CN110004367B - Preparation method of oxide dispersion strengthened FeCrAl alloy pipe - Google Patents
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- 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
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/10—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies
- C21D8/105—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies of ferrous alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
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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
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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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
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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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
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- 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
- C22C38/18—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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- 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
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/24—Ferrous alloys, e.g. steel alloys containing chromium with vanadium
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- 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
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/28—Ferrous alloys, e.g. steel alloys containing chromium with titanium or zirconium
Abstract
The invention belongs to the technical field of nuclear power pipe preparation, and particularly discloses a preparation method of an Oxide Dispersion Strengthened (ODS) FeCrAl alloy pipe for a nuclear fuel cladding material, aiming at realizing the localization of a high-strength ODS-FeCrAl alloy thin-wall pipe. The preparation of the ODS-FeCrAl alloy pipe adopts a cold rolling and pass heat treatment process, and is characterized in that: the rolling speed is controlled to be 100-600 r/min, and the deformation of the pipe is controlled to be 10-50%. The heat treatment of each pass adopts a vacuum annealing mode, the annealing temperature is 700-1050 ℃, and the heat preservation time is 30-90 minutes. The preparation method of the tube does not influence the particle size and dispersion state of the Y-Al-O oxide strengthening phase in the ODS-FeCrAl alloy, the prepared tube has a crystal structure with fine grains and uniform tissue, and the ODS tube has excellent strength and creep resistance as well as excellent oxidation resistance and radiation swelling resistance.
Description
Technical Field
The invention belongs to the technical field of nuclear power pipe preparation, and particularly relates to a preparation method of an Oxide Dispersion Strengthened (ODS) FeCrAl alloy pipe for a nuclear fuel cladding material.
Background
In 2011, nuclear power safety crisis caused by tsunami in a nuclear power plant in fukushima of japan promotes global nuclear power safety awareness to an unprecedented level, and research and development of accident fault-tolerant fuels are carried forward. Fault tolerant fuels are designed to resist severe accident conditions for extended periods of time while ensuring performance under normal operating conditions comparable to or better than existing fuel systems. Oxide Dispersion strengthening (Oxide Dispersion)The on Strengthheened, ODS) FeCrAl alloy is one of candidate materials for accident fault-tolerant fuel cladding due to the advantages of excellent creep resistance, oxidation resistance, radiation swelling resistance, small neutron economic loss, high strength and the like. Different from an as-cast FeCrAl alloy, the ODS-FeCrAl alloy matrix contains high-density dispersion distribution and nano-size Y2O3And Y-Al-O oxide particles inhibit grain boundary and dislocation movement through pinning in plastic deformation or dislocation creep, so that the hardness and strength of the alloy are remarkably increased and the plasticity and ductility are reduced.
The high-strength ODS-FeCrAl alloy brings processing difficulty to the pipe, and is especially used for preparing a thin-wall pipe. At present, the ODS-FeCrAl pipes which are successfully rolled and reported are only the MA956 USA and the PM2000 series Germany. The development and preparation of ODS-FeCrAl alloy in China are relatively late, the nuclear power equipment and materials are mostly imported, and the backward of the materials severely restricts the development of the nuclear power industry in China. In order to break through the monopoly abroad, a series of ODS-FeCrAl alloy pipes are prepared by adopting a cold rolling mode on the basis of material preparation, and fine and dispersed Y-Al-O composite oxides in the alloy ensure excellent mechanical properties, oxidation resistance, corrosion resistance and wear resistance.
Disclosure of Invention
The invention provides a preparation method of an ODS-FeCrAl alloy pipe for a nuclear fuel cladding material, and aims to break the monopoly of preparation of foreign high-strength ODS-FeCrAl alloy pipes. The invention adopts a cold rolling and pass heat treatment mode, reduces the nonuniformity of tube blank preparation by regulating and controlling pass reduction quantity, heat treatment conditions and pass diameter/wall ratio, and obtains the ODS-FeCrAl precision tube with Y-Al-O nano oxide dispersion distribution and small grain size.
The technical scheme of the invention is as follows:
a preparation method of an ODS-FeCrAl alloy pipe is characterized by comprising the following steps:
A) preparing ODS-FeCrAl alloy powder by using a mechanical alloying method or an internal oxidation method;
B) implementing ODS-FeCrAl alloying by using a hot isostatic pressing process;
C) after sheath removal, hot forging the alloy into a rod;
D) after heat treatment, a tube blank is manufactured by adopting a piercing process;
E) and reducing the diameter and/or the wall thickness of the tube blank by adopting a cold rolling and pass heat treatment process until the tube with the size requirement is obtained.
