CN114807741A - Method for improving performance of austenitic stainless steel based on carbide precipitation - Google Patents
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- C21D2211/00—Microstructure comprising significant phases
- C21D2211/004—Dispersions; Precipitations
Abstract
The invention discloses a method for improving the performance of austenitic stainless steel based on carbide precipitation, and belongs to the field of metal material manufacturing. Aiming at austenitic stainless steel with low Ti/C ratio and Si, the invention firstly promotes the dissolution of primary carbide by utilizing methods of vacuum consumable remelting, high-temperature homogenization and the like in the preparation process of alloy, secondly adopts cold working deformation to prepare a large amount of deformation twin crystals in the alloy, and finally realizes the fine dispersion precipitation of secondary carbide TiC in the alloy through low-temperature aging treatment. The carbide particles can pin dislocation to improve the strength of the material, and simultaneously provide a large amount of non-coherent phase interfaces to absorb vacancies to improve the radiation swelling resistance of the material.
Description
Technical Field
The invention relates to the technical field of metal material manufacturing, in particular to a method for improving the performance of austenitic stainless steel based on carbide precipitation.
Background
The austenitic stainless steel materials such as 316Ti, 15-15Ti and the like have good comprehensive mechanical property and processing property, and are widely applied to the manufacturing of fuel cladding of the fourth-generation advanced nuclear energy system. The nuclear-grade austenitic stainless steel material is an austenitic single-phase structure, has a small amount of precipitated phases in crystal, and mainly depends on solid solution strengthening, grain boundary strengthening and deformation strengthening. Ferritic/martensitic stainless steels such as T91 are another class of fuel cladding materials with high potential for use, with a large number of martensite laths and precipitates within the martensite grains. Due to the existence of a large number of intracrystalline interfaces and second phases, the alloy strength and the radiation swelling resistance of the iron-horse steel are superior to those of austenitic stainless steel under medium and low temperature conditions. Therefore, there is a need for further improvement of chemical composition and processing technology of austenitic stainless steel, which can improve the warm strength and radiation swelling resistance thereof.
Disclosure of Invention
In order to improve the strength and the radiation swelling resistance of the austenitic stainless steel, the invention aims to provide a method for improving the performance of the austenitic stainless steel based on carbide precipitation, which can promote the fine dispersion precipitation of carbides in the austenitic stainless steel, in particular to form deformation twin crystals in crystal grains of the austenitic stainless steel by applying cold deformation, and then carry out low-temperature aging treatment to promote the precipitation of the carbides in a deformation twin crystal area. The strength and the anti-swelling performance of the material are improved by utilizing the second phase pinning dislocation and the phase interface to absorb vacancies.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
a method for improving the properties of austenitic stainless steels based on carbide precipitation, the method comprising the steps of:
(1) alloy smelting and thermal deformation: carrying out double vacuum smelting and thermal deformation cogging on austenitic stainless steel;
(2) cold working deformation of the alloy: carrying out cold deformation processing on the alloy subjected to thermal deformation cogging for multiple times;
(3) aging treatment: the carbide is induced to be precipitated through low-temperature long-term aging heat treatment, so that the medium-temperature strength and the radiation swelling resistance of the austenitic stainless steel are improved.
In the step (1), the austenitic stainless steel before smelting comprises the following chemical components in percentage by weight: 0.04-0.08% of C, 15.5-20.0% of Cr, 14.5-16.5% of Ni, 0.4-2.0% of Si, 1.5-3.0% of Mn, 0.2-0.5% of Ti, 1.3-2.5% of Mo, 0.003-0.004% of B and the balance of Fe.
In the step (1), the weight ratio of Ti/C in the chemical components of the alloy is not more than 5, and the low Ti/C can reduce the precipitation of carbide TiC in the smelting process of the alloy.
In the step (1), the content of the chemical component Si of the alloy is preferably 1.0-2.0 wt.%, and the addition of the Si element can reduce the activity of C in the melt and inhibit TiC precipitation. Meanwhile, the alloy stacking fault energy can be reduced, and the formation of deformation twin crystals is promoted.
