CN115927790A - Preparation method of high-strength and high-plasticity austenitic stainless steel with medium nitrogen content - Google Patents
Preparation method of high-strength and high-plasticity austenitic stainless steel with medium nitrogen content Download PDFInfo
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Abstract
The invention discloses a preparation method of high-strength and high-plasticity austenitic stainless steel with medium nitrogen content, which comprises the following steps: step 1, putting austenitic stainless steel into a smelting device, heating the austenitic stainless steel in vacuum until the austenitic stainless steel is molten, and introducing nitrogen into the smelting device in a bottom blowing mode to carry out nitrogen alloying treatment on the molten austenitic stainless steel; step 2, carrying out cold deformation on the austenitic stainless steel subjected to the nitrogen alloying treatment in the step 1 after homogenizing annealing; step 3, carrying out insufficient annealing treatment on the austenitic stainless steel deformed in the step 2, and finally carrying out water quenching to room temperature; wherein, the austenitic stainless steel in the step 1 comprises 0.1-0.2% of nitrogen by mass percent. According to the invention, the austenitic stainless steel is subjected to nitrogen alloying treatment and then is subjected to cold deformation and insufficient annealing treatment, so that the yield strength of the material can be effectively improved, and good plasticity is kept.
Description
Technical Field
The invention belongs to the technical field of stainless steel smelting and processing, and particularly relates to a preparation method of high-strength and high-plasticity austenitic stainless steel with medium nitrogen content.
Background
Austenitic stainless steel means stainless steel having an austenitic structure at normal temperature. The steel has a stable austenite structure when it contains about 18% of Cr, 8% to 25% of Ni, and 0.1% of C. The austenitic chromium-nickel stainless steel comprises a famous 18Cr-8Ni steel and a high Cr-Ni series steel developed by increasing the contents of Cr and Ni and adding Mo, cu, si, nb, ti and the like on the basis of the steel. Austenitic stainless steel is one of alloys widely used because of its excellent corrosion resistance, good mechanical properties, and the like. 304 austenitic stainless steel is among the most widely used. However, the practical application of the austenitic matrix of 304 steel is limited due to its relatively low yield strength, and thus, the application of the austenitic matrix to structural members such as automobile chassis and load-bearing members is limited. Thus, a great deal of research has been conducted in the prior art to improve the yield strength of 304 austenitic stainless steels. For example, in patent nos.: 201410753437.2, named as: a Chinese patent of a preparation method of 304 austenitic stainless steel with average grain size less than 100nm discloses a preparation method of 304 austenitic stainless steel with the grain size less than 100 nm. The method comprises the steps of hot rolling 304 austenitic stainless steel to a plate with the thickness of 4-5 mm, wherein the microstructure is austenite, the grain size is 18-20 mu m, and the structure is relatively uniform; and then the 304 austenitic stainless steel with the grain size less than 100nm is prepared by three-stage cold rolling-annealing process treatment. The patent points out that the mechanical properties of the experimental steel prepared by the method are carried out, and the yield strength of the stainless steel is 1100-1200 MPa and the tensile strength is 1250-1350 MPa. And it is not said whether such high yield strength and tensile strength stainless steel can be obtained by the above method in practical application. Even if stainless steel having such high yield strength and tensile strength is actually obtained, three stages of cold rolling-annealing treatment, i.e., three times of cooling-heating-cooling treatment, are required after completion of hot rolling due to the manufacturing method. The preparation process is quite complex, is only limited to be used in a laboratory in the actual application process, and is not suitable for actual production application.
Disclosure of Invention
The invention aims to solve the technical problem that the preparation process of the austenitic stainless steel with high strength and high plasticity is relatively complex in the prior art; the preparation method of the high-strength and high-plasticity austenitic stainless steel with medium nitrogen content is provided, so that the technical effect of improving the strength and plasticity of the austenitic stainless steel is realized on the premise of not increasing the difficulty and complexity of the preparation process.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high-strength and high-plasticity austenitic stainless steel with medium nitrogen content comprises the following steps:
step 2, cooling the austenitic stainless steel subjected to the nitrogen alloying treatment in the step 1, and then performing cold rolling deformation or cold drawing deformation;
step 3, carrying out insufficient annealing treatment on the austenitic stainless steel deformed in the step 2, and finally carrying out water quenching to room temperature;
wherein, the austenitic stainless steel in the step 1 comprises 0.1-0.2% of nitrogen by mass percent.
