CN104264087B - The preparation method of a kind of Zr-Nb-Cu system alloy - Google Patents
The preparation method of a kind of Zr-Nb-Cu system alloy Download PDFInfo
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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
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- 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
Abstract
The present invention relates to the preparation method of a kind of Zr-Nb-Cu system alloy, it is according to forging → quenching → hot extrusion → → first time cold rolling cold rolling and annealing → cold rolling and annealing for the third time with annealing → second time of annealing first, wherein, first time cold rolling and annealing be by annealing first after product to carry out first time cold rolling, after deflection reaches 50 ~ 70%, at 500 ~ 550 DEG C, carry out anneal; Cold rolling and the annealing of second time be by cold rolling for first time and annealing after product to carry out second time cold rolling, after deflection reaches 50 ~ 70%, at 500 ~ 550 DEG C, carry out anneal; Third time cold rolling and annealing be by cold rolling for second time and annealing after product to carry out third time cold rolling, after deflection reaches 50 ~ 70%, at 450 ~ 520 DEG C, carry out anneal.The second-phase of the Zr-Nb-Cu system alloy prepared by the present invention is small and dispersed distribution, and compares traditional technology, and its corrosion resistance nature improves more than 25%.
Description
Technical field
The invention belongs to alloy heat processing technique technical field, be specifically related to the preparation method of a kind of Zr-Nb-Cu system alloy.
Background technology
Zirconium alloy is light water reactor dyestuff cladding material, and the performance of zirconium alloy cladding determines the burnup of nuclear fuel, and the economy of nuclear power is also closely related with it, therefore has higher requirement to the performance of Reactor fuel element cladding material zirconium alloy.The corrosion resistance nature that the new zirconium alloy of commercial applications is as good in M5, Zirlo and E110 have at present.Domestic also at exploitation N18, N36 and C7 new zirconium alloy.Because C7 zirconium alloy with the addition of a small amount of Cu element on Zr-1Nb alloy basis, with Zr-Nb alloy phase ratio, its matrix α
zr/ β
zrall can there is considerable change in the behavior of growing up of phase transformation and second phase particles.And the comparatively large and skewness of the Zr-Nb-Cu system alloy second phase particles size that the complete processing of prior art is prepared, affect the corrosion resistance nature of alloy.
Summary of the invention
Technical problem to be solved by this invention overcomes the deficiencies in the prior art, the preparation method of a kind of Zr-Nb-Cu system alloy is provided, the distribution of the second phase particles of Zr-Nb-Cu system alloy prepared by the method less and even dispersion, makes the corrosion resistance nature of alloy significantly improve.
For solving above technical problem, the present invention adopts following technical scheme:
A preparation method for Zr-Nb-Cu system alloy, described preparation method comprises the following steps:
(1) forge: the zirconium alloy product containing Nb and Cu element is forged at 800 ~ 900 DEG C;
(2) quench: quench after the product after step (1) being forged is incubated 20 ~ 40min at 1000 ~ 1050 DEG C;
(3) hot extrusion: the product after step (2) being quenched carries out hot extrusion at 550 ~ 600 DEG C;
(4) anneal first: the product after step (3) hot extrusion is annealed at 500 ~ 550 DEG C;
(5) three cold rolling and annealing: the product after step (4) being annealed first carries out three cold rolling and annealing again, obtained Zr-Nb-Cu system alloy;
In step (5), described three concrete steps that are cold rolling and annealing are as follows:
First time is cold rolling and anneal: it is cold rolling that the product after described step (4) being annealed first carries out first time, after deflection reaches 50 ~ 70%, at 500 ~ 550 DEG C, carries out anneal;
Cold rolling and the annealing of second time: the product after cold rolling for first time and annealing is carried out second time cold rolling, after deflection reaches 50 ~ 70%, carry out anneal at 500 ~ 550 DEG C;
Third time cold rolling and annealing: the product after cold rolling for second time and annealing is carried out third time cold rolling, after deflection reaches 50 ~ 70%, carry out anneal at 450 ~ 520 DEG C.
Described first time, cold rolling and in annealing annealing time was 0.5 ~ 1.5 hour.
Cold rolling and in annealing the annealing time of described second time is 0.5 ~ 1.5 hour.
Described third time, cold rolling and in annealing annealing time was 1.5 ~ 4 hours.
Described annealing time is first 2 ~ 4 hours.
Described Zr-Nb-Cu system alloy is that Zr and inevitable impurity form by Nb0.6-1.2wt.%, Cu0.01-0.1wt.%, surplus.
