CN114622141B - High-temperature oxidation resistant Zr-containing low-activation ferritic martensitic steel - Google Patents

High-temperature oxidation resistant Zr-containing low-activation ferritic martensitic steel Download PDF

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CN114622141B
CN114622141B CN202210279585.XA CN202210279585A CN114622141B CN 114622141 B CN114622141 B CN 114622141B CN 202210279585 A CN202210279585 A CN 202210279585A CN 114622141 B CN114622141 B CN 114622141B
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邱日盛
曾文
刘庆
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Chongqing University
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    • 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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    • 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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    • C21D8/0226—Hot rolling
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    • 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
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium 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
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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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    • 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
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/005—Ferrite
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    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/008—Martensite

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Abstract

The invention discloses a high-temperature oxidation resistant low-activation ferrite martensitic steel containing Zr, which comprises the following chemical components, by weight, 8.0-10.0 wt% of Cr, 0.2-1.0 wt% of Mn, 0.3-0.9 wt% of Si, 1.0-1.8 wt% of W, 0.15-0.25 wt% of C, 0.01-0.1 wt% of Ti, 0.1-0.3 wt% of V, 0.05-1.1 wt% of Zr, 0.01-0.1 wt% of N, less than 0.015wt% of P, less than 0.01wt% of S, and the balance of Fe and inevitable impurities. The high-temperature oxidation resistance of the ferrite/martensite steel is greatly improved, and the high-temperature oxidation resistance of the ferrite/martensite steel is at least 2-3 times that of the conventional common ferrite/martensite steel.

