CN112410674A - Rare earth-containing copper-rich precipitated phase reinforced martensitic stainless steel and preparation method thereof - Google Patents
Rare earth-containing copper-rich precipitated phase reinforced martensitic stainless steel and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of alloys, and particularly relates to a rare earth-containing copper-rich precipitation phase strengthened martensitic stainless steel and a preparation method thereof. The martensite stainless steel containing the rare earth and copper-rich precipitated phase reinforcement provided by the invention comprises C, Si, Mn, Cr, Ni, Al, N, Nb, V, Mo, Cu, Ca, rare earth, Fe and inevitable impurities; the rare earth comprises La and/or Ce. According to the invention, the N element is added to replace part of the C element, so that the strength and the plasticity can be ensured, and the weakening degree of the corrosion resistance of the stainless steel is reduced to the greatest extent; the Cu-rich phase can generate precipitation strengthening effect on the martensitic stainless steel; the solid-solution rare earth atoms and Cu atoms attract each other at a close distance to form a rare earth and Cu atom cluster, so that nucleation of Cu-rich second-phase particles is promoted in the aging process. The embodiment shows that the martensite stainless steel reinforced by the rare earth-containing copper-rich precipitated phase has good mechanical property and plasticity.
Description
Technical Field
The invention belongs to the technical field of alloys, and particularly relates to a rare earth-containing copper-rich precipitation phase strengthened martensitic stainless steel and a preparation method thereof.
Background
Martensite (martentite) is a structural name for ferrous materials, and is a supersaturated solid solution of carbon in α -Fe; martensitic stainless steel is stainless steel whose mechanical properties can be adjusted by heat treatment, in general, it is a type of hardenable stainless steel. The martensitic stainless steel contains not less than 12 wt.% of Cr, and can obtain higher hardness, strength and wear resistance and simultaneously have certain corrosion resistance by adjusting the content of Cr and C and combining certain quenching and tempering heat treatment processes. Based on the characteristics of the material, the martensitic stainless steel is mainly applied to the fields of steam turbine blades, bearings, wear-resistant parts, cutters, medical instruments and the like.
In the production of martensitic stainless steels, the strength of the martensitic stainless steel is often increased by increasing the content of C element, but this method also impairs the workability of the martensitic stainless steel. In response to this phenomenon, the workability can be improved by low temperature tempering, however, the tempering process is accompanied by the precipitation and coarsening of Cr carbide in large quantities, resulting in a decrease in the Cr content in the alloy matrix, which in turn results in a decrease in the plasticity and corrosion resistance of the alloy. The prior martensitic stainless steel cannot give consideration to good mechanical property, plasticity and excellent corrosion resistance.
Disclosure of Invention
In view of the above, the present invention aims to provide a martensitic stainless steel reinforced by a rare earth-containing copper-rich precipitated phase, which has good mechanical properties, plasticity and excellent corrosion resistance.
In order to achieve the purpose of the invention, the invention provides the following technical scheme:
the invention provides a rare earth-containing copper-rich precipitated phase reinforced martensitic stainless steel, which comprises the following elements in percentage by mass:
0.015 to 0.095% of C, 0.1 to 1.3% of Si, 0.10 to 0.95% of Mn, 10.0 to 15.5% of Cr, 0.05 to 2.20% of Ni0.001 to 0.600% of Al, 0.05 to 0.16% of N, 0.001 to 0.120% of Nb, 0.01 to 0.13% of V, 0.10 to 0.55% of Mo, 1.1 to 2.6% of Cu, 0.0005 to 0.0050% of Ca, 0.005 to 0.080% of rare earth, and the balance of Fe and inevitable impurities;
the rare earth comprises La and/or Ce.
Preferably, when Cr is more than or equal to 12.25 wt.%, rare earth in the rare earth-containing copper-rich precipitated phase strengthened martensitic stainless steel is 0.010-0.080 wt.%, rare earth is La and Ce, and the mass ratio of the La to the Ce is (0.4-0.5): 1.
preferably, when the Ca is 0.002 to 0.005 wt.%, the rare earth content in the rare earth-containing copper-rich precipitation phase reinforced martensitic stainless steel is 0.005 to 0.03 wt.%.
Preferably, the mass percentage of N in the rare earth-containing copper-rich precipitation phase strengthened martensitic stainless steel is more than or equal to that of C; the sum of the mass percentages of N and C is more than or equal to the sum of the mass percentages of Nb and V.
Preferably, the structure of the rare earth-containing copper-rich precipitated phase reinforced martensitic stainless steel comprises more than or equal to 80 vol.% of martensite, and the balance is ferrite and/or retained austenite.
The invention also provides a preparation method of the rare earth-containing copper-rich precipitated phase strengthened martensitic stainless steel, which comprises the following steps:
smelting alloy raw materials and then casting to obtain a casting blank;
carrying out homogenization treatment, deformation treatment, heat preservation heat treatment and aging heat treatment on the casting blank in sequence to obtain the high-strength steel containing the rare earth;
the deformation treatment is hot rolling and curling which are sequentially carried out, or forging and annealing which are sequentially carried out.
Preferably, the temperature of the homogenization treatment is 1000-1250 ℃, and the time is 30-120 min.
