CN115478220A - Ferrite/martensite heat-resistant steel for lead-bismuth pile and preparation method thereof - Google Patents

Ferrite/martensite heat-resistant steel for lead-bismuth pile and preparation method thereof Download PDF

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CN115478220A
CN115478220A CN202211139895.8A CN202211139895A CN115478220A CN 115478220 A CN115478220 A CN 115478220A CN 202211139895 A CN202211139895 A CN 202211139895A CN 115478220 A CN115478220 A CN 115478220A
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furnace
ingot
smelting
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forging
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曾泽瑶
罗许
黄洁
刘序江
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26—Methods of annealing
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    • C21D1/34—Methods of heating
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    • 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
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0205—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips of ferrous alloys
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    • 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
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
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    • 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
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0247—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/04—Making ferrous alloys by melting
    • C22C33/06—Making ferrous alloys by melting using master alloys
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
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    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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Abstract

The invention relates to ferrite/martensite heat-resistant steel for a lead-bismuth pile and a preparation method thereof, wherein the ferrite/martensite heat-resistant steel comprises the following chemical components in percentage by mass: c:0.08-0.12%, si:0.5-3.0%, al:0.5-4.50%, cr:9.0-12.0%, V:0.20-0.30%, nb:0.04-0.08%, ta:0.08-0.22%, W:1.5-2.0%, B:0.006-0.01%, ce:0.05 to 1.2 percent of Mo, ni, mn, co and the like as residual elements, less than or equal to 0.008 percent of S, less than or equal to 0.008 percent of P and the balance of Fe. The alloy is prepared by the steps of smelting, forging, normalizing, tempering and the like. The invention not only has good liquid lead corrosion resistance, but also has good room temperature and high temperature mechanical properties, and simultaneously effectively improves the lead bismuth corrosion resistance or the radiation resistance or the high temperature oxidation resistance of the martensitic stainless steel, and can greatly reduce the cost of raw materials.

Description

Ferrite/martensite heat-resistant steel for lead-bismuth pile and preparation method thereof
Technical Field
The invention relates to the technical field of nuclear power materials, in particular to ferrite/martensite heat-resistant steel for a lead bismuth stack and a preparation method thereof.
Background
With the rapid development of global economy and the increasing living standard of human beings, the demand of people for electric energy is sharply increased. The traditional fossil energy sources such as coal, petroleum, natural gas and the like not only have the problem of environmental pollution, but also are non-renewable resources. Nuclear energy is the most promising energy source which is efficient, low-carbon, clean and capable of being relied on. At present, 9 nuclear power reactor units are available in China, the main reactor type is a pressurized water reactor, the pressurized water reactor mainly utilizes uranium-235 as a fission fuel, and the uranium-235 only accounts for 0.7% of natural uranium. For a pressurized water reactor type, only about 0.45% of the input uranium resources can be consumed in one burning, and the remaining 99% cannot be utilized. The fast reactor can improve the utilization rate of uranium resources to 60-70%. Among six reference reactor types of fast reactors (sodium-cooled fast reactor, lead-cooled fast reactor, gas-cooled fast reactor, high-temperature gas-cooled reactor, molten salt reactor and supercritical water reactor), the lead-cooled fast reactor adopts liquid lead or lead-bismuth alloy as a coolant, has higher inherent safety, has unique advantages in the aspects of regenerative fuel circulation, radioactive waste aftertreatment, reactor system simplification, material change period shortening and the like, and is focused internationally.
The selection of core structure materials is one of the key problems limiting the development and application of the lead-cooled fast reactor. Because the temperature of the core of the lead-cooled fast reactor is high, the irradiation dose is high, the corrosion of the coolant is strong, the density is high, the flow rate is fast, and the core has strong erosion and corrosion effects on the material, the component elements in the structural material, such as Ni, can be gradually dissolved and mass-transferred into the coolant, and meanwhile, the coolant can also be diffused into the material along the crystal boundary to generate corrosion damage, thereby affecting the safe operation of the reactor. 9-12 (wt.%) Cr ferrite/martensite heat-resistant steel has the characteristics of excellent mechanical property, heat resistance, low expansion, neutron irradiation resistance and the like, is widely applied to the nuclear power field, and is a key structural material required by lead-cooled fast reactor construction. However, the liquid lead corrosion resistance of common ferrite/martensite, such as T/P91 heat-resistant steel, is poor, and how to improve the liquid lead corrosion resistance is an urgent problem to be solved.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a ferrite/martensite heat-resistant steel for a lead-bismuth pile and a method for manufacturing the same, which can purify molten steel, refine grains, and modify inclusions by appropriate rare earth content, thereby improving plasticity, strength, high-temperature oxidation property, and corrosion property of the steel.