In the step (1), the alloy smelting adopts a double-vacuum smelting process of vacuum induction smelting and a vacuum consumable remelting process, and the quantity of TiC in the ingot can be further reduced in the vacuum consumable remelting process.
In the step (1), the consumable ingot is subjected to high-temperature homogenization treatment for 12-15h at 1200-1250 ℃ before thermal deformation cogging and is cooled by water, TiC carbide precipitated in the ingot is dissolved, element homogenization diffusion is promoted, and the dissolved carbide is prevented from being precipitated again in the subsequent thermal deformation process; and after the thermal deformation of the alloy is finished, water quenching and cooling are carried out, so that carbide is prevented from being separated out in the cooling process.
Processing the alloy into a plate with the thickness of 1.0-3.0mm by multi-pass cold rolling in the cold deformation processing of the step (2); annealing treatment is carried out after each cold rolling deformation, the annealing treatment temperature is 1020-1060 ℃, the annealing time is not more than 30min, and the precipitation of TiC in the annealing process is reduced; the annealing treatment after each cold rolling deformation adopts gas quenching cooling, so that the cooling rate is increased to avoid TiC precipitation in the cooling process; after the final annealing treatment is finished, performing 15-30% cold deformation on the plate to prepare deformation twin crystals in the alloy structure.
In the step (3), the alloy is subjected to low-temperature aging treatment, wherein the aging temperature is 400-.
After the final cold rolling deformation of the alloy sheet is finished, a large number of deformation twin crystals can be formed in the crystal grains. After the cold-deformation alloy plate is subjected to low-temperature aging treatment, a large amount of fine TiC carbide particles can be formed in a deformation twin crystal area, and the size of the TiC carbide particles is not more than 100 nm.
TiC is an important second phase in Ti-containing austenitic stainless steel, generally having a geometric shape, with dimensions of about several microns, distributed discretely within the crystal. These large-sized TiC particles belong to primary carbides and are mainly formed in a liquid-phase melt in the alloy smelting process. Because the number of primary carbides is small and the size is large, the contribution to the alloy strength is small. In addition to being formed in the liquid phase, TiC carbides may also precipitate during thermal deformation or heat treatment of the alloy. These carbides precipitated in the solid phase are called secondary carbides. The secondary TiC particles are small in size, about hundreds of nanometers, are generally preferentially nucleated and separated at defect positions such as crystal boundaries, dislocation and the like, and can play a certain role in precipitation strengthening.
The invention introduces a large amount of deformation twin crystals in the crystal through cold deformation. The deformed twin crystal has the characteristics of high lamella density and small lamella thickness, and can provide a large number of initial nucleation positions for carbide precipitation. In low temperature, long time aging treatment, TiC nucleates in great amount on twin crystal face and dislocation line in the deformation twin crystal area. Because the heat treatment temperature is lower, the precipitation of carbide takes nucleation as the main part and grows up as the auxiliary part to form a fine and dispersed distribution state. Starting from the analysis of the structure-performance relationship, the fine and dispersed TiC particles can mainly bring two-point performance improvement to austenitic stainless steel. First, TiC can hinder dislocation motion and improve alloy strength. Second, because TiC generally does not have a coherent relationship with the austenite matrix, the precipitation of a large amount of carbides will create a large amount of non-coherent interfaces in the alloy. The non-coherent interface is a common vacancy well, can effectively absorb vacancies, avoids vacancy aggregation and cavity formation in the irradiation process, and further improves the irradiation swelling resistance of the material.
The invention has the following beneficial effects:
the invention is carried out aiming at austenitic stainless steel with low Ti/C ratio and Si, the process method prepares a large amount of deformation twin crystals in the alloy through cold deformation, twin crystal boundaries and dislocations provide a large amount of nucleation positions for carbide precipitation, and TiC is induced to be finely dispersed and precipitated in alloy crystals in low-temperature and long-time aging treatment, so that the strength and the radiation swelling resistance of the alloy are improved.
