CN105834691A - High-throughput preparation method of zirconium alloy - Google Patents
High-throughput preparation method of zirconium alloy Download PDFInfo
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- CN105834691A CN105834691A CN201610291063.6A CN201610291063A CN105834691A CN 105834691 A CN105834691 A CN 105834691A CN 201610291063 A CN201610291063 A CN 201610291063A CN 105834691 A CN105834691 A CN 105834691A
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- zircaloy
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- cold rolling
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- 229910001093 Zr alloy Inorganic materials 0.000 title claims abstract description 78
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000005260 corrosion Methods 0.000 claims abstract description 34
- 230000007797 corrosion Effects 0.000 claims abstract description 32
- 238000005097 cold rolling Methods 0.000 claims abstract description 18
- 238000000137 annealing Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000956 alloy Substances 0.000 claims abstract description 13
- 238000010894 electron beam technology Methods 0.000 claims abstract description 10
- 238000012360 testing method Methods 0.000 claims abstract description 9
- 238000003466 welding Methods 0.000 claims abstract description 9
- 238000012216 screening Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 46
- 239000000463 material Substances 0.000 claims description 24
- 230000004907 flux Effects 0.000 claims description 19
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 16
- 239000000523 sample Substances 0.000 claims description 15
- 229910045601 alloy Inorganic materials 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000005259 measurement Methods 0.000 claims description 8
- 238000005275 alloying Methods 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 229910008933 Sn—Nb Inorganic materials 0.000 claims description 5
- 229910052758 niobium Inorganic materials 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 5
- 229910052718 tin Inorganic materials 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 230000004584 weight gain Effects 0.000 claims description 3
- 235000019786 weight gain Nutrition 0.000 claims description 3
- 240000004808 Saccharomyces cerevisiae Species 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 238000012827 research and development Methods 0.000 abstract description 3
- 238000005253 cladding Methods 0.000 description 3
- 239000003758 nuclear fuel Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- OOAWCECZEHPMBX-UHFFFAOYSA-N oxygen(2-);uranium(4+) Chemical compound [O-2].[O-2].[U+4] OOAWCECZEHPMBX-UHFFFAOYSA-N 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- FCTBKIHDJGHPPO-UHFFFAOYSA-N uranium dioxide Inorganic materials O=[U]=O FCTBKIHDJGHPPO-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
- B21B1/24—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length in a continuous or semi-continuous process
- B21B1/28—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length in a continuous or semi-continuous process by cold-rolling, e.g. Steckel cold mill
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K15/00—Electron-beam welding or cutting
- B23K15/06—Electron-beam welding or cutting within a vacuum chamber
-
- 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
-
- 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
- B21B2271/00—Mill stand parameters
- B21B2271/02—Roll gap, screw-down position, draft position
Abstract
The invention discloses a high-throughput preparation method of zirconium alloy. According to the high-throughput preparation method of the zirconium alloy, zirconium alloy plates containing different elements are welded together through a vacuum electron beam welding technique, so that preparation of a single plate containing quasi-continuous elements is achieved; and multi-pass cold rolling, intermediate annealing and final annealing are conducted on the single plate containing the quasi-continuous elements, a high-temperature and high-pressure water or steam corrosion test is conducted on the single plate containing the quasi-continuous elements, the relation between the corrosion resistance of the zirconium alloy and the elements is established, screening of the elements of the zirconium alloy is achieved, high-performance zirconium alloy materials are obtained accordingly, and the research and development progress of high-performance zirconium alloy is accelerated.
Description
Technical field
The present invention relates to Zirconium alloy material preparing technical field, particularly relate to the high flux preparation method of a kind of zircaloy.