Described Zr-Nb-Cu system alloy is Zr-1Nb-0.01Cu alloy or Zr-1.1Nb-0.05Cu alloy.
Described Zr-Nb-Cu system second phase particles in alloy is small and dispersed distribution.
Due to the enforcement of technique scheme, the present invention compared with prior art tool has the following advantages:
The Zr-Nb-Cu system alloy phase ratio prepared with traditional preparation methods, the Zr-Nb-Cu system alloy that preparation method of the present invention prepares, the distribution of the size of particles of its second-phase less and even dispersion, corrosion resistance nature improves more than 25%.
Accompanying drawing explanation
The second phase particles distribution metallograph of the Zr-1Nb-0.01Cu alloy of Fig. 1 prepared by embodiment 1;
The second phase particles distribution metallograph of the Zr-1Nb-0.01Cu alloy of Fig. 2 prepared by embodiment 2;
The second phase particles distribution metallograph of the Zr-1.1Nb-0.05Cu alloy of Fig. 3 prepared by embodiment 3;
The second phase particles distribution metallograph of the Zr-1Nb-0.01Cu alloy of Fig. 4 prepared by comparative example 1;
The second phase particles distribution metallograph of the Zr-1Nb-0.01Cu alloy of Fig. 5 prepared by comparative example 2;
The second phase particles distribution metallograph of the Zr-1.1Nb-0.05Cu alloy of Fig. 6 prepared by comparative example 3;
Fig. 7 is the surrosion graphic representation of the prepared Zr-1Nb-0.01Cu alloy of embodiment 1 and comparative example 1;
Fig. 8 is the surrosion graphic representation of the prepared Zr-1Nb-0.01Cu alloy of embodiment 2 and comparative example 2;
Fig. 9 is the surrosion graphic representation of the prepared Zr-1.1Nb-0.05Cu alloy of embodiment 3 and comparative example 3.
Embodiment
Below by specific embodiment, the invention will be further described.
The preparation method of Zr-Nb-Cu system of the present invention alloy, comprises the following steps:
(1) forge: the zirconium alloy product containing Nb and Cu element is forged at 800 ~ 900 DEG C;
(2) quench: carry out quench (quenching can be carried out in atmosphere) after the product after step (1) being forged is incubated 20 ~ 40min at 1000 ~ 1050 DEG C;
(3) hot extrusion: the product after step (2) being quenched carries out hot extrusion at 550 ~ 600 DEG C;
(4) anneal first: the product after step (3) hot extrusion is annealed at 500 ~ 550 DEG C, anneals 2 ~ 4 hours;
(5) three cold rolling and annealing: the product after step (4) being annealed first carries out three cold rolling and annealing again, obtained Zr-Nb-Cu system alloy;
In step (5), three times concrete steps that are cold rolling and annealing are as follows:
First time is cold rolling and anneal: it is cold rolling that the product after step (4) being annealed first carries out first time, after deflection reaches 50 ~ 70%, at 500 ~ 550 DEG C, carries out anneal, anneals 0.5 ~ 1.5 hour;
Cold rolling and the annealing of second time: the product after cold rolling for first time and annealing is carried out second time cold rolling, after deflection reaches 50 ~ 70%, carry out anneal at 500 ~ 550 DEG C, anneal 0.5 ~ 1.5 hour;
Third time cold rolling and annealing: the product after cold rolling for second time and annealing is carried out third time cold rolling, after deflection reaches 50 ~ 70%, carry out anneal at 450 ~ 520 DEG C, anneal 1.5 ~ 4 hours.
Described first time, cold rolling and in annealing annealing time was 0.5 ~ 1.5 hour.
Cold rolling and in annealing the annealing time of described second time is 0.5 ~ 1.5 hour.
Described third time, cold rolling and in annealing annealing time was 1.5 ~ 4 hours.
Described annealing time is first 2 ~ 4 hours.