The technical scheme adopted by the invention is as follows:
the invention provides ferrite/martensite heat-resistant steel for a lead-bismuth pile, which comprises the following chemical components in percentage by mass: c:0.08-0.12%, si:0.5-3.0%, al:0.5-4.50%, cr:9.0-12.0%, V:0.20-0.30%, nb:0.04-0.08%, ta:0.08-0.22%, W:1.5-2.0%, B:0.006-0.01%, ce:0.05 to 1.2 percent of Mo, ni, mn and Co as residual elements, less than or equal to 0.008 percent of S, less than or equal to 0.008 percent of P and the balance of Fe.
A preparation method of ferrite/martensite heat-resistant steel for a lead-bismuth pile comprises the following steps:
s1, smelting: adopting single smelting of vacuum induction smelting or double smelting of vacuum induction smelting and vacuum consumable arc smelting;
s2, forging and cogging;
s3, normalizing;
and S4, tempering.
Further, the single smelting comprises the following steps: adding pure iron, ferrochrome, ferrovanadium, cerium and other materials in the weight percentage into 150kg vacuum induction smelting furnace, and vacuumizing the 150kg pressure induction smelting furnace with ultimate vacuum degree of 6 x 10 -2 Pa, power supply power of 160kW, frequency of 2500Hz, vacuum degree of less than 10- 1 When Pa, starting to transmit power to heat the smelting material, wherein the initial power is 40kW, gradually increasing the power, and maintaining and controlling the power after a molten pool appears to avoid splashing;
adjusting the power to 10-15kW after the furnace burden is melted down, refining for 50-80 minutes and keeping the vacuum degree less than or equal to 10- 3 Pa, removing O, N and H elements;
adding deoxidizer Ca in an amount of 0.05-0.1 wt%, controlling the temperature of the molten steel to be 150-200 deg.C higher than the melting point, pouring into an ingot mold under electrification, and cooling;
and after the air pressure in the furnace is balanced with the atmospheric pressure, casting the solution into a mold to obtain an ingot, discharging the ingot out of the furnace after the mold is cooled, demolding after the mold is cooled, taking out the heat-resistant steel, and cutting off a dead head of the ingot to obtain the ingot to be processed.
Further, the duplex smelting comprises the following steps: adding pure iron, ferrochromium, ferrovanadium, cerium and other materials in the weight percentage into 150kg of vacuum induction smelting furnace, and vacuumizing the 150kg of pressure induction smelting furnace to the ultimate vacuum degree of 6 multiplied by 10 -2 Pa, power supply power of 160kW, frequency of 2500Hz, and vacuum degree of less than 10 -1 When Pa, starting to transmit power to heat the smelting material, wherein the initial power is 40kW, gradually increasing the power, and maintaining and controlling the power after a molten pool appears to avoid splashing;
after the furnace burden is melted down, the power is adjusted to 10-15kW, and refining is carried out for 40-60 minutes with the vacuum degree less than or equal to 10 -3 Pa, removing O, N and H elements;
adding deoxidizer Ca in an amount of 0.05-0.1 wt%, controlling the temperature of the molten steel to be 150-200 deg.C higher than the melting point, pouring into an ingot mold under electrification, and cooling;
and after the air pressure in the furnace is balanced with the atmospheric pressure, casting the solution into a mold to obtain an ingot, discharging the ingot out of the furnace after the mold is cooled, demolding after the mold is cooled, taking out the heat-resistant steel, cutting off a dead head of the ingot to obtain the ingot to be processed, processing the ingot into a consumable electrode, and performing secondary smelting by using a vacuum consumable arc smelting furnace to finally obtain the alloy ingot.
Further, the forging and cogging includes: heating the heating furnace to 680-880 ℃, charging, heating to 1120-1220 ℃ along with the furnace, preserving heat for 3-8 hours, homogenizing, discharging, forging, and finishing forging by three times of fire; forging for the first time by fire, and upsetting for multiple times to obtain a square billet; then carrying out remelting and heating on the square billet, keeping the temperature at 1080-1220 ℃ for 1-8 hours, discharging from the furnace, and forging for the second fire time, wherein the second fire time adopts unidirectional drawing forging to obtain a rectangular billet; then, after the furnace is returned and the temperature is kept for 1 to 8 hours at the temperature of 1080 to 1220 ℃, forging for the third firing time, and performing die forging on the third firing time to obtain a round bar blank; and cooling with water after forging.
Further, the normalizing process includes: putting the round bar blank into a heat treatment furnace, normalizing at 950-1100 ℃ for 80-180min, and then carrying out oil cooling quenching.
Further, the tempering treatment comprises: putting the round bar blank into a box type heat treatment furnace, tempering the round bar blank at 700-850 ℃, keeping the temperature for 80-180min, and then cooling in air.
Further, the tempering treatment is followed by a pretreatment comprising: before pretreatment, surface polishing is carried out, the surface roughness is less than 0.7, then the temperature is raised to 700-800 ℃ along with the furnace, the temperature is kept for 10-20h, and finally the air cooling is carried out to the room temperature.
