CN117187705A - Heat treatment method of low-Cr and high-toughness alloy - Google Patents
Heat treatment method of low-Cr and high-toughness alloy Download PDFInfo
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Abstract
The application discloses a heat treatment method of a low-Cr and high-strength and high-toughness alloy, and belongs to the technical field of novel structural materials. The low Cr and high strength and toughness alloy consists of Cr, al, mo, nb, si, V, hf, ga, ni, la, fe and impurities, is processed by combining high-temperature solid solution, low-temperature rolling and twice annealing heat treatment processes, and simultaneously regulates and controls heat treatment process parameters, so that the alloy with different grain states is obtained, and has high mechanical strength and high toughness at room temperature and excellent mechanical property at a high temperature of 400 ℃.
Description
Technical Field
The application belongs to the technical field of novel structural materials, and particularly relates to a heat treatment method of a low-Cr high-strength and high-toughness alloy.
Background
The nuclear industry field puts higher demands on accident fault tolerance and related service performance of fuel cladding materials of nuclear reactors, wherein high strength and high toughness performance under room temperature and high temperature conditions are particularly important.
The traditional nuclear reactor fuel cladding material is a zirconium alloy material, and the zirconium alloy material has very excellent service performance, but has very low fault tolerance rate, and the characteristics that the zirconium alloy is contacted with water vapor to rapidly generate a large amount of hydrogen and cause hydrogen explosion when an accident occurs bring about great hidden trouble. Therefore, the development of FeCrAl alloy with higher accident fault tolerance rate is improved on the schedule in the field of nuclear industry, the toughness of the alloy can be obviously enhanced by the lower Cr content, and meanwhile, the high-density solid solution second phase in the FeCrAl alloy has the characteristics of capturing irradiation defects and inhibiting irradiation damage and has very excellent high-temperature irradiation damage resistance. Therefore, the high-performance FeCrAl alloy becomes the nuclear fuel cladding material with the most commercial prospect in the construction of advanced four-generation reactors and nuclear fusion reactors, has wide development and application prospect, but the currently developed FeCrAl alloy has the defects of high strength and poor plasticity all the time and has particularly weak high-temperature performance.
Disclosure of Invention
The application discloses a heat treatment method of a low-Cr and high-strength-toughness alloy, which aims to further improve the commercial value of FeCrAl alloy. The alloy prepared by the method has high mechanical strength and toughness at room temperature and excellent mechanical properties at a high temperature of 400 ℃.
In order to achieve the above purpose, the present application provides the following technical solutions:
the low Cr and high strength and toughness alloy comprises the following components in percentage by mass: cr:12.5-14.5%, al:3.5-5.5%, mo:1.5-2.5%, nb:1-3%, si:0.1-0.3%, V:0.1-0.2%, hf:0.1-0.2%, ga:0-0.2%, ni:0.1-0.2%, la:0.05-0.1%, C: less than or equal to 0.008 percent, N: less than or equal to 0.005 percent, O: less than or equal to 0.003 percent, and the balance of iron. The alloy also contains impurities, the impurity content accords with the standards of the current commercial industrial pure iron and ferritic stainless steel, and the impurity content is not taken as a discussion content in the application, so the impurity content is neglected.
Preferably, the total mass percentage content of the Cr, al and Si alloy elements is more than or equal to 16.5%, so that the better room-temperature mechanical strength of the FeCrAl-based alloy can be maintained, and meanwhile, in order to prevent the alloy from being broken in the running and processing preparation processes of a reactor caused by the aggravation of the hardening and embrittlement tendency of the FeCrAl-based alloy, the content of Cr and Al should be strictly controlled and reduced on the basis of ensuring that the FeCrAl-based alloy has better high-temperature steam oxidation resistance.
Preferably, the total mass percentage content of Mo, nb, V and Ga alloy elements is more than or equal to 3 percent, so that a large number of dispersed Laves second phase particles can be separated out, and the room temperature mechanical property and the high temperature strength of the alloy are improved.