Description

High-temperature oxidation resistant low-activation ferrite martensitic steel containing Zr
Technical Field
The invention belongs to the technical field of metal materials, relates to martensitic steel, and particularly relates to low-activation martensitic steel containing Zr and resisting high-temperature oxidation.
Background
The common ferrite martensitic steel contains high-activation elements such as Mo, nb, ni, co, al and the like, and the activation period after neutron irradiation is long, which causes problems on the post-treatment of nuclear reactor structural materials. In order to solve this problem, low-activation ferrite/martensite steels containing low-activation elements as main components have been produced. Among the low-activation elements, cr, W, V, mn, ti, zr, ta, si, etc., which are commonly used in steel, have an effect of improving the high-temperature oxidation resistance of steel, but the contents of these elements also need to be controlled. For example, cr and Si are ferrite forming elements in steel, and the formation of delta ferrite is caused by too high content of Cr and Si, so that the mechanical property of the steel is reduced; mn element is added into steelThe diffusion of the matrix is accelerated and accelerated 23 C 6 Coarsening of carbides reduces the stability of the matrix.
Ferritic martensitic steel has been widely used as a structural material for key parts of boilers, turbines, etc. and is considered as a main candidate material for fourth-generation nuclear reactors because of its advantages of small thermal expansion coefficient, good thermal conductivity and thermal fatigue resistance, excellent creep resistance and oxidation resistance, and relatively low price.
Compared with the prior nuclear reactor technology, the fourth generation nuclear reactor has more severe working conditions and higher operating temperature range, the temperature of the fuel cladding can reach 650-700 ℃, and the material is required to have good high-temperature oxidation resistance. However, the maximum service temperature of the current common ferrite/martensite steel is lower than 600 ℃, and when the common ferrite/martensite steel is exposed for a long time at the temperature higher than the maximum service temperature, the common ferrite/martensite steel is seriously oxidized, so that the base material is gradually oxidized and corroded, and finally the mechanical property of the material is reduced. Therefore, how to improve the high temperature oxidation resistance of the ferrite/martensite steel so as to improve the maximum use temperature is a problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a Zr-containing low-activation ferritic martensitic steel with high-temperature oxidation resistance, which solves the problem that the highest service temperature of the existing ferritic martensitic steel is lower due to poor high-temperature oxidation resistance.
The technical scheme of the invention is as follows:
the chemical components of the martensite steel with Zr low activation and high temperature oxidation resistance comprise, by weight, 8.0-10.0 wt% of Cr, 0.2-1.0 wt% of Mn, 0.3-0.9 wt% of Si, 1.0-1.8 wt% of W, 0.15-0.25 wt% of C, 0.01-0.1 wt% of Ti, 0.1-0.3 wt% of V, 0.05-1.1 wt% of Zr, 0.01-0.1 wt% of N, less than 0.015wt% of P, less than 0.01wt% of S, and the balance of Fe and inevitable impurities.
Preferably, the chemical components of the high-temperature oxidation resistant Zr-containing low-activation ferrite martensite steel comprise, by weight, 8.0-10.0 wt% of Cr, 0.2-1.0 wt% of Mn, 0.3-0.9 wt% of Si, 1.0-1.8 wt% of W, 0.15-0.25 wt% of C, 0.01-0.1 wt% of Ti, 0.1-0.3 wt% of V, 0.1-1.1 wt% of Zr, 0.01-0.1 wt% of N, less than 0.015wt% of P, less than 0.01wt% of S, and the balance Fe and inevitable impurities.
Preferably, the chemical components of the high-temperature oxidation resistant Zr-containing low-activation ferrite martensite steel comprise, by weight, 8.0-10.0 wt% of Cr, 0.2-1.0 wt% of Mn, 0.3-0.9 wt% of Si, 1.0-1.8 wt% of W, 0.15-0.25 wt% of C, 0.01-0.1 wt% of Ti, 0.1-0.3 wt% of V, 0.3-1.1 wt% of Zr, 0.01-0.1 wt% of N, less than 0.015wt% of P, less than 0.01wt% of S, and the balance Fe and inevitable impurities.
Preferably, the chemical components of the high-temperature oxidation resistant Zr-containing low-activation ferritic martensitic steel in percentage by weight are 8.0-10.0 wt% of Cr, 0.2-1.0 wt% of Mn, 0.3-0.9 wt% of Si, 1.0-1.8 wt% of W, 0.15-0.25 wt% of C, 0.01-0.1 wt% of Ti, 0.1-0.3 wt% of V, 0.5-1.1 wt% of Zr, 0.01-0.1 wt% of N, less than 0.015wt% of P, less than 0.01wt% of S, and the balance Fe and inevitable impurities.
Preferably, the chemical components of the high-temperature oxidation resistant Zr-containing low-activation ferritic martensitic steel in percentage by weight are 8.5-9.5 wt% of Cr, 0.4-0.6 wt% of Mn, 0.5-0.7 wt% of Si, 1.4-1.7 wt% of W, 0.15-0.22 wt% of C, 0.01-0.02 wt% of Ti, 0.18-0.26 wt% of V, 0.1-1.1 wt% of Zr, 0.02-0.05 wt% of N, 0.01-0.013 wt% of P, 0.001-0.003 wt% of S, and the balance Fe and unavoidable impurities.