Further, the austenitic stainless steel in the step 1 further comprises the following components in percentage by mass: less than or equal to 0.07 percent of carbon, 0.2 to 0.4 percent of silicon, 1.0 to 1.3 percent of manganese, 18 to 20.5 percent of chromium, 5 to 8 percent of nickel, less than or equal to 0.006 percent of aluminum, 0.2 to 0.3 percent of copper, 0.1 to 0.2 percent of molybdenum, less than or equal to 0.035 percent of phosphorus, and the balance of iron.
Further, the temperature of heating in the smelting device in the step 1 is 1500-1550 ℃.
Further, in the step 1, the process of introducing nitrogen into the smelting device and the process of carrying out nitrogen alloying treatment are both carried out while the temperature in the smelting device is kept at 1500-1550 ℃.
Further, after nitrogen is introduced into the smelting device in the step 1, the introduction of nitrogen is stopped when the air pressure in the smelting device reaches 0.1-0.12MPa, and the air pressure in the smelting device is kept unchanged.
Further, the treatment time of the nitrogen alloying treatment in the step 1 is 15min-30min.
Further, the deformation amount of cold rolling deformation or cold drawing deformation in the step 2 is 50-90%.
Further, the annealing temperature of the insufficient annealing treatment in the step 3 is 800-850 ℃.
Further, the annealing time of the insufficient annealing treatment in the step 3 is 1min-3min.
Further, the smelting device is a smelting furnace.
The beneficial effects of the invention are:
according to the invention, the austenitic stainless steel containing 0.1-0.2 mass% of nitrogen is subjected to nitrogen alloying treatment and then cold deformation and insufficient annealing treatment, so that the yield strength of the material can be effectively improved, good plasticity (elongation) is kept, stress/strain induced martensite phase transformation is inhibited, and the size effect and hydrogen embrittlement tendency caused by stress concentration and volume expansion are avoided, so that the finally obtained material can be widely applied to stressed structural members with high requirements on size precision and under severe environmental conditions. Meanwhile, the addition of nitrogen in the invention can properly reduce the content of expensive element Ni in the alloy and reduce the cost; the whole preparation process is relatively simple in process, and extra process cost is not required to be increased.
Drawings
FIG. 1 is a strain-stress plot of sample 304N of example 1 of the present invention and sample 304 of comparative example 1;
FIG. 2 is an EBSD phase diagram of sample 304N of example 1 of the present invention and sample 304 of comparative example 1 before and after deformation;
FIG. 3 is a KAM phase diagram before and after deformation of sample 304N of example 1 of the present invention and sample 304 of comparative example 1;
FIG. 4 is TEM bright field image, weak beam dark field image and SAED image of sample 304N of example 1 and sample 304 of comparative example 1 before deformation according to the present invention;
fig. 5 is TEM bright field images of sample 304N of example 1 of the present invention and sample 304 of comparative example 1 after deformation.
Detailed Description
The embodiment of the invention provides a preparation method of high-strength and high-plasticity austenitic stainless steel with medium nitrogen content, so as to solve the technical problem that the preparation process of austenitic stainless steel with high strength and high plasticity is relatively complex in the prior art.
The general idea adopted by the invention is as follows:
the embodiment of the invention provides a preparation method of high-strength and high-plasticity austenitic stainless steel with medium nitrogen content, which comprises the following steps: step 1, putting austenitic stainless steel into a smelting device, heating the austenitic stainless steel in vacuum until the austenitic stainless steel is molten, and introducing nitrogen into the smelting device to carry out nitrogen alloying treatment on the molten austenitic stainless steel; step 2, cooling the austenitic stainless steel subjected to the nitrogen alloying treatment in the step 1, and then performing cold rolling deformation or cold drawing deformation; step 3, carrying out insufficient annealing treatment on the austenitic stainless steel deformed in the step 2, and finally carrying out water quenching to room temperature; wherein, the austenitic stainless steel in the step 1 comprises 0.1-0.2% of nitrogen by mass percent.
