CN114160604A - Stainless steel seamless pipe and preparation method and application thereof - Google Patents
Stainless steel seamless pipe and preparation method and application thereof Download PDFInfo
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- CN114160604A CN114160604A CN202111390160.8A CN202111390160A CN114160604A CN 114160604 A CN114160604 A CN 114160604A CN 202111390160 A CN202111390160 A CN 202111390160A CN 114160604 A CN114160604 A CN 114160604A
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- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 60
- 239000010935 stainless steel Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000010622 cold drawing Methods 0.000 claims abstract description 111
- 238000010438 heat treatment Methods 0.000 claims abstract description 100
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 60
- 239000010959 steel Substances 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims description 76
- 230000008569 process Effects 0.000 claims description 60
- 238000001953 recrystallisation Methods 0.000 claims description 40
- 238000001192 hot extrusion Methods 0.000 claims description 36
- 238000001125 extrusion Methods 0.000 claims description 15
- 238000003723 Smelting Methods 0.000 claims description 8
- 229910000963 austenitic stainless steel Inorganic materials 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 2
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 2
- 235000014121 butter Nutrition 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 239000004571 lime Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 4
- 238000007670 refining Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 55
- 239000013078 crystal Substances 0.000 description 52
- 230000000052 comparative effect Effects 0.000 description 20
- 238000005242 forging Methods 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 7
- 230000008859 change Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000000137 annealing Methods 0.000 description 5
- 238000009740 moulding (composite fabrication) Methods 0.000 description 5
- 239000002893 slag Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000002159 abnormal effect Effects 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000005097 cold rolling Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/06—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of tubes or metal hoses; Combined procedures for making tubes, e.g. for making multi-wall tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C1/00—Manufacture of metal sheets, metal wire, metal rods, metal tubes by drawing
- B21C1/16—Metal drawing by machines or apparatus in which the drawing action is effected by other means than drums, e.g. by a longitudinally-moved carriage pulling or pushing the work or stock for making metal sheets, bars, or tubes
- B21C1/22—Metal drawing by machines or apparatus in which the drawing action is effected by other means than drums, e.g. by a longitudinally-moved carriage pulling or pushing the work or stock for making metal sheets, bars, or tubes specially adapted for making tubular articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C23/00—Extruding metal; Impact extrusion
- B21C23/02—Making uncoated products
- B21C23/04—Making uncoated products by direct extrusion
- B21C23/08—Making wire, bars, tubes
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/10—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies
- C21D8/105—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies of ferrous alloys
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/001—Austenite
Abstract
The invention relates to the field of seamless steel pipes, in particular to a stainless steel seamless pipe and a preparation method and application thereof, wherein the preparation method comprises the following steps: and (3) cold-drawing the pipe in a small deformation, medium deformation and large deformation mode respectively, wherein the pipe needs to be subjected to solution heat treatment after each cold-drawing is finished, and finally the stainless steel seamless pipe with uniform internal grain structure size is obtained. According to the invention, the grain structure in the stainless steel seamless pipe has the effects of refining and uniformly distributing by adopting a mode of combining different deformation with heat treatment, and finally, a uniform structure with the grain size of 4-6 grade and the grade difference of less than 2 grade is realized. Meanwhile, the large-caliber stainless steel seamless steel pipe with the uniformly distributed grain structures, the outer diameter of the pipe being larger than 800mm and the wall thickness being larger than 10mm can be manufactured by adopting the manufacturing process, and the large-caliber stainless steel seamless steel pipe can be used for a main pipeline system of an advanced nuclear power station.
Description
Technical Field
The invention relates to the field of seamless steel pipes, in particular to a stainless steel seamless pipe and a preparation method and application thereof.
Background
In the advanced nuclear power technology, large-diameter stainless steel pipes with various specifications are usually required in a primary loop system and a secondary loop system of a reactor, such as 316 and 321 series austenitic stainless steel seamless pipes with the outer diameter of 508 and 914 mm. The current large-caliber seamless pipe manufacturing technology generally adopts integral pipe forging, cold rolling, bar machining and the like.
In the prior art, hot extrusion forming has the advantages of improved metal deformability, high product comprehensive quality, wide range and the like, is widely applied to forming of difficult-to-machine materials, and becomes one of important methods for hot forming of high-alloy and special alloy seamless steel pipes. The seamless steel pipe manufactured by the technology has excellent comprehensive mechanical property, uniform structure and good surface quality, and is a key technology for manufacturing high-performance materials in the industries of nuclear power, thermal power, petrochemical industry and the like. After extrusion of the pipe, it is often necessary to machine the inner and outer surfaces. Currently, a 360 MN vertical extruder with northern heavy industry is provided in China, and the specification range of the product is 325-1200mm in outer diameter and 20-200mm in wall thickness; the 500 MN vertical extruder for Hebei Darun heavy industry has the product specification range of 406 mm in outer diameter and 1472mm in wall thickness of 30-220 mm. According to the disclosure of CN 108998650A, G115 large-caliber thick-wall seamless steel pipes with different specifications of 325-1200mm outer diameter, 20-180 mm wall thickness and 12500mm length can be produced by a hot extrusion process. Therefore, the seamless steel pipe with the outer diameter of more than or equal to 325mm and the wall thickness of less than 20mm can not be directly manufactured by the hot extrusion technology at present.
