CN112877612A - Preparation method of high-manganese TWIP steel - Google Patents
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- CN112877612A CN112877612A CN202110021142.6A CN202110021142A CN112877612A CN 112877612 A CN112877612 A CN 112877612A CN 202110021142 A CN202110021142 A CN 202110021142A CN 112877612 A CN112877612 A CN 112877612A
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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
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
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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
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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Abstract
The invention provides a preparation method of high-manganese TWIP steel, which is characterized in that a steel ingot obtained by smelting is forged and subjected to solution treatment, hot rolling, cold rolling, annealing and water cooling. The weight percentage of the chemical components is as follows: 20 to 25 percent of Mn, 0.4 to 1.2 percent of C, 8 to 15 percent of Ni, 0.1 to 0.5 percent of Si, 1 to 3 percent of Cr, less than or equal to 0.03 percent of P, less than or equal to 0.01 percent of S and the balance of Fe. The tensile strength of the steel reaches 893MPa in a hydrogen environment, the total elongation of the steel can reach 64%, the method can improve the strength and the hydrogen embrittlement resistance of the TWIP steel, and can provide good requirements for the TWIP steel in subsequent processing.
Description
Technical Field
The invention relates to a preparation method of high-manganese TWIP steel, belonging to the field of hydrogen embrittlement resistance manufacturing of steel materials.
Background
TWIP steel (twin crystal induced plasticity steel) has excellent properties such as good strength and ductility, and good delayed fracture resistance, and is widely used in the fields of automobiles, buildings, and the like. However, the TWIP steel with high Mn content has a series of related problems in the smelting and preparation processes, so the research on the problems exists, so that the performance can be improved, and the method has important significance for the manufacture and production of TWIP steel.
At present, the fields of aviation, automobiles, hydrogen energy sources and the like are in a period of high-speed development, but the fields can face the problem of hydrogen embrittlement when important parts are prepared in a hydrogen environment, particularly in a high-pressure hydrogen environment, so that the strength and the elongation of the important parts are reduced, and the problems of fatigue, premature fracture and the like caused by hydrogen occur. Some conventional methods, while reducing the hydrogen embrittlement to some extent, still face cost issues. TWIP steel is one of the industrial materials, and the Stacking Fault Energy (SFE) of the TWIP steel is 20-50mJ/m2The martensite phase transformation is inhibited, twin crystals are easy to form, dislocation slippage is hindered, and crack propagation is delayed. And the hydrogen embrittlement resistance of the alloy can be greatly improved after the alloy is optimized and improved, and the alloy is H2The environment preparation work also has high strength and ductility which are required in the field, and the cost is relatively reduced compared with 316 austenitic stainless steel and the like.
Aiming at the problems existing at present, the invention can effectively improve the hydrogen embrittlement resistance of the TWIP steel and simultaneously improve the hydrogen embrittlement resistance of the TWIP steel in H2The strength and the plasticity of the TWIP steel also meet the requirements under the environment, and the TWIP steel can meet the requirements under high pressure H2The preparation process under the environment and the practical application provide corresponding reference and selection.
Disclosure of Invention
The invention provides a preparation method of high-manganese TWIP steel, which is prepared by adopting a vacuum induction melting method, wherein raw Fe and Ni are firstly added during melting, Cr is added after deoxidation, and Mn is added 3-5 min before tapping. The obtained steel ingot is further subjected to forging, solution treatment, hot rolling, cold rolling, heat treatment and the like. So as to meet the performance requirements of high strength, high elongation and hydrogen embrittlement resistance.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the high-manganese TWIP steel is characterized in that the high-manganese TWIP steel comprises, by weight, 20% -25% of Mn, 0.4% -1.2% of C, 8% -15% of Ni, 0.1% -0.5% of Si, 1% -3% of Cr, less than or equal to 0.03% of P, less than or equal to 0.01% of S, and the balance Fe.