In the preparation method, nitrogen can be dissolved into austenite through nitrogen alloying treatment, so that the effect of effectively improving the yield strength of the stainless steel is achieved, meanwhile, the stability of the austenite can be improved, and the condition that the austenite is subjected to martensite phase transformation at the initial deformation stage or under the stress condition to cause the stainless steel material to yield too early is avoided. And the dissolved nitrogen can also improve the stacking fault energy of the austenitic stainless steel, promote the plane slip of dislocation, and improve the dislocation accommodation density in crystal grains, thereby maintaining the rheological stress of the austenitic stainless steel under a high strain condition and enabling the stainless steel material to have high strength and high plasticity. Because the austenitic stainless steel contains 0.1 to 0.2 percent of nitrogen, the recrystallization process can be effectively promoted, the time required by insufficient annealing is greatly shortened, and the austenitic matrix structure which is not completely recrystallized can be obtained within 1 to 3 minutes, namely the obtained austenitic matrix structure has three grain distribution states which are respectively: fully recrystallized, partially recrystallized, and unrecrystallized mixed texture. The heterogeneous structures with different hardness, namely the in-situ composite material, are formed in the austenite phase, the yield strength of the stainless steel material can be effectively improved through the grain distribution of the soft and hard combination, and meanwhile, the tensile strength of the stainless steel material can be further improved through the back stress strengthening between the soft and hard grains, and good plasticity is kept.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without inventive step, are within the scope of protection of the invention. Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
The use of "first," "second," and similar terms in the description and claims of the present application do not denote any order, quantity, or importance, but rather the terms are used to distinguish one element from another. Similarly, the singular forms "a," "an," or "the" and similar referents do not denote a limitation of quantity, but rather denote the presence of at least one, unless the context clearly dictates otherwise. The terms "comprises," "comprising," or the like, mean that the elements or items listed before "comprises" or "comprising" encompass the features, integers, steps, operations, elements, and/or components listed after "comprising" or "comprising," and do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. "upper", "lower", "left", "right", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly.
Example 1
A preparation method of high-strength and high-plasticity austenitic stainless steel with medium nitrogen content comprises the following steps:
Placing 304 austenitic stainless steel into a smelting crucible of a smelting furnace, sealing the smelting furnace, starting a vacuum device to pump the interior of the smelting furnace to 100Pa (because the interior of the smelting furnace cannot be pumped to complete vacuum in the actual operation process, the interior of the smelting furnace can be regarded as vacuum after the pressure in the smelting furnace reaches 100 Pa), and then starting a heating device of the smelting furnace to heat the 304 austenitic stainless steel to be molten, wherein the heating temperature is 1550 ℃. And then introducing industrial nitrogen (wherein the purity of the nitrogen is more than 99%) into the smelting furnace in a bottom blowing mode until the pressure in the smelting furnace reaches 0.1MPa, stopping introducing the nitrogen, and closing the smelting furnace. The smelting furnace is kept for 15min under the conditions that the nitrogen pressure is 0.1MPa and the temperature of the 304 austenitic stainless steel melt is 1550 ℃, so that the nitrogen can be fully dissolved in the 304 austenitic stainless steel melt.
Wherein the 304 austenitic stainless steel comprises the following components in percentage by mass: 0.074% of carbon, 0.25% of silicon, 1.11% of manganese, 18.2% of chromium, 8.07% of nickel, 0.15% of nitrogen, 0.006% of aluminum, 0.26% of copper, 0.14% of molybdenum, 0.035% of phosphorus and the balance of iron.
