CN113981347B - High-strength-plasticity heterostructure zirconium alloy and preparation method thereof - Google Patents
High-strength-plasticity heterostructure zirconium alloy and preparation method thereof Download PDFInfo
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- 229910001093 Zr alloy Inorganic materials 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 36
- 238000005096 rolling process Methods 0.000 claims abstract description 22
- 229910000734 martensite Inorganic materials 0.000 claims abstract description 17
- 230000009467 reduction Effects 0.000 claims abstract description 12
- 238000004321 preservation Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000498 cooling water Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 27
- 239000000956 alloy Substances 0.000 abstract description 21
- 229910045601 alloy Inorganic materials 0.000 abstract description 20
- 238000000034 method Methods 0.000 abstract description 19
- 238000010791 quenching Methods 0.000 abstract description 8
- 230000000171 quenching effect Effects 0.000 abstract description 8
- 230000008569 process Effects 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 7
- 238000009826 distribution Methods 0.000 description 7
- 238000000635 electron micrograph Methods 0.000 description 4
- 230000006872 improvement Effects 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005098 hot rolling Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000005482 strain hardening Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000013532 laser treatment Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/186—High-melting or refractory metals or alloys based thereon of zirconium or alloys based thereon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C16/00—Alloys based on zirconium
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Abstract
The invention discloses a heterojunction with high strength and plasticityThe zirconium alloy and the preparation method thereof, the beta quenching zirconium alloy is heated to 620-730 ℃ for long-time heat preservation for 3-48 h, and is cooled to room temperature to obtain alpha phase and beta phase with high stability; subsequently, the alloy is heated to 750 ℃ to T β The temperature is kept for 10-40 min, then high-temperature rolling deformation with the reduction of 30-80% is carried out, water or oil is used for rapid cooling after rolling deformation, the temperature of cooling water is between room temperature and 100 ℃, and the temperature of cooling oil is between room temperature and 250 ℃. The heterostructure zirconium alloy prepared by the method not only comprises a micron-scale equiaxial alpha primary phase and a submicron-scale flaky alpha' martensite phase, but also comprises an equiaxial metastable beta phase. Compared with the traditional method, the zirconium alloy prepared by the method has the strength of 950MPa and the plasticity improved by more than 40 percent compared with the traditional method.
Description
Technical Field
The invention belongs to the field of metal materials, and relates to a high-strength-plasticity heterostructure zirconium alloy and a preparation method thereof.
Background
The zirconium alloy is the only commercial nuclear reactor cladding tube material at present due to low neutron absorption cross section, good corrosion resistance and mechanical property, and is an irreplaceable key structure for developing nuclear power and nuclear power ships. Meanwhile, with the gradual extension of the refueling period of nuclear reactor kernel fuel, the gradual increase of reactor operating power and the improvement of safety and reliability, various service performances, especially mechanical properties (< 500 MPa), of the existing zirconium alloy cladding tube material cannot meet the actual requirements, so that the research and development of a zirconium alloy material with more excellent mechanical properties becomes one of the problems to be solved urgently in the field of nuclear industry.
In recent years, the preparation of heterostructures in alloys has become one of the main ideas for the preparation of high performance alloys. The heterogeneous distribution of the shape, size, element concentration and the like of grains/phases in the alloy can cause the difference of the deformation degree of the alloy in different areas in the deformation process, and in order to coordinate the deformation and improve the uniform deformation capability of the alloy, a heterogeneous interface can often generate a large amount of geometrical necessary dislocation to generate back stress on an easily deformable area, thereby improving the strain hardening capability of the alloy. At present, heterostructures have been primarily used in zirconium alloys. For example, the article "Characterization of microstructure and hardness of a Zr-2.5Nb alloy surface-treated by pulsed laser" describes that the zirconium alloy surface treated by pulsed laser has two characteristic regions, one surface region is a twin crystal martensite sheet with a structure of hundreds of nanometers wide, and the subsurface layer is a region where twin crystal martensite and a matrix are mixed. The heterostructure with the microstructure gradually changed from the surface to the core is beneficial to improving the alloy performance, but the depth of laser treatment is limited, and the improvement on the mechanical property of the alloy is also limited. Chinese patent No. CN202010879410.3 describes a method for obtaining a mixed heterostructure of primary α phase and α 'martensite phase by rolling and heat treatment, in which the two phases are uniformly distributed, and a large amount of α' martensite makes the alloy strength sufficiently improved, but the alloy lacks an effective plasticizing mechanism. Similarly, in order to improve the plasticity of the alloy in martensitic steels, the metastable austenite phase obtained by the quenching repartitioning heat treatment process contributes to the improvement in the plasticity of the martensitic steel. How to obtain the metastable beta-phase in a zirconium alloy rich in martensite is a scientific question that has never been reported.