The preparation method of the ODS-FeCrAl alloy pipe is characterized by comprising the following steps: the ODS-FeCrAl alloy prepared by hot isostatic pressing or hot extrusion is subjected to decoating and then forging treatment, wherein the hot forging temperature is 1100-1250 ℃. Turning the bar stock after hot forging to remove surface defects, then perforating the bar stock, carrying out short-time heat treatment on the bar stock before perforation, releasing the processing stress remained in the previous procedure, keeping the temperature at 800-1000 ℃ for 40-80 minutes, and rolling the steel blank into a primary tube blank by adopting a periodic tube rolling mill.
The preparation method of the ODS-FeCrAl alloy pipe is characterized by comprising the following steps: and cold rolling at room temperature at a rolling speed of 100-600 rpm. In the cold rolling process, the alloy pipe needs to be subjected to stress relief annealing once for rolling, and the reasons are that the ODS-FeCrAl alloy has high strength, large deformation resistance and strong work hardening, and stress concentration and cracking are easy to occur in the deformation process. The heat treatment adopts a vacuum annealing mode, the annealing temperature is 700-1150 ℃, and the heat preservation time is 30-90 minutes. Unlike FeCrAl alloy, the ODS-FeCrAl alloy has a high complete recrystallization temperature (more than 1350 ℃) and the annealing temperature is set below the ODS-FeCrAl alloy complete recrystallization temperature. If the annealing temperature is too low and the time is short, the stress of the pipe still exists, and the pipe is cracked due to stress concentration during the next rolling; if the annealing temperature is too high and the annealing time is longer, the possibility of growing Y-Al-O composite nano oxide particles in the ODS alloy exists, the strengthening effect of precipitated phase particles on the alloy is reduced, and therefore the heat treatment condition of each pass is considered according to the alloy components and the stability of the precipitated phase of the oxide.
The preparation method of the ODS-FeCrAl alloy pipe is characterized by comprising the following steps: the deformation of the sectional area of the tube of each pass of rolled tube is 10-50 percent; the deformation of the rolled tube is gradually increased along with the gradual reduction of the tube diameter and the wall thickness, and is increased from the initial 10-30 percent to 30-50 percent.
The preparation method of the ODS-FeCrAl alloy pipe is characterized by comprising the following steps: the ODS-FeCrAl alloy pipe mainly comprises 14-22 wt% of Cr, 3-5 wt% of Al, 0.15-0.5 wt% of Y and the balance of Fe, and preferably mainly comprises 14-20 wt% of Cr, 3-5 wt% of Al, 0.2-0.4 wt% of Y and the balance of Fe. The content of other alloy elements such as Ti, W, V, Zr, Si and the like can be designed according to actual needs.
The advantages of the invention are as follows: the processing of the high-strength ODS-FeCrAl alloy pipe is completed by adopting the process of room temperature cold rolling and pass heat treatment, the technical blockade in the field is broken through, and the mass production of the ODS-FeCrAl seamless pipe is realized. The process is simple and economical, the processing period is short, the thin-wall pipe is prepared on the premise of not influencing the dispersion strengthening of the Y-Al-O nano oxide, the obtained pipe has a crystal structure with fine grains and uniform tissue, the size precision is high, the inner surface and the outer surface are smooth and clean, and the excellent mechanical and creep-resistant performance of the pipe is ensured. The preparation method of the tube does not influence the particle size and dispersion state of the Y-Al-O oxide strengthening phase in the ODS-FeCrAl alloy, the prepared tube has a crystal structure with fine grains and uniform tissue, and the ODS tube has excellent strength and creep resistance as well as excellent oxidation resistance and radiation swelling resistance.
Drawings
FIG. 1 shows ODS-FeCrAl alloy tube obtained in example 1 of the present invention.
FIG. 2 is a transmission electron micrograph (scale 100 nm) of a dispersed phase of a nanocomposite oxide in an ODS-FeCrAl alloy obtained in example 2 of the present invention.
FIG. 3 shows ODS-FeCrAl alloy tube obtained in example 3 of the present invention.
Detailed Description
The invention is further illustrated below with reference to examples and figures.
Example 1
Mechanical ball milling of FeCrAl and Y by using QX-QM20 high-energy ball mill2O3Powder is subjected to hot consolidation by a hot isostatic pressing process to obtain a powder with the chemical composition of Fe-14Cr-3.0Al-1.0W-0.1Si-0.5Y (by mass)Percent, the same below) of ODS-FeCrAl alloy. The alloy is forged into a phi 26mm round bar at 1150 ℃, surface defects are removed after turning, and the bar blank smoothness is increased by properly polishing. Then the tube blank with the diameter of 24 multiplied by 5mm is manufactured by perforating after the heat treatment at the speed of 800 ℃/60 min. And (3) cold rolling the perforated pipe blank by using a three-high mill, increasing the annealing schedule from 800 ℃/1h to 1000 ℃/1h along with the increase of the pass, increasing the pass deformation from 20 percent to 40 percent, and finally rolling the pipe blank into the pipe with the phi 9.5 multiplied by 0.3mm as shown in figure 1. The rolling process parameters are referred to in table 1. The room temperature mechanical properties show that the ODS-FeCrAl alloy pipe prepared by the embodiment has the yield strength of 838MPa, the tensile strength of 924MPa and the elongation of 16.5%.
