CN116445828B - Ultra-pure austenitic stainless steel and preparation method thereof - Google Patents
Ultra-pure austenitic stainless steel and preparation method thereof Download PDFInfo
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- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
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Abstract
The invention relates to the technical field of metallurgy, and particularly discloses ultra-pure austenitic stainless steel and a preparation method thereof. The ultra-pure austenitic stainless steel comprises the following components ：C≤0.007％,Mn≤0.05％,Si≤0.30％,S≤0.002％,P≤0.01％,Ni:14.5％～15.0％,Cr:16.5％～17.0％,Mo:2.20％～2.50％,Al≤0.01％,H≤0.0002％,O≤0.0015％,N≤0.015％,Cu≤0.10％, by weight percent, and the balance of Fe and unavoidable impurities. According to the invention, through designing alloy components, the proportion of each component is reasonable, and Mo, ni and Cr elements are synergistic, so that the corrosion resistance of austenitic stainless steel can be obviously improved, and the proper Cr/Ni/Mo proportion is beneficial to fundamentally reducing the formation of ferrite and controlling the content of ferrite; meanwhile, by strictly controlling harmful elements and residual elements, the ultra-pure austenitic stainless steel has the advantages of low inclusion content and high purity, and has good ductility, plasticity and impact toughness.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to ultra-pure austenitic stainless steel and a preparation method thereof.
Background
Austenitic stainless steel has been widely used in various industries because of its excellent combination of high-temperature strength, toughness, corrosion resistance, weldability, and the like. With the rapid development of the industries such as nuclear industry, ocean engineering and the like, the service environment of steel materials is increasingly complex, and some precise parts or special equipment may require materials to have good corrosion resistance, oxidation resistance and mechanical properties, and particularly, nuclear grade austenitic stainless steel requires very low nonmetallic inclusion, which requires the design and research of special austenitic stainless steel to meet more strict requirements.
The 316 austenitic stainless steel is CrNiMo stainless steel, can be applied to semiconductor equipment, pipelines of nuclear power projects and in-pile shielding rods, and in order to improve the high-temperature intergranular stress corrosion resistance of the steel, a certain amount of Mo element needs to be added into the steel, so that Wen-ferrite is easier to form compared with other austenitic stainless steel, the hot workability and the hot formability of the steel are reduced, the steel is toughened and embrittled, the high-temperature durability of the steel is influenced, and the service life of the steel is further reduced; meanwhile, the internal inclusion of the 316-series austenitic stainless steel prepared by the existing smelting process is less than or equal to 1.0 level, the purity is lower, the purity required by the semiconductor and nuclear power steel is higher, otherwise, a crack source is formed at the interface of two phases in the high-temperature use process, so that the nuclear leakage is caused, the life and property safety of human beings is seriously endangered, and the control of the ferrite content and the inclusion content in the steel becomes important. Therefore, the development of the ultra-pure austenitic stainless steel with compact structure, good plasticity and high purity has very important significance.
Disclosure of Invention
In view of the above, the invention provides an ultrapure austenitic stainless steel and a preparation method thereof, and by designing alloy components, the proportion of each component is reasonable, the level of ferrite content less than 1% is realized, the content of inclusion is less, the purity is high, and meanwhile, the alloy has good ductility, plasticity and impact toughness.
In order to achieve the above purpose, the embodiment of the invention adopts the following technical scheme:
in a first aspect, the present invention provides an ultrapure austenitic stainless steel comprising, in weight percent, ：C≤0.007％,Mn≤0.05％,Si≤0.30％,S≤0.002％,P≤0.01％,Ni:14.5％～15.0％,Cr:16.5％～17.0％,Mo:2.20％～2.50％,Al≤0.01％,H≤0.0002％,O≤0.0015％,N≤0.015％,Cu≤0.10％, the balance Fe and unavoidable impurities.
Compared with the prior art, the ultra-pure austenitic stainless steel provided by the invention has the following advantages:
According to the invention, through designing alloy components, the proportion of each component is reasonable, the content of Cr element is controlled to be 16.5% -17.0%, the content of Mo element is controlled to be 2.20% -2.50%, the content of Ni element is controlled to be 14.5% -15.0%, mo, ni and Cr elements are cooperated, the corrosion resistance of austenitic stainless steel can be obviously improved, and the proper Cr/Ni/Mo proportion is beneficial to fundamentally reducing the formation of ferrite and controlling the content of ferrite; meanwhile, by strictly controlling harmful elements and residual elements, the ultra-pure austenitic stainless steel has the advantages of low inclusion content and high purity, and has good ductility, plasticity and impact toughness.