Drawings
FIG. 1 is an SEM microstructural morphology photograph of the sample obtained in example 1.
FIG. 2 is a SEM microstructural morphology photograph of the sample obtained in comparative example 1.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1:
the method is characterized in that a master alloy ingot is prepared by adopting vacuum induction melting and vacuum consumable remelting, and the alloy ingredients before melting are as follows (wt%): 0.06% of C, 17.0% of Cr, 15.0% of Ni, 2.0% of Si, 1.5% of Mn, 0.24% of Ti, 1.50% of Mo and the balance of Fe. The alloy Ti/C weight ratio was 4. And after the consumable ingot is smelted, carrying out high-temperature homogenization treatment at 1200 ℃ for 12h in a muffle furnace, and then cooling by water. The consumable ingot is forged and hot rolled to form a hot rolled plate with a thickness of 10 mm. The hot rolled plate is prepared into a cold rolled plate with the thickness of 2.5mm through two cold rolling and two annealing treatments. The annealing heat treatment of the cold-rolled sheet is carried out in a vacuum gas quenching furnace, and the heat treatment system is 1050 ℃ multiplied by 20 min. And after the last heat treatment is finished, cold deformation is applied to the plate through cold rolling, the thickness of the deformed plate is 1.9mm, and the deformation is about 24%. Sampling on the cold-deformed plate, and carrying out low-temperature long-time heat treatment at 450 ℃ for 120 h. The SEM microstructure of the resulting sample is shown in FIG. 1.
Example 2:
the method is characterized in that a master alloy ingot is prepared by adopting vacuum induction melting and vacuum consumable remelting, and the alloy ingredients before melting are as follows (wt%): 0.06% of C, 17.0% of Cr, 15.0% of Ni, 2.0% of Si, 1.5% of Mn, 0.24% of Ti, 1.50% of Mo and the balance of Fe. The alloy Ti/C weight ratio was 4. And after the consumable ingot is smelted, carrying out high-temperature homogenization treatment at 1200 ℃ for 12h in a muffle furnace, and then cooling by water. The consumable ingot is forged and hot rolled to form a hot rolled plate with a thickness of 10 mm. The hot rolled plate is prepared into a cold rolled plate with the thickness of 2.5mm through two cold rolling and two annealing treatments. The annealing heat treatment of the cold-rolled sheet is carried out in a vacuum gas quenching furnace, and the heat treatment system is 1050 ℃ multiplied by 20 min. And after the last heat treatment is finished, cold deformation is applied to the plate through cold rolling, the thickness of the deformed plate is 2.0mm, and the deformation is about 20%. Sampling on the cold-deformed plate, and carrying out low-temperature long-time heat treatment at 450 ℃ for 480 h.
Comparative example 1:
the method is characterized in that a master alloy ingot is prepared by adopting vacuum induction melting and vacuum consumable remelting, and the alloy ingredients before melting are as follows (wt%): 0.06% of C, 16.0% of Cr, 15.0% of Ni, 0.4% of Si, 1.5% of Mn, 0.36% of Ti, 1.50% of Mo and the balance of Fe. The alloy Ti/C weight ratio was 6. And after the consumable ingot is smelted, carrying out high-temperature homogenization treatment at 1200 ℃ for 12h in a muffle furnace, and then cooling by water. The consumable ingot is forged and hot rolled to form a hot rolled plate with a thickness of 10 mm. The hot rolled plate is prepared into a cold rolled plate with the thickness of 2.5mm through two cold rolling and two annealing treatments. The annealing heat treatment of the cold-rolled sheet is carried out in a vacuum gas quenching furnace, and the heat treatment system is 1050 ℃ multiplied by 20 min. And after the last heat treatment is finished, cold deformation is applied to the plate through cold rolling, the thickness of the deformed plate is 2.05mm, and the deformation is about 18%. Sampling on the cold-deformed plate, and carrying out low-temperature long-time heat treatment at 550 ℃ for 120 h. The SEM microstructure of the resulting sample is shown in FIG. 2.
The tensile properties at room temperature were measured for the samples obtained in the above examples and comparative examples, and the results are shown in Table 1.
