CN103938024B - A kind of zirconium alloy and preparation method thereof - Google Patents
A kind of zirconium alloy and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of zirconium alloy and preparation method thereof, this zirconium alloy comprises: the Zr of the Bi of 0.05 ~ 0.8wt%, the Mo of 0.05 ~ 1.0wt%, the Cr of 0.4 ~ 1.2wt%, the Fe of 0.1 ~ 0.5wt% and surplus.Compared with existing zirconium alloy, the present invention with the addition of Mo and Bi on the basis of Zr-Fe-Cr alloy simultaneously.First, Fe and Cr element forms the Zr(FeCr of small and dispersed distribution)
2precipitated phase can improve the intensity of Zr alloy, and meanwhile, Fe and the Cr element adding suitable proportioning can improve Corrosion Resistance of Zirconium Alloys; Secondly, add the strengthening phase that appropriate Mo element can obtain small and dispersed in alloy, the hot strength of zirconium alloy and creep-resistant property are improved; Again, the interpolation of Bi element can further improve the tensile strength of alloy, and can balance the fragility that Mo element brings, and improves the plasticity of zirconium alloy.
Description
Technical field
The invention belongs to technical field of alloy material, particularly relate to a kind of zirconium alloy and preparation method thereof.
Background technology
Zirconium alloy has lower neutron-absorption cross-section, good heat conductivility, good high-temperature resistant water corrosive nature and Flouride-resistani acid phesphatase energy for growth, and therefore in water cooled nuclear reactor, zirconium alloy is widely used as the can material of fuel stick and the structural element of nuclear reactor core.
Along with power producer technology is towards the future development improving fuel burnup and reduce dyestuff cycle cost, improve reactor efficiency, improve safe reliability, the performances such as the corrosion resistance of key core parts fuel element can material zirconium alloy, hydrogen sucking function, mechanical property and irradiation dimensional stability are had higher requirement.Under arms under condition under (stress of irradiation, high temperature, high pressure and complexity), can there is creep and fatigue in fuel element, creep property is one of the major issue that will consider when working in water-cooled power reactor of zirconium alloy.
At present, the zirconium alloy of industrial-scale production mainly contains two series: zirconium tin system and zirconium niobium system.The former representative is Zr-2 alloy, and the representative of the latter is Zr-2.5Nb alloy.Zirconium alloy interalloy element selection principle is: a neutron absorption that obviously can not increase zirconium retains face; Two will can not damage processing performance too much while the patience improving zirconium and intensity.In zirconium tin system alloy, comprehensively adding (Zr-2 alloy) of tin, iron, chromium, nickel, the thermal conductivity of the intensity of material and solidity to corrosion, Corrosion Resistant Film can be improved, reduce the susceptibility of condition of surface to corrosion; Not nickeliferous in Zr-4 alloy, and suitably increase iron level, this alloy corrosion hydrogen－sucking amount is because the general left and right of Zr-2.In zirconium niobium system alloy, when the addition of niobium reaches the solid solubility limit of α-Zr under use temperature, the corrosion resistance nature of alloy is best.
Wherein, the most ripe, most widely used is the zirconium alloy being referred to as Zr-2, Zr-4 alloy.Zr-2 and Zr-4 alloy has higher high-temperature resistant water and the feature such as steam corrosion performance and suitable strength and ductility because of it, is used as the fuel element can of water-cooled power reactor for a long time.
But along with nuclear fuel assembly is to the long-lived phase, the development in high burnup direction, require that the zirconium alloy as reactor structural material must have better anti-corrosion, creep resistance, the over-all propertieies such as radioprotective growth, and Zr-2 and Zr-4 alloy can meet fuel burnup design load is generally 33GWd/tU, do not meet the demands, therefore need to study the novel zirconium alloy with higher-strength and plasticity for reactor structural material, and the research tendency of existing novel zirconium alloy is on the basis to Zr-Nb system and Zr-Sn-Nb system alloy carries out the adjustment of alloying constituent content and adds other alloying elements, or both carry out reaching the object improving alloy monolithic performance simultaneously.