The ultra-pure austenitic stainless steel provided by the invention is designed based on the following thought:
C: carbon is an austenite element, can inhibit ferrite formation and improve the strength of the material, is easy to combine with chromium element to form carbide, reduces the content of chromium element in solid solution in steel, and forms a primary cell around the carbide, thereby reducing the corrosion resistance of austenitic stainless steel. Therefore, the upper limit of the content of C element in the steel is set to 0.007% in the present invention.
Mn: manganese is an austenite element, and can stabilize an austenite phase and enlarge an austenite phase region; however, during welding, harmful gas with low vapor pressure is generated on the surface of molten metal, and the harmful gas is solidified and then adheres to the inner wall of the pipe, and is enriched with Mn in a welding heat affected zone to form oxides, so that local corrosion is generated. Therefore, the upper limit of the Mn element content in the steel is set to 0.05% in the present invention.
Ni: nickel is a main alloy element in austenitic stainless steel, can form and stabilize an austenitic phase, improves the machining performance, the stainless performance and the corrosion resistance of the alloy, and meanwhile, the combination of Ni and Cr has a synergistic effect on the austenitic stainless steel in a severe corrosion environment; however, an increase in nickel content results in an increase in the intergranular corrosion susceptibility of austenitic stainless steel. Therefore, the invention controls the Ni element content in the steel to be 14.5% -15.0%.
Si element and Al element are deoxidizing elements of austenitic stainless steel, and silicon and aluminum can synergistically improve the form of inclusions, reduce the content of gas elements in molten steel, refine grains and ensure the deoxidizing effect of the steel. Therefore, the upper limit of the content of Al element in the steel is set to 0.01% and the upper limit of the content of Si element is set to 0.30%.
S: sulfur is one of the harmful element impurities in steel, and is easy to combine with manganese element in steel to form class-A inclusion (sulfide) with lower hardness, so that the cracking risk of steel is increased. Therefore, the upper limit of the S element content in the steel is set to 0.002%.
P: phosphorus is one of the harmful element impurities in steel, increases cold brittleness of steel, deteriorates welding performance, reduces plasticity, and is particularly sensitive to irradiation embrittlement. Therefore, the upper limit of the content of P element in steel is set to 0.01%.
Cr: chromium can improve corrosion resistance and strength of stainless steel, however, chromium element is a strong ferrite forming element, and a large amount of austenite forming elements such as nickel, manganese, nitrogen and the like are required to be added to high-chromium austenitic stainless steel. Therefore, the invention controls the Cr element content in the steel to be 16.5-17.0%.
Mo: the molybdenum can improve the pitting corrosion resistance and crevice corrosion resistance of the steel in a chloride environment, can also improve the corrosion resistance of the steel in a reducing environment such as hydrochloric acid, dilute sulfuric acid and the like, and the beneficial effect of the molybdenum in the steel can be obviously increased under the action of chromium element; however, molybdenum participates in the formation of harmful secondary phases, promotes the formation of high Wen-ferrite in austenitic stainless steel, causes the reduction of hot workability and hot formability of steel, and forms unstable high-temperature oxides, which adversely affects high-temperature oxidation resistance. Therefore, the invention controls the content of Mo element in the steel to be 2.2% -2.5%.
In a second aspect, the present invention also provides a method for preparing the above ultra-pure austenitic stainless steel, comprising the steps of:
Firstly, mixing the raw materials according to a preset proportion, smelting by a vacuum induction furnace, casting, electroslag remelting and vacuum consumable remelting, and controlling the content of each element to meet the requirement of the ultra-pure austenitic stainless steel to obtain a steel ingot;
And step two, heating, forging and heat treatment are carried out on the steel ingot, so that the ultra-pure austenitic stainless steel is obtained.
Compared with the prior art, the preparation method of the ultrapure austenitic stainless steel provided by the invention has the following advantages:
The invention can effectively control the form and distribution of crystal grains in the steel by adopting a triple smelting process of vacuum induction, electroslag remelting and vacuum consumption, greatly improve the purity of the alloy and realize the control of ultrapure purification of the alloy. The prepared ultra-pure austenitic stainless steel has the advantages of compact structure, good plasticity, high purity, excellent performance and the like, nonmetallic inclusion B, D class fine system inclusions are less than 0.5 level, the other types of inclusions are not included, the grain size level is more than 6.5 level, the tensile strength R m is more than or equal to 490MPa, the yield strength Rp 0.2 is more than or equal to 220MPa, the area shrinkage ratio ψ is more than or equal to 80%, the use requirements of high-end semiconductors and nuclear power key equipment can be met, and the ultra-pure austenitic stainless steel has wide market application prospect.