TABLE 1 comparison of tensile Properties at room temperature of samples obtained in examples and comparative examples
| Yield strength (MPa) | Tensile strength (MPa) | Elongation (%) | |
| Example 1 | 892 | 978 | 20 |
| Example 2 | 868 | 969 | 24 |
| Comparative example 1 | 618 | 750 | 33 |
The above embodiments are merely illustrative and not restrictive, and those skilled in the art can make modifications to the embodiments without any inventive contribution as required after reading the present specification, but only protected by the patent laws within the scope of the claims.
Claims (9)
1. A method for improving the performance of austenitic stainless steel based on carbide precipitation is characterized in that: the method comprises the following steps:
(1) alloy smelting and thermal deformation: carrying out double vacuum smelting and thermal deformation cogging on austenitic stainless steel;
(2) cold working deformation of the alloy: carrying out cold deformation processing on the alloy subjected to thermal deformation cogging for multiple times;
(3) aging treatment: carbide precipitation is induced by low temperature long term aging heat treatment.
2. Method for improving the properties of austenitic stainless steels based on carbide precipitation according to claim 1, characterized in that: in the step (1), the austenitic stainless steel before smelting comprises the following chemical components in percentage by weight: 0.04-0.08% of C, 15.5-20.0% of Cr, 14.5-16.5% of Ni, 0.4-2.0% of Si, 1.5-3.0% of Mn, 0.2-0.5% of Ti, 1.3-2.5% of Mo, 0.003-0.004% of B and the balance of Fe.
3. Method for improving the properties of austenitic stainless steels based on carbide precipitation according to claim 1, characterized in that: in the step (1), the weight ratio of Ti/C in the chemical components of the alloy is not more than 5, and the content of Si in the chemical components of the alloy is 1.0-2.0 wt.%.
4. Method for improving the properties of austenitic stainless steels based on carbide precipitation according to claim 1, characterized in that: in the step (1), the alloy smelting adopts a double-vacuum smelting process of vacuum induction smelting and vacuum consumable remelting.
5. Method for improving the properties of austenitic stainless steels based on carbide precipitation according to claim 1, characterized in that: in the step (1), the consumable ingot is subjected to high-temperature homogenization treatment for 12-15h at 1200-1250 ℃ before thermal deformation cogging and is cooled by water; and (4) after the thermal deformation of the alloy is finished, water quenching and cooling are carried out, and then the step (2) is carried out.
6. Method for improving the properties of austenitic stainless steels based on carbide precipitation according to claim 1, characterized in that: in the cold deformation processing in the step (2), annealing treatment is carried out after each cold deformation, wherein the annealing temperature is 1020-1060 ℃ each time, the annealing treatment time is not more than 30min, and the annealing treatment adopts gas quenching cooling.
7. Method for improving the properties of austenitic stainless steels based on carbide precipitation according to claim 6, characterized in that: in the step (2), after the final annealing treatment is finished, the plate is subjected to 15-30% cold deformation.
8. Method for improving the properties of austenitic stainless steels based on carbide precipitation according to claim 1, characterized in that: in the step (3), the alloy is subjected to low-temperature aging treatment, wherein the aging temperature is 400-.
9. Method for improving the properties of austenitic stainless steels based on carbide precipitation according to claim 1, characterized in that: in the step (3), a large amount of fine TiC carbide particles with the size not larger than 100nm are formed in the deformation twin crystal area of the prepared austenitic stainless steel sample.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115491612A (en) * | 2022-09-26 | 2022-12-20 | 中国科学院金属研究所 | High-strength low-activation steel and preparation method thereof |
| CN115652210A (en) * | 2022-11-07 | 2023-01-31 | 鞍钢股份有限公司 | Austenitic stainless steel billet with ultra-low carbide content and manufacturing method thereof |
| CN115948694A (en) * | 2022-11-07 | 2023-04-11 | 鞍钢股份有限公司 | High-performance austenitic stainless steel plate with thickness of less than 45mm and manufacturing method thereof |
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