The forging boring technology is adopted to produce seamless steel pipes, which are also recognized at home and abroad. At present, the large-caliber thick-wall seamless steel pipe produced by northern heavy industry groups by adopting the technology fills the domestic blank, the outer diameter range of the product is 159 and 1066mm, and the ratio of the outer diameter to the wall thickness is less than 20. In the forging process, the blank is gradually and locally deformed on a flat anvil or between tools, the forging deformation degree is not uniform enough, the uniformity of the shape and the size of the same batch of forgings is poor, and the blank is only heated but does not participate in deformation at different parts, so that the uneven structure or the low-magnification coarse grains are caused. The pipe forging technology disclosed in CN 110964990A is also directed to the production process of large-caliber thick-wall seamless pipes. Therefore, it is impossible to produce a large-diameter, medium-thin-walled, seamless steel pipe having a uniform structure by using a forged pipe.
The perforation forming and cold drawing process are commonly used for producing large-caliber seamless steel pipes. According to the disclosure of CN 112453100A, the method adopts a mode of combining electric furnace smelting, argon oxygen furnace refining, ingot casting, electroslag remelting, forging, pipe blank processing, perforating, cold drawing and heat treatment, optimizes process parameters, and obtains the phi 762 multiplied by 48mm large-caliber nickel-based alloy seamless pipe which has the advantages of pure material, uniform components, controllable grain size and good corrosion resistance. At present, the 2600-ton cold drawing unit is owned domestically, the outer diameter range of the product is 406-1060mm, and the wall thickness can be flexibly adjusted according to a die. However, during the perforation, under the action of the roller cyclic stress, radial cracks are easily formed on the blank, longitudinal, tangential and transverse tensile stress is generated on the inner surface layer and the middle transition region, and the inner cracks are easily generated between the inner surface layer and the middle layer, so that the surface quality of the pipe is influenced. In addition, the larger the pipe diameter is, the longer the punching time is, and the larger the fluctuation of the blank temperature along the length direction of the pipe is, so that the nonuniformity of the external dimension, the grain size and the mechanical property is larger. Therefore, the large-diameter seamless steel pipe formed by the perforation process cannot meet the fields of nuclear power industry and the like with high requirements on service life and safety.
The production technology of the large-caliber pipe also comprises a perforation forming and cold rolling process, and according to the disclosure of CN 111979382A, the preparation method of the large-caliber thin-wall seamless steel pipe comprises the following steps: and heating, perforating, rolling and sizing the tube blank in sequence to obtain a sized steel tube, wherein the outer diameter of the large-caliber thin-wall seamless steel tube is more than or equal to 273mm, and the ratio of the outer diameter to the wall thickness is more than or equal to 40. The pierced billet used for cold-working is usually formed by hot piercing. In addition, the maximum cold rolling mill group in China at present is 730 units, the maximum outer diameter of the product is 711mm, and a seamless steel pipe with the outer diameter larger than 711mm cannot be manufactured. Therefore, how to solve the problem of development and mass production of large-caliber (especially the outer diameter is larger than 711 mm) seamless steel pipes is an important bottleneck of current nuclear power development.
Disclosure of Invention
The invention provides a stainless steel seamless pipe, a preparation method and application thereof, aiming at overcoming the defect that the production process in the prior art can not produce a seamless steel pipe which simultaneously meets the requirements of large caliber and uniform internal structure.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of a stainless steel seamless tube comprises the following steps:
(S.1) carrying out cold drawing on the pierced billet by a deformation amount smaller than 12%, and carrying out solution heat treatment under the condition of being lower than the recrystallization temperature after the cold drawing is finished to obtain an intermediate pipe with high size uniformity;
(S.2) carrying out cold drawing on the intermediate pipe by the deformation of 12-15%, and carrying out solution heat treatment under the condition that the temperature is higher than the recrystallization temperature after the cold drawing is finished to obtain the intermediate pipe with a refined structure;
(S.3) cold-drawing the intermediate pipe with refined structure by using the deformation amount of more than 15%, and after the cold-drawing is finished, carrying out solution heat treatment under the condition of higher than recrystallization temperature to obtain the stainless steel seamless pipe with uniform internal grain structure size.
The stainless steel seamless tube in the invention realizes the step-by-step refinement of the grain structure by adopting a mode of combining different deformation amounts with heat treatment in the preparation process, thereby enabling the size of the grain structure in the obtained stainless steel seamless tube to be kept uniform. Therefore, the mechanical property of the material can be more excellent, and the material can meet the use requirements of nuclear power industry and other fields with high requirements on service life and safety.