Optionally, in the first step, the smelting process of the vacuum induction furnace specifically includes: after mixing the raw materials, sequentially carrying out melting treatment, refining treatment and fine adjustment component treatment in a vacuum induction furnace, and tapping to obtain molten alloy steel; wherein, in the melting treatment, the temperature of the full melting is 1530-1550 ℃; in the refining treatment, the vacuum degree is less than or equal to 3Pa, the refining temperature is 1540-1570 ℃, and the refining time is 30-70 min. The optimized vacuum induction furnace smelting process is favorable for controlling impurity elements in molten steel at a lower level, reducing the number of impurities in the molten steel and improving the purity of the molten steel, thereby being favorable for improving the mechanical property of stainless steel.
Optionally, in the first step, the casting temperature is 1540 ℃ to 1560 ℃.
Optionally, in the first step, in the electroslag remelting process, the melting speed is 5.0 kg/min-6.0 kg/min, and the smelting slag adopts a DRZ-1910 slag system.
Optionally, the DRZ-1910 slag system comprises the following components in percentage by weight: 15-20% of CaF 2:50％～70％,CaO:5％～15％,Al2O3, mgO:5% -15%. The preferable slag system has good adsorption effect on inclusions, can reduce oxygen enrichment of molten steel and inclusion content, and improves purity of electrode ingot steel.
Optionally, in the step one, in the vacuum consumable remelting process, the vacuum degree is less than or equal to 0.5Pa, the current in an arcing stage is 4.0 kA-10.5 kA, the melting speed in a smelting stable stage is 2.5 kg/min-6.5 kg/min, and the current in a feeding stage is 2.5 kA-6.0 kA.
Optionally, in the second step, the heating process specifically includes: heating the steel ingot to 600-650 ℃, preserving heat for 1-2 h, then heating to 800-810 ℃ at the heating rate of 80-100 ℃/h, preserving heat for 1.5-2 h, heating to 1160-1180 ℃ at the heating rate of 80-100 ℃/h, preserving heat for 3-4 h, and forging. The invention adopts three-section heating, which is beneficial to the steel ingot in the optimal thermoplastic region, ensures the uniformity of temperature and structure, effectively controls the grain size and simultaneously avoids the occurrence of forging cracking.
Optionally, in the second step, in the forging process, the forging temperature is not less than 1000 ℃, the final forging temperature is not less than 850 ℃, the heating temperature of the blank returning to the furnace is 1140-1160 ℃, and the time for returning to the furnace is 60-90 min.
Optionally, in the second step, the heat treatment specifically includes: and (3) hot-conveying the forged steel billet to a heating furnace for high-temperature solution heat treatment, wherein the heat treatment temperature is 1000-1020 ℃, and the heat preservation time is 20-30 min. The preferable heat treatment temperature and time can ensure that ferrite is fully dissolved, and simultaneously can effectively avoid the phenomenon of crystal elongation at the edge position and ensure that the grain size of the finished steel is in a reasonable range.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph of the head-to-tail inclusion distribution of an ultrapure austenitic stainless steel provided in example 1 of the present invention;
Fig. 2 is a diagram showing the ferrite distribution of the head and tail of the ultra-pure austenitic stainless steel provided in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In order to better illustrate the present invention, the following examples are provided for further illustration.
Example 1
The embodiment of the invention provides ultra-pure austenitic stainless steel, which comprises the following chemical components in percentage by weight:
C:0.007％,Mn:0.04％,Si:0.12％,S:0.0008％,P:0.005％,Ni:14.8％,Cr:16.76％,Mo:2.35％,Al:0.004％,H:0.0001％,O:0.001％,N:0.0034％,Cu:0.02％, The balance being Fe and unavoidable impurities.
The preparation method of the ultra-pure austenitic stainless steel comprises the following steps:
S1, smelting in a vacuum induction furnace: preparing raw materials according to the main chemical components in the proportion, mixing the raw materials, sequentially carrying out melting treatment, refining treatment and fine adjustment component treatment in a vacuum induction furnace, controlling the total melting temperature to be 1540 ℃, controlling the vacuum degree in the refining period to be 3Pa, controlling the refining temperature to be 1555 ℃, controlling the refining time to be 50min, and tapping to obtain the alloy molten steel.
S2, casting: casting the alloy molten steel, cooling to obtain a steel ingot with the diameter of phi 480mm, and controlling the casting temperature to 1550 ℃ by adopting argon protection in the whole casting process.