Embodiment 1
The present embodiment provides a kind of preparation method of Zr-1Nb-0.01Cu alloy, consisting of of this Zr-1Nb-0.01Cu alloy: Nb1wt%, Cu0.01wt%, Zr surplus and inevitably impurity, and this preparation method comprises the following steps:
(1) forge: the zirconium alloy product containing Nb and Cu element is forged at 800 ~ 900 DEG C;
(2) quench: quench after the product after step (1) being forged is incubated 20min at 1020 DEG C;
(3) hot extrusion: the product after step (2) being quenched carries out hot extrusion at 550 ~ 600 DEG C;
(4) anneal first: the product after step (3) hot extrusion is annealed at 550 DEG C, anneals 2 hours;
(5) three cold rolling and annealing: the product after step (4) being annealed first carries out three cold rolling and annealing again, obtained Zr-Nb-Cu system alloy;
In step (5), three times concrete steps that are cold rolling and annealing are as follows:
First time is cold rolling and anneal: it is cold rolling that the product after step (4) being annealed first carries out first time, after deflection reaches 55%, at 520 DEG C, carries out anneal, anneals 1 hour;
Cold rolling and the annealing of second time: the product after cold rolling for first time and annealing is carried out second time cold rolling, after deflection reaches 55%, carry out anneal at 520 DEG C, anneal 1 hour;
Third time cold rolling and annealing: the product after cold rolling for second time and annealing is carried out third time cold rolling, after deflection reaches 65%, carry out anneal at 520 DEG C, anneal 2 hours.
Embodiment 2
The present embodiment provides a kind of preparation method of Zr-1Nb-0.01Cu alloy, consisting of of this Zr-1Nb-0.01Cu alloy: Nb1wt%, Cu0.01wt%, Zr surplus and inevitably impurity, and this preparation method comprises the following steps:
(1) forge: the zirconium alloy product containing Nb and Cu element is forged at 800 ~ 900 DEG C;
(2) quench: quench after the product after step (1) being forged is incubated 20min at 1020 DEG C;
(3) hot extrusion: the product after step (2) being quenched carries out hot extrusion at 550 ~ 600 DEG C;
(4) anneal first: the product after step (3) hot extrusion is annealed at 550 DEG C, anneals 2 hours;
(5) three cold rolling and annealing: the product after step (4) being annealed first carries out three cold rolling and annealing again, obtained Zr-Nb-Cu system alloy;
In step (5), three times concrete steps that are cold rolling and annealing are as follows:
First time is cold rolling and anneal: it is cold rolling that the product after step (4) being annealed first carries out first time, after deflection reaches 55%, at 550 DEG C, carries out anneal, anneals 1 hour;
Cold rolling and the annealing of second time: the product after cold rolling for first time and annealing is carried out second time cold rolling, after deflection reaches 55%, carry out anneal at 550 DEG C, anneal 1 hour;
Third time cold rolling and annealing: the product after cold rolling for second time and annealing is carried out third time cold rolling, after deflection reaches 65%, carry out anneal at 460 DEG C, anneal 4 hours.
Embodiment 3
The present embodiment provides a kind of preparation method of Zr-1.1Nb-0.05Cu alloy, consisting of of this Zr-1.1Nb-0.05Cu alloy: Nb1.1wt%, Cu0.05wt%, Zr surplus and inevitably impurity, and this preparation method comprises the following steps:
(1) forge: the zirconium alloy product containing Nb and Cu element is forged at 800 ~ 900 DEG C;
(2) quench: quench after the product after step (1) being forged is incubated 20min at 1020 DEG C;
(3) hot extrusion: the product after step (2) being quenched carries out hot extrusion at 550 ~ 600 DEG C;
(4) anneal first: the product after step (3) hot extrusion is annealed at 550 DEG C, anneals 2 hours;
(5) three cold rolling and annealing: the product after step (4) being annealed first carries out three cold rolling and annealing again, obtained Zr-Nb-Cu system alloy;
In step (5), three times concrete steps that are cold rolling and annealing are as follows:
First time is cold rolling and anneal: it is cold rolling that the product after step (4) being annealed first carries out first time, after deflection reaches 55%, at 540 DEG C, carries out anneal, anneals 1 hour;
Cold rolling and the annealing of second time: the product after cold rolling for first time and annealing is carried out second time cold rolling, after deflection reaches 55%, carry out anneal at 540 DEG C, anneal 1 hour;
Third time cold rolling and annealing: the product after cold rolling for second time and annealing is carried out third time cold rolling, after deflection reaches 65%, carry out anneal at 520 DEG C, anneal 2 hours.
Temperature during three times in the preparation method of traditional Zr-Nb-Cu alloy cold rolling and annealing cold roller and deformed is higher, and annealing time is longer, i.e. (a) first cold rolling and annealing: after cold rolling reduction reaches 50 ~ 60%, anneal 2-4 hour at 560-600 DEG C; B () second time is cold rolling and anneal: after cold rolling reduction reaches 50-60%, anneal 2-4 hour at 560-600 DEG C; C () third time is cold rolling and anneal: after cold rolling reduction reaches 50-60%, anneal 8-10 hour at 560-600 DEG C.Illustrate below by comparative example:
Comparative example 1
This comparative example provides a kind of preparation method of Zr-1Nb-0.01Cu alloy, consisting of of this Zr-1Nb-0.01Cu alloy: Nb1wt%, Cu0.01wt%, Zr surplus and inevitably impurity, this preparation method is except step (5) three times is cold rolling and except annealing process, all the other steps (i.e. step (1) ~ (4)) are identical with embodiment 1.