The application also provides a heat treatment method of the low Cr and high strength and toughness alloy, which comprises the following steps: the components are weighed according to the mass percentage to prepare a steel billet, the steel billet is hot rolled, and then the hot rolled plate is subjected to high-temperature solid solution, low-temperature rolling and two annealing heat treatments.
Preferably, the high temperature solid solution is solid solution at 1150 ℃ for 2 hours.
Preferably, the low-temperature rolling is to roll at 450 ℃ to a set thickness, the rolling ratio is 50%, air cooling is performed after rolling, and then cold rolling straightening is performed.
Preferably, the two annealing heat treatments include: the first high-temperature annealing temperature is 800-1200 ℃, the annealing time is 15-180s, and then water cooling is carried out; the second stage low temperature annealing temperature is 550-700 deg.c, annealing time is 30-120min, and the product is air cooled to room temperature.
The low Cr and high strength alloy with better strength and toughness can be prepared through the annealing combination of two passes at different temperatures and times, the room temperature strength and the room temperature toughness are excellent, the energy consumption can be obviously reduced, and the preparation cost is reduced.
The application also provides application of the low-Cr high-strength and high-toughness alloy in preparing nuclear reactor fuel cladding materials, aeroengine structural materials or power plant steam pipeline structural materials.
Compared with the prior art, the application has the following advantages and technical effects:
the application adopts the preferable Cr, al, mo, nb, si, V, hf, ga, ni, la component range, and the lower Cr and Al contents avoid the problems of serious hardening and embrittlement degree of FeCrAl-based alloy materials under the conditions of thermal aging and irradiation of the reactor operation condition; proper amounts of Mo, nb, si, V, hf and other microalloying elements and proper heat treatment processes can refine FeCrAl-based alloy matrix grains, obviously improve the strong plasticity of the alloy at room temperature, and obviously improve the recrystallization temperature and high-temperature strength of the alloy at high temperature, so that the structural stability of the total alloy at high temperature is obviously improved. The action of the alloying elements in this range, and in combination with the heat treatment process, produces the following effects, which are mainly manifested as: after the alloy is processed by high-temperature solid solution, low-temperature rolling and twice annealing heat treatment processes, the alloy in different grain states is obtained by regulating and controlling the heat treatment processes, and the Laves second phase distributed in a fine dispersion way in the finished alloy is provided, so that the mechanical properties (room temperature toughness and high temperature strength) of the alloy are obviously improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the application. In the drawings:
FIG. 1 is a heat treatment process flow of a low Cr and high strength alloy according to an embodiment of the present application;
FIG. 2 is a graph of grain size of the alloy prepared in example 9;
FIG. 3 is a Laves phase distribution plot (BSE) of the alloy prepared in example 9;
FIG. 4 is a Laves phase size diagram of the alloy prepared in example 10;
FIG. 5 is a plot of the mechanical elongation at room temperature of the alloy prepared in example 8.
Detailed Description
Various exemplary embodiments of the application will now be described in detail, which should not be considered as limiting the application, but rather as more detailed descriptions of certain aspects, features and embodiments of the application.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the application. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present application. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the application described herein without departing from the scope or spirit of the application. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present application. The specification and examples of the present application are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
The "room temperature" as used herein is calculated as 25.+ -. 2 ℃ unless otherwise indicated.
The raw materials used in the following examples of the present application are all commercially available.
The application relates to a FeCrAl-based alloy with low Cr for nuclear reactor fuel element cladding materials, which comprises the following components in percentage by mass: cr:12.5-14.5%, al:3.5-5.5%, mo:1.5-2.5%, nb:1-3%, si:0.1-0.3%, V:0.1-0.2%, hf:0.1-0.2%, ga:0-0.2%, ni:0.1-0.2%, la:0.05-0.1%, C: less than or equal to 0.008 percent, N: less than or equal to 0.005 percent, O: less than or equal to 0.003 percent, the balance being iron and impurities, the impurity content accords with the current standard of commercial industry pure iron and ferrite stainless steel. Preferably Cr:12.8%, al:4.3%, mo:2.0%, nb:1.0%, si:0.15%, V:0.15%, hf:0.15%, ga:0.1%, ni:0.15%, la:0.05%, C: less than or equal to 0.008 percent, N: less than or equal to 0.005 percent, O: less than or equal to 0.003 percent, and the balance being iron, and the impurity content accords with the standards of the prior commercial industry pure iron and ferrite stainless steel.