In the step (S.1), the aim of correcting the initial size of the pierced billet is mainly fulfilled by adopting a cold drawing method with small deformation (the deformation is less than 12%) on the pierced billet, so that the size uniformity of the obtained intermediate pipe can keep consistency. Meanwhile, the cold drawing treatment with small deformation has smaller load requirement on cold drawing equipment, so that the problem that the load of the existing equipment is insufficient can be solved. Meanwhile, because the deformation amount in the cold drawing process is small, the extrusion and deformation amplitude of the grain structure in the pierced billet is small, so that the grain structure in the pierced billet cannot meet the requirement of critical deformation amount, uneven deformation is easily generated along the wall thickness direction of the pipe, and the uneven deformation can be recovered through solution heat treatment. However, the solid solution heat treatment has a significant influence on the shape of the crystal grains inside the pipe, and if the heat treatment is performed at a temperature higher than the recrystallization temperature, abnormal growth of the crystal grains is likely to occur inside the steel pipe, and the crystal grains become very uneven. Therefore, in the present invention, the temperature at the time of the heat treatment after the cold drawing is set to be not higher than the recrystallization temperature in the step (s.1), and therefore, abnormal growth of crystal grains during the cold drawing can be prevented, thereby preventing the problem of non-uniformity of crystal grain size.
In the step (S.2), as the medium deformation of the deformation amount (12-15%) of the intermediate pipe is increased in the cold drawing process, the extrusion and deformation amplitude of the grain structure in the intermediate pipe is increased, the grains in the wall thickness direction of the pipe are sufficiently deformed by more than the critical deformation, and the internal grains can be gradually deformed, crushed and refined in the cold drawing process.
Meanwhile, after the cold drawing is finished, the temperature of the solution heat treatment is higher than the recrystallization temperature, deformed crystal grains can be fully recovered, recrystallized and grown up during the solution heat treatment, and the reformed crystal grain structure can refine the crystal grains with larger internal sizes originally through the processes of dislocation sliding grain refinement, twin crystal refinement, dynamic recrystallization and the like, so that small-sized crystal grains are formed, the grain structure size in the finally obtained intermediate pipe can be refined and uniform, and the preparation is provided for the uniform control of the subsequent finished product structure.
And finally, in the step (S.3), further performing cold drawing treatment with larger deformation on the intermediate pipe, so that the crystal grains in the intermediate pipe can be further crushed and refined, and after the solution heat treatment, a uniform 4-6 grain size structure can be realized.
More preferably, the deformation amount of the pierced billet in the step (s.1) is 8 to 12%.
The main purpose of step (s.1) in the present invention is to correct the initial size of the pierced billet and to solve the problem of insufficient load of the existing equipment, so that the deformation amount only needs to be set to less than 12%. However, after the research and development personnel tests, the correction effect on the initial size of the pierced billet is poor after the deformation is set to be less than 8%, so that under the optimal condition, the deformation of the pierced billet is set to be 8-12%.
More preferably, the deformation amount of the pierced billet in the step (s.3) is 15 to 20%.
Preferably, the temperature of the solution heat treatment in the step (S.1) is 900 to 1020 ℃.
The recrystallization temperature of the stainless steel is about 1020 ℃, so that the stainless steel below 1020 ℃ does not have the function of recrystallization in the heat treatment, thereby effectively preventing the problem of abnormal increase of crystal grains generated when the deformation is small and the heat treatment temperature is higher than the recrystallization temperature, and further enabling the size of the crystal grain structure of the finally obtained seamless pipe to be smaller and more uniform. However, when the temperature is lower than 900 ℃, it is difficult to recover the uneven deformation generated during the cold drawing, which results in a decrease in the uniformity of the grain structure. Therefore, when the temperature of the solution heat treatment in the step (S.1) is 900 to 1020 ℃, the grain size and the size uniformity can be balanced at the same time.
Preferably, the temperature of the solution heat treatment in the step (S.2) is 1020 to 1100 ℃.
In the step (s.2) of the present invention, since the amount of deformation during cold drawing is large, the internal crystal grains are gradually deformed, crushed and refined during cold drawing, which may result in a decrease in uniformity of the crystal grain size. Therefore, after 12-15% of cold drawing with medium deformation, the method can recrystallize broken crystal grains by the solution heat treatment of the Jining at a temperature slightly higher than the recrystallization temperature, so that the uniformity of the crystal grain size is greatly improved. After the temperature of the solution heat treatment is reduced to be lower than the recrystallization temperature, the recrystallization function cannot be performed, and the uniformity of the grain size is low, but after practical tests, the fact that when the temperature of the solution heat treatment is higher than 1100 ℃, the recrystallization capability of the grains can be greatly improved, the size of the grains formed by recrystallization can be greatly improved, the mechanical property of the final steel pipe is reduced, and the use is not facilitated.
Preferably, the temperature of the solution heat treatment in the step (S.3) is 1050 to 1080 ℃.
Preferably, before cold drawing, the pierced blank and the intermediate pipe material need to be polished and acid-washed, and after the treatment, the surfaces of the pierced blank and the intermediate pipe material are coated with butter lime and graphite, so that galling of the pipe material surfaces during cold drawing can be prevented.
Preferably, in the step (s.1), the pierced billet is prepared by performing a vertical hot extrusion process on a billet;
in the hot extrusion process, the extrusion ratio is 3-15, the extrusion heating temperature is 1200-1250 ℃, and the average grain size of the pierced billet obtained after hot extrusion is less than or equal to 180 mu m.