A preparation method of high-manganese TWIP steel comprises the following steps:
(1) adding the raw materials in sequence, smelting in a vacuum induction smelting furnace, introducing protective gas argon, smelting, and casting into steel ingots after smelting;
(2) forging the steel ingot obtained in the step (1) at 1000-1200 ℃, carrying out solution treatment at 900-1200 ℃, and keeping the temperature for 1-5 hours;
(3) carrying out hot rolling on the steel ingot obtained in the step (2), wherein the initial rolling temperature is 900-1200 ℃, the final rolling temperature is 800-1000 ℃, and then carrying out acid pickling;
(4) cold rolling the steel ingot obtained in the step (3) at the temperature of-20-80 ℃, and rolling for 3-8 times, wherein the cold rolling amount is 20% -50%, and the thickness of the steel ingot after rolling is 4-10 mm;
(5) and (4) annealing the steel ingot obtained in the step (4) under the protection of nitrogen, and annealing for 5-15 min at the annealing temperature of 600-1000 ℃, wherein the cooling rate is 20 ℃/s, and the steel ingot is cooled to room temperature.
Preferably, the flow rate of the protective gas argon introduced in the step (1) is 1-1.6L/min.
Preferably, the forging temperature in the step (2) is 1000-1100 ℃, the solution treatment temperature is 900-1100 ℃, and the temperature is kept for 1-3 h.
Preferably, the initial rolling temperature in the step (3) is 1000-1200 ℃, and the final rolling temperature is 800-900 ℃.
Preferably, the cold rolling temperature in the step (4) is-20-60 ℃, 5-8 times of rolling are carried out, the cold rolling amount is 20-40%, and the thickness of the rolled steel ingot is 4 mm.
Preferably, the annealing temperature in the step (5) is 600-900 ℃, and the annealing is carried out for 5-10 min.
Sample detection:
(1) the samples were mechanically abraded with #400- #2000 silicon carbide sandpaper, followed by polishing with a 1 μm diamond suspension, and finally with a slurry containing 90% CH3COOH and 10% HClO4The solution of (2) is subjected to electrochemical polishing. Further, the sample was corroded in a 5% nitric acid alcohol solution for 120 seconds, washed with absolute ethanol and dried with a blower, and then the metallographic structure thereof was observed with an optical microscope.
(2) Low strain rate tensile test (SSRT) was carried out on an Instron8801(100KN) testing machine for the examples and comparative examples, the strain rate of the tensile test being 5X 10-5s-1. Further, the experiment was started after the air pressure in the tank was stabilized.
(3) The vicinity of the crack at the stress intensity factor Δ K30 was characterized using Electron Back Scattering Diffraction (EBSD): at H2And N2The values of the average misorientation (KAM) of nuclei in the vicinity of cracks under the environment are always high, indicating that hydrogen can promote stress concentration and accelerate fatigue crack propagation. Hydrogen also promotes the formation of twin crystals to block the movement of dislocation, thereby improving the fatigue resistance of the material, so that the material is subjected to high temperature oxidation treatment2And is in N2The crack propagation gap under the environment is reduced.
The invention has the following advantages:
(1) the hydrogen embrittlement resistance of the TWIP steel is greatly improved after the process treatment, the strength of the TWIP steel can reach 893MPa in a hydrogen environment, the total elongation reaches 64%, the mechanical property of high strength and high plasticity is met, and the comprehensive performance of the TWIP steel is higher than that of the traditional steel material.
(2) The method has the advantages of simple process, easy operation, relatively low loss, capability of greatly reducing the generation of defects in the preparation process, capability of ensuring the quality of the obtained product, and wide application of the prepared parts in the high-pressure hydrogen environment.
Drawings
FIG. 1 is a metallographic picture of an example;
FIG. 2 shows an embodiment in H2SEM image of fracture morphology of stress intensity factor delta K30 under environment;
FIG. 3 shows the results of the examples and comparative examples at 5MPaN2And H2Stress-strain curve under environment;
FIG. 4 shows the measured values at 5MPaN2And H2Graph of crack propagation rate for the environmental examples and 316 stainless steel;
FIG. 5 is a graph at N2EBSD map of surface crack of stress intensity factor delta K30 under environment;
FIG. 6 is a graph at N2KAM graph of surface cracks of stress intensity factor delta K30 under environment;
FIG. 7 is a graph at H2EBSD map of surface crack of stress intensity factor delta K30 under environment;
FIG. 8 is a graph at H2KAM diagram of surface cracks of stress intensity factor delta K30 under environment.