Preferably, the open rolling temperature in the hot rolling is 1050-1220 ℃, and the finish rolling temperature is 900-920 ℃; in the hot rolling process, when the rolling temperature is from the initial rolling temperature to 975 ℃, the rolling pass is more than or equal to 3 times; when the rolling temperature is 975 ℃ to the final rolling temperature, the rolling pass is more than or equal to 2 times; the reduction rate of each pass in hot rolling is independently more than or equal to 11 percent; the curling temperature is 735-755 ℃;
preferably, the forging temperature in the forging is more than or equal to 1010 ℃, and the finish forging temperature is more than or equal to 910 ℃; the annealing temperature is 280-500 ℃, and the annealing time is 30-60 min.
Preferably, the temperature of the heat preservation heat treatment is 950-1100 ℃, and the time is 10-35 min;
the temperature of the aging heat treatment is 330-600 ℃, and the time is 10-2200 min.
The invention provides a rare earth-containing copper-rich precipitated phase reinforced martensitic stainless steel, which comprises the following elements in percentage by mass: 0.015 to 0.095% of C, 0.1 to 1.3% of Si, 0.10 to 0.95% of Mn, 10.0 to 15.5% of Cr10, 0.05 to 2.20% of Ni, 0.001 to 0.600% of Al, 0.05 to 0.16% of N, 0.001 to 0.120% of Nb0.001 to 0.120% of V, 0.01 to 0.13% of Mo, 1.1 to 2.6% of Cu, 0.0005 to 0.0050% of Ca0% of rare earth, 0.005 to 0.080% of rare earth, and the balance of Fe and inevitable impurities; the rare earth comprises La and/or Ce.
In the invention, the C element can stabilize austenite phase in a high-temperature region, thereby increasing the hardenability of the alloy and ensuring that a large amount of martensite structures are obtained after quenching; si element can be dissolved into Fe matrix lattice to obviously strengthen the alloy; the Mn element can stabilize an austenite phase in a high-temperature region, ensure that a large amount of martensite structures are obtained after quenching, and can play a solid solution strengthening effect on the alloy; cr element can ensure the corrosion resistance of the martensitic stainless steel; the Ni element can stabilize an austenite phase in a high-temperature region, ensure that a large amount of martensite structures are obtained after quenching, and can play a solid solution strengthening effect on the alloy, and meanwhile, the addition of the Ni element can reduce the ductile-brittle transition temperature of the martensitic stainless steel; al plays a role of a deoxidizer; the N element can stabilize the austenite phase in a high-temperature region, ensure that a large amount of martensite structures are obtained after quenching, improve the martensite strength through a solid solution strengthening mechanism, simultaneously, in the tempering process after quenching, the N element can be separated out to form nitride to play a role in precipitation strengthening, and particularly, the N element replaces part of C elements in the alloy, compared with the C element, the N element has weaker weakening degree on the alloy plasticity while increasing the strength of the martensitic stainless steel through solid solution strengthening, in addition, in the quenching, cooling and tempering and aging processes, the N element is easy to form nitride with Cr element, the nitride has better thermal stability and weaker coarsening tendency, can form a dispersion distribution form with small size in the tempering process, and the martensitic stainless steel can have excellent strength and plasticity by reasonably adding the N element to replace part of the C element, the weakening degree of the corrosion resistance of the alloy is reduced to the maximum extent; the Nb element can refine grains, improve strength and workability, and form fine carbides with C, thereby inhibiting the formation of coarse Cr carbides; the V element can improve the strength of the alloy and can be preferentially combined with C, N to form a fine precipitated phase, which is beneficial to inhibiting the formation of Cr carbonitride and avoiding the local occurrence of Cr-poor areas of the matrix to reduce the corrosion resistance of the alloy; the Mo element can improve the strength of the alloy through a solid solution strengthening mechanism, and can block the diffusion of Cu-rich particles of an alloy atomic phase after the Mo element is partially polymerized in a precipitated phase and a matrix interface region, so that the coarsening behavior of the precipitated phase is slowed down; in the process of tempering and aging after quenching, Cu exceeding the solid solubility of a matrix is continuously precipitated and separated out to form a large number of nano-scale second phase Cu-rich particles which are dispersedly distributed, the size of the crystal lattice of the Cu element is very close to that of the crystal lattice of the martensite matrix, the interface between the Cu element and the matrix is in a complete congruent relationship, and as the congruent degree between the precipitated phase and the matrix is high and the size of the precipitated phase is small, dislocation passes through the precipitated phase in a cutting mode during deformation of the alloy, and the interface stress field caused by the low degree of mismatch is low, the dislocation near the interface is effectively prevented from being highly enriched and further generating cracks, the martensitic stainless steel can be obviously strengthened, and the plasticity of the alloy is not influenced; the Ca element can spheroidize sulfides in the steel and improve the mechanical property of the martensitic stainless steel; the solid-solution rare earth atoms have higher migration rate under high potential concentration, the rare earth atoms and the Cu atoms have an attraction effect in a close distance, the formation of rare earth and Cu atom aggregation clusters in the component fluctuation process at a high temperature stage is promoted, the nucleation of Cu-rich second-phase particles in the tempering and aging process is promoted, the Cu-rich second-phase particles are preferentially separated out and can also serve as potential nucleation points for the separation of Cr nitrides, the regulation and control of the second-phase separation behavior in the maraging steel are facilitated, and the nitrides of Cr are refined.
