CN110724809B - Method for controlling grain size uniformity of hot-rolled high-carbon austenitic stainless steel - Google Patents

Method for controlling grain size uniformity of hot-rolled high-carbon austenitic stainless steel Download PDF

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CN110724809B
CN110724809B CN201911126633.6A CN201911126633A CN110724809B CN 110724809 B CN110724809 B CN 110724809B CN 201911126633 A CN201911126633 A CN 201911126633A CN 110724809 B CN110724809 B CN 110724809B
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刘振宇
王志国
高飞
李健
陈俊
李成刚
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Northeastern University China
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    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
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    • C21DMODIFYING 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
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18Hardening; Quenching with or without subsequent tempering
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/78Combined heat-treatments not provided for above
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
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Abstract

A method for controlling the grain size uniformity of hot-rolled high-carbon austenitic stainless steel comprises the following steps: (1) preparing a high-carbon austenitic stainless steel hot-rolled medium plate; (2) preheating at 900-920 ℃ in a heating furnace for t1 ═ 0.4-0.6 h; (3) heating the preheating plate to 1000-1010 ℃ along with the furnace for recrystallization; or taking out the plate and slowly cooling the plate, heating the heating furnace to 1000-1010 ℃, and then placing the preheating plate in the heating furnace for recrystallization; (4) heating the recrystallized slab along with a furnace to 50-100 ℃ for solution treatment; or taking out the plate and slowly cooling the plate, heating the heating furnace to 50-90 ℃, and then putting the recrystallized plate in the heating furnace for solution treatment; (5) and water quenching the solid solution plate to normal temperature. The method takes recrystallization kinetics and thermodynamics as the force points, adopts the multi-stage stepped annealing process to gradually release the deformation energy storage, obtains the medium-thickness steel plate with uniform crystal grains and adjustable crystal grain size, has strong operability, and can realize industrial application.

Description

Method for controlling grain size uniformity of hot-rolled high-carbon austenitic stainless steel
Technical Field
The invention belongs to the technical field of steel alloy materials, and particularly relates to a method for controlling grain size uniformity of hot-rolled high-carbon austenitic stainless steel.
Background
In the austenitic stainless steel with special requirements, such as the austenitic stainless steel for nuclear power fast reactor, the austenitic stainless steel is in service for a long time in a severe high-temperature environment, the requirement on the structure is high, a stable austenitic structure is obtained, and the austenitic stainless steel needs good mechanical property and high-temperature property, and more C elements are generally added; high-carbon (C content is improved by about one time compared with the conventional method) austenitic stainless steel generally has a stable single-phase austenitic structure, and the grain size and uniformity can only be regulated and controlled through recrystallization; however, due to the characteristics of sensitive diffusion of C along with temperature change and high alloy components, obvious recrystallization difference can be caused in the hot rolling process, particularly for medium and heavy plates, the special property of deformation distribution difference can promote the difference of dynamic recrystallization or dynamic recovery in the thickness direction of the plate, a structure with uneven rolling state is formed, mixed crystals can be easily caused during annealing, and the mechanical property and the corrosion resistance are deteriorated.
In the traditional medium plate hot rolling process, high-temperature continuous high-reduction hot rolling is generally adopted, the final rolling temperature is more than or equal to 900 ℃, and natural cooling is adopted after rolling; however, for high carbon stainless steel, because the deformation temperature in the thickness direction of the plate blank is different and the deformation distribution is greatly different, dynamic recrystallization and dynamic recovery degrees at different positions are different, and meanwhile, partial static recrystallization or carbide precipitation occurs in the cooling process after rolling, so that the structures at different positions of the plate thickness are not uniform; if an uneven structure is formed in the hot rolling process, during subsequent heat treatment, static recrystallization and different grain growth rates are caused due to the difference of deformation energy storage distribution, grain boundaries are mutually swallowed, mixed crystals are caused, the high-temperature strength and the fatigue performance of the material are greatly deteriorated by the mixed crystals, and the problem that the mixed crystals are very difficult to form in a high-carbon stainless steel medium plate with higher performance requirements is solved.