The technical scheme for realizing the aim of the application is as follows: the FeCrAl-based multi-element alloy material with low Cr comprises no less than 16.5 percent of Cr, al and Si alloy elements in total weight so as to maintain better high-temperature oxidation performance and corrosion resistance; the total weight percentage content of Mo, nb, V and Ta alloy elements is not less than 3 percent, so that a large number of dispersed Laves second phase particles can be separated out, and the room temperature mechanical property and the high temperature strength of the alloy are improved.
The further technical scheme for realizing the aim of the application is as follows: a FeCrAl-based multi-element alloy material is prepared by preparing a steel billet from a test alloy according to the mass percentage of chemical components in the processing process, heating the steel billet to 1150 ℃ for solid solution, rolling to set thickness, rolling to 50%, air-cooling after rolling, carrying out twice annealing after cold rolling and straightening, wherein the high-temperature annealing temperature of the first pass is 800-1200 ℃, the annealing time is 15-180s, preferably 15-30s, and then water-cooling; and then carrying out second-pass low-temperature annealing at 550-700 ℃ for 30-120min, taking out and air-cooling to room temperature, avoiding the growth of Laves second-phase particles in the processing and heat treatment processes, obtaining fine second-phase particles, and ensuring the room-temperature strengthening effect of the alloy. The process before the two annealing treatments is not an innovation point of the application, so that the process is operated by a conventional method in the field without redundant description.
The following examples serve as further illustrations of the technical solutions of the application.
FIG. 1 shows the heat treatment process flow of the low Cr and high strength and toughness alloy of the present application.
Example 1
The low Cr and high strength and toughness alloy comprises the following components in percentage by mass: cr:12.8%, al:4.3%, mo:2.0%, nb:1.0%, si:0.15%, V:0.15%, hf:0.15%, ga:0.1%, ni:0.15%, la:0.05%, C: less than or equal to 0.008 percent, N: less than or equal to 0.005 percent, O: less than or equal to 0.003 percent, and the balance being iron, and the impurity content accords with the standards of the prior commercial industry pure iron and ferrite stainless steel.
Preparing the alloy into a steel billet according to the mass percentage of chemical components, heating the steel billet to 1150 ℃ for solid solution for 2 hours, rolling the steel billet into a set thickness at 450 ℃, rolling the steel billet with a rolling ratio of 50%, air-cooling the steel billet after rolling, and carrying out twice annealing after cold rolling and straightening.
The two-pass annealing steps are as follows:
(1) High-temperature annealing: the alloy steel is put into a resistance furnace preheated to 800 ℃, kept for 30 seconds and then cooled with water.
(2) And (3) low-temperature annealing: and (3) placing the alloy steel which is quenched and cooled to the room temperature into a resistance furnace preheated to 700 ℃, preserving the heat for 30min, and taking out and air-cooling to the room temperature.
Example 2
The difference from example 1 is that the two-pass annealing step is:
(1) High-temperature annealing: the alloy steel is put into a resistance furnace preheated to 800 ℃, kept for 60 seconds and then cooled with water.
(2) And (3) low-temperature annealing: and (3) placing the alloy steel which is quenched and cooled to the room temperature into a resistance furnace preheated to 650 ℃, preserving heat for 60 minutes, and taking out and air-cooling to the room temperature.
Example 3
The difference from example 1 is that the two-pass annealing step is:
(1) High-temperature annealing: the alloy steel is put into a resistance furnace preheated to 900 ℃, kept for 15 seconds and then cooled with water.