The present invention considers to provide a kind of zirconium alloy, and this zirconium alloy is not containing tin element.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of zirconium alloy and preparation method thereof, and this zirconium alloy does not contain tin element and has higher intensity and plasticity.
The invention provides a kind of zirconium alloy, comprising:
Bi0.05~0.8wt%；
Mo0.05~1.0wt%；
Cr0.4~1.2wt%；
Fe0.1~0.5wt%；
Zr surplus.
Preferably, the content of described Bi is 0.3 ~ 0.8wt%.
Preferably, the content of described Mo is 0.2 ~ 1.0wt%.
Present invention also offers a kind of preparation method of zirconium alloy, comprise the following steps:
A) by Bi, Mo, Cr, Fe and Zr mixing, melting, obtains zirconium alloy; Wherein the content of the content of Bi to be the content of 0.05 ~ 0.8wt%, Mo be 0.05 ~ 1.0wt%, Cr is the content of 0.4 ~ 1.2wt%, Fe is 0.1 ~ 0.5wt%, and surplus is Zr.
Preferably, described step a) is specially:
A1) mixed by Zr and Bi, melting, obtains Zr-Bi master alloy;
A2) by described Zr-Bi master alloy, Zr, Fe, Cr and Mo mixing, melting, obtains zirconium alloy; Wherein the content of the content of Bi to be the content of 0.05 ~ 0.8wt%, Mo be 0.05 ~ 1.0wt%, Cr is the content of 0.4 ~ 1.2wt%, Fe is 0.1 ~ 0.5wt%, and surplus is Zr.
Preferably, described step a2) in melting be 5 × 10 in vacuum tightness
-4~ 5 × 10
-3carry out under the condition of Pa.
Preferably, described step a2) in melting number of times be 4 ~ 6 times.
Preferably, described step a2) in melting carry out in non-consumable arc furnace.
Preferably, described step a2) in melting carry out under the protection of rare gas element.
Preferably, described rare gas element is argon gas.
The invention provides a kind of zirconium alloy and preparation method thereof, this zirconium alloy comprises: the Zr of the Bi of 0.05 ~ 0.8wt%, the Mo of 0.05 ~ 1.0wt%, the Cr of 0.4 ~ 1.2wt%, the Fe of 0.1 ~ 0.5wt% and surplus.Compared with existing zirconium alloy, the present invention with the addition of Mo and Bi on the basis of Zr-Fe-Cr alloy simultaneously.First, Fe and Cr element is the principal element forming second-phase in zirconium alloy, the Zr(FeCr of small and dispersed distribution)
2precipitated phase can improve the intensity of Zr alloy, and meanwhile, Fe and the Cr element of suitable proportioning adds the corrosion resistance nature that can make raising zirconium alloy in zirconium alloy to; Secondly, add the strengthening phase that appropriate Mo element can obtain small and dispersed in alloy, the hot strength of zirconium alloy and creep-resistant property are improved; Again, the interpolation of Bi element can further improve the tensile strength of alloy, and can balance the fragility that Mo element brings, and improves the plasticity of zirconium alloy.
Accompanying drawing explanation
Fig. 1 is the tensile stress-strain curve figure of the zirconium alloy obtained in the embodiment of the present invention 1;
Fig. 2 is the tensile stress-strain curve figure of the zirconium alloy obtained in the embodiment of the present invention 2;
Fig. 3 is the tensile stress-strain curve figure of the zirconium alloy obtained in the embodiment of the present invention 3;
Fig. 4 is the tensile stress-strain curve figure of the zirconium alloy obtained in the embodiment of the present invention 1 ~ 3;
Fig. 5 is the hardness of zirconium alloy and the broken line graph of Bi relation with contents that obtain in the embodiment of the present invention 1 ~ 3 and comparative example 1.
Embodiment
The invention provides a kind of zirconium alloy, comprising:
Bi0.05~0.8wt%；
Mo0.05~1.0wt%；
Cr0.4~1.2wt%；
Fe0.1~0.5wt%；
Zr surplus.