Therefore, related personnel greatly improve the hot rolling process; patent CN101724789A discloses a hot rolling process for medium and heavy plates, which adopts two stages, namely, a mode of gradually deforming from big to small in a recrystallization zone and a non-grain boundary zone respectively, and then carrying out solid solution at a certain temperature; but mainly focuses on the change of the mechanical property of the material, the problem of uniform structure in the hot rolling state and the full thickness direction after solid solution is not discussed, and the adopted material is mainly low-carbon stainless steel, and the comparative example is also low-carbon austenitic stainless steel; in addition, patent CN101748342 discloses a manufacturing method of a high-strength 18Cr-8Ni stainless steel hot-rolled medium plate, which mainly adopts a high-temperature continuous hot rolling and an online solid solution mode, and similarly, the manufacturing method also mainly focuses on the mechanical properties of the material, and does not consider the deformation behavior and the structure condition of the stainless steel in the full thickness direction; therefore, for stainless steel which is high in carbon and needs to be used in a severe environment, the solid solution process or annealing process should be controlled more intensively while considering the hot rolling process, because the final delivery is in a solid solution state, and the rolled structure needs to be adjusted by the static recrystallization and grain growth process.
Disclosure of Invention
Aiming at the problems in the preparation technology of the hot-rolled high-carbon stainless steel medium plate, the invention provides a method for controlling the grain size uniformity of hot-rolled high-carbon austenitic stainless steel, and uneven deformation energy storage is regulated and controlled by improving the process. Synchronous recrystallization nucleation occurs at a lower temperature, the required grain size is achieved through high-temperature short-time solid solution,
the method of the invention is carried out according to the following steps:
1. preparing a high-carbon austenitic stainless steel hot-rolled medium plate; the high-carbon austenitic stainless steel hot-rolled medium plate contains 0.04-0.1% of C by mass percent, and the thickness is more than or equal to 10 mm;
2. placing a high-carbon austenitic stainless steel hot-rolled medium plate in a heating furnace, preheating at 900-920 ℃, wherein the preheating time t1 is (0.4-0.6) h, and obtaining a preheating plate; wherein h is the thickness of the high-carbon stainless steel hot-rolled medium plate, and the unit is mm; the unit of t1 is min;
3. heating the preheating plate to 1000-1010 ℃ along with the furnace for recrystallization; or taking out the preheating plate, placing the preheating plate in a slow cooling environment, heating the heating furnace to 1000-1010 ℃ under the condition that the cooling speed is less than or equal to 5 ℃/min, and then placing the preheating plate in the heating furnace for recrystallization; recrystallizing for 0.6-1.2 h to obtain a recrystallized plate; wherein t2 is in units of min;
4. heating the recrystallized slab along with a furnace to 50-100 ℃ for solution treatment; or taking out the recrystallized slab, placing the recrystallized slab in a slow cooling environment, heating the heating furnace to 50-100 ℃ under the condition that the cooling speed is less than or equal to 5 ℃/min, and then placing the recrystallized slab in the heating furnace for solution treatment; the solution treatment time t3 is (0.4-1.0) h, and then a solution plate is obtained; wherein t3 is in units of min;
5. and water quenching the solid solution plate to normal temperature to prepare the high-carbon austenitic stainless steel plate with uniform grain size after the solid solution treatment.
In the step 3, when the preheating plate is heated along with the furnace, the heating speed is controlled to be less than or equal to 5 ℃/min.
In the step 4, when the temperature of the recrystallization plate rises along with the furnace, the temperature rising speed is controlled to be less than or equal to 5 ℃/min.
In the step 3, when the preheating plate is taken out and placed in a slow cooling environment, the cooling time of the preheating plate is controlled to be less than or equal to 20 min.
In the step 4, when the recrystallized slab is taken out and placed in a slow cooling environment, the cooling time of the recrystallized slab is controlled to be less than or equal to 20 min.
The grain size of the austenitic stainless steel plate is 45-90 mu m, and the grain size difference of different positions in the thickness direction is less than or equal to 8 mu m.
The main idea of the invention is to avoid directly giving larger driving force to the rolling state uneven structure, prevent the inconsistency of nucleation mode and grain growth rate of the structures in different states caused by the difference of recrystallization thermodynamics/kinetics, and gradually release the deformation energy storage in stages; the low-temperature preheating section mainly has the main function of homogenizing deformation energy storage among adjacent crystal grains through recovery or partial precipitation, and the stage is mainly used for regulating and controlling the nonuniform deformation energy storage; then, synchronous recrystallization nucleation occurs at a lower temperature, and the lower temperature recrystallization nucleation is adopted to mainly prevent abnormal growth of dynamically recrystallized grains in a hot rolling state and abnormal growth of formed subgrain; on the basis, the required grain size is achieved through high-temperature short-time solid solution, and in the stage, grains grow up at the same rate or secondary recrystallization occurs at the same rate; meanwhile, the temperature rise or slow cooling along with the furnace is adopted between the stages to prevent the generation of thermal stress in the repeated heating process and influence on the local recrystallization behavior.