(2) And (3) low-temperature annealing: and (3) placing the alloy steel which is quenched and cooled to the room temperature into a resistance furnace preheated to 650 ℃, preserving heat for 30min, and taking out and air-cooling to the room temperature.
Example 4
The difference from example 1 is that the two-pass annealing step is:
(1) High-temperature annealing: the alloy steel is put into a resistance furnace preheated to 900 ℃, kept for 30 seconds and then cooled with water.
(2) And (3) low-temperature annealing: and (3) placing the alloy steel which is quenched and cooled to the room temperature into a resistance furnace preheated to 600 ℃, preserving the heat for 60 minutes, and taking out and air-cooling to the room temperature.
Example 5
The difference from example 1 is that the two-pass annealing step is:
(1) High-temperature annealing: the alloy steel is put into a resistance furnace preheated to 1000 ℃, kept for 15 seconds and then cooled with water.
(2) And (3) low-temperature annealing: and (3) placing the alloy steel which is quenched and cooled to the room temperature into a resistance furnace preheated to 650 ℃, preserving heat for 60 minutes, and taking out and air-cooling to the room temperature.
Example 6
The difference from example 1 is that the two-pass annealing step is:
(1) High-temperature annealing: the alloy steel is put into a resistance furnace preheated to 1000 ℃, kept for 30 seconds and then cooled with water.
(2) And (3) low-temperature annealing: and (3) placing the alloy steel which is quenched and cooled to the room temperature into a resistance furnace preheated to 600 ℃, preserving heat for 120min, and taking out and air-cooling to the room temperature.
Example 7
The difference from example 1 is that the two-pass annealing step is:
(1) High-temperature annealing: the alloy steel is put into a resistance furnace preheated to 1100 ℃, kept for 15 seconds and then cooled with water.
(2) And (3) low-temperature annealing: and (3) placing the alloy steel which is quenched and cooled to the room temperature into a resistance furnace preheated to 600 ℃, preserving the heat for 60 minutes, and taking out and air-cooling to the room temperature.
Example 8
The difference from example 1 is that the two-pass annealing step is:
(1) High-temperature annealing: the alloy steel is put into a resistance furnace preheated to 1100 ℃, kept for 30 seconds and then cooled with water.
(2) And (3) low-temperature annealing: and (3) placing the alloy steel which is quenched and cooled to the room temperature into a resistance furnace preheated to 550 ℃, preserving heat for 120min, and taking out and air-cooling to the room temperature.
Example 9
The difference from example 1 is that the two-pass annealing step is:
(1) High-temperature annealing: the alloy steel is put into a resistance furnace preheated to 1200 ℃, kept for 15 seconds, and then cooled with water.
(2) And (3) low-temperature annealing: and (3) placing the alloy steel which is quenched and cooled to the room temperature into a resistance furnace preheated to 650 ℃, preserving heat for 60 minutes, and taking out and air-cooling to the room temperature.
Example 10
The difference from example 1 is that the two-pass annealing step is:
(1) High-temperature annealing: the alloy steel is put into a resistance furnace preheated to 1200 ℃, kept for 15 seconds, and then cooled with water.
(2) And (3) low-temperature annealing: and (3) placing the alloy steel which is quenched and cooled to the room temperature into a resistance furnace preheated to 550 ℃, preserving heat for 120min, and taking out and air-cooling to the room temperature.
Comparative example 1
The difference is that the step of two-pass annealing is omitted as in example 1.
Performance test:
the tensile test was performed on the above examples and comparative examples according to GB/T2975-2018 steel and steel product mechanical property test sampling positions and sample preparation standards, and the results are shown in Table 1.
TABLE 1
Remarks: the numerical sequence of the heat treatment process is as follows: high temperature annealing temperature-high temperature annealing time(s) -low temperature annealing temperature-low temperature annealing time (min).