Background technology
Zircaloy is little because having thermal neutron absorption cross section, good with the compatibility of uranium dioxide, and there is the advantages such as the high-temperature resistant water corrosive nature of excellence, good comprehensive mechanical property and preferable thermal conductivity, and it is widely used as a kind of important feature material of cladding nuclear fuels in water cooled nuclear reactor.The zircaloy developed in the world at present mainly has the big series of Zr-Sn, Zr-Nb and Zr-Sn-Nb tri-, and the Zr-4 alloy in Zr-Sn system can not meet high burnup fuel assembly and extend the requirement of refulling cycle.At present, in order to deepen the burnup of nuclear fuel, extending the refulling cycle, reduce nuclear power cost further, need to develop the fuel assembly of high burnup, the performance of zircaloy is had higher requirement by this.Zircaloy decay resistance in high-temperature high pressure water is to affect the topmost factor of its service life, and its decay resistance is had a significant impact by composition, so the water-fast side corrosive nature improving zircaloy is crucial.Use high flux preparation and characterizing method can quickly set up the relation between Corrosion Resistance of Zirconium Alloys and composition, it is achieved the optimization of zircaloy composition, accelerate the research and development process of advanced zirconium alloys.
In order to better adapt to the situation of China's nuclear power developing, high flux preparation and characterizing method is used quickly to set up the relation of Corrosion Resistance of Zirconium Alloys and composition on the basis of existing zircaloy, realize the screening of zircaloy composition, and then develop the advanced zirconium alloys material with China's independent intellectual property right, the situation breaking away from nuclear-used zirconium alloy cladding materials and being completely dependent on import is had profound significance.
Summary of the invention
The technical problem to be solved is to provide the high flux preparation method of a kind of zircaloy, high flux preparation method is used to obtain the zircaloy block materials of quasi-continuous composition, single piece of material obtains multicomponent alloy simultaneously, quickly set up the relation of Corrosion Resistance of Zirconium Alloys and composition, realize the screening of zircaloy composition, and then develop the Zirconium alloy material of higher performance.
The present invention solves above-mentioned technical problem by following technical proposals: the high flux preparation method of a kind of zircaloy, it is characterised in that it comprises the following steps:
Step one, selection have alloy based on application prospect or commercial Zr-Sn, Zr-Nb and Zr-Sn-Nb tri-big series zircaloy；
Step 2, use vacuum electron beam welding machine realize vacuum electron beam welding, are fitted together by the zircaloy sheet material of heterogeneity, it is achieved the monolithic preparation of plates of quasi-continuous composition；
Step 3, monolithic sheet material to above-mentioned quasi-continuous composition carry out that multi-pass is cold rolling, and draught per pass is 40%-55%, carries out the intermediate annealing of 550-600 ° of C/1-2 h between two passages are cold rolling, finally carries out 550-600 ° of C/1-5 h annealing；
Step 4, above-mentioned final annealing is processed after sheet material put into autoclave carry out the corrosion test of high-temperature high pressure water or steam, it is thus achieved that cover the corrosion sample of oxide-film；
Step 5, corrode the thickness of sample oxidation film with light microscope or SEM point-to-point measurement, by electron probe point-to-point measurement alloying component, reduction formula 15mg/dm according to oxide thickness with Corrosion Resistance of Zirconium Alloys classical relation, i.e. oxidation weight gain with oxide thickness2=1 mm, quickly sets up the relation of Corrosion Resistance of Zirconium Alloys and composition, it is achieved the screening of zircaloy composition, and then obtains the zircaloy composition of multiple fine corrosion resistance.
Preferably, the zircaloy sheet material of 2-6 block heterogeneity is fitted together by described step 2, can obtain the block materials of quasi-continuous composition, also can carry out the iron-enriched yeast of oxide thickness and alloying component simultaneously.
Preferably, the multi-pass in described step 3 is cold rolling cold rolling for 2-4 passage, it is thus achieved that suitably cold rolling reduction.
Preferably, in the autoclave in described step 4, the medium of corrosion test is high-temperature high pressure water or superheated vapour or the LiOH aqueous solution or LiOH+ boric acid aqueous solution, carries out the decay resistance of multiple condition and characterizes and be conducive to the preferred of composition.
The most progressive effect of the present invention is: the high flux preparation method of zircaloy of the present invention can obtain the zircaloy block materials of quasi-continuous composition, the zircaloy composition of excellent anti-corrosion performance, i.e. composition corresponding to oxide thickness smaller area can be preferably gone out in conjunction with oxide thickness.Visible high flux prepares the information can very enriched the impact of Corrosion Resistance of Zirconium Alloys with study on characterization composition, it is simple to filter out the new zirconium alloy that decay resistance is more excellent.