The invention has the advantages that:
1. creatively provides an idea of staged and gradual release of deformation energy storage, takes the joint adjustment of recrystallization thermodynamics and kinetics as a starting point, separately carries out the reversion of a deformed tissue, recrystallization nucleation and grain growth, and prevents different static recrystallization rates of tissues in different states from being mutually swallowed under the condition of higher temperature;
2. considering the diffusion problem of the element C in the stainless steel, the deformation energy storage is adjusted by means of the whole process of recovery, precipitation and recrystallization nucleation, thereby not only avoiding carbide precipitation caused by low-temperature solid solution, but also avoiding abnormal growth of crystal grains caused by high-temperature solid solution, and providing a specific process route, having strong operability and realizing industrial application;
3. the influence of thermal stress on recrystallization in the repeated heating process is considered, and external influence factors are avoided by adopting a mode of furnace temperature rise or slow cooling.
Drawings
FIG. 1 is a microstructure diagram of a high carbon austenitic stainless steel hot rolled medium plate and a high carbon austenitic stainless steel plate after solution treatment at different positions in the thickness direction in examples 1 and 2 of the present invention; in the figure, (a), (b) and (c) are high carbon austenitic stainless steel hot rolled medium plates, (d), (e) and (f) are example 1, and (g), (h) and (i) are example 2; (a) (d) and (g) are skin layers, (b), (e) and (h) are taken from the skin layers to the total thickness 1/4, (c), (f) and (i) are central parts;
FIG. 2 is a microstructure diagram of a hot-rolled medium plate of a high carbon austenitic stainless steel and a high carbon austenitic stainless steel plate after solution treatment in different positions in the thickness direction in example 3 of the present invention; in the figure, (a), (b) and (c) are high carbon austenitic stainless steel hot rolled medium plates, (d), (e) and (f) are example 3; (a) and (d) is a skin layer, (b) and (e) are taken to be 1/4 total thickness from the skin layer, (c) and (f) are central parts;
FIG. 3 is a microstructure diagram of high carbon austenitic stainless steel sheets after solution treatment according to comparative examples 1 to 3 of the present invention at different positions in the thickness direction; in the figure, (a), (b) and (c) are comparative examples 1, (d), (e) and (f) are comparative examples 2, and (g), (h) and (i) are comparative examples 3; (a) the skin layers, (b), (e) and (h) are at total thickness 1/4 from the skin layers, and (c), (f) and (i) are the center.
Detailed Description
The grade and the components of the steel treated in the embodiment of the invention adopt the standard GB/T4238-2015.
The high-carbon austenitic stainless steel hot-rolled medium plate has a thickness of 10-100 mm.
In the embodiment of the invention, the solution treatment adopts a box-type resistance furnace, and finally the steel is water-quenched to room temperature after being taken out of the furnace.
In the embodiment of the invention, the solid solution plate is randomly sampled in the full thickness direction, and after sand paper grinding, mechanical polishing and electrolytic corrosion, an OLYMPUS metallographic microscope is adopted to observe the structure and count the grain size, according to the standard GB/T6394-.
Example 1
The mark of a high-carbon austenitic stainless steel hot-rolled medium plate is 07Cr17Ni12Mo2, the uniform code is S31609, the high-carbon austenitic stainless steel hot-rolled medium plate contains 0.04-0.1 wt% of C according to mass percent, the thickness is 70mm, and microstructures at different positions in the thickness direction are shown in figures 1(a), (b) and (C);
placing a high-carbon austenitic stainless steel hot-rolled medium plate in a heating furnace, preheating at 900 ℃ for 35min after t1 is 0.5h, and obtaining a preheating plate;
heating the preheating plate to 1000 ℃ along with the furnace for recrystallization, and controlling the heating speed to be 1-5 ℃/min; recrystallizing for 42min at t 2h 0.6h to obtain a recrystallized slab;
heating the recrystallized slab along with a furnace to 50 ℃ for solution treatment, and controlling the heating speed to be 1-5 ℃/min; the solution treatment time t3 is 0.4h 8min, and then a solid solution plate is obtained;
the solid solution plate is water-quenched to normal temperature to prepare a solid solution treated high-carbon austenitic stainless steel plate with uniform grain size, the microstructure is shown in figures 1(d), (e) and (f), and the average grain sizes of the surface layer, the quarter part and the core part are respectively as follows: 70 μm, 73 μm and 68 μm.