Table 1 example 1 rolling process parameters
Example 2
Mechanical ball milling of FeCrAl and Y by high-energy ball mill2O3And extruding the powder by a hot isostatic pressing process to obtain an ODS-FeCrAl alloy with the chemical composition of Fe-20Cr-5.0Al-0.25 Ti-0.3Y. The alloy is forged into a phi 24.5mm round rod at 1200 ℃, surface defects are removed after turning, and then the phi 22X 5mm tube blank is manufactured after heat treatment at 700 ℃/60min and perforation. The perforated tube blank is cold-rolled by a three-roll mill, the annealing temperature is increased from 700 ℃ to 950 ℃ in the tube cold rolling process, the heat preservation time is not changed, the pass deformation is increased from 15% to 35%, and the rolled ODS-FeCrAl tube has excellent mechanical properties because of the nano oxide strengthening phase which is dispersed and distributed as shown in figure 2: the tensile strength at room temperature reaches 1180MPa, the yield strength at room temperature reaches 1100MPa, and the elongation is 12 percent.
Table 2 example 2 rolling process parameters
Example 3
Mechanical ball milling of FeCrAl and Y by high-energy ball mill2O3And carrying out hot consolidation on the powder by using a hot isostatic pressing process to obtain an ODS-FeCrAl alloy with the chemical composition of Fe-16Cr-5Al-0.3 Ti-2W-0.15Y. The alloy is forged into a phi 25mm round bar at 1150 ℃, surface defects are removed after turning, and then the phi 24X 5mm tube blank is manufactured after heat treatment at 800 ℃/60min and perforation. And (3) cold rolling the perforated pipe blank by using a three-high mill, wherein the annealing temperature is increased from 800 ℃ to 1000 ℃, the deformation of each pass is increased from 25% to 40%, and finally the pipe blank is rolled into a pipe with the diameter of 10 multiplied by 0.5mm as shown in figure 3. The alloy is subjected to mechanical test, the yield strength at room temperature is 987MPa, the tensile strength is 1013MPa, and the elongation is 14%.
Table 3 example 3 rolling process parameters
Example 4
Mechanical ball milling of FeCrAl and Y by high-energy ball mill2O3And carrying out hot consolidation on the powder by using a hot isostatic pressing process to obtain an ODS-FeCrAl alloy with the chemical composition of Fe-16Cr-4.5Al-0.2 Ti-1.5W-0.4Y. The alloy is forged into a phi 25mm round bar at 1150 ℃, surface defects are removed after turning, and then the phi 24X 5mm tube blank is manufactured after heat treatment at 800 ℃/60min and perforation. And (3) cold rolling the perforated pipe blank by using a three-high mill, wherein the annealing temperature is increased from 800 ℃ to 1000 ℃, the deformation of each pass is increased from 25% to 40%, and finally the pipe blank is rolled into a pipe with the diameter of 10 multiplied by 0.5mm as shown in figure 3. The alloy is subjected to mechanical test, the yield strength at room temperature is 1007MPa, the tensile strength is 1142MPa, and the elongation is 13.5%.
Table 4 example 4 rolling process parameters
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (6)
1. The preparation method of the oxide dispersion strengthening FeCrAl alloy pipe is characterized in that the oxide dispersion strengthening FeCrAl alloy pipe contains 14-22 wt% of Cr, 3-5 wt% of Al, 0.15-0.5 wt% of Y and the balance of Fe in percentage by weight; the preparation method comprises the following steps:
A) preparing ODS-FeCrAl alloy powder by using a mechanical alloying method;
B) implementing ODS-FeCrAl alloying by using a hot isostatic pressing process;
C) after sheath removal, forging the alloy into a rod;
D) after heat treatment, a tube blank is manufactured by adopting a piercing process;
E) reducing the diameter and/or the wall thickness of the tube blank by adopting a cold rolling and pass heat treatment process until a tube with the size requirement is obtained; wherein, cold rolling is carried out at room temperature, the pass heat treatment temperature is 700-1050 ℃, the heat preservation time is 30-90 minutes, the deformation of the sectional area of the pipe in each pass is 10-50%, and the deformation of the sectional area of the pipe in each pass is gradually increased along with the reduction of the wall thickness, and is increased from 10-30% to 30-50%.
