CN111139347B - Method for rapidly refining metastable austenite grain structure - Google Patents

Method for rapidly refining metastable austenite grain structure Download PDF

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CN111139347B
CN111139347B CN202010055323.6A CN202010055323A CN111139347B CN 111139347 B CN111139347 B CN 111139347B CN 202010055323 A CN202010055323 A CN 202010055323A CN 111139347 B CN111139347 B CN 111139347B
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rolling
temperature
deformation
rapidly
metastable austenite
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CN111139347A (en
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史金涛
张辉平
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Henan Dundao Intelligent Technology Co ltd
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Huanghe Science and Technology College
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    • 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0221Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
    • C21D8/0236Cold rolling
    • 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
    • C21D1/18Hardening; 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
    • C21D1/26Methods of annealing
    • 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
    • C21D1/74Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • 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
    • C21D1/74Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/773Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
    • 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
    • C21D6/00Heat treatment of ferrous alloys
    • C21D6/04Hardening by cooling below 0 degrees Celsius
    • 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
    • C21D2211/00Microstructure comprising significant phases
    • C21D2211/001Austenite
    • 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
    • C21D2211/00Microstructure comprising significant phases
    • C21D2211/008Martensite

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Heat Treatment Of Sheet Steel (AREA)
  • Heat Treatment Of Steel (AREA)

Abstract

The invention relates to the field of metal material processing, in particular to a method for quickly refining metastable austenite grain structure, which can realize the refinement of metastable austenite grain, quickly improve the mechanical property and the processing deformation characteristic of original steel, and belongs to the field of metal material processing. Finally obtaining the austenite structure with refined grains.