The test result of the embodiment shows that the rare earth-containing copper-rich precipitation phase strengthened martensitic stainless steel has the tensile strength of 1396-1455 MPa, the yield strength of 1076-1165 MPa and the elongation of 22-24%.
Drawings
FIG. 1 is a TEM image of the rare earth-containing Cu-rich precipitated phase-strengthened martensitic stainless steel obtained in example 1.
Detailed Description
The invention provides a rare earth-containing copper-rich precipitated phase reinforced martensitic stainless steel, which comprises the following elements in percentage by mass:
0.015 to 0.095% of C, 0.1 to 1.3% of Si, 0.10 to 0.95% of Mn, 10.0 to 15.5% of Cr, 0.05 to 2.20% of Ni0.001 to 0.600% of Al, 0.05 to 0.16% of N, 0.001 to 0.120% of Nb, 0.01 to 0.13% of V, 0.10 to 0.55% of Mo, 1.1 to 2.6% of Cu, 0.0005 to 0.0050% of Ca, 0.005 to 0.080% of rare earth, and the balance of Fe and inevitable impurities;
the rare earth comprises La and/or Ce.
In the invention, the martensite stainless steel containing the rare earth and copper-rich precipitation phase reinforcement comprises 0.015-0.095% of C, preferably 0.02-0.06% of C, and more preferably 0.035-0.045% of C by mass percentage. In the present invention, the element C stabilizes the austenite phase in a high temperature region, increases the hardenability of the alloy, and ensures that a large amount of martensite structure is obtained after quenching.
In the invention, the martensite stainless steel containing the rare earth copper-rich precipitation phase strengthening comprises 0.1-1.3% of Si, preferably 0.35-1.15%, and more preferably 0.40-0.70% by mass percentage. In the present invention, Si element can significantly strengthen the alloy by being dissolved into the lattice of the Fe matrix.
In the invention, the martensite stainless steel containing the rare earth copper-rich precipitation phase strengthening comprises 0.10-0.95% of Mn, preferably 0.45-0.90%, and more preferably 0.65-0.85% by mass percentage. In the invention, Mn element can stabilize austenite phase in a high temperature region, ensure that a large amount of martensite structure is obtained after quenching, and can play a solid solution strengthening effect on the alloy.
In the invention, the martensite stainless steel containing the rare earth copper-rich precipitation phase strengthening comprises 10.0-15.5% of Cr, preferably 11.0-15.0%, and more preferably 11.5-14.5% by mass. In the present invention, the Cr element can ensure the corrosion resistance of the martensitic stainless steel.
In the invention, the martensite stainless steel containing the rare earth and copper-rich precipitation phase strengthening comprises 0.05-2.20% of Ni, preferably 0.08-2.10%, and more preferably 0.1-2.0% by mass. In the invention, the Ni element can stabilize austenite phase in a high-temperature region, ensure that a large amount of martensite structures are obtained after quenching, and can play a solid solution strengthening effect on the alloy. Meanwhile, the addition of the Ni element can reduce the ductile-brittle transition temperature of the martensitic stainless steel.
In the invention, the martensite stainless steel containing the rare earth copper-rich precipitation phase strengthening comprises 0.001-0.600% of Al, preferably 0.05-0.55%, and more preferably 0.10-0.30% by mass. In the present invention, Al functions as a deoxidizer.
In the invention, the martensite stainless steel containing the rare earth and copper-rich precipitation phase strengthening comprises 0.05-0.16% of N, preferably 0.06-0.13%, and more preferably 0.07-0.10% by mass. In the invention, the N element can stabilize the austenite phase in a high-temperature region, ensure that a large amount of martensite structures are obtained after quenching, and improve the martensite strength through a solid solution strengthening mechanism; meanwhile, in the tempering process after quenching, N element can be separated out to be nitride, and the precipitation strengthening effect is achieved. According to the invention, partial C element in the alloy is replaced by N element, and compared with C element, the N element has weaker weakening degree on the plasticity of the alloy while increasing the strength of the martensitic stainless steel through solid solution strengthening; in the quenching, cooling and tempering and aging processes, the N element and the Cr element are easy to form nitrides, the nitrides have good thermal stability and weaker coarsening tendency, and can form a dispersion distribution form with small size in the tempering process.
In the invention, the mass percentage of N in the rare earth-containing copper-rich precipitation phase strengthened martensitic stainless steel is preferably not less than that of C.
In the invention, the martensite stainless steel containing the rare earth copper-rich precipitated phase reinforcement comprises 0.001-0.120% of Nb, preferably 0.010-0.100%, and more preferably 0.025-0.075% by mass percentage. In the present invention, the Nb element can refine grains, improve strength and workability, and form fine carbides with C, thereby suppressing the formation of coarse carbides of Cr.
In the invention, the martensite stainless steel containing the rare earth and copper-rich precipitation phase strengthening comprises 0.01-0.13% of V, preferably 0.02-0.12% of V, and more preferably 0.03-0.10% of V. In the invention, the V element can improve the strength of the alloy and can be preferentially combined with C, N to form a fine precipitated phase, thereby being beneficial to inhibiting the formation of Cr carbonitride and avoiding the local occurrence of Cr-poor areas of the matrix so as to reduce the corrosion resistance of the alloy.
In the invention, the sum of the mass percentages of N and C in the rare earth-containing copper-rich precipitation phase reinforced martensitic stainless steel is preferably more than or equal to the sum of the mass percentages of Nb and V.