Disclosure of Invention
The invention aims to overcome the defects of the existing zirconium alloy and the preparation method thereof, and provides a high-strength plastic heterostructure zirconium alloy and the preparation method thereof.
The invention is realized by the following technical scheme:
a preparation method of a high-strength plastic heterostructure zirconium alloy comprises the following steps:
step 1, heating beta-quenched zirconium alloy to 620-730 ℃, preserving heat, and then cooling to room temperature;
Preferably, the heat treatment and heat preservation time in the step 1 is 3h-48h.
Preferably, 750 ℃ to T in step 2 β The heat treatment and the heat preservation time are 10min-40min.
Preferably, the cooling mode after rolling deformation in the step 2 is water cooling or oil cooling.
Preferably, the temperature of the cooling water is from room temperature to 100 ℃.
Preferably, the temperature of the cooling oil is from room temperature to 250 ℃.
The microstructure of the heterostructure zirconium alloy comprises a micron-sized equiaxial alpha primary phase, a submicron-sized flaky alpha' martensite phase and a submicron-sized equiaxial beta phase.
Preferably, the tensile strength of the heterostructure zirconium alloy reaches 911-959MPa, and the uniform elongation is 4.7-5.8%.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides a preparation method of high-strength plastic heterostructure zirconium alloy, which comprises the steps of firstly, carrying out long-time heat preservation on beta quenching state zirconium alloy at a lower temperature of 620-730 ℃ before the traditional rolling process to ensure that alloy elements are fully redistributed between an alpha phase and a beta phase, according to an alloy phase diagram, although the content of the beta phase is low at the lower temperature, the concentration of beta stable elements is higher, and the beta phase with high stability is limited because the beta stable elements are diffused outwards due to shorter time in a high temperature region during hot rolling, so that the stability of the part of the beta phase is enough to be kept during hot rolling quenching. The preparation method is simple in process flow, the zirconium alloy with the heterostructure can be obtained through the process convenient to operate, extra back stress strengthening can be provided for the zirconium alloy through heterogeneous deformation, and the plasticity of the zirconium alloy can be improved while the strength of the zirconium alloy is kept. Compared with the traditional method, the zirconium alloy prepared by the method has the strength of 950MPa and the plasticity improved by more than 40 percent compared with the traditional method.
Secondly, the zirconium alloy after low-temperature annealing is carried out at 750 ℃ to T β The heat preservation and rolling are carried out between the two layers, so that a certain amount of equiaxial alpha primary phase can be generated, and the residue of flaky grain boundary alpha primary phase can be avoided.
In addition, the rolled sample is rapidly cooled in water or oil, which contributes to the transformation of the high temperature β phase into the fine α' martensite phase.
Finally, the high temperature β phase will completely transform into martensite when the temperature of the coolant is sufficiently low, and therefore, setting the temperature of the cooling water to 100 ℃ or the temperature of the cooling oil to 250 ℃ makes the martensitic transformation of the high temperature β phase not completely occur, which may also leave a certain amount of β phase remaining, which is advantageous for improving the plasticity of the alloy.
Drawings
FIG. 1 is an electron micrograph of the distribution of the morphology of the structure in the zirconium alloy of example 1 of the present invention.
FIG. 2 is an electron micrograph of the phase distribution in the zirconium alloy of example 1 of the present invention.
FIG. 3 is a graph of tensile engineering stress-strain for the zirconium alloy of example 1 of the present invention.
FIG. 4 is an electron micrograph of the texture morphology distribution in the zirconium alloy of comparative example 1 of the present invention.
FIG. 5 is an electron micrograph of the phase distribution in the zirconium alloy of comparative example 1 of the present invention.
FIG. 6 is a tensile engineering stress-strain plot of the zirconium alloy of comparative example 1 of the present invention.
Detailed Description
The present invention will now be described more fully hereinafter with reference to the accompanying drawings, in which the invention is shown by way of illustration and not by way of limitation.
A preparation method of a high-strength plastic heterostructure zirconium alloy comprises the following steps:
step 1, heating a beta quenching state zirconium alloy to 620-730 ℃, preserving heat for 3-48 h, and then cooling to room temperature to obtain an alpha phase and a beta phase with high stability;
And the cooling mode after rolling deformation is water cooling or oil cooling.
The temperature of the cooling water is from room temperature to 100 ℃. The temperature of the cooling oil is between room temperature and 250 ℃.
