CN115287542A - High-strength low-magnetic steel with uniform nano twin crystal distribution and preparation method thereof - Google Patents
High-strength low-magnetic steel with uniform nano twin crystal distribution and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- 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
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
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- 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
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- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
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Abstract
The invention discloses a high-strength low-magnetic steel with uniform nano twin crystal distribution and a preparation method thereof, and is characterized in that the proportion of the total length of an annealing twin crystal interface in an austenite matrix before deformation and introduction of nano twin crystals in the total length of all high-angle interfaces is lower than 35%. The method comprises the steps of carrying out solid solution treatment on a section bar which is obtained by casting, forging or rolling Fe, mn, si and C elements and is obtained by smelting at 1050-1150 ℃ for 30-120 minutes, then carrying out rolling deformation at 800-1000 ℃, then carrying out annealing at 800-1000 ℃ for 15-30 minutes, and then introducing deformed nano twin crystals at room temperature. The high-strength low-magnetic steel prepared by the method has the advantages of more quantity of nano twin crystals introduced by room-temperature deformation, more uniform distribution, higher strength and plasticity, simple manufacturing process and low cost.
Description
Technical Field
The invention belongs to the field of high-strength steel, and particularly relates to a method for preparing high-strength low-strength magnetic steel by introducing nanometer twin crystals. The high-strength low-magnetic steel prepared by the method has higher strength and plasticity, and can be widely applied to the fields of electric power, machinery, rail transit, buildings, national defense, military industry and the like.
Background
Along with the demand that the structure subtracts heavy improvement, the demand of the low magnet steel of superhigh strength is bigger and bigger. To ensure low magnetic properties, the low magnetic steel must have a stable face centered cubic structure of the austenitic matrix at room temperature. However, for the austenitic steel with the face-centered cubic structure, the traditional methods of solid solution strengthening, deformation strengthening, fine grain strengthening and precipitation strengthening are adopted to improve the strength and simultaneously obviously reduce the plasticity or toughness of the material. Therefore, how to improve the strength on the premise of ensuring excellent ductility and toughness is the primary technical problem facing the current development of high-strength low-magnetic steel.
Luokeji proposes a strengthening method for introducing a twin crystal structure with a nanometer scale into a polycrystalline material; and a large amount of nanometer twin crystals are introduced into the pure Cu film through pulse electrodeposition, and the combination of the yield strength of about 900MPa and the fracture strain of about 13 percent is realized. The nano twin structure prepared by the pulse electrodeposition can be used for preparing a thin film sample only, although the strength of the material can be remarkably improved and the plasticity and the toughness are not damaged or are slightly damaged. In order to introduce a nanometer twin crystal structure into a block sample, luoke and the like develop a dynamic plastic deformation method with high strain rate. However, the dynamic plastic deformation method with high strain rate can only realize small sheet-shaped samples in a laboratory, and is difficult to realize the industrial preparation of large-size samples.
The invention discloses a method for improving the yield strength of twin-induced plastic steel by introducing nano deformation twin crystals through simple unidirectional deformation (a method for preparing the twin-induced plastic steel with high yield strength, ZL2017 1 0604528.3). The twin induced plasticity steel prepared by the method not only has greatly increased yield strength, but also has higher elongation. However, since the orientation of each crystal grain is different, the crystal grain having a partially unfavorable orientation is inevitably not subjected to twinning deformation. Therefore, the introduction of deformation twins by simple unidirectional deformation on the grain scale is not necessarily uniform, and the improvement of the strength is not very remarkable. If the nano deformation twin crystal with higher density can be introduced more uniformly on the grain size, the comprehensive mechanical properties of high strength and excellent plasticity and toughness can be realized in the low-magnetic face-centered cubic twin induced plasticity steel.