In the invention, the martensite stainless steel containing the rare earth and copper-rich precipitation phase strengthening comprises 0.10-0.55% of Mo, preferably 0.15-0.50%, and more preferably 0.18-0.25% by mass. In the present invention, Mo element can improve the strength of the alloy by a solid solution strengthening mechanism. Meanwhile, after the Mo element is subjected to segregation in the precipitated phase and matrix interface region, the diffusion of Cu-rich particles in the alloy atomic phase can be hindered, so that the coarsening behavior of the precipitated phase is slowed down.
In the invention, the martensite stainless steel containing the rare earth and copper-rich precipitated phase reinforcement comprises 1.1-2.6% of Cu, preferably 1.3-2.2%, and more preferably 1.6-2.0% by mass. In the invention, Cu element is precipitated and separated out continuously in the tempering process after quenching to form a coherent precipitated phase with a nano scale; specifically, in the invention, Cu exceeding the solid solubility of the matrix is continuously precipitated and separated out in the aging heat process after quenching, a large number of nano-scale second phase Cu-rich particles which are dispersed and distributed are formed, the lattice size of the Cu-rich particles is very close to that of the martensite matrix, and the interface between the Cu-rich particles and the martensite matrix is in a complete coherent relationship. Because the coherence between the precipitated phase and the matrix is high and the size of the precipitated phase is small, dislocation passes through the precipitated phase in a cutting mode when the alloy is deformed, and an interface stress field caused by the low mismatching degree is low, so that the dislocation near the interface is effectively prevented from being highly enriched and further generating cracks, the high-density nanoscale Cu-rich phase can generate a remarkable precipitation strengthening effect on the martensitic stainless steel, and the elongation of the alloy cannot be adversely affected.
In the present invention, the rare earth-containing copper-rich precipitate-phase-strengthened martensitic stainless steel includes, by mass%, 0.0005 to 0.0050% of Ca, preferably 0.0008 to 0.004%, and more preferably 0.001 to 0.002%. In the invention, Ca element can spheroidize sulfide in steel and improve the mechanical property of the martensitic stainless steel.
In the invention, the rare earth-containing copper-rich precipitation phase strengthened martensitic stainless steel comprises 0.005-0.080% of rare earth, preferably 0.01-0.07%, and more preferably 0.015-0.05% by mass. In the invention, the rare earth is La and/or Ce. In the invention, the attraction effect of the rare earth atoms and the Cu atoms in a close range promotes the formation of rare earth and Cu atom aggregation clusters in the component fluctuation process at a high temperature stage, promotes the nucleation of Cu-rich second-phase particles in the tempering and aging process, and the preferential precipitation of the Cu-rich second-phase particles can also serve as potential nucleation points of Cr nitride precipitation, thereby being beneficial to regulating and controlling the second-phase precipitation behavior in the maraging steel and refining the Cr nitride.
In the invention, the martensite stainless steel strengthened by the rare earth-containing copper-rich precipitation phase comprises the balance of Fe and inevitable impurities in percentage by mass. In the present invention, the impurities preferably include S and/or P. In the invention, the content of the impurity P in the rare earth-containing copper-rich precipitated phase strengthened martensitic stainless steel is preferably less than or equal to 0.02 percent by mass; the impurity S is preferably less than or equal to 0.03%. The invention strictly controls harmful impurity elements to prevent the impurity elements from generating adverse effects on the microstructure of the rare earth-containing high-strength steel.
In the invention, when Cr is more than or equal to 12.25 wt.%, the rare earth in the rare earth-containing copper-rich precipitation phase strengthened martensitic stainless steel is preferably 0.010-0.080 wt.%, and more preferably 0.020-0.070%; the rare earth is La and Ce, and the mass ratio of the La to the Ce is preferably (0.4-0.5): 1, more preferably (0.42 to 0.48): 1. in the invention, the rare earth element can promote the formation of the dispersed VC and CrN precipitated phases while promoting the formation of the anti-corrosion layer through the cooperation with Cr and N, C, and is beneficial to reducing the formation of local Cr-poor areas.
In the invention, when the Ca content is 0.002-0.005 wt.%, the rare earth content in the rare earth-containing copper-rich precipitation phase reinforced martensitic stainless steel is preferably 0.005-0.03 wt.%, and more preferably 0.01-0.025%; the rare earth comprises La and/or Ce. In the invention, through reasonable content configuration of Ca and rare earth elements, the formation of dispersed and fine Ca and rare earth-containing sulfide is promoted, thereby not only being beneficial to refining as-cast structure, but also being beneficial to improving the cutting performance of steel.
In the invention, the structure of the rare earth-containing copper-rich precipitated phase reinforced martensitic stainless steel preferably comprises more than or equal to 80 vol.% of martensite, and the balance of ferrite and/or retained austenite. In the invention, the structure of the rare earth-containing copper-rich precipitated phase reinforced martensitic stainless steel preferably comprises martensite at least 80 Vol.%, and more preferably 80-92 Vol.%; the residual austenite is preferably 3-7 vol.%, more preferably 5 vol.%; the balance being ferrite.
In the invention, the corrosion resistance of the martensitic stainless steel can be improved by increasing the Cr content, the low-temperature impact toughness of the steel can be reduced, and the impact toughness of the martensitic stainless steel can be improved by adding more rare earth elements; meanwhile, due to the difference of La valence electronic structures and Ce valence electronic structures, the La valence electronic structures and the Ce valence electronic structures can promote the formation of the Cr-containing anti-corrosion layer, and the mass content ratio of the La to the Ce is controlled within the range of 0.4-0.5, so that the formation of VC and CrN second-phase particles which are fine in size and distributed in a dispersion mode is facilitated.
