CN102260841B - Method for preparing zirconium-niobium alloy with alpha/beta dual-state organization - Google Patents
Method for preparing zirconium-niobium alloy with alpha/beta dual-state organization Download PDFInfo
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- CN102260841B CN102260841B CN201110195057A CN201110195057A CN102260841B CN 102260841 B CN102260841 B CN 102260841B CN 201110195057 A CN201110195057 A CN 201110195057A CN 201110195057 A CN201110195057 A CN 201110195057A CN 102260841 B CN102260841 B CN 102260841B
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Abstract
The invention relates to a method for preparing a zirconium-niobium alloy with an alpha/beta dual-state organization, which mainly comprises the following steps of: firstly obtaining an alpha single-phase martensite or basket-shaped organization from the zirconium-niobium alloy and then rolling the alloy to deform at the temperature of 20-600 DEG C, wherein the deformation amount is 30%-60% and the alloy is air-cooled to room temperature after the alloy is deformed; and coating a layer of static high-temperature anti-oxidizing paint on the deformed alloy, putting the alloy in a furnace for annealing treatment after the paint is dried and the furnace temperature reaches 800-900 DEG C, taking out the alloy after heat-preserving for 0.5-2 hours and air-cooling the alloy to room temperature. The final heat-treatment process in the invention can be used for final heat treatment of the cold-deformed zirconium-niobium alloy and is also suitable for the final heat treatment of the hot-deformed zirconium-niobium alloy. The invention has the advantages that: the strength and the impact toughness of the zirconium-niobium alloy with the dual-state organization are respectively increased by about 2 times and 0.6 times of that of a zirconium-niobium alloy with the basket-shaped organization and an equiaxial organization, the strength is increased by about 100 MPa, and meanwhile, the excellent tensile ductility is remained.
Description
Technical field
The present invention relates to a kind of preparing method's of alloy material, particularly a kind of zirconium-niobium alloy preparation method.
Background technology
Zirconium-niobium alloy has been widely used in preparing key members such as pressure tube, pressurized vessel owing to have advantages such as excellent anticorrosive performance, stable anti-radiation performance, higher intensity, low density in chemical industry and nuclear industry.The main structural state of zirconium-niobium alloy has the α single-phase martensite, equiaxed structure, three kinds of structural states of basket shape tissue.
The α single-phase martensite in the insulation of β phase region, treats to change into fully β back shrend mutually by zirconium-niobium alloy, martensitic transformation takes place obtain.Microstructure characteristics is that α crystal grain is very big, and α single-phase martensite intensity is higher than basket shape tissue and equiaxed structure, but plasticity is relatively poor.
Basket shape tissue in the insulation of β phase region, treats to change into fully β back shrend mutually by zirconium-niobium alloy, obtains in the annealing of alpha+beta phase region again.Microstructure characteristics is that the α that original β intragranular shortens is the structure that the basket shape weaves, and strip β is distributed between the α phase mutually.The stretching plastic of basket shape organizational groups is better than Wei Shi body tissue or α single-phase martensite, and fatigue property is lower than equiaxed structure, and fracture toughness property is not as synusia shape tissue.
Equiaxed structure can obtain through the recrystallization annealing processing by after the zirconium-niobium alloy distortion.Microstructure characteristics is etc. that axle α is distributed in the β phase matrix mutually.Equiaxed structure has good stretching plastic and fatigue strength, but its high temperature endurance performance (like creep rupture strength, high temperature creep), fracture toughness property are not as basket shape tissue and synusia shape tissue.
Along with the continuous development of nuclear industry and chemical industry, the long lifetime of the zirconium alloy member of under high temperature and high pressure environment, being on active service requires strong gradually.The bifurcation tissue that in the TiAl alloy, has obtained broad research is the set of equiaxed structure and synusia shape tissue.This tissue is in stratiform α/β tissue, the discrete axle α phase that waits of the some amount that distributing.Equiaxed structure has very high plasticity and fatigue strength, and lamellar structure has high fracture toughness property, excellent high temperature creep property and high temperature endurance performance.The bifurcation tissue combines stratiform and the advantage that waits axle shape tissue, and existing high plasticity, fatigue strength has good high temperature endurance performance again.Yet in zirconium alloy, do not see the report of allied organization so far, if can prepare zirconium alloy, with significantly improving the work-ing life of zirconium alloy member under high temperature and high pressure environment with bifurcation tissue.
Summary of the invention
The object of the present invention is to provide a kind of α/β bifurcation that has that can significantly improve alloy impelling strength, intensity and have a high stretching plastic to organize the preparation method of zirconium-niobium alloy.The present invention is out of shape and thermal treatment zirconium-niobium alloy, the bifurcation tissue that obtains to have axle primary such as certain volume fractional and synusia shape α/β to organize.