According to the heterostructure zirconium alloy obtained by the preparation method, the microstructure of the heterostructure zirconium alloy comprises a micron-scale equiaxial alpha primary phase, a submicron-scale flaky alpha' martensite phase and a submicron-scale equiaxial beta phase. The tensile strength of the zirconium alloy with the heterostructure reaches 911-959MPa, and the uniform elongation is 4.7-5.8%.
Example 1:
a preparation method of a high-strength-plasticity heterostructure zirconium alloy comprises the following steps:
step 1, heating beta-quenched zirconium alloy to 620 ℃, preserving heat for 12 hours, and then cooling to room temperature;
and 2, heating the zirconium alloy obtained in the step 1 to 870 ℃, preserving heat for 20min, then carrying out high-temperature rolling deformation with the reduction of 75%, and cooling the rolled zirconium alloy to room temperature in room-temperature oil.
The microstructure and morphology of the alloy obtained in this example are shown in fig. 1, the phase distribution is shown in fig. 2, and the micron-sized equiaxed alpha primary phase, the submicron-sized flaky alpha' martensite phase and the submicron-sized equiaxed beta phase are uniformly distributed. The alloy strength-plasticity curve treated by the process of the invention is shown in figure 3, which shows extremely high strength/plasticity combination, the tensile strength reaches 959MPa, and the uniform elongation still reaches 5.4%.
Example 2:
a preparation method of a high-strength-plasticity heterostructure zirconium alloy comprises the following steps:
step 1, heating beta-quenched zirconium alloy to 680 ℃, preserving heat for 48 hours, and then cooling to room temperature;
and 2, heating the zirconium alloy obtained in the step 1 to 870 ℃, preserving heat for 20min, then carrying out high-temperature rolling deformation with the reduction of 75%, and cooling the zirconium alloy to room temperature in room-temperature oil after rolling.
The zirconium alloy prepared by the process shows extremely high strength/plasticity combination, the tensile strength reaches 941MPa, and the uniform elongation still reaches 5.3%.
Example 3:
a preparation method of a high-strength plastic heterostructure zirconium alloy comprises the following steps:
step 1, heating beta-quenched zirconium alloy to 730 ℃, preserving heat for 3 hours, and then cooling to room temperature;
and 2, heating the zirconium alloy obtained in the step 1 to 870 ℃, preserving heat for 20min, then carrying out high-temperature rolling deformation with the reduction of 75%, and cooling the rolled zirconium alloy to room temperature in room-temperature oil.
The zirconium alloy prepared by the process shows extremely high strength/plasticity combination, the tensile strength reaches 957MPa, and the uniform elongation rate still reaches 4.8 percent.
Example 4:
a preparation method of a high-strength plastic heterostructure zirconium alloy comprises the following steps:
step 1, heating beta-quenched zirconium alloy to 620 ℃, preserving heat for 12 hours, and then cooling to room temperature;
and 2, heating the zirconium alloy obtained in the step 1 to 750 ℃, preserving heat for 40min, then performing high-temperature rolling deformation with the reduction of 80%, and cooling the zirconium alloy to room temperature in room-temperature oil after rolling.
The zirconium alloy prepared by the process shows extremely high strength/plasticity combination, the tensile strength reaches 911MPa, and the uniform elongation still reaches 4.7 percent.
Example 5:
a preparation method of a high-strength-plasticity heterostructure zirconium alloy comprises the following steps:
step 1, heating beta quenching state zirconium alloy to 620 ℃, preserving heat for 12 hours, and then cooling to room temperature;
and 2, heating the zirconium alloy obtained in the step 1 to 940 ℃, preserving heat for 10min, then performing high-temperature rolling deformation with the reduction of 30%, and cooling the zirconium alloy to room temperature in room-temperature oil after rolling.
The zirconium alloy prepared by the process shows extremely high strength/plasticity combination, the tensile strength reaches 951MPa, and the uniform elongation still reaches 5.2%.
Example 6:
a preparation method of a high-strength plastic heterostructure zirconium alloy comprises the following steps:
step 1, heating beta-quenched zirconium alloy to 620 ℃, preserving heat for 12 hours, and then cooling to room temperature;
and 2, heating the zirconium alloy obtained in the step 1 to 870 ℃, preserving heat for 20min, then performing high-temperature rolling deformation with the reduction of 80%, and cooling the rolled zirconium alloy to room temperature in water at 100 ℃.
The zirconium alloy prepared by the process shows extremely high strength/plasticity combination, the tensile strength reaches 968MPa, and the uniform elongation still reaches 5.8%.