Compared with the prior art, the invention has the following beneficial effects:
the heat-resistant steel prepared by the invention not only has good liquid lead corrosion resistance, but also has good room temperature and high temperature mechanical properties, and can effectively improve the lead and bismuth corrosion resistance, the radiation resistance and the high temperature oxidation resistance of the martensitic stainless steel, and greatly reduce the cost of raw materials.
Drawings
FIG. 1 is a schematic view of a normalized structure in example 3 of the present invention.
Detailed Description
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
The invention provides ferrite/martensite heat-resistant steel for a lead-bismuth pile, which comprises the following chemical components in percentage by mass: c:0.08-0.12%, si:0.5-3.0%, al:0.5-4.50%, cr:9.0-12.0%, V:0.20-0.30%, nb:0.04-0.08%, ta:0.08-0.22%, W:1.5-2.0%, B:0.006-0.01%, ce:0.05 to 1.2 percent of Mo, ni, mn and Co as residual elements, less than or equal to 0.008 percent of S, less than or equal to 0.008 percent of P and the balance of Fe.
The chromium-nickel equivalent of the alloy steel is balanced by adjusting elements such as C, si, al and the like, so that ferrite and martensite structures with different proportions are obtained, and a large amount of carbides are contained, so that the alloy is ensured to have excellent room-temperature and high-temperature mechanical properties.
The addition of Ce is simple substance Ce or cerium-iron intermediate alloy.
The proper rare earth content can purify molten steel, refine crystal grains, deteriorate inclusion, and improve the plasticity, strength, high-temperature oxidation performance and corrosion performance of the steel. The rare earth elements have a large radius, and cause large lattice distortion, thereby tending to segregate at each interface in the steel. The rare earth elements are segregated at the grain boundary, so that the grain boundary bonding force can be enhanced, for example, ce rare earth elements are easily segregated at the grain boundary, occupy vacancies on the grain boundary, reduce the enrichment of harmful elements such as P and S and the like at the grain boundary, and purify the grain boundary. Meanwhile, ce can reduce the growth speed of the oxide film and improve the anti-stripping performance of the oxide film. The rare earth element can be used as Cr oxide film 2 O 3 Nucleation of (C) by Cr 2 O 3 Can be quickly generated under the condition of low chromium concentration, and secondly, the rare earth elements promote the diffusion of chromium elements in the alloyThe rare earth elements are partially gathered on the oxide layer and the surface of a matrix, so that the effect of optimizing the structure of the oxide layer on the surface of the steel can be achieved, and the fusion reactor taking lead base or lead bismuth as a coolant has a favorable effect.
C is the most basic alloy element in steel, and as an interstitial solid solution strengthening element, the increase of the content of carbon and nitrogen leads to the increase of the strength of the steel and the reduction of the toughness. The carbon content of heat resistant steels is usually strictly controlled within a certain range under high temperature creep conditions.
Cr is a typical ferrite forming element, is also the most basic additive element in heat-resistant steel, is a main element in the heat-resistant steel for improving steam oxidation and corrosion capacity, and can improve the high-temperature strength of the steel. When Cr is enough, the Cr can react with the Cr to form a protective film on the surface of the alloy matrix, so that the diffusion of atoms and metal ions is prevented, and the oxidation process is delayed.
W is a refractory metal element and is used as a solute atom, so that the recrystallization temperature of the Fe-based solid solution can be increased. W belongs to ferrite forming elements and strong carbide forming elements, can effectively improve the high-temperature strength and creep property of the heat-resistant steel, and can ensure excellent radiation brittleness resistance in a reactor core by using W to replace Mo.
V is a ferrite forming element, and the main function of V is to form fine carbon nitride in the martensite heat-resistant steel to play a role in precipitation strengthening, so that the high-temperature strength of the steel is effectively improved, and V replaces Nb, and the addition of Ti can avoid irradiation embrittlement caused at high temperature. .
B is a interstitial solid solution element which can enter into the vacancy at the grain boundary to stabilize the grain boundary, thereby improving the strength of the grain boundary. The content of B in the material is increased, and M can be effectively inhibited 23 C 6 The coarsening of the material improves the creep property of the material. However, too high a B content necessitates the formation of BN by lowering the N content, while too low an N content leads to the loss of the MX phase and, on the contrary, to a negative effect on the creep behaviour.
Si and Al are strong ferrite forming elements and are beneficial to improving heat resistanceThe steel is resistant to high-temperature oxidation, but the addition of more Si or Al increases the tendency of delta ferrite precipitation, and sigma phase is easily formed to destroy the ductility and toughness of the alloy when exposed to a high-temperature environment for a long time. Strong binding capacity of Si and oxygen, uniform, compact and stable rich SiO generated by reaction 2 ，Al 2 O 3 The oxide layer can effectively reduce the diffusion rate of alloy elements and inhibit the dissolution corrosion of structural materials, so that the alloy steel is ensured to have the liquid lead corrosion resistance.