Step 2, cold deformation treatment
And (3) carrying out homogenization annealing and cooling on the austenitic stainless steel subjected to the nitrogen alloying treatment in the step (1), and then carrying out cold drawing to 50% of deformation, wherein the diameter of the obtained semi-finished product is 6mm.
Step 3, insufficient annealing treatment
And (3) cutting the deformed semi-finished austenitic stainless steel in the step (2) into required shapes and sizes, annealing for 3min at the temperature of 800 ℃, and finally water quenching to room temperature to obtain high-strength and high-plasticity austenitic stainless steel samples. The sample obtained in this example was designated as 304N sample.
Example 2
A preparation method of high-strength and high-plasticity austenitic stainless steel with medium nitrogen content comprises the following steps:
Placing 304 austenitic stainless steel into a smelting crucible of a smelting furnace, sealing the smelting furnace, starting a vacuum device to pump the pressure in the smelting furnace to 100Pa, and then starting a heating device of the smelting furnace to heat the 304 austenitic stainless steel to be molten, wherein the heating temperature is 1500 ℃. And then introducing industrial nitrogen (wherein the purity of the nitrogen is more than 99%) into the smelting furnace until the pressure in the smelting furnace reaches 0.11MPa, stopping introducing the nitrogen, and closing the smelting furnace. The smelting furnace is kept for 20min under the conditions that the nitrogen pressure is 0.11MPa and the temperature of the 304 austenitic stainless steel melt is 1500 ℃, so that the nitrogen can be fully dissolved in the 304 austenitic stainless steel melt.
Wherein the 304 austenitic stainless steel comprises the following components in percentage by mass: 0.03 percent of carbon, 0.3 percent of silicon, 1.3 percent of manganese, 19.1 percent of chromium, 6.6 percent of nickel, 0.17 percent of nitrogen, 0.005 percent of aluminum, 0.24 percent of copper, 0.15 percent of molybdenum, 0.02 percent of phosphorus and the balance of iron.
Step 2, cold deformation treatment
And (3) annealing and cooling the austenitic stainless steel subjected to the nitrogen alloying treatment in the step (1), and then performing cold drawing to 50% of deformation, wherein the diameter of the obtained semi-finished product is 6mm.
Step 3, insufficient annealing treatment
And (3) cutting the deformed semi-finished austenitic stainless steel in the step (2) into required shapes and sizes, annealing for 2min at 830 ℃, and finally water quenching to room temperature to obtain high-strength and high-plasticity austenitic stainless steel samples.
Example 3
A preparation method of high-strength and high-plasticity austenitic stainless steel with medium nitrogen content comprises the following steps:
Placing 304 austenitic stainless steel into a smelting crucible of a smelting furnace, sealing the smelting furnace, starting a vacuum device to pump the interior of the smelting furnace to 100Pa, and then starting a heating device of the smelting furnace to heat the 304 austenitic stainless steel to be molten, wherein the heating temperature is 1530 ℃. And then introducing industrial nitrogen (wherein the purity of the nitrogen is more than 99%) into the smelting furnace until the pressure in the smelting furnace reaches 0.12MPa, stopping introducing the nitrogen, and closing the smelting furnace. And keeping the pressure of nitrogen in the smelting furnace at 0.12MPa and the temperature of the 304 austenitic stainless steel melt at 1530 ℃ for 30min to ensure that the nitrogen can be fully dissolved in the 304 austenitic stainless steel melt.
Wherein the 304 austenitic stainless steel comprises the following components in percentage by mass: 0.04% of carbon, 0.40% of silicon, 1.21% of manganese, 18.5% of chromium, 5.3% of nickel, 0.19% of nitrogen, 0.006% of aluminum, 0.21% of copper, 0.12% of molybdenum, 0.02% of phosphorus and the balance of iron.
Step 2, cold deformation treatment
And (3) annealing and cooling the austenitic stainless steel subjected to the nitrogen alloying treatment in the step (1), and then performing cold drawing to 50% of deformation, wherein the diameter of the obtained semi-finished product is 6mm.
