CN115181858A - Control method for ferrite content of large-size austenitic stainless steel component - Google Patents

Control method for ferrite content of large-size austenitic stainless steel component Download PDF

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Publication number
CN115181858A
CN115181858A CN202110358922.XA CN202110358922A CN115181858A CN 115181858 A CN115181858 A CN 115181858A CN 202110358922 A CN202110358922 A CN 202110358922A CN 115181858 A CN115181858 A CN 115181858A
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forging
stainless steel
austenitic stainless
ferrite
ferrite content
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高明
李小兵
张龙
李昊泽
马颖澈
刘奎
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Institute of Metal Research of CAS
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16Remelting metals
    • C22B9/18Electroslag remelting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21JFORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • B21J5/002Hybrid process, e.g. forging following casting
    • 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/005Modifying the physical properties by deformation combined with, or followed by, heat treatment of ferrous alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/04Making ferrous alloys by melting
    • 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
    • C21D2211/005Ferrite

Abstract

The invention discloses a method for controlling ferrite content of a large-size austenitic stainless steel component, and belongs to the field of homogenization control of a structure of an oversized ingot type stainless steel forging. Aiming at the problem that a high-temperature homogenization procedure is added before the forging of a large-ingot austenitic stainless steel forging, the electroslag ingot is required to be treated at 1160-1240 ℃ for 50-100 h of homogenization time, so that ferrite forming elements such as Cr, mo and the like in the stainless steel before forging are uniformly distributed in a matrix, and the ferrite content in the finished forging is greatly reduced. When the manufacturing cost of the austenitic stainless steel forging needs to be further controlled, the atmosphere control needs to be carried out on the homogenization treatment process, and the oxidation loss cost of the large-size stainless steel component is reduced. The method can control the ferrite content of the large-size austenitic stainless steel forging to be below 1vol.% according to GB/T13305-2008 standard after omnibearing dissection.