Ta is a refractory element, and the addition of Ta can refine austenite grains, improve the anti-irradiation performance of steel, reduce the ductile-brittle transition temperature of the steel, and improve the high-temperature creep property and the room-temperature tensile property of the steel. Excessive addition of Ta easily coarsens the carbide and reduces the mechanical properties.
Ce can not only purify molten steel, but also refine the solidification structure of steel, and change the property, form and distribution of inclusions, thereby improving various properties of steel. As a surface active element, the crystal boundary diffusion activation energy can be increased, the crystal boundary sliding can be hindered, the surface energy of crystal boundary cracks can be increased, and the method is very effective for improving the endurance strength; in addition, rare earth Ce element can inhibit the growth speed of an oxide layer of the heat-resistant steel in a high-temperature state, the formed oxide layer is well combined with a matrix, and the matrix can be protected from further oxidation under the action of high-temperature circulation.
A preparation method of ferrite/martensite heat-resistant steel for a lead-bismuth pile comprises the following steps:
s1, smelting;
adopting single smelting of vacuum induction smelting or double smelting of vacuum induction smelting and vacuum consumable arc smelting;
wherein the specific process of the single smelting is as follows: adding the pure iron, the ferrochrome, the ferrovanadium, the cerium metal and other ingredients according to the actual weight percentage into a 150kg vacuum induction smelting furnace, and carrying out the operation on the 150kg pressure induction smelting furnaceVacuum pumping is carried out, and the ultimate vacuum degree is 6 multiplied by 10 -2 Pa, power supply power of 160kW, frequency of 2500Hz, and vacuum degree of less than 10 -1 When Pa, starting to transmit power to heat the smelting material, wherein the initial power is 40kW, gradually increasing the power, and maintaining and controlling the power after a molten pool appears to avoid splashing;
after the furnace burden is melted down, the power is adjusted to 10-15kW, refining is carried out for 50-80 minutes, and the vacuum degree is less than or equal to 10 -1 Pa, removing O, N and H elements;
adding deoxidizer Ca in an amount of 0.05-0.1 wt%, controlling the temperature of the molten steel to be 150-200 deg.C higher than the melting point, pouring into an ingot mold under electrification, and cooling;
and after the air pressure in the furnace is balanced with the atmospheric pressure, casting the solution into a mold to obtain an ingot, discharging the ingot out of the furnace after the mold is cooled, demolding after the mold is cooled, taking out the heat-resistant steel, and cutting off a dead head of the ingot to obtain the ingot to be processed.
The specific process of duplex smelting is as follows: adding pure iron, ferrochromium, ferrovanadium, yttrium metal and other ingredients in the weight percentage into a 150kg vacuum induction smelting furnace, vacuumizing the 150kg pressure induction smelting furnace, wherein the ultimate vacuum degree is 6 multiplied by 10 -2 Pa, power supply power of 160kW, frequency of 2500Hz, and vacuum degree of less than 10 -1 When Pa, starting to transmit power to heat the smelting material, wherein the initial power is 40kW, gradually increasing the power, and maintaining and controlling the power after a molten pool appears to avoid splashing;
after the furnace burden is melted down, the power is adjusted to 10-15kW, refining is carried out for 40-60 minutes, and the vacuum degree is less than or equal to 10 -1 Pa, removing O, N and H elements;
adding deoxidizer Ca in an amount of 0.05-0.1 wt%, controlling the temperature of the molten steel to be 150-200 deg.C higher than the melting point, pouring into an ingot mold under electrification, and cooling;
and after the air pressure in the furnace is balanced with the atmospheric pressure, casting the solution into a mold to obtain an ingot, discharging the ingot out of the furnace after the mold is cooled, demolding after the mold is cooled, taking out the heat-resistant steel, cutting off a dead head of the ingot to obtain the ingot to be processed, processing the ingot into a consumable electrode, and performing secondary smelting by using a vacuum consumable arc smelting furnace to finally obtain the alloy ingot.
S2, forging and cogging;
the forging and cogging process comprises the following specific steps: heating the heating furnace to 680-880 ℃, charging, heating to 1120-1220 ℃ along with the furnace, preserving heat for 3-8 hours, homogenizing, discharging, forging, and finishing forging by three times of fire; forging for the first time by fire, and upsetting for multiple times to obtain a square billet; then carrying out remelting heating on the square billet, keeping the temperature at 1080-1220 ℃ for 1-8 hours, discharging from the furnace and forging for the second firing time, and carrying out unidirectional drawing forging on the second firing time to obtain a rectangular billet; then, after the furnace is returned and the temperature is kept for 1 to 8 hours at the temperature of 1080 to 1220 ℃, forging for the third firing time, and performing die forging for the third firing time to obtain a round bar blank; and cooling with water after forging.
S3, normalizing;
the normalizing treatment comprises the following specific processes: putting the round bar blank into a box type heat treatment furnace, normalizing the bar blank or the plate blank at 950-1100 ℃, keeping the temperature for 80-180min, and then carrying out oil cooling quenching.