Accompanying drawing explanation
Fig. 1 is that the sample of the present invention corrodes 100 in 360 ° of C/18.6 MPa/0.01 M/LiOH aqueous solution
Solder side side oxide thickness and the change curve schematic diagram of alloying component during d.
Detailed description of the invention
Provide present pre-ferred embodiments below in conjunction with the accompanying drawings, to describe technical scheme in detail.
The high flux preparation method of zircaloy of the present invention comprises the following steps:
Step one, selection have alloy based on application prospect or commercial Zr-Sn, Zr-Nb and Zr-Sn-Nb tri-big series zircaloy；
Step 2, use vacuum electron beam welder realize vacuum electron beam welding, are fitted together by the zircaloy sheet material of heterogeneity, it is achieved the monolithic preparation of plates of quasi-continuous composition；
Step 3, monolithic sheet material to above-mentioned quasi-continuous composition carry out that multi-pass is cold rolling, and draught per pass is 40%-55%, carries out the intermediate annealing of 550-600 ° of C/1-2h between two passages are cold rolling, finally carries out 550-600 ° of C/1-5 h annealing；
Step 4, above-mentioned sheet material is put into the corrosion test carrying out high-temperature high pressure water or steam in autoclave, it is thus achieved that cover the corrosion sample of oxide-film；
Step 5, corrode the thickness of sample oxidation film with light microscope or SEM point-to-point measurement, by electron probe point-to-point measurement alloying component, reduction formula 15mg/dm according to oxide thickness with Corrosion Resistance of Zirconium Alloys classical relation, i.e. oxidation weight gain with oxide thickness2=1 um, quickly sets up the relation of Corrosion Resistance of Zirconium Alloys and composition, it is achieved the screening of zircaloy composition, and then obtains the zircaloy composition of multiple fine corrosion resistance.
Described step 2 can be to be fitted together by the zircaloy sheet material of 2-6 block heterogeneity.Multi-pass in described step 3 is cold rolling cold rolling for 2-4 passage.In autoclave in described step 4, the medium of corrosion test is high-temperature high pressure water or superheated vapour or the LiOH aqueous solution or LiOH+ boric acid aqueous solution.
Embodiment one: the concrete preparation process of the high flux preparation method of zircaloy of the present invention is as follows:
Step one, composition based on commercialization or Zr-Sn, Zr-Nb and Zr-Sn-Nb tri-big series zircaloy having application prospect, devise the alloy that composition is Zr-1.8Sn-0.5Nb-0.2Fe-0.2Cr, Zr-1.5Sn-0.2Fe-0.1Cr and Zr-1.0Sn-0.22Nb-0.12Fe.
Step 2, the alloy sheets of mentioned component use vacuum electron beam welding machine carry out vacuum electron beam welding；
Step 3, solder side is polished after, being parallel to weld seam, that the monolithic sheet material of above-mentioned quasi-continuous composition is carried out three passages is cold rolling, and draught per pass is 45%, carries out 560 ° of C/1.5 between two passages are cold rolling
The intermediate annealing of h, finally carries out 580 ° of C/3
H makes annealing treatment.
Step 4, it is perpendicular to weld seam sample shear is cut into sheet sample, put into after cleaning by standard method pickling and deionized water and autoclave carries out 360 ° of C/18.6
The high-temperature high pressure water corrosion test of the MPa/0.01 M/LiOH aqueous solution, it is thus achieved that cover the corrosion sample of oxide-film.
Step 5, corrode the thickness of sample oxidation film with light microscope or SEM point-to-point measurement, by electron probe point-to-point measurement alloying component, quickly set up the relation of Corrosion Resistance of Zirconium Alloys and composition, realize the screening of zircaloy composition, and then obtain the zircaloy composition of multiple fine corrosion resistance.
The zircaloy block materials of quasi-continuous composition can be obtained as shown in Figure 1 by the high flux preparation method of above-mentioned zircaloy, can preferably go out the zircaloy composition of excellent anti-corrosion performance, i.e. composition corresponding to oxide thickness smaller area in conjunction with oxide thickness.Visible high flux prepares the information can very enriched the impact of Corrosion Resistance of Zirconium Alloys with study on characterization composition, it is simple to filter out the new zirconium alloy that decay resistance is more excellent.