Detailed Description
The invention is described in more detail below by way of examples:
the high-manganese TWIP steel comprises the following chemical components in percentage by weight: 20 to 25 percent of Mn, 0.4 to 1.2 percent of C, 8 to 15 percent of Ni, 0.1 to 0.5 percent of Si, 1 to 3 percent of Cr, less than or equal to 0.03 percent of P, less than or equal to 0.01 percent of S and the balance of Fe.
According to the invention, during vacuum induction smelting of the high-manganese TWIP steel, raw Fe and Ni are firstly added, Cr is added after deoxidation, and Mn is added 3-5 min before tapping.
Example (b):
the TWIP steel comprises the following chemical components in percentage by weight: 24% of Mn, 0.55% of C, 9% of Ni, 0.25% of Si, 1.2% of Cr, 0.02% of P, 0.01% of S and the balance of Fe. The method comprises the following specific steps:
(1) adding the raw materials in sequence, smelting in a vacuum induction smelting furnace, introducing protective gas with argon flow of 1.2L/min, and casting into steel ingots after smelting;
(2) forging the steel ingot obtained in the step (1) at 1050 ℃, carrying out solution treatment at 1100 ℃, and keeping the temperature for 1.5 h;
(3) carrying out hot rolling on the steel ingot obtained in the step (2), wherein the initial rolling temperature is 1050 ℃, the final rolling temperature is 850 ℃, and then carrying out acid pickling;
(4) cold rolling the steel ingot obtained in the step (3) at room temperature, wherein the cold rolling amount is 35%, and the thickness of the steel ingot after rolling is 4 mm;
(5) and (4) annealing the steel ingot obtained in the step (4) under the protection of nitrogen, annealing for 8min at the annealing temperature of 700 ℃, and cooling to room temperature at the cooling rate of 20 ℃/s.
Comparative example:
the TWIP steel of the comparative example comprises the following chemical components in percentage by weight: mn was 24%, C was 0.55%, P was 0.03%, S was 0.01%, and the balance was Fe, and Ni, Si, and Cr were not added to the chemical compositions of the examples. The comparative example was prepared in the same manner as in the examples, and the properties thereof were measured and processed in the same manner as in the examples.
Low strain rate tensile testing (SSRT) was conducted on an Instron8801 testing machine for examples and comparative examples to give 5MPaH2And N2The performance test results of the stress-strain curve of the TWIP steel sample under the environment are shown in tables 1 and 2.
TABLE 1 examples and comparative examples in N2Results of environmental Performance test
Experimental Material | Yield strength/MPa | Tensile strength/MPa | Total elongation/% |
Examples | 335 | 901 | 62.0 |
Comparative example | 307 | 811 | 53.5 |
TABLE 2 examples and comparative examples in H2Results of environmental Performance test
Experimental Material | Yield strength/MPa | Tensile strength/MPa | Total elongation/% |
Examples | 339 | 893 | 64.0 |
Comparative example | 294 | 767 | 51.5 |
In this example, the metallographic structure of the sample was observed by an optical microscope, and the metallographic structure analysis showed that: the grain size is not obviously influenced under the cold rolling at normal temperature, the grain size is kept at about 25 mu m, and twin crystals appear in partial grains. At H2The fracture morphology is observed by a Scanning Electron Microscope (SEM) under the environment, and the twin crystal can be found. Calculating the Stacking Fault Energy (SFE) based on an Olson-Cohen thermodynamic model to obtain the SFE of 36.72mJ/m2It is shown that the present embodiment suppresses the martensitic transformation, thereby promoting the twinning shapeAnd (4) obtaining.
In order to evaluate the hydrogen embrittlement resistance of the TWIP steel of the present invention, this example was also conducted in 5MPaH with 316 stainless steel2And N2The fatigue crack propagation rate in the environment is compared with the stress intensity factor delta K, and it can be seen that the steel has higher hydrogen embrittlement resistance compared with 316 stainless steel. In addition, compare at 5MPaH2And N2Has stronger fatigue crack propagation rate ratio (H) under hydrogen embrittlement effect stress intensity factor delta K30 under the environment2/N2) See table 3. Therefore, the TWIP steel can reduce hydrogen embrittlement sensitivity and has excellent hydrogen embrittlement resistance.