S4, tempering;
the specific process of the tempering treatment is as follows: and (3) putting the normalized sample into a box-type heat treatment furnace, tempering the round bar blank or the plate blank at 700-850 ℃, keeping the temperature for 80-180min, and then cooling in air.
The tempering treatment can be optionally performed with pretreatment, and the pretreatment specifically comprises the following steps: before pretreatment, surface polishing is carried out, the surface roughness is less than 0.7, then the temperature is raised to 700-800 ℃ along with a box type resistance furnace, the temperature is kept for 10-20h, and finally air cooling is carried out to the room temperature.
The purpose of this step is to more effectively exhibit the film forming properties of Si and Al and promote the addition of rare earth element Ce to SiO surface 2 ，(Cr，Al) 2 O 3 The composite oxide film exerts the rare earth element Ce to inhibit the growth speed of an oxide layer of the heat-resistant steel in a high-temperature state, the formed oxide layer is well combined with a matrix, the matrix can be protected from further oxidation under the action of high-temperature circulation, the characteristic has good protection effect on a liquid lead bismuth environment and a high-radiation environment, the surface Si-Al-rich oxide film layer is prepared by pretreatment, and the surface dense SiO film layer can be formed by pretreatment to obtain a film 2 ，(Cr，Al) 2 O 3 Composite oxide film type ferriteA body heat resistant steel.
After normalizing at 950-1100 ℃ and tempering heat treatment at 700-850 ℃, the tensile strength of the alloy at room temperature mechanical property is more than 620MPa, the yield strength is more than 320MPa, the elongation is more than 10 percent, and the reduction of area is more than 40 percent.
After normalizing at 950-1100 ℃ and tempering heat treatment at 700-850 ℃, the tensile strength of the alloy is more than 330MPa, the yield strength is more than 220MPa, the elongation is more than 10 percent and the reduction of area is more than 30 percent at 550 ℃.
The invention is further illustrated by the following three specific examples:
example 1
The ferrite/martensite heat-resistant steel corroded by the ferrite/martensite heat-resistant steel (lead bismuth) for the lead bismuth pile comprises the following chemical components in percentage by weight: c:0.08%, si:0.5%, al:4.5%, cr:9.0%, V:0.20%, nb:0.04%, ta:0.08%, W:1.5%, B:0.006%, ce:0.05 percent of Mo, ni, mn, co and the like as residual elements, less than or equal to 0.008 percent of S, less than or equal to 0.008 percent of P and the balance of Fe.
S1, smelting
Adopting a vacuum induction smelting mode, calculating the ingredients of pure iron, ferrochromium, ferrovanadium, cerium and the like according to the actual added weight percentage, putting the ingredients into a vacuum induction smelting furnace, vacuumizing the 150kg pressure induction smelting furnace, wherein the ultimate vacuum degree is 6 multiplied by 10 - 2 Pa, power supply power of 160kW, frequency of 2500Hz, and vacuum degree of less than 10 -1 When Pa, starting to transmit power to heat the smelting material, wherein the initial power is 40kW, gradually increasing the power, and maintaining and controlling the power after a molten pool appears to avoid splashing;
after the furnace burden is melted down, the power is adjusted to 10-15kW, refining is carried out for 40 minutes, and the vacuum degree is less than or equal to 10 -3 Pa, removing O, N and H elements;
adding deoxidizer Ca accounting for 0.05% of the total weight, controlling the temperature of the molten steel to be 150 ℃ higher than the melting point, pouring the molten steel into an ingot mold in a charged manner, and cooling;
and after the air pressure in the furnace is balanced with the atmospheric pressure, casting the solution into a mold to obtain an ingot, discharging the ingot out of the furnace after the mold is cooled, demolding after the mold is cooled, taking out the heat-resistant steel, and cutting off a dead head of the ingot to obtain the ingot to be processed.
S2, forging and cogging
Heating the heating furnace to 680 ℃, charging, heating to 1120 ℃ along with the furnace, keeping the temperature for 8 hours, discharging from the furnace, forging, and finishing the forging by three times of fire; performing first hot forging for multiple times to obtain a square billet; then, carrying out remelting heating on the billet, keeping the temperature at 1220 ℃ for 1 hour, discharging from the furnace, forging a second fire, and carrying out unidirectional drawing forging on the second fire to obtain a rectangular billet; then, after the furnace is returned and the temperature is kept for 1 hour at 1220 ℃, forging a third fire, and performing die forging on the third fire to obtain a round bar blank; and cooling with water after forging.
S3, normalizing treatment
Putting the round bar blank into a box type heat treatment furnace, normalizing the round bar blank at 950 ℃, keeping the temperature for 180min, and then carrying out oil cooling quenching.
S4, tempering
Putting the round bar blank into a box type heat treatment furnace, tempering the round bar blank at 700 ℃, keeping the temperature for 180min, and then cooling in air.