Description

Control method for ferrite content of large-size austenitic stainless steel component
Technical Field
The invention relates to the technical field of homogenization control of a structure of an oversized ingot type stainless steel forging, in particular to a method for controlling the ferrite content of a large-size austenitic stainless steel component. The method can provide powerful guarantee for preparing the large stainless steel forging with high performance in the fields of military industry, chemical industry, nuclear power and the like.
Background
The austenitic stainless steel has the advantages of excellent corrosion resistance, good structure stability, higher service temperature (up to 700 ℃), good welding performance, excellent processing performance and the like, can be used in severe environments of high temperature, high pressure, corrosive atmosphere and physical ray radiation, and the manufactured large-size forgings are widely applied to the major fields of military industry, chemical industry, nuclear power and the like. In order to reduce the element segregation and impurity element content of large-size forgings, an electroslag remelting mode is often adopted during the preparation of the large-size forgings, but with the increase of the ingot shapes of austenitic stainless steel forgings, the cooling speed after electroslag smelting is very slow, so that ferrite forming elements such as Cr, mo and the like in a matrix are locally enriched to cause the ferrite content of finished forgings to exceed the standard, and embrittlement transformation is generated under the high-temperature service condition to seriously affect the performance stability of alloy high-temperature structures. At present, the realization of the low-ferrite content quantitative control of large-size austenitic stainless steel forgings (such as cake-shaped forgings with the diameter larger than 2000mm and the thickness larger than 500 mm) becomes one of the major technical bottlenecks to be solved for the domestic application of the large-size forgings, particularly in the field of nuclear power, the ferrite embrittlement tendency is more obvious due to the requirement of long-term service in a high-temperature environment, and the industrial application of the large-size forgings is severely restricted. Therefore, some effective control means for ferrite reduction of large-size austenitic stainless steel forgings need to be explored.
Disclosure of Invention
The method is simple and feasible, and a high-temperature homogenization procedure is added after the electroslag remelting procedure of the large-size austenitic stainless steel is completed, so that ferrite forming elements such as Cr, mo and the like in the stainless steel before forging are uniformly distributed in a matrix, and the ferrite content in the finished product forged piece is greatly reduced.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for controlling the ferrite content of a large-size austenitic stainless steel member comprises the following steps:
(1) Preparing an austenitic stainless steel casting electrode bar;
(2) Preparing an electroslag ingot: remelting and refining the austenitic stainless steel electrode bar in the step (1) by adopting an electroslag remelting process to obtain an electroslag ingot;
(3) High-temperature homogenization treatment of electroslag ingots: carrying out high-temperature homogenization treatment on the electroslag ingot obtained in the step (2) by using a heat treatment furnace, and carrying out water cooling treatment after homogenization treatment;
(4) Forging an electroslag ingot: fully cutting off the head and the tail of the electroslag ingot treated in the step (3), and forging and deforming the electroslag ingot with the head and the tail removed by adopting an upsetting-pulling deformation mode, wherein the integral forging ratio of a forge piece needs to be controlled in the forging process;
(5) Heat treatment of electroslag ingots: carrying out solution heat treatment on the forged piece obtained after forging in the step (4), and after treatment, requiring water quenching and cooling;
in the step (1), the diameter of the cast electrode rod is 200-300 mm.
In the step (2), the electroslag remelting process is carried out in an argon atmosphere and CaF is adopted 2 -CaO-Al 2 O 3 A slag system; the specification of the electroslag ingot is phi 1250-1300 mm.
In the step (3), the treatment temperature of the high-temperature homogenization treatment is 1160-1240 ℃, and the heat preservation time is 50-100 h.
In the step (4), the cutting height of the head and the tail of the electroslag ingot is required to be more than 150mm; in the forging deformation process, the initial forging temperature is 1050-1180 ℃, the final forging temperature is more than or equal to 850 ℃, the heat preservation time of each fire is 3-20 hours, and the deformation time of each fire is 20-70 min; the integral forging ratio requirement of the forge piece is more than 4.
In the step (5), the treatment temperature of the heat treatment process is 1060 +/-10 ℃.
And (3) carrying out comprehensive dissection on the forged piece obtained after the heat treatment in the step (5), and evaluating the content of ferrite in the forged piece according to the GB/T13305-2008 standard, wherein the content of ferrite in the forged piece can be controlled below 1% (vol.%).
Analyzing the surface position of the forging according to the comprehensive anatomical requirement, wherein the surface position is 1/4, 1/2 and 3/4 of the radial thickness of the forging respectively; analyzing the center position of the forging to be 1/4, 1/2 and 3/4 of the radial thickness of the forging respectively; the surface position and the center position of the forging piece both comprise two positions of 0 degree and 180 degrees.
When the ferrite is evaluated according to the GB/T13305-2008 standard, a view field with the most serious ferrite content in the whole section of the inspection surface is selected for determination, the magnification is 300 times, and the actual view field diameter is guaranteed to be 0.267mm.
The invention has the following advantages and beneficial effects:
(1) The method can realize the low-quantitative control of the ferrite content of different parts in the finished product of the large-size austenitic stainless steel forging, and can be controlled below 1% (vol.%) according to the detection method of the ferrite content of the most serious field of view executed according to the GB/T13305-2008 standard.
(2) By controlling the atmosphere in the homogenization treatment process, the oxidation loss cost of the large-size stainless steel component can be obviously reduced.
Drawings
FIG. 1 shows a 10X 10mm electroslag ingot taken from 20t austenitic stainless steel 3 And (3) carrying out detected ferrite content and morphology graph according to GB/T13305-2008 standard after 1230 ℃ homogenization treatment of the small-size sample.
FIG. 2 shows a 10X 10mm electroslag ingot taken from 20t austenitic stainless steel 3 Graph of the relation between the treatment time and the ferrite content detected according to the GB/T13305-2008 standard after the 1230 ℃ homogenization treatment of the small-sized samples.
FIG. 3 shows the ferrite corrosion morphology at the position of 180 degrees and 1/2 of the radial thickness of the surface of the large-size finished forging in example 2; wherein: (a) without high temperature homogenization; (b) after high temperature homogenization treatment.