The invention also provides a preparation method of the rare earth-containing copper-rich precipitated phase strengthened martensitic stainless steel, which comprises the following steps:
smelting alloy raw materials and then casting to obtain a casting blank;
carrying out homogenization treatment, deformation treatment, heat preservation heat treatment and aging heat treatment on the casting blank in sequence to obtain the high-strength steel containing the rare earth;
the deformation treatment is hot rolling and curling which are sequentially carried out, or forging and annealing which are sequentially carried out.
The invention obtains a casting blank by casting after smelting alloy raw materials.
In the invention, the alloy raw materials are subject to the element composition and proportion of the rare earth-containing high-strength steel. In the invention, the purity of the alloy raw material is preferably more than or equal to 99.99%. In the present invention, the source of the alloy raw material is not particularly limited, and commercially available alloy raw materials known to those skilled in the art may be used.
In the present invention, the melting facility is preferably a vacuum furnace. In the invention, the smelting temperature is preferably 1570-1690 ℃, and more preferably 1600-1650 ℃; the time is preferably 10 to 35min, and more preferably 12 to 20 min. In the invention, the vacuum degree of the smelting is preferably 0.1-0.2 Pa.
The casting is not particularly limited in the present invention, and casting known to those skilled in the art may be employed. The size of the casting slab is not particularly limited in the present invention, and in the embodiment of the present invention, the size of the casting slab may be 300mm × 250mm × 120 mm.
After a casting blank is obtained, the casting blank is subjected to homogenization treatment in sequence to obtain a homogenized slab.
In the invention, the temperature of the homogenization treatment is preferably 1000-1250 ℃, and more preferably 1050-1200 ℃; the time is preferably 30 to 120min, and more preferably 50 to 100 min. The temperature of the present invention is preferably raised from room temperature to the homogenization treatment temperature. In the present invention, the rate of temperature rise to the homogenization treatment temperature is preferably not less than 5 ℃/min, and more preferably 5 to 8 ℃/min.
After the homogenized plate blank is obtained, the homogenized plate blank is subjected to deformation treatment to obtain a curled blank or an annealed blank.
In the present invention, the deformation treatment is hot rolling and curling which are sequentially performed, or forging and annealing which are sequentially performed. In the present invention, when the deformation treatment is hot rolling and curling which are sequentially performed, a curled blank is obtained; and when the deformation treatment is forging and annealing treatment which are sequentially carried out, an annealed blank is obtained. In the invention, the hot rolling temperature is preferably 1050-1220 ℃, more preferably 10550-1200 ℃; the finishing temperature is preferably 900-920 ℃, and more preferably 905-915 ℃. In the invention, in the hot rolling process, when the rolling temperature is from the initial rolling temperature to 975 ℃, the rolling pass is preferably more than or equal to 3 times, and more preferably 3-6 times; when the rolling temperature is 975 ℃ to the final rolling temperature, the rolling pass is preferably more than or equal to 2 times, and more preferably 2-6 times. In the invention, the reduction rate of each pass in the hot rolling is preferably equal to or more than 11%, more preferably 11-35%, and still more preferably 15-34% independently. In the invention, the curling temperature is preferably 735-755 ℃, and more preferably 740-750 ℃. In the invention, when the curling is finished, the temperature of the obtained coiled plate is preferably not less than 630 ℃, more preferably 630-685 ℃, and more preferably 635-680 ℃. The invention preferably carries on laminar flow cooling to the hot rolled plate obtained by hot rolling to the curling temperature; the laminar cooling is not particularly limited in the present invention, and may be laminar cooling known to those skilled in the art.
After the curling, the invention preferably further comprises the step of sequentially carrying out primary annealing, surface scale removal and cold rolling on the curled material obtained by curling to obtain a curled blank. In the invention, the temperature of the primary annealing is preferably 930-990 ℃, and more preferably 940-980 ℃; the time is preferably 20 to 45min, and more preferably 25 to 40 min. The invention achieves the temperature of primary annealing by raising the temperature; the heating rate is preferably 20-25 ℃/s, and more preferably 21-24 ℃/s. The present invention is not particularly limited to the removal of the surface scale, and the technical means for removing the surface scale, which are well known to those skilled in the art, such as acid pickling, may be used. In the invention, the temperature of the cold rolling is preferably 18-40 ℃, and more preferably 20-30 ℃. In the invention, the reduction rate of each pass in the cold rolling is preferably less than or equal to 38%, and more preferably 25-38%. In the embodiment of the invention, the number of cold rolling passes is 2; the total deformation was 60%.
In the invention, the forging temperature in the forging is preferably not less than 1010 ℃, and more preferably 1010-1050 ℃; the finish forging temperature is preferably not less than 910 ℃, and more preferably 910-980 ℃. In the present invention, the total deformation rate of the forging is preferably not less than 40%, more preferably 40 to 60%. In the invention, the annealing treatment temperature is preferably 280-500 ℃, and more preferably 300-480 ℃; the time is preferably 30 to 60min, and more preferably 35 to 55 min. Preferably, the forged plate obtained after forging is air-cooled to the annealing temperature; the air cooling is not particularly limited in the present invention, and air cooling known to those skilled in the art may be employed. The annealing plate obtained after annealing is preferably cooled to room temperature by air; the air cooling is not particularly limited in the present invention, and air cooling known to those skilled in the art may be employed.