Preferably, the chemical components of the high-temperature oxidation resistant Zr-containing low-activation ferritic martensitic steel comprise, by weight, 8.5-9.5% of Cr, 0.4-0.6% of Mn, 0.5-0.7% of Si, 1.4-1.7% of W, 0.15-0.22% of C, 0.01-0.02% of Ti, 0.18-0.26% of V, 0.3-1.1% of Zr, 0.02-0.05% of N, 0.01-0.013% of P, 0.001-0.003% of S, and the balance Fe and inevitable impurities.
Preferably, the chemical components of the high-temperature oxidation resistant Zr-containing low-activation ferritic martensitic steel comprise, by weight, 8.5-9.5% of Cr, 0.4-0.6% of Mn, 0.5-0.7% of Si, 1.4-1.7% of W, 0.15-0.22% of C, 0.01-0.02% of Ti, 0.18-0.26% of V, 0.5-1.1% of Zr, 0.02-0.05% of N, 0.01-0.013% of P, 0.001-0.003% of S, and the balance Fe and inevitable impurities.
Preferably, the chemical components of the high-temperature oxidation resistant Zr-containing low-activation ferritic martensitic steel in percentage by weight are 9.5wt% of Cr, 0.49wt% of Mn, 0.62wt% of Si, 1.64wt% of W, 0.18wt% of C, 0.02wt% of Ti, 0.21wt% of V, 0.5wt% of Zr, 0.03wt% of N, 0.011wt% of P, 0.001wt% of S and the balance of Fe.
Preferably, the chemical components of the high-temperature oxidation resistant Zr-containing low-activation ferritic martensitic steel in percentage by weight are 8.9wt% of Cr, 0.44wt% of Mn, 0.60wt% of Si, 1.48wt% of W, 0.16wt% of C, 0.01wt% of Ti, 0.19wt% of V, 1.01wt% of Zr, 0.04wt% of N, 0.010wt% of P, 0.001wt% of S and the balance of Fe.
The processing technology of the Zr-containing low-activation ferritic martensitic steel with high temperature oxidation resistance comprises the following steps:
(1) Weighing raw material components according to the weight ratio and carrying out vacuum melting; (2) Forging at 950-1200 ℃, and cooling the blank to room temperature after forging; (3) Hot rolling at 850-1150 deg.c with single rolling deformation of 20-30% and total rolling deformation of 80%, and air cooling to room temperature; (4) Normalizing the rolled and formed plate at 950-1150 ℃ and tempering at 740-780 ℃.
The technical scheme of the invention has the following beneficial effects:
for the ferrite martensite steel which is in service for a long time and has the most extensive usage amount in a high-temperature environment, the problem of low high-temperature oxidation resistance is solved by increasing the Zr content, and the high-temperature oxidation resistance is at least 2-3 times of that of the current common ferrite martensite steel. And, it was found that the high temperature oxidation resistance thereof is improved as the Zr content is increased, but the high temperature oxidation resistance thereof is in a decreasing trend after the Zr content is increased to a certain value, and in the present invention, it was found that the high temperature oxidation resistance thereof is the best at 0.5% Zr content, which is 3.5 times that of the commercial T91 ferrite/martensite steel.
Drawings
FIG. 1 shows the surface oxide morphology after oxidizing in air at 650 ℃ for 400h in example 1 of the present invention.
FIG. 2 is the surface oxide morphology after the oxidation of example 2 of the present invention in air at 650 deg.C for 400 h.
FIG. 3 shows the surface oxide morphology after oxidizing example 3 in air at 650 ℃ for 400 h.
FIG. 4 is the surface oxide morphology after the oxidation of example 4 of the present invention in air at 650 deg.C for 400 h.
FIG. 5 is the morphology of the surface oxide of comparative example 1 of the present invention after oxidation in air at 650 ℃ for 400 h.
FIG. 6 is an oxidation weight gain curve of inventive examples 1-4 and comparative example 1 oxidized in air at 650 ℃ for 400 hours.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to fully understand the objects, features and effects of the invention. The present invention relates to a process or an apparatus, which is conventional in the art unless otherwise specified. The following noun terms have meanings commonly understood by those skilled in the art unless otherwise specified.
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
The high temperature oxidation resistant Zr-containing low activation ferrite martensitic steel comprises, by weight, 8.0-10.0 wt% of Cr, 0.2-1.0 wt% of Mn, 0.3-0.9 wt% of Si, 1.0-1.8 wt% of W, 0.15-0.25 wt% of C, 0.01-0.1 wt% of Ti, 0.1-0.3 wt% of V, 0.05-1.1 wt% of Zr, 0.01-0.1 wt% of N, less than 0.015wt% of P, less than 0.01wt% of S, and the balance Fe and inevitable impurities.
The Zr-containing low activation ferritic martensitic steel resistant to high temperature oxidation according to the present invention can be prepared by a conventional method in the art, for example, by the following method, according to the following steps: (1) Weighing raw material components according to the weight ratio and carrying out vacuum melting; (2) Forging at 950-1200 ℃, and cooling the blank to room temperature after forging; (3) Hot rolling at 850-1150 deg.c with single rolling deformation of 20-30% and total rolling deformation of 80%, and air cooling to room temperature; (4) Normalizing the rolled and formed plate at 950-1150 ℃ and tempering at 740-780 ℃.
The oxidation resistance measurement method in the following examples is as follows:
the high temperature oxidation resistance of the steel is characterized by the weight gain of the sample after oxidation in air at high temperature for a long time. The weight gain method is to calculate the oxidation weight gain value of the steel after the test is finished. Cutting a high-temperature oxidation sample on a steel plate after heat treatment, wherein the specification of the sample is a rectangle of 30 multiplied by 10 multiplied by 5mm, the thickness of the sample is uniform, the shape of the sample is regular, the surface of the sample is polished and polished to a mirror surface, all edges are polished smoothly, and finally, the sample is cleaned by acetone and alcohol and dried.
The sample should be measured to an accuracy of 0.02mm, at least 3 points measured, and the average taken. The analytical balance precision is 0.0001g, and the vernier caliper precision is 0.02mm.
The oxidation weight gain per unit area (K) was calculated by the following formula (1)
K＝(m 0 -m 1 )/(S 0 X t) formula (1)
In the formula (1), m 0 Mass of sample before test, g;
m 1 sample mass after test, g;
S 0 m is the original surface area of the sample 2 ；
t is the test time, h.
Example 1
The composition of the Zr-containing low activation ferritic martensitic steel resistant to high temperature oxidation of the present example is shown in table 1.
The preparation method of the Zr-containing low activation ferritic martensitic steel resistant to high temperature oxidation of this example is as follows:
(1) Weighing raw material components according to the weight ratio and carrying out vacuum melting; (2) forging: the initial forging temperature of the ingot blank is 1150 ℃, the final forging temperature is 950 ℃, and the blank is air-cooled to the room temperature after the forging is finished; (3) hot rolling: then hot rolling is carried out within the temperature range of 1000 ℃, the single rolling deformation is 20 percent, the total rolling deformation is 80 percent, and the steel is cooled to room temperature in air; (4) normalizing and tempering treatment: normalizing and tempering the rolled and formed plate, wherein the normalizing process is 980-30 min, and the tempering process is 760-90 min.
The appearance of the oxide on the surface of the obtained steel sample after being oxidized for 400 hours at 650 ℃ is shown in figure 1, the oxide is granular, the size is relatively fine and uniform, and the weight gain is 0.316mg/cm 2 。
Example 2
The composition of the Zr-containing low activation ferritic martensitic steel resistant to high temperature oxidation of this example is shown in table 1.
The method for preparing the Zr-containing low activation ferritic martensitic steel resistant to high temperature oxidation of this example is the same as that of example 1.
The appearance of the oxide on the surface of the obtained steel sample after being oxidized for 400 hours at 650 ℃ is shown in figure 2, the oxide is granular, the size is fine and uniform, and the weight gain is 0.272mg/cm 2 。
Example 3
The composition of the Zr-containing low activation ferritic martensitic steel resistant to high temperature oxidation of this example is shown in table 1.
The method of manufacturing the Zr-containing low activation ferritic martensitic steel resistant to high temperature oxidation of this example is the same as that of example 1.
The appearance of the oxide on the surface of the obtained steel sample after being oxidized for 400 hours at 650 ℃ is shown in figure 3, the oxide is granular, the size is relatively fine and uniform, and the weight gain is 0.180mg/cm 2 。
Example 4
The composition of the Zr-containing low activation ferritic martensitic steel resistant to high temperature oxidation of the present example is shown in table 1.
The method of manufacturing the Zr-containing low activation ferritic martensitic steel resistant to high temperature oxidation of this example is the same as that of example 1.
The appearance of the oxide on the surface of the obtained steel sample after being oxidized for 400 hours at 650 ℃ is shown in figure 4, the oxide is granular, the size is relatively fine and uniform, and the weight gain is 0.196mg/cm 2 。
Comparative example 1
Commercial T91 ferritic/martensitic steel was used, the composition of which is shown in table 1.
Steel sampleThe morphology of the surface oxide after oxidation at 650 ℃ for 400 hours is shown in FIG. 5, the shape of the oxide is composed of large-sized lamellar particles and small-sized particles, and the weight gain is 0.624mg/cm 2 。
The oxidation kinetics curves of examples 1-4 and comparative example 1 are shown in fig. 6, and it can be seen that the high temperature oxidation resistance of examples 1-4 is significantly better than that of comparative example 1. In examples 1 to 4, the oxidation weight gain exhibited a phenomenon of decreasing first and then increasing as the Zr content increased, and the high temperature oxidation resistance of example 3 was the best, about 3.5 times as high temperature oxidation resistance of comparative example 1.
TABLE 1 chemical composition (wt%) of ferritic martensitic steel
Figure BDA0003556319980000051
Figure BDA0003556319980000061