2. The method for preparing an oxide dispersion strengthened FeCrAl alloy pipe according to claim 1, wherein the method comprises the following steps: in the step C), after the sheath is removed, the forging temperature of the alloy is 1100-1250 ℃.
3. The method for preparing an oxide dispersion strengthened FeCrAl alloy pipe according to claim 1, wherein the method comprises the following steps: and D), performing heat treatment on the bar blank before perforation, wherein the temperature is 800-1000 ℃, and the heat preservation time is 40-80 minutes.
4. The method for preparing an oxide dispersion strengthened FeCrAl alloy pipe according to claim 1, wherein the method comprises the following steps: and E), cold rolling at room temperature at the rolling speed of 100-600 r/min.
5. The method for preparing an oxide dispersion strengthened FeCrAl alloy pipe according to claim 1, wherein the method comprises the following steps: and E), cold rolling at room temperature, wherein the heat treatment mode of each pass adopts vacuum annealing.
6. The method for preparing an oxide dispersion strengthened FeCrAl alloy pipe according to claim 1, wherein the method comprises the following steps: the oxide dispersion strengthening FeCrAl alloy pipe comprises, by weight, 14-20% of Cr, 3-5% of Al, 0.2-0.4 wt% of Y and the balance of Fe.
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| CN201811422686.8A CN109594017A (en) | 2018-11-27 | 2018-11-27 | A kind of preparation method of oxide dispersion intensifying FeCrAl alloy pipe |
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| CN110125383B (en) * | 2019-04-25 | 2020-04-17 | 江苏大学 | Method for manufacturing high-purity iron-chromium-aluminum alloy powder |
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| CN110918649A (en) * | 2019-10-16 | 2020-03-27 | 宁夏北鼎新材料产业技术有限公司 | FeCrAl alloy tube material for light water reactor cladding and rolling method thereof |
| CN110863153B (en) * | 2019-12-05 | 2021-04-06 | 中国核动力研究设计院 | Preparation method of FeCrAl-based ODS alloy material for advanced nuclear fuel element cladding |
| CN111020346B (en) * | 2019-12-05 | 2021-04-27 | 中国核动力研究设计院 | Preparation method of FeCrAl-based ODS alloy material for nuclear reactor |
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| CN110863152B (en) * | 2019-12-05 | 2021-03-26 | 中国核动力研究设计院 | Preparation method of FeCrAl-based ODS alloy for nuclear reactor accident-resistant fuel element cladding |
| CN110835716B (en) * | 2019-12-05 | 2021-08-31 | 中国核动力研究设计院 | Preparation method of FeCrAl-based ODS alloy for nuclear reactor core |
| CN110760760B (en) * | 2019-12-05 | 2020-12-04 | 中国核动力研究设计院 | Preparation method of FeCrAl-based alloy for nuclear reactor structural material |
| CN111057958B (en) * | 2019-12-22 | 2022-01-14 | 中国科学院金属研究所 | Corrosion-resistant, anti-irradiation and high-strength super ODS steel and preparation method thereof |
| CN112355078A (en) * | 2020-10-26 | 2021-02-12 | 有研工程技术研究院有限公司 | Aluminum oxide dispersion strengthened copper alloy pipe and preparation method and application thereof |
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| CN113736966B (en) * | 2021-08-27 | 2023-04-28 | 西安交通大学 | FeCrAl-based alloy with double heterostructure and preparation method thereof |
| CN114134429A (en) * | 2021-12-03 | 2022-03-04 | 中国核动力研究设计院 | ODS ferrite stainless steel fuel cladding tube and preparation method thereof |
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| CN115171920A (en) * | 2022-06-14 | 2022-10-11 | 中国核动力研究设计院 | Double-layer composite cladding tube for nuclear fuel, nuclear fuel and preparation method |
| CN115161564B (en) * | 2022-07-12 | 2023-04-18 | 中国核动力研究设计院 | FeCrAl stainless steel cladding tube and preparation method thereof |
| CN117403141A (en) * | 2023-10-24 | 2024-01-16 | 上海交通大学 | High-strength corrosion-resistant oxide dispersion strengthening steel and preparation method thereof |
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| CN1259515C (en) * | 2004-07-13 | 2006-06-14 | 天津市天材科技发展有限公司 | Method for making ferrite stainless steel seamless pipes and cold working process thereof |
| CN101328562B (en) * | 2008-07-17 | 2011-01-26 | 中国科学院等离子体物理研究所 | Oxide dispersion strengthening low activity martensitic steel material and preparation thereof |
| JP2018070897A (en) * | 2015-03-02 | 2018-05-10 | 国立大学法人北海道大学 | Iron-chromium-aluminum oxide-dispersed strengthened steel and method for producing the same |
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