In the high manganese iron-based shape memory alloy with low stacking fault energy, research shows that when the density of annealing twin interfaces in the matrix, namely the total length of the annealing twin interfaces, accounts for the fraction of all high-angle interfaces, is reduced, the amount of closely-packed hexagonal martensite introduced by deformation is more, and the distribution on the grain scale becomes more uniform (Wen Yu Hua, nature Communications,2014,5, P4964). The similarity of the twin shear and the shearing process of the hexagonal close-packed martensite is considered, the density of an annealing twin crystal interface in the face-centered cubic twin induced plastic steel is reduced, nano deformation twin crystals with higher density can be introduced more uniformly, and the comprehensive mechanical properties of high strength and excellent plasticity and toughness are realized. The technical problem existing in the prior art of reducing the density of an annealing twin crystal interface in the face-centered cubic twin induced plasticity steel is an industrialized method.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides high-strength low-magnetic steel with uniform nano twin crystal distribution. Another object of the present invention is to provide an industrial method for preparing such high strength low magnetic steel with uniform nano twinning distribution. The method can prepare the austenite matrix with low annealing twin crystal interface density, and can introduce nano deformation twin crystals with higher density more uniformly after deformation.
The invention provides high-strength low-magnetic steel with uniform nano twin distribution, which consists of Mn, si, C and Fe elements and is characterized in that the proportion of the total length of annealing twin boundaries in an austenite matrix before introduction of nano twin to the fraction of all high-angle interfaces (more than or equal to 15 ℃) is less than 35%, and the high-strength steel comprises the following elements in percentage by mass: 12 to 25 percent of Mn, 0 to 3 percent of Si, 0.6 to 1.4 percent of C and the balance of Fe.
The invention provides high-strength non-magnetic steel with uniform nanometer twin crystal distribution, which is prepared by the method provided by the invention, the preparation method comprises the steps of carrying out solution treatment on a profile which is obtained by casting, forging or rolling Fe, mn, si and C elements and is obtained by smelting at 1050-1150 ℃ for 30-120 minutes, then carrying out rolling deformation with the rolling reduction of 10-30% at 800-1000 ℃, and then annealing at 800-1000 ℃ for 15-30 minutes, wherein the proportion of the total length of an annealing twin crystal boundary in an austenitic matrix to the fraction of all high-angle interfaces (more than or equal to 15 ℃) is lower than 35%, and the mass percentage content of each element is as follows: mn is 12 to 25 percent, si is 0 to 3 percent, C is 0.6 to 1.4 percent, and the balance is Fe; or the section bar which is obtained by casting, forging or rolling Fe, mn, si and C elements obtained by smelting is subjected to solution treatment and then is deformed by continuous multi-pass rolling, wherein the initial rolling temperature is 1050 to 1150 ℃, the final rolling temperature is 800 to 950 ℃, the total rolling reduction is 20 to 30 percent, and then annealing is carried out at 850 to 950 ℃ for 15 to 30 minutes, the section bar is characterized in that the proportion of the total length of annealing twin crystal boundaries in an austenite matrix to the total length fraction of all high-angle interfaces (more than or equal to 15 ℃) is less than 35 percent, and the weight percentage content of each element is as follows: mn is 12 to 25 percent, si is 0 to 3 percent, C is 0.6 to 1.4 percent, and the balance is Fe; and after annealing at 850-950 ℃ for 15-30 minutes, the section with low annealing twin interface density is stretched, compressed, rolled, twisted or sheared and deformed at room temperature for 20-90 percent to introduce deformed nano twin crystal, and then annealing at 350-450 ℃ for 30-90 minutes to improve the plasticity of the high-strength low-magnetic steel.
When the carbon content in the alloy is more than 0.6%, a second phase is easily precipitated during rolling and annealing. The selection of the temperature is extremely important for preventing the precipitation of the second phase, and the optimum rolling temperature in the present invention is 800 to 1000 ℃. The annealing temperature also has influence on the grain boundary characteristic distribution of subsequent metals, the proportion of annealing twin boundaries is increased due to overhigh annealing temperature, and the second phase is separated due to overlow annealing temperature, so the optimal annealing temperature range is 850-950 ℃. Too long annealing time also leads to an increase in the proportion of annealed twin interfaces, so the optimum annealing time is 15 to 30 minutes. The annealing twin crystal interface mainly takes an immovable coherent twin crystal interface with low energy as a main part. When the proportion of the total length of the annealing twin crystal interface in the austenite matrix to the total length fraction of all high-angle interfaces (more than or equal to 15 ℃) is more than 45%, the large amount of the annealing twin crystal interface can hinder the coordinated deformation of crystal grains and inhibit the introduction of deformation twin crystals in crystal grains with unfavorable orientation. When the proportion of the total length of the annealing twin crystal interface in the austenite matrix in the steel prepared by the optimized rolling process and the annealing process to the total length fraction of all high-angle interfaces is less than 35%, the uniformity of the deformation twin crystal introduced into the crystal grains can be remarkably improved. However, when the proportion is less than 25%, further reduction of the proportion does not significantly improve the uniformity of the deformed twin crystal introduced into the crystal grains.