FIG. 4 shows the ferrite corrosion morphology at the position of 1/2 and 180 degrees of the radial thickness of the surface of the large-size finished product forging in embodiment 3.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples. It should be understood that these small embodiments are merely illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
Carrying out high-temperature homogenization treatment on 30t austenitic stainless steel (316) electroslag ingot with the diameter of 1250mm, wherein the treatment system is as follows: the high-temperature homogenization temperature is 1230 ℃, and the homogenization treatment time is 6-72 hours; the experimental samples were taken from the electroslag ingot described above and the dimensions were selected to be 10mm x 10mm. After high-temperature homogenization treatment, comparing the ferrite content before and after high-temperature homogenization, and quantitatively counting the ferrite content corresponding to samples with different homogenization times, wherein the test standard is a field-of-view method for selecting the most serious ferrite content in the whole section of the test surface specified in GB/T13305-2008 standard. The magnification is 300 times, and the actual field diameter is guaranteed to be 0.267mm. The results of the experiment are shown in FIGS. 1 and 2. It can be seen that the test sample is uniformly treated at the high temperature of 1230 ℃/72h, and the ferrite test result is reduced to 0.84% from 18.22% before treatment. The example results strongly demonstrate the effectiveness of high temperature homogenization to control ferrite.
Example 2
The method comprises the steps of carrying out electroslag remelting, high-temperature homogenization, forging deformation, heat treatment and the like on a 30T austenitic stainless steel forging product with the target phi 1250mm, and analyzing the ferrite content of the forging according to the GB/T13305-2008 standard through omnibearing dissection. The specific implementation process is as follows:
(1) The diameter specification of the electrode rod is phi 220mm.
(2) The specific process parameters of electroslag remelting are listed in table 1.
TABLE 1 electroslag remelting Process parameters
Diameter specification Protective atmosphere Slag system
Φ1250mm Ar CaF 2 -CaO-Al 2 O 3
(3) After electroslag remelting, the electroslag ingot is homogenized at high temperature, and the specific process parameters are listed in table 2.
TABLE 2 high temperature homogenization Process parameters
Temperature of treatment Time of treatment Protective atmosphere Cooling method
1220℃ 80-100h Ar Water cooling
(4) After homogenization at high temperature, the mixture is forged and deformed, and the specific process parameters are listed in Table 3.
TABLE 3 Hot forging deformation Process parameters
Total forging ratio Deformation mode Temperature of start forging Finish forging temperature
13.5 Upsetting and drawing process 1180℃ 850℃
(5) After hot forging deformation, the steel is subjected to solution heat treatment, and specific process parameters are listed in Table 4.
TABLE 4 solution Heat treatment Process parameters
Charging temperature Rate of temperature rise Temperature keeping Time of heat preservation Cooling method
900℃ ≤50℃/h 1050℃ 18h Water cooling
(6) And (3) carrying out overall dissection on the forged piece after heat treatment, and determining according to a view field with the most serious ferrite content in the whole section of the selected inspection surface specified in the GB/T13305-2008 standard. The magnification is 300 times, and the actual diameter of the visual field is guaranteed to be 0.267mm. Carrying out overall dissection on the forged piece: the surface positions comprise 1/4, 1/2 and 3/4 of the radial thickness of the forging; the core part position comprises 1/4, 1/2 and 3/4 of the radial thickness of the forging. The location portion should include both 0 ° and 180 °. The test results are shown in Table 5, and the ferrite test results of the forgings under the same conditions but without high-temperature homogenization are also shown. The corrosion morphology of the sample ferrite is shown in figure 3.
TABLE 5 ferrite analysis results of samples in different positions of the whole-dimensional anatomy of finished forgings
Figure BDA0003004719420000061
Example 3
The method comprises the steps of carrying out electroslag remelting, high-temperature homogenization, forging deformation, heat treatment and the like on a 30T austenitic stainless steel forging product with a target phi of 1250mm, and analyzing the ferrite content of the forging according to the GB/T13305-2008 standard through omnibearing anatomy. The specific implementation process is as follows:
(1) The diameter of the electrode rod is phi 220mm.
(2) The specific process parameters of electroslag remelting are listed in table 1.
TABLE 1 electroslag remelting Process parameters
Diameter specification Protective atmosphere Slag system
Φ1250mm Ar CaF 2 -CaO-Al 2 O 3
(3) After electroslag remelting, the electroslag ingot is homogenized at high temperature, and the specific process parameters are listed in table 2.
TABLE 2 high temperature homogenization Process parameters
Temperature of treatment Time of treatment Protective atmosphere Cooling method
1200℃ 100h Ar Water cooling
(4) After homogenization at high temperature, the mixture is forged and deformed, and the specific process parameters are listed in Table 3.
TABLE 3 Hot forging deformation Process parameters
Total forging ratio Deformation mode Temperature of start forging Finish forging temperature
13.5 Upsetting and drawing process 1180℃ 850℃
(5) After hot forging deformation, the steel is subjected to solution heat treatment, and specific process parameters are listed in Table 4.
TABLE 4 solution Heat treatment Process parameters
Charging temperature Rate of temperature rise Temperature of heat preservation Time of heat preservation Cooling method
900℃ ≤50℃/h 1055℃ 20h Water cooling
(6) And (3) carrying out overall dissection on the forged piece after heat treatment, and determining according to a view field with the most serious ferrite content in the whole section of the selected inspection surface specified in the GB/T13305-2008 standard. The magnification is 300 times, and the actual diameter of the visual field is guaranteed to be 0.267mm. Carrying out overall dissection on the forged piece: the surface positions comprise 1/4, 1/2 and 3/4 of the radial thickness of the forging; the core part position comprises 1/4, 1/2 and 3/4 of the radial thickness of the forging. The position portion should include both 0 ° and 180 °. The test results are shown in Table 10. The ferrite corrosion morphology of the sample is shown in FIG. 4.
TABLE 10 ferrite analysis results of samples in different positions for omnibearing dissection of finished product forgings
Test site Ferrite content/%)
1/4 of the radial thickness of the surface 0
1/2,0 degree of surface radial thickness 0
1/2 of surface radial thickness, 180 ° 0
3/4 of the radial thickness of the surface 0
1/4 of the radial thickness of the core 0
The radial thickness of the core part is 1/2,0 ° 0
1/2 of the radial thickness of the core part, 180 ° 0
3/4 of the radial thickness of the core 0