Example 7:
a preparation method of a high-strength-plasticity heterostructure zirconium alloy comprises the following steps:
step 1, heating beta-quenched zirconium alloy to 620 ℃, preserving heat for 12 hours, and then cooling to room temperature;
and 2, heating the zirconium alloy obtained in the step 1 to 870 ℃, preserving heat for 20min, then performing high-temperature rolling deformation with the reduction of 80%, and cooling the rolled zirconium alloy in oil at 250 ℃ to room temperature.
The zirconium alloy prepared by the process shows extremely high strength/plasticity combination, the tensile strength reaches 947MPa, and the uniform elongation still reaches 6.1%.
Comparative example 1:
this comparative example produced a two-phase heterostructure comprising an alpha primary phase and an alpha' martensite phase using conventional techniques, the difference from the above examples 1-7 resulting in poor plasticity.
The traditional preparation method of the zirconium alloy with the heterostructure comprises the following steps:
step 1, heating the beta quenching state zirconium alloy to 870 ℃, preserving heat for 30min, wherein the total rolling reduction rate is 75%, preserving heat for 5min at 870 ℃ after rolling, and then quenching with oil at room temperature.
And 2, heating the zirconium alloy obtained in the step 1 to 400 ℃, preserving heat for 60min, performing stress relief annealing, and then cooling to room temperature in an air mode.
The morphology of the alloy structure obtained by the comparative example is shown in fig. 4, the phase distribution is shown in fig. 5, the structure is almost all micron-sized equiaxed alpha primary phase and submicron-sized flaky alpha' martensite phase, and the content of beta phase is almost zero. The strength-plasticity curve of the alloy obtained by the comparative example is shown in fig. 6, and shows a lower uniform elongation of 3.5%.
The invention aims to overcome the defects of the conventional zirconium alloy and a preparation method thereof, and provides a zirconium alloy with a three-phase heterostructure and a preparation method thereof. Meanwhile, the strain hardening capacity of the alloy is obviously improved by utilizing the residual metastable beta phase, so that the zirconium alloy with high strength and large elongation is obtained. The preparation process of the zirconium alloy is easy to operate, short in flow and low in equipment requirement.
The above contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention should not be limited thereby, and any modification made on the basis of the technical idea proposed by the present invention falls within the protection scope of the claims of the present invention.
Claims (2)
1. A high-strength plastic heterostructure zirconium alloy, wherein the microstructure of the heterostructure zirconium alloy comprises a micron-sized equiaxed alpha primary phase, a submicron-sized flaky alpha' martensite phase and a submicron-sized equiaxed beta phase;
the high-strength plastic heterostructure zirconium alloy comprises the following steps:
step 1, heating beta-quenched zirconium alloy to 620-730 ℃, preserving heat for 3-48 h, and then cooling to room temperature;
step 2, heating the zirconium alloy obtained in the step 1 to 750-T β Carrying out heat treatment and heat preservation for 10-40 min, then carrying out high-temperature rolling deformation with the reduction of 30-80%, and cooling to obtain the zirconium alloy with the heterostructure;
the cooling mode is water cooling or oil cooling, the temperature of the cooling water is between room temperature and 100 ℃, and the temperature of the cooling oil is between room temperature and 250 DEG C
2. A high strength plastic heterostructure zirconium alloy as claimed in claim 1, wherein the heterostructure zirconium alloy has a tensile strength of 911-959MPa and a uniform elongation of 4.7-5.8%.
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| CN102260841B (en) * | 2011-07-13 | 2012-09-19 | 燕山大学 | Method for preparing zirconium-niobium alloy with alpha/beta dual-state organization |
| CN102586709B (en) * | 2012-04-05 | 2013-10-02 | 重庆大学 | Method for performing thermal treatment on zirconium alloy |
| CN102660719B (en) * | 2012-05-18 | 2015-01-07 | 重庆大学 | Machining process for zirconium alloy |
| CN104046846A (en) * | 2014-07-02 | 2014-09-17 | 燕山大学 | Multilevel high-strength high-plasticity titanium-zirconium-based alloy and preparation method thereof |
| CN112126875B (en) * | 2020-08-27 | 2021-07-13 | 西安交通大学 | Multi-level heterostructure dual-phase alloy and hot rolling method thereof |
| CN113025933B (en) * | 2021-03-08 | 2022-03-08 | 燕山大学 | Intermetallic compound toughened heterostructure zirconium alloy and preparation method thereof |
| CN113174551B (en) * | 2021-03-30 | 2022-08-09 | 西安交通大学 | Dual-phase high-strength high-plasticity titanium alloy with heterogeneous laminated structure and preparation method thereof |
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