Wherein, the content of Fe is preferably 0.2 ~ 0.4wt%, then is preferably 0.3 ~ 0.4wt%.
The content of Cr is preferably 0.4 ~ 1.0wt%, then is preferably 0.6 ~ 1.0wt%.
Fe and Cr element is the forming element of second-phase in zirconium alloy mainly, the Zr(FeCr of small and dispersed distribution)
2precipitated phase can improve the intensity of zirconium alloy, and, the corrosion resistance nature of zirconium alloy in 500 DEG C of superheated vapours or supercritical water can be made by the content of adjustment Fe and Cr element in zirconium alloy.
The content of described Mo is preferably 0.2 ~ 1.0wt%, then is preferably 0.2 ~ 0.8wt%, is more preferably 0.2 ~ 0.6wt%.
Mo element has solution strengthening and dispersion-strengthened action, the mechanical property of zirconium alloy can be improved, and Mo element also has grain refining effect makes structure refinement, the strengthening phase compared with small and dispersed can be obtained, improve hot strength and the creep-resistant property of zirconium alloy, but its interpolation can cause the fragility of zirconium alloy to increase, and has a certain impact to the corrosion resistance nature of zirconium alloy.
The content of described Bi is preferably 0.1 ~ 0.8wt%, then is preferably 0.3 ~ 0.8wt%, is more preferably 0.3 ~ 0.5wt%.
Bi element can improve corrosion resistance nature and the plasticity of zirconium alloy, but its too high levels can cause zirconium alloy plasticity to decline, and intensity reduces.
The present invention is by the adjustment composition of Chrome metal powder and the content of each composition, interpolation as Fe element can suppress Mo element on the impact of Corrosion Resistance of Zirconium Alloys, the interpolation of Bi element can balance the fragility that Mo element brings, improve plasticity and the corrosion resistance nature of zirconium alloy, and the interpolation of Cr element effectively can suppress the segregation of Bi element, utilize influencing each other of each element, and then the mechanical property such as the hot strength of raising zirconium alloy entirety and creep-resistant property.
Present invention also offers the preparation method of above-mentioned zirconium alloy, comprise the following steps: a) by Bi, Mo, Cr, Fe and Zr mixing, melting, obtains zirconium alloy; Wherein the content of the content of Bi to be the content of 0.05 ~ 0.8wt%, Mo be 0.05 ~ 1.0wt%, Cr is the content of 0.4 ~ 1.2wt%, Fe is 0.1 ~ 0.5wt%, and surplus is Zr.
Wherein, according to the present invention, described Bi, Mo, Cr, Fe and Zr element are all same as above, do not repeat them here.
Described in the present invention, step a) is specially: a1) Zr and Bi is mixed, melting, obtains Zr-Bi master alloy; A2) by described Zr-Bi master alloy, Zr, Fe, Cr and Mo mixing, melting, obtains zirconium alloy.
Described step a1) in melting method be method well known to those skilled in the art, there is no special restriction, the condition of described melting is also method well known to those skilled in the art, there is no special restriction.
Described step a2) in melting method be method well known to those skilled in the art, there is no special restriction, the present invention preferably carries out melting in non-consumable arc furnace.In the present invention, described step a2) in melting be preferably less than 5 × 10 in vacuum tightness
-3carry out under the condition of Pa, more preferably vacuum tightness is 5 × 10
-4~ 5 × 10
-3pa.Described step a2) in melting preferably carry out under the protection of rare gas element, described rare gas element is rare gas element well known to those skilled in the art, and there is no special restriction, described in the present invention, rare gas element is preferably argon gas.For making the abundant blending dispersion of each component of zirconium alloy even, step a2 of the present invention) in melting number of times be preferably 4 ~ 6 times.
Because component each in zirconium alloy of the present invention influences each other, improve intensity and the plasticity of zirconium alloy, simplify manufacturing procedure, and be conducive to processing and the size control of product forms.