After obtaining the coiled blank or the annealing blank, the invention sequentially carries out heat preservation heat treatment and aging heat treatment on the coiled blank or the annealing blank to obtain the rare earth-containing high-strength steel.
In the invention, the temperature of the heat preservation heat treatment is preferably 950-1100 ℃, and more preferably 1000-1050 ℃; the time is preferably 10 to 35min, and more preferably 15 to 30 min. According to the invention, the temperature of the coiling blank or the annealing blank is preferably raised to the temperature of the heat preservation heat treatment; in the invention, the temperature rise rate is preferably not less than 20 ℃/s, and more preferably 20-35 ℃/s.
After the heat preservation heat treatment, the plate obtained by the heat preservation heat treatment is preferably rapidly cooled; the rapid cooling method is preferably water quenching or oil quenching. In the present invention, the cooling rate of the rapid cooling is preferably not less than 1.2 ℃/s, more preferably not less than 5 ℃/s. The invention preferably cools the plate obtained by heat preservation and heat treatment to room temperature quickly.
In the invention, the temperature of the aging heat treatment is preferably 330-600 ℃, more preferably 350-550 ℃; the time is preferably 10 to 2200min, and more preferably 20 to 72 min.
In the present invention, the temperature of the aging heat treatment is preferably obtained by raising the temperature; the heating rate is preferably more than or equal to 35 ℃/s, more preferably 35-60 ℃/s, and further preferably 40-60 ℃/s.
After the aging heat treatment, the aging heat treatment plate obtained by the failure heat treatment is preferably cooled to room temperature in air to obtain the rare earth-containing copper-rich precipitation phase strengthened martensitic stainless steel.
In order to further illustrate the present invention, the following will describe the rare earth-containing copper-rich precipitated phase strengthened martensitic stainless steel and the preparation method thereof in detail with reference to the examples, but they should not be construed as limiting the scope of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
By mass percentage, the martensitic stainless steel containing the rare earth copper-rich precipitation phase strengthening material is designed to have the components of 0.035% of C, 0.32% of Si, 0.92% of Mn, 11.9% of Cr, 0.22% of Ni, 0.06% of Al, 0.088% of N, 0.05% of Nb, 0.09% of V, 0.25% of Mo, 1.96% of Cu, 0.0012% of Ca, 0.016% of La, 0.009% of Ce0.011% of S, 0.008% of P and the balance of Fe;
according to the designed composition of the martensite stainless steel element reinforced by the rare earth-containing copper-rich precipitated phase, the alloy raw material is placed in a vacuum smelting furnace, smelted under the vacuum degree of 0.1Pa and the temperature of 1650 ℃ and then cast to obtain a casting blank with the size of 300mm multiplied by 250mm multiplied by 120 mm;
heating the casting blank to 1250 ℃ at the heating rate of 6 ℃/min, preserving heat for 45min at 1250 ℃, cooling to 1100 ℃ for hot rolling, wherein in the process of gradually reducing the hot rolling temperature, rolling for 6 times at the beginning temperature of 975 ℃ and rolling for 4 times at the end temperature of 975 ℃ to obtain a hot rolled blank with the thickness of 7mm, wherein the reduction rate of each time is 30%, and the end rolling temperature is 910 ℃; cooling the hot-rolled blank to 752 ℃ in air for curling; and (3) heating the obtained coil blank to 1010 ℃ at the speed of 20 ℃/s, preserving heat for 30min, performing water quenching, heating the plate blank obtained by water quenching to 490 ℃ at the speed of 40 ℃/s, preserving heat at 490 ℃ for 60min, performing aging heat treatment, and finally cooling in air to room temperature to obtain the rare earth-containing copper-rich precipitation phase strengthened martensitic stainless steel.
The martensitic stainless steel containing the rare earth-rich copper precipitated phase strengthened in example 1 was subjected to transmission electron microscopy and the TEM image obtained is shown in FIG. 1. As can be seen from fig. 1, the martensitic stainless steel strengthened by the rare earth-containing copper-rich precipitated phase provided by the invention contains dispersed black particles, and the black particles are a second phase precipitated.
Example 2
By mass percentage, the elements of the martensite stainless steel with the strengthened rare earth-rich copper precipitation phase comprise 0.048% of C, 0.53% of Si, 0.78% of Mn, 13.1% of Cr, 0.26% of Ni, 0.12% of Al, 0.095% of N, 0.07% of Nb, 0.09% of V, 0.18% of Mo, 1.85% of Cu, 0.0008% of Ca, 0.008% of La, 0.015% of Ce0.015%, 0.015% of S, 0.007% of P and the balance of Fe;
according to the designed composition of the martensite stainless steel element reinforced by the rare earth-containing copper-rich precipitated phase, the alloy raw material is placed in a vacuum smelting furnace, smelted under the vacuum degree of 0.1Pa and the temperature of 1635 ℃, and then cast to obtain a casting blank with the size of 300mm multiplied by 250mm multiplied by 120 mm;
heating the casting blank to 1250 ℃ at the heating rate of 6 ℃/min, preserving heat for 45min at 1250 ℃, cooling to 1100 ℃ for hot rolling, wherein in the process of gradually reducing the hot rolling temperature, rolling for 6 times at the beginning temperature of 975 ℃ and rolling for 4 times at the end temperature of 975 ℃ to obtain a hot rolled blank with the thickness of 7mm, wherein the reduction rate of each time is 30%, and the end rolling temperature is 910 ℃; cooling the hot-rolled blank to 743 ℃ in air and curling; and (3) heating the obtained coil blank to 1010 ℃ at the speed of 20 ℃/s, preserving heat for 30min, performing water quenching, heating the plate blank obtained by water quenching to 490 ℃ at the speed of 40 ℃/s, preserving heat at 490 ℃ for 60min, performing aging heat treatment, and finally cooling in air to room temperature to obtain the rare earth-containing copper-rich precipitation phase strengthened martensitic stainless steel.