Description

Method for rapidly refining metastable austenite grain structure
Technical Field
The invention relates to the field of metal material processing, in particular to a method for quickly refining metastable austenite grain structure, which can realize metastable austenite grain refinement and quickly improve the mechanical property and the processing deformation characteristic of original steel, and belongs to the field of metal material processing.
Background
The austenitic stainless steel becomes an important engineering material in modern industry due to excellent corrosion resistance and formability, but the strength and hardness of the austenitic stainless steel are low, and the product is easy to scratch, wear or yield deformation to cause failure, so that the quality and the service life of the product are reduced.
For stainless steel, the strengthening effect is achieved mainly through processing strengthening and fine grain strengthening, and particularly for steel types which can generate deformation induced martensite transformation, the purpose of fine grain can be achieved through deformation induced martensite. Therefore, the current method for strengthening the stainless steel is realized by plastic deformation, but the efficiency of the traditional plastic deformation method for generating processing strengthening or deformation induced phase transformation to form fine grain strengthening is low. Under the current conditions of energy crisis and environmental crisis, a method for rapidly generating processing strengthening and deformation induced martensite refined grains needs to be found.
Disclosure of Invention
In view of the above situation, the present invention provides a method for rapidly refining metastable austenite grain structure, which aims to solve the problem of low efficiency of the traditional plastic deformation method for producing processing strengthening or deformation induced phase transformation to form fine grain strengthening, and provides a method for rapidly processing strengthening, rapidly producing deformation induced martensite, and refining grains to achieve fine grain strengthening.
The technical scheme is that the method comprises the following steps:
step 1: adopting a casting blank or hot rolled slab steel capable of generating deformation induced martensite as an initial material, and carrying out solution quenching or annealing treatment on the casting blank or the hot rolled blank;
step 1: carrying out surface milling on the casting blank or the hot rolling blank obtained in the step (1), and then carrying out multi-pass rapid rolling processing on the milled casting blank or the milled hot rolling plate blank;
step 3, placing the casting blank or the hot rolled slab processed in the step 2 into a low-temperature or ultralow-temperature cooling pretreatment medium for processing;
and 4, step 4: performing multi-pass rolling processing on the plate treated in the step 3, and performing low-temperature or ultralow-temperature cooling pretreatment on the casting blank or the hot rolled plate blank before each pass of rolling;
and 5: and (4) annealing the material treated in the step (4) by vacuum heat treatment.
In the above or some embodiments, the annealing temperature in step 1 is 800 ℃ to 1200 ℃ and the holding time is 1 to 8 hours.
In the above or some embodiments, the rapid rolling in the step 2 adopts cold rolling or hot rolling for multi-pass rapid rolling processing, and the rolling deformation is 20% -95%.
In the above or some embodiments, the casting blank or the hot rolled slab is placed in a low-temperature or ultra-low-temperature cooling pretreatment medium for treatment for 1-60 minutes for standby, wherein the temperature of the cooling pretreatment medium is-196 ℃ to-30 ℃.
In the above or some embodiments, in step 4, the plate before each rolling pass is treated in the low-temperature or ultralow-temperature cooling pretreatment medium for 1 to 5 minutes to obtain the steel material capable of rapidly promoting the martensitic transformation, wherein the deformation amount of each rolling pass in the rolling process is 2 to 10 percent.
In the above or some embodiments, the heat treatment temperature in the step 4 is 500-1200 ℃ for 1-20 minutes.
In the above or some embodiments, in step 1, the heat treatment of the cast or hot rolled slab should be vacuum treatment or protective atmosphere treatment.
In the above or some embodiments, in step 2, the cold rolling and the hot rolling may be performed rapidly, and the deformation may be stopped with a residual amount of 5% to 10% of the total deformation.
In the above or some embodiments, in step 3, the cooling pretreatment medium is liquid nitrogen or a liquid nitrogen-alcohol mixture, a liquid nitrogen-acetone mixture.
In the above or some embodiments, the material after being rolled at the ultra-low temperature in step 5 is placed in a vacuum heat treatment furnace to be subjected to recrystallization annealing treatment.
The method provided by the invention has the advantages that the diffusion and migration capacity of atoms in the material is obviously reduced and the deformation heat generated in the rolling deformation process is quickly consumed mainly through the low-temperature effect of the ultralow-temperature environment, so that the generation of dynamic recovery or recrystallization in the rolling process is effectively inhibited, the deformation defects such as dislocation, dislocation cells/walls, substructures and the like are continuously accumulated to reach higher density while the structure is obviously refined, meanwhile, the low-temperature effect can more quickly accelerate the transformation of metastable austenitic stainless steel into martensite, the grain structure of the martensite is finer, and fine martensite grains are utilized for annealing treatment to finally obtain the grain-refined austenitic structure.
In addition, the invention is different from the traditional cold rolling and hot rolling and the current more advanced ultra-low temperature rolling. The invention discloses a Chinese patent, a processing method for obviously improving the deformability and mechanical property of a high-strength aluminum alloy, wherein the patent publication numbers are CN103343306A and a method for rapidly promoting deformation to induce martensite transformation, the patent publication number is CN105177259A, and the ' journal of metals ' 2016 (quantitative analysis and structure characterization of martensite transformation induced by 304 austenitic stainless steel ultra-low temperature rolling deformation) ' discloses an alloy processing method, the whole process of the alloy processing method is ultra-low temperature deformation, the method can complete the improvement of material property, however, the processing method has high cost and high industrial application threshold in the process of processing period, is not beneficial to the popularization of the technology, the whole process of ultra-low temperature deformation is a processing technology with larger deformation amount, and is difficult to ensure the yield, but the invention carries out rapid traditional deformation before carrying out ultra-low temperature deformation, thus being beneficial to the deformation processing and forming of materials, the method can improve the yield, greatly shorten the processing period, and quickly accumulate martensite formation by using the advantage of ultralow temperature deformation at the near-end stage, thereby realizing the double optimization effects of improving the mechanical property of the material and maintaining the high-molding material. Compared with the prior processing method, the invention is simpler, has low cost increase and is beneficial to the popularization of the technology.