Claims (6)

1. A low activation ferritic martensitic steel containing Zr resistant to high temperature oxidation, characterized in that: the chemical components by weight percentage are 8.5 to 9.5 weight percent of Cr, 0.4 to 0.6 weight percent of Mn, 0.5 to 0.7 weight percent of Si, 1.4 to 1.7 weight percent of W, 0.15 to 0.22 weight percent of C, 0.01 to 0.02 weight percent of Ti, 0.18 to 0.26 weight percent of V, 0.1 to 1.1 weight percent of Zr, 0.02 to 0.05 weight percent of N, 0.01 to 0.013 weight percent of P, 0.001 to 0.003 weight percent of S, and the balance of Fe and inevitable impurities.
2. The Zr-containing low activation ferritic martensitic steel as claimed in claim 1 being resistant to high temperature oxidation characterized in that: the chemical components by weight percentage are 8.5 to 9.5 weight percent of Cr, 0.4 to 0.6 weight percent of Mn, 0.5 to 0.7 weight percent of Si, 1.4 to 1.7 weight percent of W, 0.15 to 0.22 weight percent of C, 0.01 to 0.02 weight percent of Ti, 0.18 to 0.26 weight percent of V, 0.3 to 1.1 weight percent of Zr, 0.02 to 0.05 weight percent of N, 0.01 to 0.013 weight percent of P, 0.001 to 0.003 weight percent of S, and the balance of Fe and inevitable impurities.
3. The Zr containing low activation ferritic martensitic steel as claimed in claim 2 being resistant to high temperature oxidation characterized in that: the chemical components by weight percentage are 8.5 to 9.5 weight percent of Cr, 0.4 to 0.6 weight percent of Mn, 0.5 to 0.7 weight percent of Si, 1.4 to 1.7 weight percent of W, 0.15 to 0.22 weight percent of C, 0.01 to 0.02 weight percent of Ti, 0.18 to 0.26 weight percent of V, 0.5 to 1.1 weight percent of Zr, 0.02 to 0.05 weight percent of N, 0.01 to 0.013 weight percent of P, 0.001 to 0.003 weight percent of S, and the balance of Fe and inevitable impurities.
4. The Zr-containing low activation ferritic martensitic steel as claimed in claim 1 being resistant to high temperature oxidation characterized in that: the chemical components by weight percentage are 9.5wt% of Cr, 0.49wt% of Mn, 0.62wt% of Si, 1.64wt% of W, 0.18wt% of C, 0.02wt% of Ti, 0.21wt% of V, 0.5wt% of Zr, 0.03wt% of N, 0.011wt% of P, 0.001wt% of S and the balance of Fe.
5. The Zr-containing low activation ferritic martensitic steel as claimed in claim 1 being resistant to high temperature oxidation characterized in that: the chemical components by weight percentage are 8.9wt% of Cr, 0.44wt% of Mn, 0.60wt% of Si, 1.48wt% of W, 0.16wt% of C, 0.01wt% of Ti, 0.19wt% of V, 1.01wt% of Zr, 0.04wt% of N, 0.010wt% of P, 0.001wt% of S and the balance of Fe.
6. The Zr low-activation ferritic martensitic steel with resistance to high-temperature oxidation according to any one of claims 1 to 5, characterized in that the processing of said Zr low-activation ferritic martensitic steel with resistance to high-temperature oxidation comprises the following steps:
(1) Weighing raw material components according to the weight ratio and carrying out vacuum melting; (2) Forging at 950-1200 ℃, and cooling the blank to room temperature after forging; (3) Hot rolling at 850-1150 deg.c with single rolling deformation of 20-30% and total rolling deformation of 80%, and air cooling to room temperature; (4) Normalizing the rolled and formed plate at 950-1150 ℃ and tempering at 740-780 ℃.
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CN113913706A (en) * 2021-10-14 2022-01-11 中国科学院合肥物质科学研究院 Anti-irradiation low-activation steel-based structural material capable of forming self-healing hydrogen permeation resistant layer through thermal oxidation

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JP2000290756A (en) * 1999-04-06 2000-10-17 Sumitomo Metal Ind Ltd HIGH Cr MARTENSITIC HEAT RESISTANT STEEL EXCELLENT IN HOT WORKABILITY
JP2010065322A (en) * 2009-12-04 2010-03-25 Babcock Hitachi Kk Ferritic heat resistant steel
CN103305765A (en) * 2013-06-14 2013-09-18 中国科学院金属研究所 Low activation martensitic steel with resistance to high temperature oxidation and high strength
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