1739 11.5
3-3 1357 1485 1.4(脆断)
3-4 1231 1869 9.6
3-5 1262 1834 9.9
3-6 1262 1825 11.0
3-7 1237 1740 10.3
3-8 1250 1744 11.0
3-9 1249 1700 9.1
3-10 1246 1696 9.4
4-1 1330 1450 1.1(脆断)
表4部分试样三点弯曲性能(试样厚度2.0mm)
试样 载荷力/kN 弯曲角/°
3-1 24.5 62.3
3-2 23.1 56.9
3-4 24.9 44.9
3-7 23.0 56.3
其中，“-”表示未进行该处理，“残奥量”表示以面积计的残余奥氏 体含量。
如图2的极化曲线所示，本发明钢材的点蚀电位达到了270mV。其中，所采用的电解质溶液为3.5％NaCl生理盐水，参考电极为KCl饱和甘汞电极，对电极为铂电极。
从以上说明可知，本发明的钢材经本发明的热处理方法后得到的成形构件兼具高硬度、高韧性与高耐晶间腐蚀能力，同时其生产成本并没有显著提高，具有较高的工业价值。
虽然已经参考优选实施例对本发明进行了描述，但在不脱离本发明的范围的情况下，可以对其进行各种改进。尤其是，只要不存在冲突，各个实施例中所提到的各项技术特征均可以任意方式组合起来。本发明并不局限于文中公开的特定实施例，而是包括落入权利要求的范围内的所有技术方案。

Claims (14)

  1. 一种高强度不锈钢，其特征在于，以重量含量计，所述高强度不锈钢包括0.2-0.35％的C、0.7-3.50％的Mn、0.6-2.0％的Si、11-17％的Cr、小于等于0.20％的Nb、小于等于0.20％的Ti，余量为Fe和杂质。
  2. 如权利要求1所述的高强度不锈钢，其特征在于，C含量为0.2-0.3％，Cr含量为12.0-14％，Nb含量小于等于0.10％，Ti含量小于等于0.10％。
  3. 如权利要求1或2所述的高强度不锈钢，其特征在于，以重量含量计，还包括由以下元素组成的组中的一种或多种：
    2.0％以下的Mo；
    1.0％以下的W；
    1.0％以下的V；
    3.0％以下的Cu；
    4.0％以下的Ni；
    0.4％以下的Zr。
  4. 一种高强度不锈钢的热处理工艺，其特征在于，所述热处理工艺包括以下步骤：
    步骤a：将权利要求1至3中任一项所述的高强度不锈钢加热至1000～1200℃后保温1～3600s；
    步骤b：将经过所述步骤a处理后的所述高强度不锈钢冷却至100℃以下；以及
    步骤c，将经过所述步骤b处理后的所述高强度不锈钢加热至150～400℃后保温10～10000s，然后以任意冷却方式冷却到室温。
  5. 如权利要求4所述的热处理工艺，其特征在于，在所述步骤a中，加热至1000～1100℃后保温60～3600s。
  6. 如权利要求4所述的热处理工艺，其特征在于，在所述步骤a中，以10℃/s以上的加热速率快速加热至1050～1200℃后保温1～600s。
  7. 如权利要求6所述的热处理工艺，其特征在于，在所述步骤a中，以20℃/s以上的加热速率快速加热至1050～1200℃后保温1～30s。
  8. 如权利要求4至6中任一项所述的热处理工艺，其特征在于， 在所述步骤a与所述步骤b之间，所述高强度不锈钢被热冲压成形为所需构件形状。
  9. 如权利要求4至6中任一项所述的热处理工艺，其特征在于，在所述步骤b中，以10℃/s以上的平均冷速冷却至室温。
  10. 一种成形构件，其特征在于，所述成形构件由权利要求1至3中任一项所述的高强度不锈钢制成，所述成形构件的微观组织以面积计由5％-30％的残余奥氏体，70％-95％的马氏体，低于1％的Nb、Ti碳化物，以及低于2％的Cr的碳化物构成。
  11. 如权利要求10所述的成形构件，其特征在于，微观组织以面积计由5％-20％的残余奥氏体，低于0.3％的Nb、Ti碳化物，以及低于0.5％的Cr的碳化物，其余为马氏体构成。
  12. 如权利要求10或11所述的成形构件，其特征在于，残余奥氏体以板条或薄膜状存在，平均厚度小于300纳米。
  13. 如权利要求10或11所述的成形构件，其特征在于，所述微观组织为回火组织。
  14. 如权利要求10或11所述的成形构件，其特征在于，所述成形构件由权利要求4所述的热处理工艺制成。
PCT/CN2019/111884 2018-11-14 2019-10-18 高强度不锈钢、热处理工艺及成形构件 WO2020098448A1 (zh)

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