S3, electroslag remelting: after cleaning and finishing the surface of the steel ingot, carrying out electroslag remelting, wherein argon is adopted for protection smelting in the whole process, the smelting speed is controlled to be 5.5kg/min, the smelting slag adopts a DRZ-1910 slag system, and the chemical components of the slag are as follows in percentage by weight: caF 2:60％,CaO:10％,Al2O3:20%, mgO:10%.
S4, vacuum consumable remelting: and (3) carrying out vacuum consumable remelting on the steel ingot subjected to electroslag remelting, wherein the vacuum degree of a vacuum consumable furnace is controlled to be 0.5Pa, the current in an arcing stage is 8.0kA, the melting speed in a smelting stabilization stage is 4.5kg/min, and the current in a feeding stage is 4.0kA.
S5, forging: polishing the steel ingot subjected to vacuum consumable remelting, heating to 620 ℃, preserving heat for 1.5h, then heating to 805 ℃ at a heating rate of 90 ℃/h, preserving heat for 1.7h, heating to 1170 ℃ at a heating rate of 90 ℃/h, preserving heat for 3.5h, and forging to produce the steel ingot. In the forging process, the forging temperature is controlled to be 1000 ℃, the final forging temperature is controlled to be 850 ℃, the heating temperature of blank furnace returning is controlled to be 1150 ℃, and the furnace returning time is controlled to be 80 minutes. After final forging, the forged steel billet is heated to a heating furnace for high-temperature solution heat treatment to obtain the ultra-pure austenitic stainless steel, wherein the heat treatment temperature is controlled to be 1010 ℃, and the heat preservation time is 25min.
Example 2
The embodiment of the invention provides ultra-pure austenitic stainless steel, which comprises the following chemical components in percentage by weight:
C:0.006％,Mn:0.03％,Si:0.14％,S:0.001％,P:0.006％,Ni:14.75％,Cr:16.78％,Mo:2.32％,Al:0.008％,H:0.00009％,O:0.001％,N:0.004％,Cu:0.02％, The balance being Fe and unavoidable impurities.
The preparation method of the ultra-pure austenitic stainless steel comprises the following steps:
S1, smelting in a vacuum induction furnace: preparing raw materials according to the main chemical components in the proportion, mixing the raw materials, sequentially carrying out melting treatment, refining treatment and fine adjustment component treatment in a vacuum induction furnace, controlling the total melting temperature to be 1530 ℃, controlling the vacuum degree in the refining period to be 3Pa, controlling the refining temperature to be 1540 ℃, controlling the refining time to be 30min, and tapping to obtain the alloy molten steel.
S2, casting: casting the alloy molten steel, cooling to obtain a steel ingot with the diameter of phi 480mm, and controlling the casting temperature to be 1540 ℃ by adopting argon protection in the whole casting process.
S3, electroslag remelting: after cleaning and finishing the surface of the steel ingot, carrying out electroslag remelting, wherein argon is adopted for protection smelting in the whole process, the smelting speed is controlled to be 5.0kg/min, the smelting slag adopts a DRZ-1910 slag system, and the chemical components of the slag are as follows in percentage by weight: caF 2:50％,CaO:15％,Al2O3:20%, mgO:15%.
S4, vacuum consumable remelting: and (3) carrying out vacuum consumable remelting on the steel ingot subjected to the electroslag remelting, wherein the vacuum degree of a vacuum consumable furnace is controlled to be 0.5Pa, the current in an arcing stage is 4.0kA, the melting speed in a smelting stabilization stage is 2.5kg/min, and the current in a feeding stage is 2.5kA.
S5, forging: and polishing the steel ingot subjected to vacuum consumable remelting, heating to 600 ℃, preserving heat for 1h, then heating to 800 ℃ at a heating rate of 80 ℃/h, preserving heat for 1.5h, heating to 1160 ℃ at a heating rate of 80 ℃/h, preserving heat for 3h, and forging. In the forging process, the forging temperature is controlled to be 1020 ℃, the final forging temperature is controlled to be 860 ℃, the heating temperature of blank furnace returning is controlled to be 1140 ℃, and the furnace returning time is controlled to be 60 minutes. After final forging, the forged steel billet is heated to a heating furnace for high-temperature solution heat treatment to obtain the ultra-pure austenitic stainless steel, wherein the heat treatment temperature is controlled to be 1000 ℃, and the heat preservation time is controlled to be 20min.
Example 3
The embodiment of the invention provides ultra-pure austenitic stainless steel, which comprises the following chemical components in percentage by weight:
C:0.006％,Mn:0.03％,Si:0.13％,S:0.0009％,P:0.005％,Ni:14.78％,Cr:16.71％,Mo:2.30％,Al:0.006％,H:0.0001％,O:0.0009％,N:0.0038％,Cu:0.025％, The balance being Fe and unavoidable impurities.