The grain size of the material is mainly determined by the temperature and time of the high temperature annealing section, and the higher the temperature, the stronger the driving force provided to the recrystallization process, wherein fig. 2 is a graph of the grain size of the alloy prepared in example 9. As can be seen from FIG. 2, the average grain size is about 40-60 μm, and the room temperature mechanical property and the high temperature mechanical property of the material subjected to the twice annealing are obviously improved, which is related to the formation and growth of the dispersed Laves phase in the twice annealing process. The distribution diagram of Laves phase at subgrain boundaries in the crystal of example 9 is shown in fig. 3, the size diagram of Laves phase of example 10 is shown in fig. 4, and it can be seen that Laves phase is dispersed and distributed in subgrain boundaries and crystal, the effect of improving mechanical properties of the material is good, and the mechanical stretching curve of the alloy prepared in example 8 at room temperature is shown in fig. 5.
In connection with the discussion above and Table 1, it can be seen from examples 1 to 10 that: when the alloy composition is determined, the temperature of the first annealing is raised to help improve the toughness of the material, and the temperature and time of the first annealing mainly determine the size of grains; the temperature and time of the second annealing are mainly used for regulating and controlling the precipitated Laves phase, and the pinning effect of the second phase particles in the grain boundary migration process plays a role in enhancing the room temperature strength and the high temperature strength of the material.
Example 11
The difference from example 8 is that the Ga content is 0%, specifically: the low Cr and high strength and toughness alloy comprises the following components in percentage by mass: cr:12.8%, al:4.3%, mo:2.0%, nb:1.0%, si:0.15%, V:0.15%, hf:0.15%, ga:0%, ni:0.15%, la:0.05%, C: less than or equal to 0.008 percent, N: less than or equal to 0.005 percent, O: less than or equal to 0.003 percent, and the balance being iron, and the impurity content accords with the standards of the prior commercial industry pure iron and ferrite stainless steel.
After the treatment, the alloy is subjected to tensile test, the room temperature yield strength of the alloy is 632MPa, the tensile strength of the alloy is 807MPa, and the elongation of the alloy is 10.42%; the high-temperature tensile strength at 400 ℃ is 561MPa.
Comparative example 2
The difference from example 8 is that the total mass percentage content of Cr, al and Si alloy elements is less than 16.5%, specifically: the low Cr and high strength and toughness alloy comprises the following components in percentage by mass: cr:12.5%, al:3.5%, mo:2.0%, nb:1.0%, si:0.1%, V:0.15%, hf:0.15%, ga:0.1%, ni:0.15%, la:0.05%, C: less than or equal to 0.008 percent, N: less than or equal to 0.005 percent, O: less than or equal to 0.003 percent, and the balance being iron, and the impurity content accords with the standards of the prior commercial industry pure iron and ferrite stainless steel.
After the treatment, the alloy is subjected to a tensile test, the room temperature yield strength of the alloy is 627MPa, the tensile strength is 793MPa, and the elongation is 11.41%; the high-temperature tensile strength at 400 ℃ is 550MPa.
Comparative example 3
The difference from example 8 is that the total mass percentage content of Mo, nb, V and Ga alloy elements is less than 3%, specifically: the low Cr and high strength and toughness alloy comprises the following components in percentage by mass: cr:12.8%, al:4.3%, mo:1.5%, nb:1.0%, si:0.15%, V:0.1%, hf:0.15%, ga:0.1%, ni:0.15%, la:0.05%, C: less than or equal to 0.008 percent, N: less than or equal to 0.005 percent, O: less than or equal to 0.003 percent, and the balance being iron, and the impurity content accords with the standards of the prior commercial industry pure iron and ferrite stainless steel.
After the treatment, the alloy is subjected to a tensile test, the room temperature yield strength of the alloy is 604MPa, the tensile strength is 764MPa, and the elongation is 9.42%; the high-temperature tensile strength at 400 ℃ is 524MPa.
Comparative example 4
The difference is that the content of Mo element is replaced by Nb in equal mass percent as in example 8.