Example 2
The ferrite/martensite heat-resistant steel corroded by ferrite/martensite heat-resistant steel (lead bismuth) for the lead bismuth pile comprises the following chemical components in percentage by weight: c:0.12%, si:3.0%, al:0.50%, cr:12.0%, V:0.30%, nb:0.08%, ta:0.22%, W:2.0%, B:0.01%, ce:1.2 percent of Mo, ni, mn, co and the like as residual elements, less than or equal to 0.008 percent of S, less than or equal to 0.008 percent of P and the balance of Fe.
S1, smelting
Adopts Vacuum Induction Melting (VIM) + vacuum consumable arc melting (VAR)'
The ingredients are calculated according to the actual added weight percentage and put into a vacuum induction melting furnace, the 150kg pressure induction melting furnace is vacuumized, and the ultimate vacuum degree is 6 multiplied by 10 -2 Pa, power supply power of 160kW, frequency of 2500Hz, and vacuum degree of less than 10 - 1 When Pa, starting to transmit power to heat the smelting material, wherein the initial power is 40kW, gradually increasing the power, and maintaining and controlling the power after a molten pool appears to avoid splashing;
lowering after furnace burden is moltenThe power reaches 10-15kW, refining is carried out for 60 minutes, and the vacuum degree is less than or equal to 10 -3 Pa, removing O, N and H elements;
adding a deoxidizer Ca accounting for 0.1 percent of the total weight, controlling the temperature of the molten steel to be 200 ℃ higher than the melting point, pouring the molten steel into an ingot mold in a charged manner, and cooling;
after the air pressure in the furnace is balanced with the atmospheric pressure, casting the solution into a mold to obtain an ingot, after the mold is cooled, discharging the ingot out of the furnace, demolding after cooling, taking out heat-resistant steel, cutting off a dead head of the ingot to obtain an ingot to be processed, processing the ingot into a consumable electrode, and performing secondary smelting by using a vacuum consumable arc smelting furnace to finally obtain an alloy ingot;
s2, forging and cogging
Heating the heating furnace to 880 ℃, charging, heating to 1220 ℃ along with the furnace, preserving heat for 3 hours, discharging and forging, and finishing the forging by three times of heating; performing first hot forging for multiple times to obtain a square billet; then carrying out remelting heating on the square billet, keeping the temperature at 1080 ℃ for 8 hours, discharging from the furnace, forging a second fire, and carrying out unidirectional drawing forging on the second fire to obtain a rectangular billet; then, after the furnace is returned and the temperature is kept for 8 hours at 1080 ℃, forging a third fire, and performing die forging on the third fire to obtain a round bar blank; and cooling with water after forging.
S3, normalizing treatment
Putting the round bar blank into a box type heat treatment furnace, normalizing the round bar blank at 1100 ℃, keeping the temperature for 80min, and then carrying out oil cooling quenching.
S4, tempering
Putting the round bar blank into a box type heat treatment furnace, tempering the round bar blank at 850 ℃, keeping the temperature for 80min, and then cooling in air.
Example 3
The ferrite/martensite heat-resistant steel corroded by ferrite/martensite heat-resistant steel (lead bismuth) for the lead bismuth pile comprises the following chemical components in percentage by weight: c:0.10%, si:2.0%, al:2.20%, cr:10.0%, V:0.25%, nb:0.06%, ta:0.18%, W:1.85%, B:0.008%, ce:0.8 percent of Mo, ni, mn, co and the like as residual elements, less than or equal to 0.008 percent of S, less than or equal to 0.008 percent of P and the balance of Fe.
S1, smelting
Adopts Vacuum Induction Melting (VIM) + vacuum consumable arc melting (VAR)'
The ingredients are calculated according to the actual added weight percentage and put into a vacuum induction melting furnace, the 150kg pressure induction melting furnace is vacuumized, and the ultimate vacuum degree is 6 multiplied by 10 -2 Pa, power supply power of 160kW, frequency of 2500Hz, and vacuum degree of less than 10 - 1 When Pa, starting to transmit power to heat the smelting material, wherein the initial power is 40kW, gradually increasing the power, and maintaining and controlling the power after a molten pool appears to avoid splashing;
after the furnace burden is melted down, the power is adjusted to 15kW, and refining is carried out for 60 minutes with the vacuum degree less than or equal to 10 -1 Pa, removing O, N and H elements;
adding deoxidizer Ca accounting for 0.08 percent of the total weight, controlling the temperature of the molten steel to be 180 ℃ higher than the melting point, pouring the molten steel into an ingot mold in a charged manner, and cooling;
after the air pressure in the furnace is balanced with the atmospheric pressure, casting the solution into a mold to obtain an ingot, discharging the ingot out of the furnace after the mold is cooled, demolding after the mold is cooled, taking out heat-resistant steel, cutting off a dead head of the ingot to obtain an ingot to be processed, processing the ingot into a consumable electrode, and performing secondary smelting by using a vacuum consumable arc smelting furnace to finally obtain an alloy ingot;
s2, forging and cogging
Heating the heating furnace to 780 ℃, charging, heating to 1200 ℃ along with the furnace, keeping the temperature for 6 hours, discharging from the furnace, forging, and finishing the forging by three times of fire; performing first hot forging for multiple times to obtain a square billet; then, carrying out remelting and heating on the billet, keeping the temperature at 1200 ℃ for 1.5 hours, discharging the billet from the furnace, and forging a second fire, wherein the second fire adopts unidirectional drawing forging to obtain a rectangular billet; then, after the furnace is returned and the temperature is kept for 1.5 hours at 1200 ℃, forging a third fire, and performing die forging on the third fire to obtain a round bar blank; and cooling with water after forging.