The temperature of low-temperature annealing after 20 to 90 percent of deformation nanometer twin crystal is introduced by stretching or compressing or rolling or twisting or shearing deformation at room temperature cannot be higher than 450 ℃, and the annealing time cannot exceed 90 minutes. Higher and longer anneals will introduce second phases that reduce the plasticity of the steel.
Drawings
FIG. 1 is an EBSD map of samples of example 1 prepared by the present invention before deformation introduction of nano twins, wherein gray is the high angle interface and black is the annealing twin boundary interface, and the total length of the annealing twin boundary accounts for about 33.26% of the fraction of the total high angle interface.
FIG. 2 is an EBSD map of a sample prepared according to the present invention before deformation of the sample into nano twin crystal, wherein gray is a high angle interface and black is an annealing twin boundary interface, and the total length of the annealing twin boundary accounts for about 22.58% of the fraction of the total high angle interface.
FIG. 3 is an EBSD graph of the sample of comparative example 1 before nano-twin crystal introduction by deformation, wherein gray is a high angle interface, and black is an annealing twin boundary interface, wherein the proportion of the total length of the annealing twin boundary to the fraction of the total high angle interface is about 45.72%.
FIG. 4 is a TEM photograph of nano twins in the sample of example 6 prepared by the present invention.
Fig. 5 is a TEM photograph of nano twins in the sample of comparative example 3.
FIG. 6 is a graph of engineering stress-strain curves when samples of example 6 and comparative example 3 prepared in accordance with the present invention are stretched.
Detailed Description
The following examples are given to further illustrate the present invention. It should be noted that the examples given are not to be construed as limiting the scope of the invention, and that the invention is not to be limited thereto but rather is to be construed as broadly as possible within the scope of the invention as defined in the claims appended hereto.
Examples 1 to 10.
The chemical compositions of the alloys of examples 1-10 of the present invention are shown in Table 1. In the specific implementation process, the invention provides a method and a process for preparing high-strength non-magnetic steel, wherein the process flow comprises the following steps: solution treatment → high temperature rolling treatment → high temperature annealing treatment → stretching or compressing or rolling or twisting or shearing deformation → low temperature annealing treatment. The high temperature rolling process performed on examples 1-10 is shown in tables 2 and 3. The annealed twin boundary fraction in the structure after the high temperature annealing treatment of examples 1 to 10 was measured by the EBSD method, and the results are shown in table 4. The mechanical properties of the samples after introduction of the nano twins of examples 1-10 are shown in table 4.
Comparative examples 1 to 4.
The chemical composition of the alloys of comparative examples 1 to 4 is shown in table 1. In comparative examples 1 to 4, the solution treatment process is the same as in examples 1 to 10, except that the solution treatment is directly followed by cold deformation to introduce nanometer twin crystals, and the process flow is as follows: solution treatment → stretching or compression or rolling or torsion or shear deformation → low temperature annealing treatment. The annealed twin boundary fraction in the alloy after the solution treatment was detected by the EBSD method and the results are shown in table 4. Comparative examples 1-4 the mechanical properties of the samples after introduction of the nano twins are shown in table 4.
Table 1 chemical composition of the example alloys and the comparative example alloys.
Table 2 high temperature rolling and annealing process performed on the alloys of examples 1-6.
Table 3 high temperature rolling and annealing process performed on the alloys of examples 7-10.
Table 4 annealing twin boundary fraction and cold deformation + annealing process in the structure after high temperature rolling and annealing process of the alloy of examples and the alloy of comparative examples and corresponding mechanical properties.