In the hot extrusion process of the thick-wall pipe, the extrusion heating temperature is usually more than 1200 ℃ and even more than 1250 ℃, and the grain size of the pipe blank is usually more than 200 mu m. When the extrusion ratio is small, the recrystallization of crystal grains is insufficient and the problem of non-uniformity of crystal grains in the wall thickness direction is easily generated, and the crystal grains still exhibit a coarse phenomenon. The good hot extrusion pierced billet is a precondition for preparing the large-caliber stainless steel seamless pipe with uniform crystal grains, so that the extrusion ratio is required to be at least not less than 3.0.
Preferably, the billet used for preparing the pierced billet is subjected to at least one secondary remelting process during smelting;
after the secondary remelting process, the level contents of D-type punctiform inclusions and B-type chain-shaped inclusions in the steel billet are respectively not more than 1.5 level and 1.0 level.
The steel billet subjected to the secondary remelting process has extremely low content of non-metallic inclusions, and the lower non-metallic inclusions have a beneficial effect on uniform growth of crystal grains.
A stainless steel seamless pipe is prepared by the method;
the outer diameter of the stainless steel seamless pipe is more than or equal to 600mm, and the wall thickness is less than 20 mm;
the grain size of a grain structure in the stainless steel seamless pipe is 4-6 grades, and the grain size range is less than 2.
More preferably, the outer diameter of the stainless steel seamless pipe is not less than 800 mm.
More preferably, the thickness of the stainless steel seamless pipe is not less than 10 mm.
Preferably, the stainless steel seamless pipe is an austenitic stainless steel pipe for nuclear power
The application of the stainless steel seamless pipe in a nuclear power station main pipeline system.
Therefore, the invention has the following beneficial effects:
(1) according to the invention, the grain structure in the stainless steel seamless pipe is refined and uniformly distributed by adopting a mode of combining different deformation with heat treatment, and finally, a uniform structure with the grain size of 4-6 grades and the grade difference of less than 2 grades is realized;
(2) the manufacturing process can be used for manufacturing the large-caliber stainless steel seamless steel with uniformly distributed grain structures, the outer diameter of the tube is more than 800mm, and the wall thickness is more than 10 mm;
(3) the large-caliber stainless steel seamless steel pipe prepared by the method can be used for a main pipeline system of an advanced nuclear power station.
Drawings
FIG. 1 is a diagram showing a large-diameter stainless steel pipe prepared by the present invention.
FIG. 2 is a photograph showing the structure of a stainless steel pipe produced by the present invention.
Detailed Description
The invention is further described with reference to the drawings and the specific embodiments. Those skilled in the art will be able to implement the invention based on these teachings. Moreover, the embodiments of the present invention described in the following description are generally only some embodiments of the present invention, and not all embodiments. Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
Example 1.
The outer diameter of the large-diameter austenitic stainless steel pipe prepared by the embodiment is in the specification
813mm×15mm×5000mm。
Firstly, smelting a steel ingot by adopting an AOD furnace and slag remelting process, and forging and forming to prepare a billet. The steel billet comprises the following chemical components in percentage by mass: 0.045 of C, 0.35 of Si, 1.56 of Mn, 0.010 of P, 0.001 of S, 12.35 of Ni, 17.45 of Cr, 0.015 of Co, 0.0004 of H, 0.0012 of B, 0.060 of N and the balance of Fe. The steel billet contains class A nonmetallic inclusion 0, class B nonmetallic inclusion 0.5, class C nonmetallic inclusion 0.5 and class D nonmetallic inclusion 1.0, and the lower nonmetallic inclusion has a beneficial effect on uniform growth of grains.
The billet is prepared into a pierced billet by adopting a vertical hot extrusion process, the temperature of the hot extrusion process is 1250 ℃, and the specification of the extruded tube is
813mm by 15mm by 5000 mm. The extrusion ratio is 5.2, the average grain size of the vertical hot extrusion pierced billet is 150 mu m, and the mother pipe with excellent quality is prepared by the hot extrusion process.
The main manufacturing process comprises the following steps:
the vertical hot extrusion pierced billet adopts a three-step combined cold drawing process, and cold drawing passes are divided into at least four times.
In the first step, a small deformation of 9.1 percent plus annealing mode below the recrystallization temperature is adopted, the size deviation of the vertical extruded tube is mainly corrected, and the intermediate tube with high size uniformity is ensured to be obtained.
The elongation coefficient (area ratio of the pipe after cold drawing to the pipe before cold drawing) of the cold drawing deformation is 1.1, and the number of cold drawing is 1. And carrying out solution heat treatment after cold drawing deformation, wherein the heat treatment temperature is 900 ℃.
The second step and the third step respectively adopt a heat treatment mode of 14.1 percent and 14.5 percent of medium deformation plus the temperature about higher than the recrystallization temperature to realize the gradual refinement of the structure, the cold drawing pass is 2 times, the elongation coefficients of the cold drawing deformation are 1.164 and 1.17 respectively, the main deformation stage of the pipe is realized, and the change of the appearance size and the full recrystallization of crystal grains are realized. And carrying out solution heat treatment after cold drawing deformation, wherein the heat treatment temperature is 1025 ℃.