Example 3
By mass percentage, the elements of the martensite stainless steel with the strengthened rare earth-rich copper precipitation phase comprise 0.048% of C, 0.53% of Si, 0.78% of Mn, 13.1% of Cr, 0.26% of Ni, 0.12% of Al, 0.095% of N, 0.07% of Nb, 0.09% of V, 0.18% of Mo, 1.85% of Cu, 0.0008% of Ca, 0.008% of La, 0.015% of Ce0.015%, 0.015% of S, 0.007% of P and the balance of Fe;
according to the designed composition of the martensite stainless steel element reinforced by the rare earth-containing copper-rich precipitated phase, the alloy raw material is placed in a vacuum smelting furnace, smelted under the vacuum degree of 0.1Pa and the temperature of 1635 ℃, and then cast to obtain a casting blank with the size of 300mm multiplied by 250mm multiplied by 120 mm;
heating the casting blank to 1250 ℃ at the heating rate of 6 ℃/min, preserving heat for 45min at 1250 ℃, cooling to 1100 ℃ for hot rolling, wherein in the process of gradually reducing the hot rolling temperature, rolling for 6 times at the beginning temperature of 975 ℃ and rolling for 4 times at the end temperature of 975 ℃ to obtain a hot rolled blank with the thickness of 7mm, wherein the reduction rate of each time is 30%, and the end rolling temperature is 910 ℃; cooling the hot-rolled blank to 752 ℃ in air for curling; heating the obtained coil blank to 965 ℃ at the speed of 22 ℃/s, keeping the temperature for 40min at the temperature, annealing, removing surface oxide skin by acid cleaning, and carrying out cold rolling at room temperature, wherein the number of cold rolling passes is 2, the total deformation is 60%, and thus a cold rolled blank is obtained; and (3) heating the obtained cold rolled blank to 1010 ℃ at the speed of 22 ℃/s, preserving heat for 30min, performing water quenching, heating the plate blank obtained by water quenching to 490 ℃ at the speed of 40 ℃/s, preserving heat at 490 ℃ for 60min, performing aging heat treatment, and finally performing air cooling to room temperature to obtain the rare earth-containing copper-rich precipitation phase strengthened martensitic stainless steel.
Example 4
By mass percentage, the elements of the martensite stainless steel with the strengthened rare earth-rich copper precipitation phase comprise 0.048% of C, 0.53% of Si, 0.78% of Mn, 13.1% of Cr, 0.26% of Ni, 0.12% of Al, 0.095% of N, 0.07% of Nb, 0.09% of V, 0.18% of Mo, 1.85% of Cu, 0.0008% of Ca, 0.008% of La, 0.015% of Ce0.015%, 0.015% of S, 0.007% of P and the balance of Fe;
according to the designed composition of the martensite stainless steel element reinforced by the rare earth-containing copper-rich precipitated phase, the alloy raw material is placed in a vacuum smelting furnace, smelted under the vacuum degree of 0.1Pa and the temperature of 1635 ℃, and then cast to obtain a casting blank with the size of 300mm multiplied by 250mm multiplied by 120 mm;
heating the casting blank to 1250 ℃ at the heating rate of 6 ℃/min, preserving heat for 45min, cooling to 1030 ℃, and starting forging to obtain a forging blank with the thickness of 20mm (the final forging temperature is 930 ℃); keeping the temperature of the forging blank at 435 ℃ for 40min for annealing; and (3) heating the obtained annealing blank to 1010 ℃ at the speed of 30 ℃/s, preserving heat for 30min, performing water quenching, heating the plate blank obtained by water quenching to 490 ℃ at the speed of 35 ℃/s, preserving heat at 490 ℃ for 60min, performing aging heat treatment, and finally performing air cooling to room temperature to obtain the rare earth-containing copper-rich precipitation phase strengthened martensitic stainless steel.
According to GB/T228.1-2010 part 1 of the tensile test of metallic materials: room temperature test method, the room temperature tensile test was performed on the rare earth-containing copper-rich precipitated phase-strengthened martensitic stainless steel obtained in examples 1 to 4, and the test results are shown in table 1.