The present invention relates to a kind of water cooled nuclear reactor is used as the high flux preparation method of cladding nuclear fuels zircaloy, the most quickly set up high flux preparation and the characterizing method of Corrosion Resistance of Zirconium Alloys and composition relation, belong to Zirconium alloy material preparing technical field.The present invention uses vacuum electron beam welding technology to be welded together by the zircaloy sheet material of heterogeneity, it is achieved the monolithic preparation of plates of quasi-continuous composition；The monolithic sheet material of above-mentioned quasi-continuous composition is carried out multi-pass cold rolling, intermediate annealing and final annealing process, and it is carried out the corrosion test of high-temperature high pressure water or steam, set up the relation of Corrosion Resistance of Zirconium Alloys and composition, realize the screening of zircaloy composition, and then the Zirconium alloy material of acquisition higher performance, accelerate the research and development process of advanced zirconium alloys.
Particular embodiments described above; solve the technical problem that the present invention, technical scheme and beneficial effect are further described; it is it should be understood that; the foregoing is only the specific embodiment of the present invention; it is not limited to the present invention; all within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. done, should be included within the scope of the present invention.
Claims (4)
1. the high flux preparation method of a zircaloy, it is characterised in that it comprises the following steps:
Step one, selection have alloy based on application prospect or commercial Zr-Sn, Zr-Nb and Zr-Sn-Nb tri-big series zircaloy；
Step 2, use vacuum electron beam welding machine realize vacuum electron beam welding, are fitted together by the zircaloy sheet material of heterogeneity, it is achieved the monolithic preparation of plates of quasi-continuous composition；
Step 3, monolithic sheet material to above-mentioned quasi-continuous composition carry out that multi-pass is cold rolling, and draught per pass is 40%-55%, carries out the intermediate annealing of 550-600 ° of C/1-2 h between two passages are cold rolling, finally carries out 550-600 ° of C/1-5 h annealing；
Step 4, above-mentioned final annealing is processed after sheet material put into autoclave carry out the corrosion test of high-temperature high pressure water or steam, it is thus achieved that cover the corrosion sample of oxide-film；
Step 5, corrode the thickness of sample oxidation film with light microscope or SEM point-to-point measurement, by electron probe point-to-point measurement alloying component, reduction formula 15mg/dm according to oxide thickness with Corrosion Resistance of Zirconium Alloys classical relation, i.e. oxidation weight gain with oxide thickness2=1 mm, quickly sets up the relation of Corrosion Resistance of Zirconium Alloys and composition, it is achieved the screening of zircaloy composition, and then obtains the zircaloy composition of multiple fine corrosion resistance.
2. the high flux preparation method of zircaloy as claimed in claim 1, it is characterized in that, the zircaloy sheet material of 2-6 block heterogeneity is fitted together by described step 2, it is thus achieved that the block materials of quasi-continuous composition, carries out the iron-enriched yeast of oxide thickness and alloying component simultaneously.
3. the high flux preparation method of zircaloy as claimed in claim 1, it is characterised in that the multi-pass in described step 3 is cold rolling cold rolling for 2-4 passage, it is thus achieved that suitably cold rolling reduction.
4. the high flux preparation method of zircaloy as claimed in claim 1, it is characterized in that, in autoclave in described step 4, the medium of corrosion test is high-temperature high pressure water or superheated vapour or the LiOH aqueous solution or LiOH+ boric acid aqueous solution, carries out the decay resistance of multiple condition and characterizes and be conducive to the preferred of composition.
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| CN201610291063.6A CN105834691A (en) | 2016-05-05 | 2016-05-05 | High-throughput preparation method of zirconium alloy |
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| CN201610291063.6A CN105834691A (en) | 2016-05-05 | 2016-05-05 | High-throughput preparation method of zirconium alloy |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116487079A (en) * | 2023-04-03 | 2023-07-25 | 中国核动力研究设计院 | Method for qualitatively testing nuclear fuel microcell burnup based on electronic probe |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116487079A (en) * | 2023-04-03 | 2023-07-25 | 中国核动力研究设计院 | Method for qualitatively testing nuclear fuel microcell burnup based on electronic probe |
| CN116487079B (en) * | 2023-04-03 | 2024-01-30 | 中国核动力研究设计院 | Method for qualitatively testing nuclear fuel microcell burnup based on electronic probe |
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