It can be seen from table 4 that the high strength non-magnetic steel prepared according to the present invention has higher strength, which can be increased by up to about 16%, without reducing plasticity, compared to the comparative example in which nano twins are introduced by direct cold deformation. In order to verify the influence of the invention on the annealing twin interface fraction, fig. 1, 2 and 3 show the structures before the deformation introduction of nano-twins in example 1, example 7 and comparative example 1, respectively, were examined with EBSD. The results show that: the high-strength non-magnetic steel prepared by the method obviously reduces the fraction of annealing twin crystal interface in the structure before the introduction of nano twin crystal strengthening, and the fraction is lower than 35 percent. In order to verify the influence of reducing the annealing twin interface fraction on the introduction of nano twin by deformation, transmission electron microscope tests were carried out on the samples of example 6 and comparative example 3 by using the TEM technique, and the photographs are shown in fig. 4 and 5. Through observation and analysis, the nanometer twin crystal introduced by deformation after the fraction of the annealing twin crystal interface is reduced is thinner in thickness, smaller in distance and more uniform in distribution. In order to more intuitively compare and reduce the influence of the annealing twin interface fraction on the mechanical properties of the deformed nanometer twin strengthened nonmagnetic steel, fig. 6 is an engineering stress-strain curve of the samples of example 6 and comparative example 3 when the samples are stretched. It can be seen that the strength and plasticity of the sample of example 6 prepared by the process of the present invention are higher than those of comparative example 3. This is due to the fine and uniformly distributed nano twins in the sample of example 6.
Claims (11)
1. A high-strength low-magnetic steel with uniform nano twin distribution is characterized in that: the steel comprises the following elements in percentage by mass: the material comprises 12 to 25 percent of Mn, 0 to 3 percent of Si, 0.6 to 1.4 percent of C and the balance of Fe, the preparation process comprises high-temperature annealing, the proportion of the total length of annealing twin crystal interfaces in an austenitic matrix after annealing to the total length fraction of all high-angle interfaces is lower than 35 percent, and the high-angle interfaces refer to interfaces with angles larger than or equal to 15 degrees.
2. A method of high strength low magnetic steel with uniform nano twinning distribution according to claim 1, characterized by: the method comprises the steps of casting, forging or rolling into a section, solution treatment, rolling and high-temperature annealing.
3. A method according to claim 2, characterized in that: the section bar preparation comprises casting or forging or rolling to form a section bar, and the solid solution treatment is carried out for 30 to 120 minutes at 1050 to 1150 ℃.
4. A method according to any one of claims 2-3, characterized in that: the rolling is carried out under the condition that rolling deformation is carried out under the rolling reduction of 10 to 30 percent at 800 to 1000 ℃ or continuous multipass rolling deformation is carried out, wherein the initial rolling temperature is 1050 to 1150 ℃, the final rolling temperature is 800 to 950 ℃, and the rolling total rolling reduction is 20 to 30 percent.
5. A method according to claim 4, characterized in that: the high-temperature annealing is carried out at 800-1000 ℃ for 15-30 minutes, the proportion of the total length of annealing twin crystal interfaces in the austenitic matrix after annealing to the total length fraction of all high-angle interfaces is less than 35%, wherein the high-angle interfaces refer to interfaces with angles larger than or equal to 15 degrees.
6. A method according to claim 4, characterized in that the proportion of the total length of the annealed twin interfaces in the austenitic matrix after annealing to the total length fraction of all high-angle interfaces is less than 25%, wherein a high-angle interface means an interface with an angle of 15 ° or more.
7. A method according to any one of claims 5 or 6, wherein: the high-temperature annealing is carried out at 850 to 950 ℃ for 15 to 30 minutes.
8. A method for preparing the high-strength low-magnetic steel as claimed in any one of claims 5 or 6, which is characterized by further comprising room-temperature deformation after high-temperature annealing, wherein the room-temperature deformation is performed by drawing or compressing or rolling or twisting or shearing deformation at room temperature for 20-90% to introduce deformation nanometer twin crystals.
9. A method for preparing the high-strength low-magnetic steel as claimed in claim 7, wherein the method further comprises room temperature deformation after high temperature annealing, wherein the room temperature deformation is performed by drawing or compressing or rolling or twisting or shearing deformation at room temperature for 20-90% to introduce deformation nanometer twin crystals.
10. A method for producing high strength low magnetic steel as claimed in claim 8, characterized in that the steel is annealed at 350 to 450 ℃ for 30 to 90 minutes after deformation at room temperature.
11. A method for producing high strength low magnetic steel according to claim 9, characterized in that the steel is annealed at 350 to 450 ℃ for 30 to 90 minutes after deformation at room temperature.
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| CN116083699A (en) * | 2023-04-10 | 2023-05-09 | 中北大学 | TWIP steel with adjustable and controllable performance and preparation process thereof |
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