TABLE 3 in N2And H2Fatigue crack growth rate ratio at Δ K30 for the environmental 316 steel and the example TWIP steel
The test results show that the invention is effective, the hydrogen embrittlement resistance of the TWIP steel is improved, and the TWIP steel is H-shaped2Compared with a comparative example, the mechanical property is also improved under the environment, the total elongation reaches 64 percent, and the tensile strength reaches 893 MPa.
Claims (8)
1. The high-manganese TWIP steel is characterized by comprising, by weight, 20-25% of Mn, 0.4-1.2% of C, 8-15% of Ni, 0.1-0.5% of Si, 1-3% of Cr, less than or equal to 0.03% of P, less than or equal to 0.01% of S and the balance Fe.
2. The high-manganese TWIP steel according to claim 1, wherein raw Fe and Ni are added first during smelting, Cr is added after deoxidation, and Mn is added 3-5 min before tapping.
3. A method of producing a high manganese TWIP steel according to claims 1 to 2, characterized in that it comprises the following steps:
(1) adding the raw materials in sequence, smelting in a vacuum induction smelting furnace, introducing protective gas argon, smelting, and casting into steel ingots after smelting;
(2) forging the steel ingot obtained in the step (1) at 1000-1200 ℃, carrying out solution treatment at 900-1200 ℃, and keeping the temperature for 1-5 h;
(3) carrying out hot rolling on the steel ingot obtained in the step (2), wherein the initial rolling temperature is 900-1200 ℃, and the final rolling temperature is 800-1000 ℃, and then carrying out acid pickling;
(4) cold rolling the steel ingot obtained in the step (3) at-20-80 ℃, and rolling for 3-8 times, wherein the cold rolling amount is 20% -50%, and the thickness of the steel ingot after rolling is 4-10 mm;
(5) and (4) annealing the steel ingot obtained in the step (4) under the protection of nitrogen, and annealing for 5-15 min at the annealing temperature of 600-1000 ℃, wherein the cooling rate is 20 ℃/s, and the steel ingot is cooled to room temperature.
4. The preparation method of the high-manganese TWIP steel as claimed in claim 2, wherein the flow rate of argon gas introduced into the step (1) is 1-1.6L/min.
5. The preparation method of the high-manganese TWIP steel according to claim 2, wherein the forging temperature in the step (2) is 1000-1100 ℃, the solution treatment temperature is 900-1100 ℃, and the temperature is kept for 1-3 h.
6. The preparation method of the high-manganese TWIP steel according to claim 2, wherein the start rolling temperature in the step (3) is 1000-1200 ℃ and the finish rolling temperature is 800-900 ℃.
7. The preparation method of the high-manganese TWIP steel according to claim 2, wherein the cold rolling temperature in the step (4) is-20-60 ℃, 5-8 passes of rolling are performed, the cold rolling amount is 20-40%, and the thickness of the rolled steel ingot is 4 mm.
8. The method for preparing high-manganese TWIP steel according to claim 2, wherein the annealing temperature in the step (5) is 600-900 ℃ and the annealing time is 5-10 min.
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Citations (11)
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JPS6247428A (en) * | 1985-08-28 | 1987-03-02 | Nippon Kokan Kk <Nkk> | Manufacture of mn stainless steel having high strength and toughness at 4.2k |
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CN107574377A (en) * | 2017-09-07 | 2018-01-12 | 北京科技大学 | High manganese TWIP steel of a kind of high energy absorbing type based on nanostructured and preparation method thereof |
CN108866447A (en) * | 2017-07-14 | 2018-11-23 | 淮北益嘉益新材料科技有限公司 | A kind of high manganese TWIP steel and its manufacturing method |
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2021
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JPS6247428A (en) * | 1985-08-28 | 1987-03-02 | Nippon Kokan Kk <Nkk> | Manufacture of mn stainless steel having high strength and toughness at 4.2k |
JPS62238353A (en) * | 1986-04-09 | 1987-10-19 | Nippon Kokan Kk <Nkk> | High-manganese austenitic steel excellent in strength at high temperature |
JPS64254A (en) * | 1987-03-11 | 1989-01-05 | Nippon Steel Corp | High-hardness nonmagnetic stainless steel |
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