Drawings
FIG. 1 is a process flow diagram of the present embodiment
FIG. 2 is a photograph of the annealed structure after 70% cold rolling and 10% ultra-low temperature rolling in the present embodiment
FIG. 3 is a photograph of the annealed structure after 30% cold rolling and 20% ultra-low temperature rolling in this embodiment
FIG. 4 is a photograph of the 20% cold rolled and 10% ultra-low temperature rolled annealed structure in this embodiment
FIG. 5 is a photograph of the annealed structure of the present scheme at an ultra-low temperature of 80% after rolling
Detailed Description
The following detailed description is made with reference to the accompanying drawings.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The method comprises the following steps of (1) adopting a commercial stainless steel casting blank or hot rolled plate blank as an initial material, and carrying out surface milling on the processed initial material to prepare the plate blank with the size required by the plate blank;
step 1, adopting a casting blank or hot rolled slab steel capable of generating deformation induced martensite as an initial material, carrying out heat treatment such as solution quenching or annealing on the casting blank or hot rolled blank, wherein the treatment temperature is 800-1200 ℃, the heat preservation time is 1-8 hours, and the heat treatment on the casting blank or hot rolled blank in step 1 is vacuum treatment or argon protective atmosphere treatment, preferably quartz tube vacuum tube sealing treatment, so as to prevent the decarburization phenomenon in the heating treatment process;
step 2, performing surface milling on the casting blank or the hot rolling blank obtained in the step 1, then performing cold rolling or hot rolling on the milled casting blank or the milled hot rolling plate blank, and performing multi-pass rapid rolling processing by using a (synchronous or asynchronous) rolling mill, wherein the deformation is 20-95%, the cold rolling and the hot rolling can be performed rapidly, and the deformation is stopped when 5-10% of the residual total deformation is obtained;
step 3, placing the casting blank or the hot rolled plate blank processed in the step 2 into a low-temperature or ultralow-temperature cooling pretreatment medium for processing for 1-60 minutes for later use, wherein the temperature of the cooling pretreatment medium is-196 ℃ to-30 ℃, and the cooling pretreatment medium is liquid nitrogen or liquid nitrogen-alcohol mixed liquid or liquid nitrogen-acetone mixed liquid;
and 4, performing multi-pass rolling processing on the plate processed in the step 3 by using a rolling mill, and processing the plate in a low-temperature or ultralow-temperature cooling pretreatment medium for 1-5 minutes before each pass of rolling to obtain a steel product for rapidly promoting martensite transformation, wherein the deformation of each pass in the rolling process is 2-10%.
And 5, annealing the plate processed in the step 4 in a vacuum heat treatment at 500-1200 ℃ for 1-20 minutes, and performing recrystallization annealing treatment, preferably vacuum treatment of a quartz sealed tube, and more preferably argon protection treatment, on the plate rolled at ultralow temperature in the step 5 in a vacuum heat treatment furnace.
Example 1:
milling a commercial 304 stainless steel hot rolled plate to the condition that the upper surface and the lower surface are smooth and clean and the required size, carrying out vacuum tube sealing on the milled material, then carrying out heat preservation for 1 hour in an air furnace at 1100 ℃, rapidly carrying out water quenching after discharging, carrying out cold rolling deformation on the quenched 304 stainless steel plate at room temperature, wherein the pass deformation is 10%, carrying out one-time cold rolling, then directly carrying out the next-time rolling, namely continuously carrying out cold rolling, obtaining a rolled plate material with the deformation of 70%, then putting the cold rolled plate into liquid nitrogen for soaking for 5 minutes, carrying out ultralow-temperature rolling on the soaked rolled plate, finally carrying out the total deformation of 80%, and finally carrying out heat treatment annealing on the plate, wherein the annealing temperature is 850 ℃, and carrying out heat preservation for 5 minutes. The total processing time was 20 minutes, and fig. 2 is a photograph of the final grain structure, with a grain size of 4.5 μm.
Example 2:
a commercial 304 stainless steel hot rolled plate was milled to the upper and lower surfaces smooth and of the required dimensions. The method comprises the steps of carrying out vacuum tube sealing on a plate, then carrying out heat preservation in an air furnace at 1100 ℃ for 1 hour, carrying out rapid water quenching after discharging, carrying out cold rolling deformation on a quenched 304 stainless steel plate at room temperature, wherein the pass deformation is 10%, carrying out one-pass cold rolling, then directly carrying out the next-pass rolling, namely carrying out continuous cold rolling, obtaining a rolled plate with the deformation of 30%, then placing the cold rolled plate into liquid nitrogen for soaking for 10 minutes, then carrying out ultralow-temperature rolling on the soaked rolled plate, and finally obtaining the plate with the total deformation of 50%. Finally, the plate is annealed by heat treatment, the annealing temperature is 850 ℃, and the temperature is kept for 5 minutes. The total processing time was 25 minutes, and fig. 3 is a photograph of the final grain structure, with a grain size of 8.7 μm.
Example 3:
a commercial 304 stainless steel hot rolled plate was milled to the upper and lower surface finish and required dimensions. The method comprises the steps of performing vacuum tube sealing on a plate, then preserving heat in an air furnace at 1100 ℃ for 1 hour, discharging the plate, performing rapid water quenching, performing cold rolling deformation on a quenched 304 stainless steel plate at room temperature, wherein the pass deformation is 10%, performing one-pass cold rolling, then performing the next-pass rolling, namely continuous cold rolling, to obtain a rolled plate with the deformation of 20%, then placing the cold rolled plate into liquid nitrogen to perform soaking for 10 minutes, performing ultralow-temperature rolling on the soaked rolled plate, finally performing heat treatment annealing on the plate, wherein the total deformation is 30%, the annealing temperature is 850 ℃, preserving heat for 5 minutes, the total processing time is 25 minutes, and fig. 4 is a final crystal grain structure photo and the crystal grain size is 10 mu m.
Comparative example 1:
milling a commercial 304 stainless steel hot-rolled plate into a smooth upper surface and a smooth lower surface, sealing a tube of the milled material in vacuum, preserving heat for 1 hour in an air furnace at 1100 ℃, rapidly quenching the tube by water after discharging, and soaking the quenched 304 stainless steel plate for 30 minutes. Then directly carrying out ultra-low temperature cold rolling deformation to obtain a rolled plate with 80% deformation, and finally carrying out heat treatment annealing on the plate, wherein the annealing temperature is 850 ℃, and the heat preservation time is 5 minutes. The total processing time was 50 minutes, and fig. 5 is a photograph of the final grain structure, and the grain size was 5.5 μm.
Comparative examples 2 and 3
The experimental method was substantially identical to comparative example 1 except that the deformation was 50% and 20%, respectively, the working time was 40 minutes and 30 minutes, respectively, and the final grain size was measured to be about 10 micrometers and 20 micrometers, respectively.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (10)