And fourthly, adopting 20.2% of large deformation amount drawing and 1050 ℃ solution heat treatment, wherein the elongation coefficient of cold-drawing deformation is 1.254. And carrying out solution heat treatment after cold drawing deformation, wherein the heat treatment temperature is 1050 ℃. Through deformation and solution heat treatment processes, the full deformation of crystal grains and the full recrystallization of the crystal grains are mainly promoted, and the growth of the crystal grain size of the pipe is controlled by combining the heat treatment process, so that a uniform internal crystal grain structure is obtained.
The photograph of the stainless steel seamless steel pipe produced in this example is shown in FIG. 1. FIG. 2 is a photograph of the internal structure of the seamless steel tube made of stainless steel according to this example, after the final solution heat treatment, the average grain size was 85 μm, the grain size rating was 4, and the grain size difference was 2.
Example 2.
The outer diameter of the large-diameter austenitic stainless steel pipe prepared by the embodiment is in the specification
610mm×10mm×6000mm。
Firstly, smelting a steel ingot by adopting an AOD furnace and slag remelting process, and forging and forming to prepare a billet. The steel billet comprises the following chemical components in percentage by mass: c0.045, Si 0.35, Mn 1.25, P0.015, S0.001, Ni 12.5, Cr 17.32, Co 0.012, H0.0005, B0.0015, N0.070 and the balance of Fe. The steel billet contains class A nonmetallic inclusion 0, class B nonmetallic inclusion 0.5, class C nonmetallic inclusion 0 and class D nonmetallic inclusion 0.5, and the lower nonmetallic inclusion has a beneficial effect on the uniform growth of crystal grains.
The main manufacturing process comprises the following steps:
the billet is prepared into a pierced billet by adopting a vertical hot extrusion process, the temperature of the hot extrusion process is 1230 ℃, and the specification of the extruded tube is
680 multiplied by 25mm, the extrusion ratio is 7.2, the average grain size of the vertical hot extrusion pierced billet is 100 mu m, and the mother pipe with excellent quality is prepared by the hot extrusion process.
The main manufacturing process comprises the following steps:
the vertical hot extrusion pierced billet adopts a three-step combined cold drawing process, and a cold drawing channel is divided into three times.
In the first step, a 12% small-deformation cold-drawing process is adopted, the size deviation of the vertical extruded tube is mainly corrected, and the intermediate tube with high size uniformity is ensured to be obtained. The elongation coefficient (area ratio of the pipe after cold drawing to the pipe before cold drawing) of the cold drawing deformation is 1.14, and the number of cold drawing is 1. After cold drawing deformation, solution heat treatment is carried out, and the heat treatment temperature is 1000 ℃.
And in the second step, a 15% medium-deformation cold-drawing process is adopted, the cold-drawing pass is 1 time, the elongation coefficient of cold-drawing deformation is 1.18, and the cold-drawing process is a main deformation stage of the pipe, so that the change of the appearance size, the full recrystallization of crystal grains and the growth of the crystal grains are realized. After cold drawing deformation, solution heat treatment is carried out, and the heat treatment temperature is 1100 ℃.
In the third step, 21.9% of large deformation is adopted, and the elongation coefficient of cold-drawing deformation is 1.28. And carrying out solution heat treatment after cold drawing deformation, wherein the heat treatment temperature is 1050 ℃. Through deformation and solution heat treatment processes, the full deformation of crystal grains is mainly promoted, and the growth of the crystal grain size of the pipe is controlled by combining the heat treatment process, so that a uniform internal crystal grain structure is obtained. After the stainless steel seamless steel pipe is subjected to final solution heat treatment, the average grain size is 75 micrometers, the grain size level is 4.5 levels, and the grain size level difference is 1.5 levels.
Example 3.
The outer diameter of the large-diameter austenitic stainless steel pipe prepared by the embodiment is in the specification
850mm×15mm×5000mm。
Firstly, smelting a steel ingot by adopting an AOD furnace and slag remelting process, and forging and forming to prepare a billet. The steel billet comprises the following chemical components in percentage by mass: 0.017 of C, 0.235 of Si, 1.03 of Mn, 0.0275 of P, 0.0012 of S, 9.85 of Ni, 19.44 of Cr, 0.015 of Co, 0.0004 of H, 0.009 of B, 0.110 of N and the balance of Fe. The steel billet contains class A nonmetallic inclusion 0, class B nonmetallic inclusion 0.5, class C nonmetallic inclusion 0.5 and class D nonmetallic inclusion 1.0, and the lower nonmetallic inclusion has a beneficial effect on uniform growth of grains.
The billet is prepared into a pierced billet by adopting a vertical hot extrusion process, the temperature of the hot extrusion process is 1200 ℃, and the specification of the extruded tube is
880X 29mm, the extrusion ratio is 15.1, the average grain size of the vertical hot extrusion pierced billet is 120 mu m, and the mother pipe with excellent quality is prepared by the hot extrusion process.
The main manufacturing process comprises the following steps:
the vertical hot extrusion pierced billet adopts a three-step combined cold drawing process, and cold drawing passes are divided into at least three times.
In the first step, a mode of annealing with small deformation of 11.3 percent and the annealing temperature lower than the recrystallization temperature is adopted, the size deviation of the vertical extruded tube is mainly corrected, and the intermediate tube with high size uniformity is ensured to be obtained.