Technical scheme of the present invention is following:
1, pre-treatment: with zirconium-niobium alloy 1000～1050
oShrend behind C insulation 0.5～1h obtains the α single-phase martensite in this alloy.The α single-phase martensite zirconium-niobium alloy that preferably again above-prepared is gone out is 600
oC insulation 0.5～1h carries out anneal, obtains basket shape tissue.
2, deformation process: to above-mentioned zirconium-niobium alloy at 20-600
oC is rolled distortion, deflection 30%-60%.(a) for the zirconium-niobium alloy with α single-phase martensite, the rolling deformation process need is at 300-600
oCarry out in the C scope, in case the crack arrest line occurs, distortion back air cooling is to room temperature; (b) for the zirconium-niobium alloy with basket shape tissue, the rolling deformation process can be at 20-600
oCarry out in the C scope.(c), texturing temperature need be incubated 20-30min when being higher than 45 ℃.
3, thermal treatment: the anti-oxidation lacquer of any static state high-temperature of zirconium-niobium alloy surface-coated one deck after the rolling distortion (is moistened KOC-02 and the anti-oxidant decarburization protective cover of putting of KOC-15 that your surfacing ltd produces like Shanghai; The model that Huangyan, Zhejiang speciality coating factory produces is 202 the anti-decarburizing coating of high-temperature oxidation resistant; The model that Wuhan inscription new high-tech material ltd produces is the anti-decarburizing coating of MP100 high-temperature oxidation resistant; The anti-decarburizing coating of model JZ-403B high-temp antioxidizing that the new heat treatment material factory of Anqiu China produces); After waiting to coat with lacquer drying, reach 800-900 etc. furnace temperature
oC puts into stove with above-mentioned alloy and carries out anneal, takes out behind insulation 0.5～2 h, and air cooling is to room temperature.
The present invention has the following advantages:
1, the present invention is out of shape and thermal treatment zirconium-niobium alloy, the bifurcation tissue that obtains to have axle primary such as certain volume fractional and synusia shape α/β to organize.This has the zirconium-niobium alloy intensity of bifurcation tissue and impelling strength has basket shape tissue and the equiaxed structure zirconium-niobium alloy has improved nearly 2 times and 0.6 times respectively, and intensity has improved about 100MPa, has kept excellent stretching plastic simultaneously.
2, the final thermal treatment process among the present invention can be used for the final thermal treatment of zirconium-niobium alloy after the cold deformation, is applicable to the final thermal treatment of zirconium-niobium alloy after the thermal distortion again.
Description of drawings
The Zr705 α single-phase martensite metallograph of Fig. 1 for adopting the inventive method to obtain.
Fig. 2 for adopt the inventive method distortion back Zr705 900 ℃ of insulation 0.5h obtain etc. axle α organize metallograph with synusia shape α/β bifurcation.
Fig. 3 for adopt the inventive method distortion back Zr705 850 ℃ of insulation 1.5h obtain etc. axle α organize metallograph with synusia shape α/β bifurcation.
Fig. 4 organizes metallograph for the Zr705 basket shape that the inventive method obtains.
Fig. 5 for adopt the inventive method distortion back Zr705 850 ℃ of insulation 1h obtain etc. axle α organize metallograph with synusia shape α/β bifurcation.
Fig. 6 for adopt the inventive method distortion back Zr705 800 ℃ of insulation 2h obtain etc. axle α organize metallograph with synusia shape α/β bifurcation.
Embodiment
Embodiment 1
With the at first shrend behind 1000 ℃ of insulation 1h of Zr705 sheet material, obtain the α single-phase martensite, as shown in Figure 1.With above-mentioned alloy 600
oBe rolled behind the C insulation 30min, deflection is 60%, and distortion back air cooling is to room temperature.(202 high-temperature oxidation resistants prevent that decarburizing coating model 202, Huangyan, Zhejiang speciality coating factory produce with the anti-oxidant anti-decarburizing coating of above-mentioned deforming alloy surface-coated one deck then; No. 230, Zhejiang Province Huangyan economic and technological development zone Lv Ting road); Put it into temperature after the drying and be in 900 ℃ the High Temperature Furnaces Heating Apparatus, take out air cooling to room temperature behind the insulation 0.5h.Can obtain etc. axle primary phase volume fraction be about 21% with the bifurcation tissue that synusia shape α/β tissue is formed, as shown in Figure 2.Deng axle primary phase grain-size is 2-4 μ m.Carry out Mechanics Performance Testing, impelling strength is 62 J/cm
2, tensile strength is 698 MPa, unit elongation is 20.5%.