S3, normalizing treatment
Putting the round bar blank into a box-type heat treatment furnace, normalizing the round bar blank at 1080 ℃ for 100min, and then carrying out oil cooling quenching to obtain a structure shown in figure 1, wherein the structure is ferrite equiaxial crystal structure.
A normalized sample was processed into a Charpy V-shaped opening pattern of 10X 55mm, and 2 parallel samples were subjected to a room temperature impact test to obtain a value of 9J,7J in impact toughness.
S4, tempering
And (3) putting the round bar blank into a box type heat treatment furnace, tempering the round bar blank at 750 ℃, keeping the temperature for 100min, and then cooling in air.
S5, pretreatment
In order to more effectively exert the film forming property of Si and Al, a pretreatment is carried out to prepare a surface Si-rich and Al-rich oxide film layer, and a pretreatment is carried out to obtain a film capable of forming SiO with a compact surface 2 ，(Cr，Al) 2 O 3 Composite oxide film type ferrite heat-resistant steel. Before pretreatment, surface polishing is carried out, the surface roughness is less than 0.7, then the temperature is raised to 780 ℃ along with a box-type resistance furnace, the temperature is kept for 10h, and then the air cooling is carried out to the room temperature.
After normalizing and tempering heat treatment, the tensile strength of the alloy at room temperature mechanical property is 620MPa, the yield strength is 330MPa, the elongation is 17 percent, and the reduction of area is 43 percent.
After normalizing and tempering heat treatment, the tensile strength of the heat-resistant steel at 550 ℃ is 349MPa, the yield strength is 242MPa, the elongation is 14 percent, and the reduction of area is 39 percent.
The invention is not the best known technology.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.

Claims (8)

1. The ferrite/martensite heat-resistant steel for the lead-bismuth pile is characterized by comprising the following chemical components in percentage by mass: c:0.08-0.12%, si:0.5-3.0%, al:0.5-4.50%, cr:9.0-12.0%, V:0.20-0.30%, nb:0.04-0.08%, ta:0.08-0.22%, W:1.5-2.0%, B:0.006-0.01%, ce:0.05 to 1.2 percent of Mo, ni, mn and Co as residual elements, less than or equal to 0.008 percent of S, less than or equal to 0.008 percent of P and the balance of Fe.
2. A method for preparing a ferritic/martensitic heat-resistant steel for a lead-bismuth stack as claimed in claim 1, characterized by comprising the steps of:
s1, smelting: adopting single smelting of vacuum induction smelting or double smelting of vacuum induction smelting and vacuum consumable arc smelting;
s2, forging and cogging;
s3, normalizing;
and S4, tempering.
3. The method for preparing the ferrite/martensite heat-resistant steel for the lead-bismuth pile according to claim 2, wherein the method comprises the following steps: the single smelting comprises the following steps: adding pure iron, ferrochromium, ferrovanadium, cerium and other materials in the weight percentage into 150kg of vacuum induction smelting furnace, and vacuumizing the 150kg of pressure induction smelting furnace to the ultimate vacuum degree of 6 multiplied by 10 -2 Pa, power supply power of 160kW, frequency of 2500Hz, and vacuum degree of less than 10 -1 When Pa, starting to transmit power to heat the smelting material, wherein the initial power is 40kW, gradually increasing the power, and maintaining and controlling the power after a molten pool appears to avoid splashing; after the furnace burden is melted down, the power is adjusted to 10-15kW, and refining is carried out for 50-80 minutes with the vacuum degree less than or equal to 10 -1 Pa, removing O, N and H elements; adding deoxidizer Ca in an amount of 0.05-0.1 wt%, controlling the temperature of the molten steel to be 150-200 deg.C higher than the melting point, pouring into an ingot mold under electrification, and cooling; and after the air pressure in the furnace is balanced with the atmospheric pressure, casting the solution into a mold to obtain an ingot, discharging the ingot out of the furnace after the mold is cooled, demolding after the mold is cooled, taking out the heat-resistant steel, and cutting off a dead head of the ingot to obtain the ingot to be processed.