Step 3, insufficient annealing treatment
And (3) cutting the deformed semi-finished austenitic stainless steel in the step (2) into required shapes and sizes, annealing for 1min at 850 ℃, and finally water quenching to room temperature to obtain high-strength and high-plasticity austenitic stainless steel samples.
Comparative example 1
Commercially available ordinary 304 austenitic stainless steel. The sample of this comparative example was designated as 304 sample.
The austenitic stainless steel samples obtained in examples 1 to 3 and comparative example 1 were subjected to tensile testing according to GB/T228.1 to 2010, and the test results were as follows:
TABLE 1 tensile test results for examples 1-3 and comparative example 1
As can be seen from the above table, the austenitic stainless steel prepared by the examples of the present invention has both superior strength and plasticity compared to the commercially available 304 stainless steel. Referring to fig. 1, the yield ratio of the sample 304N of example 1 is significantly improved to 0.76, almost twice as high as that of the sample 304 of comparative example 1, and the total elongation of 304N can be maintained at a high level of about 50%, as compared to the sample 304 of comparative example 1.
Performance test 2
To further verify the beneficial effects of the embodiments of the present invention, the sample 304N obtained in the embodiment 1 of the present invention and the sample 304 of the comparative example 1 are further examined and compared for microstructure, and the following results are obtained:
as shown in FIG. 2, the EBSD phase diagrams before and after the tensile deformation of sample 304 of the comparative example are shown in the two portions (a) and (c), respectively. In the figure, the two parts (b) and (d) are EBSD phase diagrams before and after the sample 304N of example 1 is subjected to tensile deformation. Comparing the two parts (a) and (b) in the figures, it can be seen that the 304 sample of the comparative example had a majority of austenite and a small amount of ferrite before the tensile deformation, whereas the 304N sample of example 1 had an almost completely austenitic microstructure. Comparing the two parts (c) and (d) in the figure, it can be seen that 60% or more of the austenite in the 304 sample of the comparative example is transformed into martensite, while the austenite proportion transformed into martensite in the 304N sample of the example 1 is less than 4% after the tensile deformation. The austenitic stainless steel matrix prepared by the method has high austenite content and good austenite stability after stretching deformation, thereby greatly improving the yield strength of the stainless steel.
As shown in FIG. 3, portions (e) and (g) are the austenite-shape comparison KAM plot and the martensite-shape band-shape comparison KAM plot, respectively, of the sample 304 of the comparative example. Sections (f) and (h) are the austenite-like contrast KAM plot and the martensite-like contrast KAM plot, respectively, for sample 304N of example 1. Comparing the two sections (e) and (f) in the graph, it can be seen that the dislocation density is relatively low and the distribution is not uniform in the 304 sample of the comparative example, whereas the dislocation density is high and the distribution is uniform in the 304N sample of example 1. Comparing the two parts (g) and (h) in the graph, it can be seen that the austenite of the 304N sample of example 1 has a dense slip band relative to the 304 sample of the comparative example. Therefore, the preparation method provided by the embodiment of the invention can improve the stacking fault energy of the austenitic stainless steel, promote the plane slippage of dislocation, and improve the dislocation accommodation density in crystal grains, so that the rheological stress of the austenitic stainless steel under a high strain condition is maintained, and the stainless steel material is high in strength and plasticity.
As shown in fig. 4, two parts (a) and (c) in the figure are TEM bright field images before deformation of the 304 sample of the comparative example and the 304N sample of example 1, respectively. In the figure, two parts (b) and (d) are a weak beam dark field image and a SAED image before deformation of the 304 sample of the comparative example and the 304N sample of the example 1, respectively. As can be seen from the two sections (a) and (b), the 304 samples of the comparative example had many Stacking Faults (SFs) arranged along two (111) planes between which many short dislocations were randomly distributed. As can be seen from the two sections (c) and (d) in the figure, the dislocations in the 304N sample of example 1 are regularly arranged along the (111) plane, and almost no Stacking Faults (SFs) are found. It can be seen that the addition of nitrogen has a significant effect on the microscopic microstructure of the material, changing the configuration of crystal defects in the structure.