In the step (5) of this comparative example, three times concrete steps that are cold rolling and annealing are as follows:
First time cold rolling and annealing: the product after step (4) being annealed first carries out first cold rolling, after deflection reaches 55%, carries out anneal at 580 DEG C, anneals 4 hours;
Cold rolling and the annealing of second time: the product after cold rolling for first time and annealing is carried out second time cold rolling, after deflection reaches 55%, carry out anneal at 580 DEG C, anneal 4 hours;
Third time cold rolling and annealing: the product after cold rolling for second time and annealing is carried out third time cold rolling, after deflection reaches 65%, carry out anneal at 580 DEG C, anneal 8 hours.
Comparative example 2
This comparative example provides a kind of preparation method of Zr-1Nb-0.01Cu alloy, consisting of of this Zr-1Nb-0.01Cu alloy: Nb1wt%, Cu0.01wt%, Zr surplus and inevitably impurity, this preparation method is except step (5) three times is cold rolling and except annealing process, all the other steps are identical with embodiment 2 with (i.e. step (1) ~ (4)).
In the step (5) of this comparative example, three times concrete steps that are cold rolling and annealing are as follows:
First time cold rolling and annealing: the product after step (4) being annealed first carries out first cold rolling, after deflection reaches 55%, carries out anneal at 580 DEG C, anneals 2 hours;
Cold rolling and the annealing of second time: the product after cold rolling for first time and annealing is carried out second time cold rolling, after deflection reaches 55%, carry out anneal at 580 DEG C, anneal 2 hours;
Third time cold rolling and annealing: the product after cold rolling for second time and annealing is carried out third time cold rolling, after deflection reaches 65%, carry out anneal at 580 DEG C, anneal 10 hours.
Comparative example 3
This comparative example provides a kind of preparation method of Zr-1.1Nb-0.05Cu alloy, consisting of of this Zr-1.1Nb-0.05Cu alloy: Nb1.1wt%, Cu0.05wt%, Zr surplus and inevitably impurity, this preparation method is except step (5) three times is cold rolling and except annealing process, all the other steps (i.e. step (1) ~ (4)) are identical with embodiment 3.
In the step (5) of this comparative example, three times concrete steps that are cold rolling and annealing are as follows:
First time cold rolling and annealing: the product after step (4) being annealed first carries out first cold rolling, after deflection reaches 55%, carries out anneal at 560 DEG C, anneals 4 hours;
Cold rolling and the annealing of second time: the product after cold rolling for first time and annealing is carried out second time cold rolling, after deflection reaches 55%, carry out anneal at 560 DEG C, anneal 4 hours;
Third time cold rolling and annealing: the product after cold rolling for second time and annealing is carried out third time cold rolling, after deflection reaches 65%, carry out anneal at 560 DEG C, anneal 10 hours.
Carry out metallurgical analysis to the Zr-Nb-Cu alloy prepared by embodiment 1 ~ 3 and comparative example 1 ~ 3, result is as shown in Fig. 1 ~ 6.
Comparison diagram 1 and Fig. 4, the second phase particles of embodiment 1 is small and dispersed distribution, and particle average size is 45.1nm; The second-phase size of comparative example 1 is comparatively large, and distribution of sizes is uneven, and particle average size is 60.2nm.
Comparison diagram 2 and Fig. 5, the second phase particles of embodiment 2 is small and dispersed distribution, and particle average size is 42.4nm; The second-phase size of comparative example 2 is comparatively large, and distribution of sizes is uneven, and particle average size is 67.1nm.
Comparison diagram 3 and Fig. 6, the second phase particles of embodiment 3 is small and dispersed distribution, and particle average size is 39.1nm; The second-phase size of comparative example 3 is comparatively large, and distribution of sizes is uneven, and particle average size is 58.7nm.
From above-mentioned comparing result, compare traditional technology, adopt preparation method of the present invention, in zirconium alloy, second phase particles thinning effect is obvious, and the mean sizes of second phase particles reduces more than 25%.