Claims (9)

1. A control method of ferrite content of a large-size austenitic stainless steel component is characterized by comprising the following steps: the method comprises the following steps:
(1) Preparing an austenitic stainless steel casting electrode bar;
(2) Preparing an electroslag ingot: remelting and refining the austenitic stainless steel electrode bar in the step (1) by adopting an electroslag remelting process to obtain an electroslag ingot;
(3) High-temperature homogenization treatment of electroslag ingots: carrying out high-temperature homogenization treatment on the electroslag ingot obtained in the step (2) by using a heat treatment furnace, and carrying out water cooling treatment after homogenization treatment;
(4) Forging an electroslag ingot: fully cutting off the head and the tail of the electroslag ingot treated in the step (3), and forging and deforming the electroslag ingot with the head and the tail removed by adopting an upsetting-pulling deformation mode, wherein the integral forging ratio of a forge piece needs to be controlled in the forging process;
(5) Heat treatment of electroslag ingots: and (4) carrying out solution heat treatment on the forged piece obtained after forging in the step (4), and requiring water quenching and cooling after treatment.
2. The method of controlling ferrite content of a large-sized austenitic stainless steel member according to claim 1, wherein: in the step (1), the diameter of the cast electrode rod is 200-300 mm.
3. The method of controlling the ferrite content of a large-sized austenitic stainless steel member according to claim 1, wherein: in the step (2), the electroslag remelting process is carried out in an argon atmosphere and CaF is adopted 2 -CaO-Al 2 O 3 A slag system; the specification of the electroslag ingot is phi 1250-1300 mm.
4. The method of controlling the ferrite content of a large-sized austenitic stainless steel member according to claim 1, wherein: in the step (3), the treatment temperature of the high-temperature homogenization treatment is 1160-1240 ℃, and the heat preservation time is 50-100 h.
5. The method of controlling ferrite content of a large-sized austenitic stainless steel member according to claim 1, wherein: in the step (4), the cutting height of the head and the tail of the electroslag ingot is required to be more than 150mm; in the forging deformation process, the initial forging temperature is 1050-1180 ℃, the final forging temperature is more than or equal to 850 ℃, the heat preservation time of each fire is 3-20 h, and the deformation time of each fire is 20-70 min; the integral forging ratio requirement of the forge piece is more than 4.
6. The method of controlling the ferrite content of a large-sized austenitic stainless steel member according to claim 1, wherein: in the step (5), the treatment temperature of the heat treatment process is 1060 ℃ +/-10 ℃.
7. The method of controlling the ferrite content of a large-sized austenitic stainless steel member according to claim 1, wherein: and (5) carrying out comprehensive dissection on the forged piece obtained in the step (5), and evaluating the content of ferrite in the forged piece according to the GB/T13305-2008 standard, wherein the content of the ferrite in the forged piece can be controlled to be less than 1 vol.%.
8. The method of controlling the ferrite content of a large-sized austenitic stainless steel member according to claim 7, wherein: analyzing the surface position of the forging according to the comprehensive anatomical requirement, wherein the surface position is 1/4, 1/2 and 3/4 of the radial thickness of the forging respectively; analyzing the center position of the forging to be 1/4, 1/2 and 3/4 of the radial thickness of the forging respectively; the surface position and the center position of the forging piece both comprise two positions of 0 degree and 180 degrees.
9. The method of controlling the ferrite content of a large-sized austenitic stainless steel member according to claim 8, wherein: when the ferrite is evaluated according to the GB/T13305-2008 standard, a visual field with the most serious ferrite content in the whole section of the test surface is specified and selected for measurement, the magnification is 300 times, and the actual diameter of the visual field is ensured to be 0.267mm.
CN202110358922.XA 2021-04-02 2021-04-02 Control method for ferrite content of large-size austenitic stainless steel component Pending CN115181858A (en)