The elongation coefficient (area ratio of the pipe after cold drawing to the pipe before cold drawing) of the cold drawing deformation is 1.13, and the number of cold drawing is 1. And carrying out solution heat treatment after cold drawing deformation, wherein the heat treatment temperature is 925 ℃.
And in the second step, the gradual refinement of the structure is realized by adopting a heat treatment mode of 12.5 percent of medium deformation and higher than recrystallization temperature, the cold drawing pass is 1 time, the elongation coefficient of cold drawing deformation is 1.14, and the method is a main deformation stage of the pipe and realizes the change of the appearance size and the full recrystallization of crystal grains. And carrying out solution heat treatment after cold drawing deformation, wherein the heat treatment temperature is 1020 ℃.
And thirdly, adopting 18.6% of large deformation amount drawing and 1080 ℃ solution heat treatment, wherein the elongation coefficient of cold-drawing deformation is 1.229. And carrying out solution heat treatment after cold drawing deformation, wherein the heat treatment temperature is 1080 ℃. Through deformation and solution heat treatment processes, the full deformation of crystal grains and the full recrystallization of the crystal grains are mainly promoted, and the growth of the crystal grain size of the pipe is controlled by combining the heat treatment process, so that a uniform internal crystal grain structure is obtained. After the stainless steel seamless steel pipe is subjected to final solution heat treatment, the average grain size is 65 micrometers, the grain size level is 5 grades, and the grain size difference is 2 grades.
Example 4.
The outer diameter of the large-diameter austenitic stainless steel pipe prepared by the embodiment is in the specification
813mm×15mm×5000mm。
Firstly, smelting a steel ingot by adopting an AOD furnace and slag remelting process, and forging and forming to prepare a billet. The steel billet comprises the following chemical components in percentage by mass: c0.046, Si 0.312, Mn 1.36, P0.011, S0.001, Ni 12.42, Cr 17.35, Co 0.016, H0.0003, B0.0012, N0.086 and the balance of Fe. The steel billet contains class A nonmetallic inclusion 0, class B nonmetallic inclusion 0.5, class C nonmetallic inclusion 0.5 and class D nonmetallic inclusion 1.0, and the lower nonmetallic inclusion has a beneficial effect on uniform growth of grains.
The billet is prepared into a pierced billet by adopting a vertical hot extrusion process, the temperature of the hot extrusion process is 1250 ℃, and the specification of the extruded tube is
880X 29mm, the extrusion ratio is 3, the average grain size of the vertical hot extrusion pierced billet is 165 mu m, and the mother pipe with excellent quality is prepared by the hot extrusion process.
The main manufacturing process comprises the following steps:
the vertical hot extrusion pierced billet adopts a three-step combined cold drawing process, and cold drawing passes are divided into at least three times.
In the first step, a small deformation amount of 10.8 percent and an annealing mode below the recrystallization temperature are adopted, the size deviation of the vertical extruded tube is mainly corrected, and the intermediate tube with high size uniformity is ensured to be obtained.
The elongation coefficient (area ratio of the pipe after cold drawing to the pipe before cold drawing) of the cold drawing deformation is 1.121, and the number of cold drawing is 1. And carrying out solution heat treatment after cold drawing deformation, wherein the heat treatment temperature is 900 ℃.
And in the second step, 13.6 percent of medium deformation and a heat treatment mode of which the temperature is higher than the recrystallization temperature are adopted to realize gradual refinement of the structure, the cold drawing pass is 1 time, the elongation coefficients of the cold drawing deformation are 1.157 respectively, and the cold drawing deformation is a main deformation stage of the pipe, so that the change of the appearance size and the full recrystallization of crystal grains are realized. And carrying out solution heat treatment after cold drawing deformation, wherein the heat treatment temperature is 1030 ℃.
And the third step adopts 17.6% large deformation drawing and 1060 ℃ solution heat treatment, and the elongation coefficient of cold-drawing deformation is 1.213. After cold drawing deformation, solution heat treatment is carried out, and the heat treatment temperature is 1060 ℃. Through deformation and solution heat treatment processes, the full deformation of crystal grains and the full recrystallization of the crystal grains are mainly promoted, and the growth of the crystal grain size of the pipe is controlled by combining the heat treatment process, so that a uniform internal crystal grain structure is obtained. After the stainless steel seamless steel pipe is subjected to final solution heat treatment, the average grain size is 92 micrometers, the grain size level is 4 levels, and the grain size difference is 2 levels.
Example 5.
The outer diameter of the large-diameter austenitic stainless steel pipe prepared by the embodiment is in the specification
813mm×15mm×5000mm。
Firstly, smelting a steel ingot by adopting an AOD furnace and slag remelting process, and forging and forming to prepare a billet. The steel billet comprises the following chemical components in percentage by mass: 0.036 of C, 0.31 of Si, 1.63 of Mn, 0.012 of P, 0.001 of S, 12.38 of Ni, 17.55 of Cr, 0.012 of Co, 0.0003 of H, 0.0013 of B, 0.065 of N and the balance of Fe. The steel billet contains class A nonmetallic inclusion 0, class B nonmetallic inclusion 0.5, class C nonmetallic inclusion 0.5 and class D nonmetallic inclusion 1.0, and the lower nonmetallic inclusion has a beneficial effect on uniform growth of grains.