In order to further illustrate the present invention, below in conjunction with embodiment, a kind of zirconium alloy provided by the invention and preparation method thereof is described in detail.
Reagent used in following examples is commercially available.
Embodiment 1
100gZr and 110gBi mixes by 1.1, founds, obtains Zr-Bi master alloy, and is 50wt% by the concrete content that chemical analysis obtains Bi element.
The 0.2gZr-Bi master alloy obtained in 1.1 pulverizing adds in the compound of 48.9gZr, 0.2gFe, 0.5gCr and 0.2gMo by 1.2, then utilizes non-consumable arc furnace to be 5 × 10 in vacuum tightness
-3under the condition of Pa, 0.5atm argon shield, melting 5 times, obtains zirconium alloy, and wherein the content of the content of the content of Bi to be the content of 0.2wt%, Mo be 0.4wt%, Cr to be the content of 1.0wt%, Fe be 0.4wt%, Zr is 98wt%.
Mechanics Performance Testing is carried out to the zirconium alloy obtained in 1.2, obtain its tensile strength, yield strength and unit elongation, as shown in table 1, zirconium alloy is carried out hot rolling and anneal, then carry out Mechanics Performance Testing at ambient temperature and obtain its tensile stress-strain curve, as shown in Figure 1, wherein, A is the stress-strain curve of tension specimen 1, and B is the stress-strain curve of tension specimen 2.
Embodiment 2
100gZr and 110gBi mixes by 2.1, founds, obtains Zr-Bi master alloy, and is 50wt% by the concrete content that chemical analysis obtains Bi element.
The 0.4gZr-Bi master alloy obtained in 2.1 pulverizing adds in the compound of 48.7gZr, 0.2gFe, 0.5gCr and 0.2gMo by 2.2, then utilizes non-consumable arc furnace to be 5 × 10 in vacuum tightness
-3under the condition of Pa, 0.5atm argon shield, melting 5 times, obtains zirconium alloy, and wherein the content of the content of the content of Bi to be the content of 0.4wt%, Mo be 0.4wt%, Cr to be the content of 1.0wt%, Fe be 0.4wt%, Zr is 97.8wt%.
Hot rolling and anneal are carried out to the zirconium alloy obtained in 2.2, then carry out Mechanics Performance Testing at ambient temperature and obtain its tensile stress-strain curve, as shown in Figure 2, wherein, A is the stress-strain curve of tension specimen 1, and B is the stress-strain curve of tension specimen 2.
Embodiment 3
100gZr and 110gBi mixes by 3.1, founds, obtains Zr-Bi master alloy, and is 50wt% by the concrete content that chemical analysis obtains Bi element.
The 0.6gZr-Bi master alloy obtained in 3.1 pulverizing adds in the compound of 48.5gZr, 0.2gFe, 0.5gCr and 0.2gMo by 3.2, then utilizes non-consumable arc furnace to be 5 × 10 in vacuum tightness
-3under the condition of Pa, 0.5atm argon shield, melting 5 times, obtains zirconium alloy, and wherein the content of the content of the content of Bi to be the content of 0.6wt%, Mo be 0.4wt%, Cr to be the content of 1.0wt%, Fe be 0.4wt%, Zr is 97.6wt%.
Hot rolling and anneal are carried out to the zirconium alloy obtained in 3.2, then carry out Mechanics Performance Testing at ambient temperature and obtain its tensile stress-strain curve, as shown in Figure 3, wherein, A is the stress-strain curve of tension specimen 1, and B is the stress-strain curve of tension specimen 2.
Fig. 4 is the tensile stress-strain curve synthesizing map of the zirconium alloy obtained in embodiment 1 ~ 3, and wherein a is the zirconium alloy obtained in embodiment 1, and b is the zirconium alloy obtained in embodiment 2, and c is the zirconium alloy obtained in embodiment 3.