1. The method for rapidly refining the metastable austenite grain structure is characterized by comprising the following steps of:
step 1: adopting a casting blank or hot rolled slab steel capable of generating deformation induced martensite as an initial material, and carrying out solution quenching or annealing treatment on the casting blank or the hot rolled blank;
step 2: carrying out surface milling on the casting blank or the hot rolling blank obtained in the step 1, and then carrying out multi-pass rapid rolling processing on the milled casting blank or the hot rolling plate blank;
step 3, placing the casting blank or the hot rolled slab processed in the step 2 into a low-temperature or ultralow-temperature cooling pretreatment medium for processing;
and 4, step 4: performing multi-pass rolling processing on the plate treated in the step 3, and performing low-temperature or ultralow-temperature cooling pretreatment on a casting blank or a hot-rolled plate blank before each pass of rolling;
and 5: and 4, annealing the material treated in the step 4 by vacuum heat treatment.
2. The method for rapidly refining the texture of metastable austenite grains according to claim 1, wherein the annealing temperature in step 1 is 800 ℃ to 1200 ℃ and the holding time is 1 to 8 hours.
3. The method for rapidly refining the metastable austenite grain structure according to claim 1, wherein the rapid rolling in the step 2 adopts a cold rolling or a hot rolling for multi-pass rapid rolling processing, and the rolling deformation is 20-95%.
4. The method for rapidly refining the metastable austenite grain structure according to claim 1, wherein the cast slab or the hot-rolled slab is placed in a low-temperature or ultra-low-temperature cooling pretreatment medium for 1-60 minutes for standby, wherein the temperature of the cooling pretreatment medium is-196 ℃ to-30 ℃.
5. The method for rapidly refining the metastable austenite grain structure of claim 1, wherein the plate is treated in a low-temperature or ultralow-temperature cooling pretreatment medium for 1-5 minutes before each rolling in the step 4 to obtain the steel for rapidly promoting the martensitic transformation, wherein the deformation amount of each rolling is 2-10%.
6. The method for rapidly refining the metastable austenite grain structure according to claim 1, wherein the heat treatment temperature in step 5 is 500-1200 ℃ for 1-20 minutes.
7. The method for rapidly refining the metastable austenite grain structure according to any one of claims 1 to 6, wherein the solution quenching or annealing treatment of the cast or hot-rolled slab in step 1 is vacuum treatment or argon atmosphere treatment.
8. The method for rapid refinement of the texture of metastable austenite grains according to any one of claims 1 to 6, characterized in that in step 2, said cold rolling and hot rolling are carried out rapidly, stopping the deformation with a residual total deformation of 5% to 10%.
9. The method for rapidly refining the texture of metastable austenite grains according to any of claims 1 to 6, characterized in that, in step 3, the cooling pretreatment medium is liquid nitrogen or a liquid nitrogen-alcohol mixture, a liquid nitrogen-acetone mixture.
10. The method for rapidly refining the metastable austenite grain structure of claim 1-6, wherein the material after the ultra-low temperature rolling in step 5 is placed in a vacuum heat treatment furnace for recrystallization annealing treatment.
CN202010055323.6A 2020-01-17 2020-01-17 Method for rapidly refining metastable austenite grain structure Expired - Fee Related CN111139347B (en)

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CN115637376B (en) * 2021-07-20 2024-01-16 上海交通大学 Austenitic stainless steel and heat treatment process thereof
CN114032369B (en) * 2021-10-27 2023-05-09 广东海洋大学 Method for regulating and controlling tissue structure of 304 metastable austenitic stainless steel
CN113981192B (en) * 2021-10-27 2023-02-03 广东海洋大学 Method for improving yield strength of 304 type metastable austenitic stainless steel
CN114273426B (en) * 2022-01-10 2024-04-16 南京理工大学 Method for preparing high-strength high-plasticity 316L stainless steel by high-strain warm rolling
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