As shown in fig. 5, two parts (a) and (b) in the figure are TEM bright field images after deformation of the 304 sample of the comparative example and the 304N sample of example 1, respectively. Comparing the two parts in the figure, the 304 sample generates obvious strain induced martensite phase transformation in the deformation process, while the 304N sample has no martensite phase transformation and only generates deformation twin crystals in austenite, thereby avoiding the failure problem caused by the martensite phase transformation possibly under the stress or strain condition in the service process.
Finally, it should be noted that: these embodiments are merely illustrative of the present invention and do not limit the scope of the present invention. In addition, other variations and modifications will be apparent to persons skilled in the art based on the foregoing description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.
Claims (10)
1. A preparation method of high-strength and high-plasticity austenitic stainless steel with medium nitrogen content is characterized by comprising the following steps:
step 1, putting austenitic stainless steel into a smelting device, heating the austenitic stainless steel in vacuum until the austenitic stainless steel is molten, and introducing nitrogen into the smelting device in a bottom blowing mode to carry out nitrogen alloying treatment on the molten austenitic stainless steel;
step 2, carrying out cold rolling deformation or cold drawing deformation on the austenitic stainless steel subjected to the nitrogen alloying treatment in the step 1 after carrying out homogenization annealing and cooling;
step 3, performing insufficient annealing treatment on the austenitic stainless steel deformed in the step 2, and finally performing water quenching to room temperature;
wherein, the austenitic stainless steel in the step 1 comprises 0.1-0.2% of nitrogen by mass percent.
2. A method of making a medium nitrogen content high strength and high plasticity austenitic stainless steel according to claim 1, characterized in that: the austenitic stainless steel in the step 1 further comprises the following components in percentage by mass: less than or equal to 0.07 percent of carbon, 0.2 to 0.4 percent of silicon, 1.0 to 1.3 percent of manganese, 18 to 20.5 percent of chromium, 5 to 8 percent of nickel, less than or equal to 0.006 percent of aluminum, 0.2 to 0.3 percent of copper, 0.1 to 0.2 percent of molybdenum, less than or equal to 0.035 percent of phosphorus, and the balance of iron.
3. A method of making a medium nitrogen content high strength and high plasticity austenitic stainless steel according to claim 1, characterized in that: the heating temperature in the smelting device in the step 1 is 1500-1550 ℃.
4. A method of making a medium nitrogen content high strength and high plasticity austenitic stainless steel according to claim 1, characterized in that: in the step 1, the process of introducing nitrogen into the smelting device and the process of carrying out nitrogen alloying treatment are both carried out while the temperature in the smelting device is kept at 1500-1550 ℃.
5. A method of making a medium nitrogen content high strength and high plasticity austenitic stainless steel according to claim 1, characterized in that: and in the step 1, after nitrogen is introduced into the smelting device, stopping introducing the nitrogen when the air pressure in the smelting device reaches 0.1-0.12MPa, and keeping the air pressure in the smelting device unchanged.
6. A method of making a medium nitrogen content high strength and high plasticity austenitic stainless steel according to claim 1, characterized in that: the treatment time of the nitrogen alloying treatment in the step 1 is 15min-30min.
7. A method of making a medium nitrogen content high strength and high plasticity austenitic stainless steel according to claim 1, characterized in that: and the deformation amount of cold rolling deformation or cold drawing deformation in the step 2 is 50-90%.
8. A method of making a medium nitrogen content high strength and high plasticity austenitic stainless steel according to claim 1, characterized in that: the annealing temperature of the insufficient annealing treatment in the step 3 is 800-850 ℃.
9. A method of making a medium nitrogen content high strength and high plasticity austenitic stainless steel according to claim 1, characterized in that: the annealing time of the insufficient annealing treatment in the step 3 is 1min-3min.
10. The method for preparing a medium nitrogen content high strength and high plasticity austenitic stainless steel according to claim 1, characterized by: the smelting device is a smelting furnace.
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