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Publication number Priority date Publication date Assignee Title
CN104826890A (en) * 2015-05-09 2015-08-12 山西太钢不锈钢股份有限公司 Manufacturing method of super austenitic stainless steel seamless tube
CN106893831A (en) * 2017-03-13 2017-06-27 东北大学 A kind of super austenitic stainless steel high temperature homogenization processing method
CN107557670A (en) * 2017-10-24 2018-01-09 山西太钢不锈钢股份有限公司 Austenitic stainless steel and preparation method and application
CN111663082A (en) * 2020-06-17 2020-09-15 江苏良工精密合金钢有限公司 Austenitic stainless steel precision seamless steel pipe and preparation method thereof
CN111876653A (en) * 2020-07-27 2020-11-03 四川六合特种金属材料股份有限公司 Preparation method of pure austenitic stainless steel
CN112143973A (en) * 2020-09-25 2020-12-29 山西太钢不锈钢股份有限公司 High-strength high-corrosion-resistance super austenitic stainless steel and preparation method thereof
CN112322971A (en) * 2020-10-15 2021-02-05 江苏银环精密钢管有限公司 Austenitic stainless steel seamless tube for sodium-cooled fast reactor internals and manufacturing method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104826890A (en) * 2015-05-09 2015-08-12 山西太钢不锈钢股份有限公司 Manufacturing method of super austenitic stainless steel seamless tube
CN106893831A (en) * 2017-03-13 2017-06-27 东北大学 A kind of super austenitic stainless steel high temperature homogenization processing method
CN107557670A (en) * 2017-10-24 2018-01-09 山西太钢不锈钢股份有限公司 Austenitic stainless steel and preparation method and application
CN111663082A (en) * 2020-06-17 2020-09-15 江苏良工精密合金钢有限公司 Austenitic stainless steel precision seamless steel pipe and preparation method thereof
CN111876653A (en) * 2020-07-27 2020-11-03 四川六合特种金属材料股份有限公司 Preparation method of pure austenitic stainless steel
CN112143973A (en) * 2020-09-25 2020-12-29 山西太钢不锈钢股份有限公司 High-strength high-corrosion-resistance super austenitic stainless steel and preparation method thereof
CN112322971A (en) * 2020-10-15 2021-02-05 江苏银环精密钢管有限公司 Austenitic stainless steel seamless tube for sodium-cooled fast reactor internals and manufacturing method thereof

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