The preparation method of the ultra-pure austenitic stainless steel comprises the following steps:
S1, smelting in a vacuum induction furnace: preparing raw materials according to the main chemical components in the proportion, mixing the raw materials, sequentially carrying out melting treatment, refining treatment and fine adjustment component treatment in a vacuum induction furnace, controlling the total melting temperature to 1550 ℃, controlling the vacuum degree in the refining period to 3Pa, controlling the refining temperature to 1570 ℃, controlling the refining time to 70min, and tapping to obtain the alloy molten steel.
S2, casting: casting the alloy molten steel, cooling to obtain a steel ingot with the diameter of phi 480mm, and controlling the casting temperature to 1560 ℃ by adopting argon protection in the whole casting process.
S3, electroslag remelting: after cleaning and finishing the surface of the steel ingot, carrying out electroslag remelting, wherein argon is adopted for protection smelting in the whole process, the smelting speed is controlled to be 6.0kg/min, the smelting slag adopts a DRZ-1910 slag system, and the chemical components of the slag are as follows in percentage by weight: caF 2:70％,CaO:5％,Al2O3:15%, mgO:10%.
S4, vacuum consumable remelting: and (3) carrying out vacuum consumable remelting on the steel ingot subjected to the electroslag remelting, wherein the vacuum degree of a vacuum consumable furnace is controlled to be 0.5Pa, the current in an arcing stage is 10.5kA, the melting speed in a smelting stabilization stage is 6.5kg/min, and the current in a feeding stage is 6.0kA.
S5, forging: and polishing the steel ingot subjected to vacuum consumable remelting, heating to 650 ℃, preserving heat for 2 hours, then heating to 810 ℃ at a heating rate of 100 ℃/h, preserving heat for 2 hours, heating to 1180 ℃ at a heating rate of 100 ℃/h, and preserving heat for 4 hours, and forging to produce the steel ingot. In the forging process, the forging temperature is controlled to be 1050 ℃, the final forging temperature is controlled to be 880 ℃, the heating temperature of blank returning is 1160 ℃, and the time for returning is 90min. After final forging, the forged steel billet is sent to a heating furnace for high-temperature solution heat treatment to obtain the ultra-pure austenitic stainless steel, wherein the heat treatment temperature is controlled to be 1020 ℃, and the heat preservation time is 30min.
Example 4
The embodiment of the invention provides ultra-pure austenitic stainless steel, which comprises the following chemical components in percentage by weight:
C:0.005％,Mn:0.05％,Si:0.13％,S:0.001％,P:0.004％,Ni:14.74％,Cr:16.73％,Mo:2.33％,Al:0.005％,H:0.00008％,O:0.001％,N:0.0041％,Cu:0.01％, The balance being Fe and unavoidable impurities.
The procedure for the preparation of the above-described ultrapure austenitic stainless steel is the same as in example 1.
Example 5
The embodiment of the invention provides ultra-pure austenitic stainless steel, which comprises the following chemical components in percentage by weight:
C:0.006％,Mn:0.04％,Si:0.13％,S:0.001％,P:0.005％,Ni:14.76％,Cr:16.75％,Mo:2.30％,Al:0.004％,H:0.0001％,O:0.0008％,N:0.0038％,Cu:0.015％, The balance being Fe and unavoidable impurities.
The procedure for the preparation of the above-described ultrapure austenitic stainless steel is the same as in example 1.
Any sample of the ultra-pure austenitic stainless steel prepared in examples 1 to 5 is cut, the nonmetallic inclusion content, ferrite content and grain size of the ultra-pure austenitic stainless steel are detected, and the full-section high-power result is detected as shown in table 1; performance testing was performed simultaneously and the results are shown in table 2.
FIG. 1 is a schematic view of the inclusion of the ultrapure austenitic stainless steel prepared in example 1 in a full section metallographic view on a scale of 100 μm, from which only a very small number of B, D species are seen; FIG. 2 is a schematic diagram of a full section metallographic view of ferrite of the super austenitic stainless steel prepared in example 1 under a scale of 50 μm, each sample being free of ferrite. TABLE 1 nonmetallic inclusion detection results
TABLE 2 Performance test results
As can be seen from tables 1-2, the ultra-pure austenitic stainless steel provided by the invention has extremely low content of nonmetallic inclusion and ferrite and stable austenitic structure, and simultaneously, the performance indexes such as tensile strength, yield strength, elongation, area shrinkage and the like meet the ASTM A182/A182M-2020 and GB/T1220-2007 standard requirements under the component design.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, or alternatives falling within the spirit and principles of the invention.
Claims (5)
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