4. The method for preparing the ferrite/martensite heat-resistant steel for the lead-bismuth pile according to claim 2, wherein the method comprises the following steps: the duplex smelting comprises the following steps: adding pure iron, ferrochromium, ferrovanadium, cerium and other materials in the weight percentage into 150kg of vacuum induction smelting furnace, and vacuumizing the 150kg of pressure induction smelting furnace to the ultimate vacuum degree of 6 multiplied by 10 -2 Pa, power supply power of 160kW, and frequency of 2500Hz, vacuum degree less than 10 -1 When Pa, starting to transmit power to heat the smelting material, wherein the initial power is 40kW, gradually increasing the power, and maintaining and controlling the power after a molten pool appears to avoid splashing; after the furnace burden is melted down, the power is adjusted to 10-15kW, refining is carried out for 40-60 minutes, and the vacuum degree is less than or equal to 10 -1 Pa, removing O, N and H elements; adding deoxidizer Ca in an amount of 0.05-0.1 wt%, controlling the temperature of the molten steel to be 150-200 deg.C higher than the melting point, pouring into an ingot mold under electrification, and cooling; and after the air pressure in the furnace is balanced with the atmospheric pressure, casting the solution into a mold to obtain an ingot, discharging the ingot out of the furnace after the mold is cooled, demolding after the mold is cooled, taking out the heat-resistant steel, cutting off a dead head of the ingot to obtain the ingot to be processed, processing the ingot into a consumable electrode, and performing secondary smelting by using a vacuum consumable arc smelting furnace to finally obtain the alloy ingot.
5. The method for preparing a ferritic/martensitic heat-resistant steel for a lead-bismuth stack as claimed in claim 3 or 4, wherein: the forging cogging comprises: heating the ingot in a heating furnace to 680-880 ℃, charging, heating to 1120-1220 ℃ along with the furnace, preserving heat for 3-8 hours, performing homogenization treatment, discharging from the furnace, forging, and finishing the forging by three fire times; forging for the first time by fire, and upsetting for multiple times to obtain a square billet; then carrying out remelting and heating on the square billet, keeping the temperature at 1080-1220 ℃ for 1-8 hours, discharging from the furnace, and forging for the second fire time, wherein the second fire time adopts unidirectional drawing forging to obtain a rectangular billet; then, after the furnace is returned and the temperature is kept for 1 to 8 hours at the temperature of 1080 to 1220 ℃, forging for the third firing time, and performing die forging for the third firing time to obtain a round bar blank; and cooling with water after forging.
6. The method for preparing the ferrite/martensite heat-resistant steel for the lead-bismuth pile according to claim 5, wherein the method comprises the following steps: the normalizing treatment comprises the following steps: putting the cogging sample into a heat treatment furnace, normalizing at 950-1100 ℃ for 80-180min, and carrying out oil cooling quenching.
7. The method for preparing the ferrite/martensite heat-resistant steel for the lead-bismuth pile according to claim 6, wherein the method comprises the following steps: the tempering treatment comprises the following steps: and (3) putting the normalized sample into a heat treatment furnace, tempering the normalized sample at 700-850 ℃, keeping the temperature for 80-180min, and then cooling in air.
8. The method for preparing ferrite/martensite heat-resistant steel for lead-bismuth pile according to claim 2, wherein: the tempering treatment is followed by pretreatment comprising: before pretreatment, surface polishing is carried out, the surface roughness is less than 0.7, then the temperature is raised to 700-800 ℃ along with the furnace, the temperature is kept for 10-20h, and finally the air cooling is carried out to the room temperature.
CN202211139895.8A 2022-09-19 2022-09-19 Ferrite/martensite heat-resistant steel for lead-bismuth pile and preparation method thereof Pending CN115478220A (en)

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CN116377314A (en) * 2023-06-05 2023-07-04 成都先进金属材料产业技术研究院股份有限公司 Martensitic heat-resistant steel for gas turbine and smelting method thereof

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CN103898411A (en) * 2012-12-28 2014-07-02 中国科学院金属研究所 Liquid metal corrosion resistance martensite structural material for high temperature and preparation method of material
CN113528952A (en) * 2021-06-29 2021-10-22 中国原子能科学研究院 High-silicon high-chromium ferrite/martensite heat-resistant steel resistant to liquid lead or lead bismuth corrosion and preparation method thereof

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CN103898411A (en) * 2012-12-28 2014-07-02 中国科学院金属研究所 Liquid metal corrosion resistance martensite structural material for high temperature and preparation method of material
CN113528952A (en) * 2021-06-29 2021-10-22 中国原子能科学研究院 High-silicon high-chromium ferrite/martensite heat-resistant steel resistant to liquid lead or lead bismuth corrosion and preparation method thereof

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CN116377314A (en) * 2023-06-05 2023-07-04 成都先进金属材料产业技术研究院股份有限公司 Martensitic heat-resistant steel for gas turbine and smelting method thereof
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