Example 2
The raw materials and the method are different from those in example 1 in that:
(1) taking out the preheating plate, wrapping the preheating plate with asbestos, heating the heating furnace to 1000 ℃, and then placing the preheating plate in the heating furnace for recrystallization; when the asbestos is wrapped, the cooling speed of the preheating plate is controlled to be 1-5 ℃/min, and the wrapping time of the preheating plate in the asbestos is less than or equal to 20 min;
(2) taking out the recrystallized slab, wrapping the recrystallized slab with asbestos, heating a heating furnace to 50-90 ℃, and placing the recrystallized slab in the heating furnace for solution treatment; controlling the cooling speed of the recrystallization plate to be 1-5 ℃/min when the asbestos is wrapped, and the wrapping time of the recrystallization plate in the asbestos is less than or equal to 20 min;
(3) the microstructure of the high carbon austenitic stainless steel sheet after the solution treatment is shown in fig. 1(g), (h) and (i), and the average grain sizes of the surface layer, the quarter and the core are respectively: 85 μm, 83 μm and 78 μm.
Example 3
The high-carbon austenitic stainless steel hot-rolled medium plate is adopted, the mark is 06Cr25Ni20, the uniform code is S31008, the microstructure comprises 0.08 percent of C according to the mass percent, the thickness is 50mm, and the microstructure at different positions in the thickness direction is shown in figures 2(a), (b) and (C);
the method is the same as example 1, except that:
(1) preheating at 920 ℃ for 20min at t 1;
(2) the recrystallization temperature is 1010 ℃, and the time t2 is 0.8 h-40 min;
(3) heating the recrystallized slab along with a furnace to 70 ℃ for solution treatment; the solution treatment time t3 is 0.6h and 30 min;
(4) the microstructure of the high carbon austenitic stainless steel sheet after the solution treatment is shown in fig. 2(d), (e) and (f), and the average grain sizes of the surface layer, the quarter and the core are respectively: 85 μm, 83 μm and 82 μm.
Example 4
The raw materials and the method are different from those in example 3 in that:
(1) the preheating temperature is 900 ℃;
(2) taking out the preheating plate, wrapping the preheating plate with asbestos, heating the heating furnace to 1000 ℃, and then placing the preheating plate in the heating furnace for recrystallization; controlling the cooling speed of the preheating plate to be 1-5 ℃/min when the asbestos is wrapped, and meanwhile, the wrapping time of the preheating plate in the asbestos is less than or equal to 20 min;
(3) taking out the recrystallized slab, wrapping the recrystallized slab with asbestos, heating a heating furnace to 50 ℃, and placing the recrystallized slab in the heating furnace for solution treatment; controlling the cooling speed of the recrystallization plate to be 1-5 ℃/min when the asbestos is wrapped; meanwhile, the wrapping time of the recrystallization plate in the asbestos is less than or equal to 20 min;
(4) the average grain sizes of the surface layer, the quarter part and the center part of the high-carbon austenitic stainless steel plate after solution treatment are respectively as follows: 88 μm, 85 μm and 85 μm.
Example 5
The high-carbon austenitic stainless steel hot-rolled medium plate is 07Cr19Ni10, the uniform code S30409 contains 0.04-0.1% of C by mass percent, and the thickness is 10 mm;
the method is the same as example 1, except that:
(1) preheating time t1 is 0.6h and 6 min;
(2) the recrystallization treatment time t2 is 1.2h 12 min;
(3) heating the recrystallized slab along with a furnace to 100 ℃ for solution treatment; the solution treatment time t3 is 1.0h and 10 min;
(4) the average grain sizes of the surface layer, the quarter part and the center part of the high-carbon austenitic stainless steel plate after solution treatment are respectively as follows: 48 μm, 48 μm and 45 μm.
Example 6
The raw materials and the method are the same as the example 5, and the differences are that:
(1) taking out the preheating plate, wrapping the preheating plate with asbestos, heating the heating furnace to 1000 ℃, and then placing the preheating plate in the heating furnace for recrystallization; controlling the cooling speed of the preheating plate to be 1-5 ℃/min; meanwhile, the wrapping time of the preheating plate in the asbestos is less than or equal to 20 min;
(2) taking out the recrystallized slab, wrapping the recrystallized slab with asbestos, heating a heating furnace to 100 ℃, and placing the recrystallized slab in the heating furnace for solution treatment; controlling the cooling speed of the recrystallization plate to be 1-5 ℃/min; meanwhile, the wrapping time of the recrystallization plate in the asbestos is less than or equal to 20 min;
(3) the average grain sizes of the surface layer, the quarter part and the center part of the high-carbon austenitic stainless steel plate after solution treatment are respectively as follows: 50 μm, 48 μm and 48 μm.