After the treatment, the alloy is subjected to a tensile test, the room temperature yield strength of the alloy is 613MPa, the tensile strength is 803MPa, and the elongation is 7.63%; the high-temperature tensile strength at 400 ℃ is 562MPa.
Comparative example 5
The difference from example 8 is that the first pass high temperature annealing step was omitted and the second pass low temperature annealing was directly performed after the low temperature rolling.
After the treatment, the alloy is subjected to a tensile test, the room temperature yield strength of the alloy is 627MPa, the tensile strength is 862MPa, and the elongation is 5.23%; the high-temperature tensile strength at 400 ℃ is 582MPa.
Comparative example 6
The difference from example 8 is that the second low temperature annealing step is omitted and only the first high temperature annealing step is performed.
After the treatment, the alloy is subjected to a tensile test, the room temperature yield strength of the alloy is 557MPa, the tensile strength is 726MPa, and the elongation is 12.32%; the high-temperature tensile strength at 400 ℃ is 502MPa.
Comparative example 7
The difference from example 8 is that the first pass high temperature anneal temperature is 1300 c and the anneal time is 180s.
After the treatment, the alloy is subjected to a tensile test, the room temperature yield strength of the alloy is 537MPa, the tensile strength is 692MPa, and the elongation is 11.61%; the high-temperature tensile strength at 400 ℃ is 482MPa.
Comparative example 8
The difference from example 8 is that the second pass low temperature annealing temperature was 800℃and the annealing time was 25 minutes.
After the treatment, the alloy is subjected to a tensile test, the room temperature yield strength of the alloy is 604MPa, the tensile strength is 764MPa, and the elongation is 9.77%; the high-temperature tensile strength at 400 ℃ is 504MPa.
The present application is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present application are intended to be included in the scope of the present application. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.
Claims (8)
1. The low Cr and high strength and toughness alloy is characterized by comprising the following components in percentage by mass: cr:12.5-14.5%, al:3.5-5.5%, mo:1.5-2.5%, nb:1-3%, si:0.1-0.3%, V:0.1-0.2%, hf:0.1-0.2%, ga:0-0.2%, ni:0.1-0.2%, la:0.05-0.1%, C: less than or equal to 0.008 percent, N: less than or equal to 0.005 percent, O: less than or equal to 0.003 percent, and the balance of iron.
2. The low-Cr and high-strength and high-toughness alloy according to claim 1, wherein the total mass percentage content of Cr, al and Si is not less than 16.5%.
3. The low-Cr and high-strength and high-toughness alloy according to claim 1, wherein the total mass percentage content of Mo, nb, V and Ga is not less than 3%.
4. A method for heat treatment of a low Cr and high strength and toughness alloy according to any one of claims 1 to 3, comprising the steps of: the components are weighed according to the mass percentage to prepare a steel billet, the steel billet is hot rolled, and then the hot rolled plate is subjected to high-temperature solid solution, low-temperature rolling and two annealing heat treatments.
5. The heat treatment method of a low Cr and high toughness alloy according to claim 4, wherein said high temperature solid solution is solid solution at 1150 ℃ for 2 hours.
6. The heat treatment method of low Cr and high toughness alloy according to claim 4, wherein the low temperature rolling is performed at a temperature of 450 ℃ to a set thickness, the rolling ratio is 50%, and the alloy is subjected to air cooling after rolling and then is straightened by cold rolling.
7. The method of heat treating a low Cr and high strength and toughness alloy according to claim 4, wherein the two annealing heat treatments include: the first high-temperature annealing temperature is 800-1200 ℃, the annealing time is 15-180s, and then water cooling is carried out; the second stage low temperature annealing temperature is 550-700 deg.c, annealing time is 30-120min, and the product is air cooled to room temperature.
8. Use of a low Cr and high strength alloy as claimed in any one of claims 1 to 3 in the preparation of nuclear reactor fuel cladding materials, aeroengine structural materials or power plant steam conduit structural materials.
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