TABLE 1 test results of tensile properties of martensitic stainless steels containing Cu-rich precipitated phases reinforced by rare earth elements obtained in examples 1 to 4
| Tensile strength/MPa | Yield strength/MPa | Elongation/percent | |
| Example 1 | 1396 | 1076 | 24 |
| Example 2 | 1455 | 1165 | 22 |
| Example 3 | 1422 | 1096 | 20 |
| Example 4 | 1479 | 1192 | 23 |
As can be seen from Table 1, the rare earth-containing copper-rich precipitated phase strengthened martensitic stainless steel provided by the invention has high tensile strength and yield strength and higher mechanical properties; high elongation and excellent plasticity. In addition, the martensite stainless steel containing the rare earth and rich in copper precipitation phase has high Cr content and excellent corrosion resistance.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The martensite stainless steel reinforced by the rare earth-containing copper-rich precipitated phase is characterized by comprising the following elements in percentage by mass:
0.015 to 0.095% of C, 0.1 to 1.3% of Si, 0.10 to 0.95% of Mn, 10.0 to 15.5% of Cr, 0.05 to 2.20% of Ni, 0.001 to 0.600% of Al, 0.05 to 0.16% of N, 0.001 to 0.120% of Nb, 0.01 to 0.13% of V, 0.10 to 0.55% of Mo, 1.1 to 2.6% of Cu, 0.0005 to 0.0050% of Ca, 0.005 to 0.080% of rare earth, and the balance of Fe and inevitable impurities;
the rare earth comprises La and/or Ce.
2. The martensitic stainless steel reinforced by the rare earth-containing copper-rich precipitated phase as claimed in claim 1 is characterized in that when Cr is more than or equal to 12.25 wt.%, rare earth in the martensitic stainless steel reinforced by the rare earth-containing copper-rich precipitated phase is 0.010-0.080 wt.%, rare earth is La and Ce, and the mass ratio of the La to the Ce is (0.4-0.5): 1.
3. the martensitic stainless steel reinforced by a rare earth-containing copper-rich precipitate phase according to claim 1, wherein when Ca is 0.002 to 0.005 wt.%, rare earth in the martensitic stainless steel reinforced by a rare earth-containing copper-rich precipitate phase is 0.005 to 0.03 wt.%.
4. The martensitic stainless steel reinforced by the rare earth-containing copper-rich precipitated phase as claimed in claim 1, wherein the mass percentage of N in the martensitic stainless steel reinforced by the rare earth-containing copper-rich precipitated phase is not less than that of C; the sum of the mass percentages of N and C is more than or equal to the sum of the mass percentages of Nb and V.
5. The martensitic stainless steel reinforced with a rare earth-rich copper precipitate phase as claimed in claim 1 wherein the structure of the martensitic stainless steel reinforced with a rare earth-rich copper precipitate phase comprises martensite at least equal to 80 vol.%, the balance being ferrite and/or retained austenite.
6. A method for preparing a martensitic stainless steel reinforced with a rare earth-containing copper-rich precipitate phase as claimed in any one of claims 1 to 5, characterized by comprising the steps of:
smelting alloy raw materials and then casting to obtain a casting blank;
carrying out homogenization treatment, deformation treatment, heat preservation heat treatment and aging heat treatment on the casting blank in sequence to obtain the high-strength steel containing the rare earth;
the deformation treatment is hot rolling and curling which are sequentially carried out, or forging and annealing which are sequentially carried out.
7. The method according to claim 6, wherein the homogenization treatment is carried out at a temperature of 1000 to 1250 ℃ for 30 to 120 min.
8. The production method according to claim 6, wherein the hot rolling is performed at a start rolling temperature of 1050 to 1220 ℃ and a finish rolling temperature of 900 to 920 ℃; in the hot rolling process, when the rolling temperature is from the initial rolling temperature to 975 ℃, the rolling pass is more than or equal to 3 times; when the rolling temperature is 975 ℃ to the final rolling temperature, the rolling pass is more than or equal to 2 times; the reduction rate of each pass in hot rolling is independently more than or equal to 11 percent; the curling temperature is 735-755 ℃.
9. The preparation method according to claim 6, wherein the forging temperature in the forging is not less than 1010 ℃, and the finish forging temperature is not less than 910 ℃; the annealing temperature is 280-500 ℃, and the annealing time is 30-60 min.
10. The preparation method according to claim 6, wherein the temperature of the heat-preservation heat treatment is 950 to 1100 ℃ for 10 to 35 min;
the temperature of the aging heat treatment is 330-600 ℃, and the time is 10-2200 min.
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| CN113174544A (en) * | 2021-04-21 | 2021-07-27 | 中国科学院金属研究所 | Superplastic forming nanocrystalline antibacterial martensitic stainless steel and preparation method thereof |
| CN113278892A (en) * | 2021-05-25 | 2021-08-20 | 东莞市亿丰钟表有限公司 | High-chromium high-hardness corrosion-resistant alloy steel and preparation method thereof |
| WO2024082324A1 (en) * | 2022-10-19 | 2024-04-25 | 鞍钢集团北京研究院有限公司 | High-strength and high-toughness maraging stainless steel for ultralow-temperature engineering and manufacturing method therefor |
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| CN107532259A (en) * | 2015-04-21 | 2018-01-02 | 杰富意钢铁株式会社 | Martensitic stain less steel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113174544A (en) * | 2021-04-21 | 2021-07-27 | 中国科学院金属研究所 | Superplastic forming nanocrystalline antibacterial martensitic stainless steel and preparation method thereof |
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| WO2024082324A1 (en) * | 2022-10-19 | 2024-04-25 | 鞍钢集团北京研究院有限公司 | High-strength and high-toughness maraging stainless steel for ultralow-temperature engineering and manufacturing method therefor |
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