Corrosion resistance nature test is carried out to the Zr-Nb-Cu alloy prepared by embodiment 1 ~ 3 and comparative example 1 ~ 3, draws surrosion curve, as shown in Fig. 7 ~ 9.The corrosive medium adopted is 360 ° of C/18.6MPa/3.5ppmLi+1000ppmB aqueous solution.
As can be seen from Figure 7, compare ratio 1, the corrosion resistance nature of the Zr-1Nb-0.01Cu alloy that embodiment 1 is prepared improves 25%.
As can be seen from Figure 8, compare ratio 2, the corrosion resistance nature of the Zr-1Nb-0.01Cu alloy that embodiment 2 is prepared improves 28%.
As can be seen from Figure 9, compare ratio 3, the corrosion resistance nature of the Zr-1.1Nb-0.05Cu alloy that embodiment 3 is prepared improves more than 25%.
From above-mentioned comparing result, compare traditional technology, adopt preparation method of the present invention, the corrosion resistance nature of zirconium alloy is greatly enhanced, and improves more than 25%.
Preparation method of the present invention is applicable to the preparation of Zr-(0.6-1.2) Nb-(0.01-0.1) Cu system alloy.
Above to invention has been detailed description; its object is to allow the personage being familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; and the invention is not restricted to the embodiments described; the equivalence change that all spirit according to the present invention are done or modification, all should be encompassed within protection scope of the present invention.
Claims (3)
1. a preparation method for Zr-Nb-Cu system alloy, described preparation method comprises the following steps:
(1) forge: the zirconium alloy product containing Nb and Cu element is forged at 800 ~ 900 DEG C;
(2) quench: quench after the product after step (1) being forged is incubated 20 ~ 40min at 1000 ~ 1050 DEG C;
(3) hot extrusion: the product after step (2) being quenched carries out hot extrusion at 550 ~ 600 DEG C;
(4) anneal first: the product after step (3) hot extrusion is annealed at 500 ~ 550 DEG C;
(5) three cold rolling and annealing: the product after step (4) being annealed first carries out three cold rolling and annealing again, obtained Zr-Nb-Cu system alloy;
It is characterized in that:
Described annealing time is first 2 ~ 4 hours;
In step (5), described three concrete steps that are cold rolling and annealing are as follows:
First time is cold rolling and anneal: it is cold rolling that the product after described step (4) being annealed first carries out first time, after deflection reaches 50 ~ 70%, at 500 ~ 550 DEG C, carries out anneal, and described first time, cold rolling and in annealing annealing time was 0.5 ~ 1.5 hour;
Cold rolling and the annealing of second time: the product after cold rolling for first time and annealing is carried out second time cold rolling, after deflection reaches 50 ~ 70%, carry out anneal at 500 ~ 550 DEG C, cold rolling and in annealing the annealing time of described second time is 0.5 ~ 1.5 hour;
Third time cold rolling and annealing: the product after cold rolling for second time and annealing is carried out third time cold rolling, after deflection reaches 50 ~ 70%, carry out anneal at 450 ~ 520 DEG C, described third time, cold rolling and in annealing annealing time was 1.5 ~ 4 hours;
Described Zr-Nb-Cu system alloy is that Zr and inevitable impurity form by Nb0.6-1.2wt.%, Cu0.01-0.1wt.%, surplus.
2. the preparation method of Zr-Nb-Cu system according to claim 1 alloy, is characterized in that: described Zr-Nb-Cu system alloy is Zr-1Nb-0.01Cu alloy or Zr-1.1Nb-0.05Cu alloy.
3. the preparation method of Zr-Nb-Cu system according to claim 1 alloy, is characterized in that: described Zr-Nb-Cu system second phase particles in alloy is small and dispersed distribution.
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| CN112458337B (en) * | 2020-04-13 | 2022-02-18 | 国核宝钛锆业股份公司 | Zirconium alloy and preparation method of zirconium alloy profile |
| CN112481522B (en) * | 2020-04-13 | 2021-11-12 | 国核宝钛锆业股份公司 | Zirconium alloy, preparation method of zirconium alloy and zirconium alloy section |
| CN111842486B (en) * | 2020-06-24 | 2022-06-24 | 江苏圣珀新材料科技有限公司 | Cold rolling process of high-temperature alloy GH4169 |
| CN113355619B (en) * | 2021-06-04 | 2022-08-09 | 西安交通大学 | Heat treatment method for preventing thermal mechanical processing cracking of zirconium alloy |
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| CN103650659B (en) * | 2005-12-27 | 2010-03-10 | 西北有色金属研究院 | A kind of preparation method of used by nuclear reactor zirconium-base alloy sheet material |
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