Comparative example 1
By in the compound of 49.1gZr, 0.2gFe, 0.5gCr and 0.2gMo, non-consumable arc furnace is then utilized to be 5 × 10 in vacuum tightness
-3under the condition of Pa, 0.5atm argon shield, melting 5 times, obtains zirconium alloy, and wherein the content of the content of Mo to be the content of 0.4wt%, Cr be 1.0wt%, Fe is the content of 0.4wt%, Zr is 98.2wt%.
Mechanics Performance Testing is carried out to the zirconium alloy obtained in comparative example 1, obtains its tensile strength, yield strength and unit elongation, as shown in table 1, obtain its tensile stress-strain curve, as shown in Figure 1.
Respectively hot rolling and anneal are carried out to the zirconium alloy obtained in embodiment 1 ~ 3 and comparative example, then carry out hardness test, obtain the broken line graph of the relation of itself and Bi content, as shown in Figure 5, wherein A is the zirconium alloy after hot rolling process, and B is the zirconium alloy after hot-roll annealing process.
The mechanical property of table 1 zirconium alloy
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a zirconium alloy, is characterized in that, comprising:
Bi0.05~0.8wt%；
Mo0.05~1.0wt%；
Cr0.4~1.2wt%；
Fe0.1~0.5wt%；
Zr surplus.
2. zirconium alloy according to claim 1, is characterized in that, the content of described Bi is 0.3 ~ 0.8wt%.
3. zirconium alloy according to claim 1, is characterized in that, the content of described Mo is 0.2 ~ 1.0wt%.
4. a preparation method for zirconium alloy, is characterized in that, comprises the following steps:
A) by Bi, Mo, Cr, Fe and Zr mixing, melting, obtains zirconium alloy; Wherein the content of the content of Bi to be the content of 0.05 ~ 0.8wt%, Mo be 0.05 ~ 1.0wt%, Cr is the content of 0.4 ~ 1.2wt%, Fe is 0.1 ~ 0.5wt%, and surplus is Zr.
5. preparation method according to claim 4, is characterized in that, described step a) is specially:
A1) mixed by Zr and Bi, melting, obtains Zr-Bi master alloy;
A2) by described Zr-Bi master alloy, Zr, Fe, Cr and Mo mixing, melting, obtains zirconium alloy; Wherein the content of the content of Bi to be the content of 0.05 ~ 0.8wt%, Mo be 0.05 ~ 1.0wt%, Cr is the content of 0.4 ~ 1.2wt%, Fe is 0.1 ~ 0.5wt%, and surplus is Zr.
6. preparation method according to claim 5, is characterized in that, described step a2) in melting be 5 × 10 in vacuum tightness
-4~ 5 × 10
-3carry out under the condition of Pa.
7. preparation method according to claim 5, is characterized in that, described step a2) in melting number of times be 4 ~ 6 times.
8. preparation method according to claim 5, is characterized in that, described step a2) in melting carry out in non-consumable arc furnace.
9. preparation method according to claim 5, is characterized in that, described step a2) in melting carry out under the protection of rare gas element.
10. preparation method according to claim 9, is characterized in that, described rare gas element is argon gas.
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| US5190721A (en) * | 1991-12-23 | 1993-03-02 | General Electric Company | Zirconium-bismuth-niobium alloy for nuclear fuel cladding barrier |
| CN102433465A (en) * | 2011-12-14 | 2012-05-02 | 国核宝钛锆业股份公司 | Bismuth-zirconium alloy |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5190721A (en) * | 1991-12-23 | 1993-03-02 | General Electric Company | Zirconium-bismuth-niobium alloy for nuclear fuel cladding barrier |
| CN102433465A (en) * | 2011-12-14 | 2012-05-02 | 国核宝钛锆业股份公司 | Bismuth-zirconium alloy |
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| Title |
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| Zr-Fe-Cr合金在500℃过热蒸汽中耐腐蚀性能研究;张太平等;《材料热处理技术》;20110430;第40卷(第8期);第32页表1 * |
| 添加Bi对Zr-4合金在400℃/10.3Mpa过热蒸汽中耐腐蚀性能的影响;姚美意等;《金属学报》;20120930;第48卷(第9期);摘要，第1098页左栏第2段 * |
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