Comparative example 1
The raw materials and the method of example 1 are different in that: directly heating to 1050 ℃ along with a furnace without preheating and recrystallization treatment for solid solution treatment for 60min (namely t is more than 0.6 h);
the microstructure of the product is shown in fig. 3(a), (b) and (c), and the average grain sizes of the surface layer, the quarter part and the core part are respectively as follows: 120 μm, 95 μm and 112 μm, and the steel plate has obvious mixed crystals at the same thickness position.
Comparative example 2
The raw materials and the method are different from those in example 1 in that: directly heating the preheating plate to 1050 ℃ along with a furnace without recrystallization treatment for solution treatment for 28 min;
the microstructure of the product is shown in fig. 3(d), (e) and (f), and the average grain sizes of the surface layer, the quarter part and the core part are respectively as follows: 82 μm, 70 μm and 68 μm, and the steel plate has obvious mixed crystals at the same thickness position.
Comparative example 3
The raw materials and the method are different from those in example 1 in that: the preheating plate is heated to 950 ℃ along with the furnace, then the temperature is kept for 28min (namely secondary preheating is carried out at different temperatures), and then recrystallization treatment and solid solution treatment are carried out;
the solid solution microstructure is shown in FIGS. 3(g), (h) and (i), and the average grain sizes of the surface layer, the quarter part and the core part are respectively: 110 μm, 85 μm and 58 μm, and the steel plate has obvious mixed crystals at the same thickness position.
The features and effects of the present invention are described in more detail by the examples and comparative examples, but the present invention is not limited to these examples, and other equivalent examples, such as other steel grades or other corresponding staged heat treatment processes, can be adopted without departing from the concept of the present invention.

Claims (3)

1. A method for controlling the grain size uniformity of hot-rolled high-carbon austenitic stainless steel is characterized by comprising the following steps:
(1) preparing a high-carbon austenitic stainless steel hot-rolled medium plate; the high-carbon austenitic stainless steel hot-rolled medium plate contains 0.04-0.1% of C by mass percent, and the thickness is more than or equal to 10 mm;
(2) placing a high-carbon austenitic stainless steel hot-rolled medium plate in a heating furnace, preheating at 900-920 ℃, wherein the preheating time t1= (0.4-0.6) h, and obtaining a preheating plate; wherein h is the thickness of the high-carbon stainless steel hot-rolled medium plate, and the unit is mm; the unit of t1 is min;
(3) heating the preheating plate to 1000-1010 ℃ along with the furnace for recrystallization; or taking out the preheating plate, placing the preheating plate in a slow cooling environment, heating the heating furnace to 1000-1010 ℃ under the condition that the cooling speed is less than or equal to 5 ℃/min, and then placing the preheating plate in the heating furnace for recrystallization; recrystallizing for t2= (0.6-1.2) h, and then obtaining a recrystallized board; wherein t2 is in units of min; when the preheating plate is taken out and placed in a slow cooling environment, the cooling time of the preheating plate is controlled to be less than or equal to 20 min;
(4) heating the recrystallized slab along with a furnace to 50-100 ℃ for solution treatment; or taking out the recrystallized slab, placing the recrystallized slab in a slow cooling environment, heating the heating furnace to 50-100 ℃ under the condition that the cooling speed is less than or equal to 5 ℃/min, and then placing the recrystallized slab in the heating furnace for solution treatment; the solution treatment time t3= (0.4-1.0) h, and then obtaining a solid solution plate; wherein t3 is in units of min; when the recrystallized plate is taken out and placed in a slow cooling environment, the cooling time of the recrystallized plate is controlled to be less than or equal to 20 min;
(5) water quenching the solid solution plate to normal temperature to prepare a solid solution treated high-carbon austenitic stainless steel plate with uniform grain size; the grain size of the austenitic stainless steel plate is 45-90 mu m, and the grain size difference of different positions in the thickness direction is less than or equal to 8 mu m.
2. The method for controlling the grain size uniformity of the hot-rolled high-carbon austenitic stainless steel as claimed in claim 1, wherein in the step (3), the temperature rising speed is controlled to be less than or equal to 5 ℃/min when the preheating plate is heated along with the furnace.
3. The method of claim 1, wherein in the step (4), the temperature of the recrystallized slab is raised with the furnace at a rate of 5 ℃/min or less.
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CN111549276A (en) * 2020-05-06 2020-08-18 山西太钢不锈钢股份有限公司 Grain size control method for high-carbon austenitic stainless steel medium plate
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