The billet is prepared into a pierced billet by adopting a vertical hot extrusion process, the temperature of the hot extrusion process is 1250 ℃, and the specification of the extruded tube is
880X 29mm, the extrusion ratio is 10.2, the average grain size of the vertical hot extrusion pierced billet is 125 mu m, and the mother pipe with excellent quality is prepared by the hot extrusion process.
The main manufacturing process comprises the following steps:
the vertical hot extrusion pierced billet adopts a three-step combined cold drawing process, and cold drawing passes are divided into at least three times.
In the first step, 8.1% of small deformation and annealing below the recrystallization temperature are adopted, the size deviation of the vertical extruded tube is mainly corrected, and the intermediate tube with high size uniformity is ensured to be obtained.
The elongation coefficient (area ratio of the pipe after cold drawing to the pipe before cold drawing) of the cold drawing deformation is 1.088, and the number of cold drawing is 1. And carrying out solution heat treatment after cold drawing deformation, wherein the heat treatment temperature is 950 ℃.
In the second step, the gradual refinement of the structure is realized by adopting a heat treatment mode of 14.3 percent of medium deformation and higher than recrystallization temperature, the elongation coefficients of cold-drawing deformation are respectively 1.167, and the cold-drawing deformation is a main deformation stage of the pipe, so that the change of the appearance size and the full recrystallization of crystal grains are realized. And carrying out solution heat treatment after cold drawing deformation, wherein the heat treatment temperature is 1080 ℃.
And thirdly, adopting 17.2% of large deformation amount drawing and 1050 ℃ solution heat treatment, wherein the elongation coefficient of cold-drawing deformation is 1.208. And carrying out solution heat treatment after cold drawing deformation, wherein the heat treatment temperature is 1050 ℃. Through deformation and solution heat treatment processes, the full deformation of crystal grains and the full recrystallization of the crystal grains are mainly promoted, and the growth of the crystal grain size of the pipe is controlled by combining the heat treatment process, so that a uniform internal crystal grain structure is obtained. After the stainless steel seamless steel pipe is subjected to final solution heat treatment, the average grain size is 75 micrometers, the grain size level is 4.5 levels, and the grain size level difference is 1.5 levels.
Meanwhile, the invention also adopts a variable control method, and controls the parameters in the implementation step on the basis of the embodiment 1 to obtain comparative examples 1-5.
The method comprises the following specific steps:
comparative example 1
Comparative example 1 is different from example 1 in that comparative example 1 has a solution heat treatment temperature of 850 c after cold drawing with a small deformation amount, and the remaining conditions are the same as example 1.
The average grain size of the finally obtained stainless steel seamless steel pipe is 85 micrometers, the grain size level is 4 grades, and the grain size difference is 4 grades.
Comparative example 2
Comparative example 2 is different from example 1 in that comparative example 2 has a solution heat treatment temperature of 1050 c after cold drawing with a small deformation amount, and the remaining conditions are the same as example 1.
The average grain size of the finally obtained stainless steel seamless steel pipe is 108 mu m, the grain size grade is 3.5 grade, and the grain size grade difference is 3 grade.
Comparative example 3
Comparative example 3 is different from example 1 in that comparative example 3 has deformation amounts of 8% and 10.5% in the second and third steps, and the remaining conditions are the same as example 1.
The average grain size of the finally obtained stainless steel seamless steel pipe is 105 mu m, the grain size grade is 3.5 grade, and the grain size grade difference is 2 grade.
Comparative example 4
Comparative example 4 is different from example 1 in that comparative example 4 has the same conditions as example 1 except that the temperature of the solution heat treatment after the medium deformation amount cold drawing is 1000 ℃.
The average grain size of the finally obtained stainless steel seamless steel pipe is 90 mu m, the grain size grade is 3 grades, and the grain size grade difference is 4 grades.
Comparative example 5
Comparative example 5 is different from example 1 in that comparative example 5 has a solution heat treatment temperature of 1150 ℃ after cold drawing with a small deformation amount, and the remaining conditions are the same as example 1.
The average grain size of the finally obtained stainless steel seamless steel pipe is 110 mu m, the grain size grade is 3.5 grade, and the grain size grade difference is 2 grade.
[ data analysis ]
(1) Influence of parameter change on performance of stainless steel seamless steel tube in small-deformation cold drawing process
Comparing example 1 with comparative example 1, we found that, under the same remaining conditions, after cold drawing deformation with a small deformation amount, when the solution heat treatment temperature is low, uneven deformation generated during cold drawing is hard to recover, thus resulting in a decrease in uniformity of the grain structure.
Comparing example 1 with comparative example 2, we found that under the same conditions, when the solution heat treatment temperature is higher than the recrystallization temperature after cold drawing with small deformation, the average grain size of the seamless steel pipe is abnormally increased, and the grain size difference is correspondingly increased.
Therefore, it was shown that the solution heat treatment after the cold drawing treatment with a small deformation amount has a significant influence on the size and dimensional stability of crystal grains in the final seamless steel pipe. After cold drawing with 8-12% of deformation, the grain size and the uniformity of the grain size can be obviously improved by adopting solution heat treatment at 900-1020 ℃.
(2) Influence of parameter change on performance of stainless steel seamless steel tube in medium-deformation cold drawing process
Comparing example 1 with comparative example 3, we found that, under the same remaining conditions, when the deformation amount in this step is small, the effect of crushing and refining the crystal grains is poor, resulting in a larger size of the crystal grains inside the finally obtained seamless steel pipe.
In contrast, comparative examples 4 and 5 discuss the influence of the use of too low and too high solution heat treatment temperatures on the final seamless steel pipe after cold drawing with the same medium deformation amount, respectively. We have found that when the solution heat treatment temperature is lower than the recrystallization temperature, the recrystallization step can not be performed after the crystal grains are crushed, and the grain size difference is greatly increased. When the solution heat treatment temperature is much higher than the recrystallization temperature, the grain size difference is small, but the grain size is large. Therefore, after cold drawing with medium deformation, the balance of grain size and grain size uniformity can be ensured when the temperature of the solution heat treatment is in the range of 1020-1100 ℃.
Therefore, the invention adopts a mode of combining different deformation amounts with heat treatment to enable the grain structure in the stainless steel seamless pipe to have the effects of refining and uniformly distributing, and finally realizes a uniform structure with the grain size of 4-6 grade and the grade difference less than 2 grade. Meanwhile, the large-caliber stainless steel seamless steel pipe with the uniformly distributed grain structures, the outer diameter of the pipe being larger than 800mm and the wall thickness being larger than 10mm can be manufactured by adopting the manufacturing process, and the large-caliber stainless steel seamless steel pipe can be used for a main pipeline system of an advanced nuclear power station.
Claims (10)
1. The preparation method of the stainless steel seamless pipe is characterized by comprising the following steps of:
(S.1) carrying out cold drawing on the pierced billet by a deformation amount smaller than 12%, and carrying out solution heat treatment under the condition of being lower than the recrystallization temperature after the cold drawing is finished to obtain an intermediate pipe with high size uniformity;
(S.2) carrying out cold drawing on the intermediate pipe by the deformation of 12-15%, and carrying out solution heat treatment under the condition that the temperature is higher than the recrystallization temperature after the cold drawing is finished to obtain the intermediate pipe with a refined structure;
(S.3) cold-drawing the intermediate pipe with refined structure by using the deformation amount of more than 15%, and after the cold-drawing is finished, carrying out solution heat treatment under the condition of higher than recrystallization temperature to obtain the stainless steel seamless pipe with uniform internal grain structure size.
2. The method of producing a stainless steel seamless tube according to claim 1,
the temperature of the solution heat treatment in the step (S.1) is 900-1020 ℃.
3. The method of producing a stainless steel seamless tube according to claim 1,
the temperature of the solution heat treatment in the step (S.2) is 1020-1100 ℃.
4. The method of producing a stainless steel seamless tube according to claim 1,
the temperature of the solution heat treatment in the step (S.3) is 1050-1080 ℃.
5. The method of producing a stainless steel seamless pipe according to any one of claims 1 to 4,
before cold drawing, the pierced billet and the intermediate pipe are polished and acid-washed, and after the treatment, the surfaces of the pierced billet and the intermediate pipe are coated with butter lime and graphite.
6. The method of producing a stainless steel seamless tube according to claim 1 or 2,
in the step (S.1), the pierced billet is prepared from a billet by a vertical hot extrusion process;
in the hot extrusion process, the extrusion ratio is 3-15, the extrusion heating temperature is 1200-1250 ℃, and the average grain size of the pierced billet obtained after hot extrusion is less than or equal to 180 mu m.
7. The method of producing a stainless steel seamless tube according to claim 6,
the billet used for preparing the pierced billet is subjected to at least one secondary remelting process during smelting;
after the secondary remelting process, the level contents of D-type punctiform inclusions and B-type chain-shaped inclusions in the steel billet are respectively not more than 1.5 level and 1.0 level.
8. A stainless steel seamless tube is characterized in that,
the stainless steel seamless pipe is prepared by the method of any one of claims 1 to 7;
the outer diameter of the stainless steel seamless pipe is more than or equal to 600mm, and the wall thickness is less than 20 mm;
the grain size of a grain structure in the stainless steel seamless pipe is 4-6 grades, and the grain size range is less than 2.
9. A stainless steel seamless tube according to claim 8,
the stainless steel seamless pipe is an austenitic stainless steel pipe.
10. Use of a stainless steel seamless tube according to claim 8 or 9 in a nuclear power plant main piping system.
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| CN114934163A (en) * | 2022-04-02 | 2022-08-23 | 常州市联谊特种不锈钢管有限公司 | Manufacturing method of ultralow-carbon austenitic stainless steel thin-wall seamless pipe suitable for manufacturing clamping sleeve |
| CN115505707A (en) * | 2022-09-22 | 2022-12-23 | 内蒙古北方重工业集团有限公司 | Grain size refinement manufacturing method of large-caliber TP316H stainless steel seamless steel pipe |
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