Embodiment 2
With the at first shrend behind 1050 ℃ of insulation 0.5h of Zr705 sheet material, obtain the α single-phase martensite.With above-mentioned alloy 400
oBe rolled behind the C insulation 25min, deflection is 40%, and distortion back air cooling is to room temperature.Then with the anti-oxidant anti-decarburizing coating of above-mentioned deforming alloy surface-coated one deck (the anti-decarburizing coating of high-temp antioxidizing; Model JZ-403B; The new heat treatment material factory of Anqiu China produces; Economic and technological development zone, Anqiu City, Shandong Province), puts it into temperature after the drying and be in 850 ℃ the High Temperature Furnaces Heating Apparatus, take out air cooling to room temperature behind the insulation 1.5h.Can obtain etc. axle primary phase volume fraction be about 30% with the bifurcation tissue that synusia shape α/β tissue is formed, as shown in Figure 3.Deng axle primary phase grain-size is 2-4 μ m.Carry out Mechanics Performance Testing, impelling strength is 70J/cm
2, tensile strength is 693 MPa, unit elongation is 23.8%.
Embodiment 3
With the at first shrend behind 1000 ℃ of insulation 1h of Zr705 sheet material, obtain basket shape tissue at 600 ℃ of insulation 1h subsequently, as shown in Figure 4.With above-mentioned alloy 200
oBe rolled behind the C insulation 20min, deflection is 50%, and distortion back air cooling is to room temperature.(high-temperature oxidation resistant is prevented the decarburization protective cover with the anti-oxidant anti-decarburization protective cover of above-mentioned deforming alloy surface-coated one deck; Model KOC-02, Shanghai profit that surfacing ltd, No. 2784, peace road, business section, Shanghai); Put it into temperature after the drying and be in 850 ℃ the High Temperature Furnaces Heating Apparatus; Take out air cooling to room temperature behind the insulation 1h, obtain to wait the bifurcation tissue of axle primary phase volume fraction 36%, as shown in Figure 5.Deng axle α phase grain-size is 2-4 μ m.This tissue is carried out Mechanics Performance Testing, and impelling strength is about 65 J/cm
2, tensile strength is about 682 MPa, and unit elongation is 25.6%.
Embodiment 4
With the at first shrend behind 1000 ℃ of insulation 50min of Zr705 sheet material, obtain basket shape tissue at 600 ℃ of insulation 0.5h subsequently.With above-mentioned alloy 20
oIt is rolling that C carries out multi-pass, and the accumulative total deflection of alloy is about 30%.(high-temperature oxidation resistant is prevented decarburizing coating with the anti-oxidant anti-decarburization protective cover of above-mentioned deforming alloy surface-coated one deck; Model MP100, Wuhan inscription new high-tech material ltd produces No. 17,8XXkou District Gutian, Wu Han city Wu Lu); Put it into temperature after the drying and be in 800 ℃ the High Temperature Furnaces Heating Apparatus; Take out air cooling to room temperature behind the insulation 2h, axle such as acquisition primary phase volume fraction is ~ 45% bifurcation tissue, and is as shown in Figure 6.Deng axle α phase grain-size is 2-4 μ m.This tissue is carried out Mechanics Performance Testing, and impelling strength is about 66 J/cm
2, tensile strength is about 670 MPa, and unit elongation is 26.2%.
Table 1 bifurcation is organized Zr705 and basket shape and is waited the axle shape to organize the mechanical property of Zr705 to contrast
Claims (3)
1. one kind has α/β bifurcation and organizes the preparation method of zirconium-niobium alloy, it is characterized in that:
(1) pre-treatment: with zirconium-niobium alloy 1000～1050
oShrend behind C insulation 0.5～1h obtains the α single-phase martensite in this alloy;
(2) deformation process: to above-mentioned zirconium-niobium alloy at 300-600
oC is rolled distortion, deflection 30%-60%, and distortion back air cooling is to room temperature;
(3) thermal treatment: the anti-oxidation lacquer of alloy-coated one deck static state high-temperature with after the above-mentioned distortion after waiting to coat with lacquer drying, reaches 800-900 etc. furnace temperature
oC puts into stove with above-mentioned alloy and carries out anneal, takes out behind soaking time 0.5～2 h, and air cooling is to room temperature.
2. one kind has α/β bifurcation and organizes the preparation method of zirconium-niobium alloy, it is characterized in that:
(1) pre-treatment: with zirconium-niobium alloy 1000～1050
oShrend behind C insulation 0.5～1h obtains the α single-phase martensite in this alloy, the α single-phase martensite zirconium-niobium alloy that above-prepared is gone out is 600
oC insulation 0.5～1h carries out anneal, obtains basket shape tissue;
(2) deformation process: to above-mentioned zirconium-niobium alloy at 20-600
oC is rolled distortion, deflection 30%-60%, and distortion back air cooling is to room temperature;
(3) thermal treatment:, after waiting to coat with lacquer drying, treat that furnace temperature reaches 800-900 with the anti-oxidation lacquer of alloy-coated one deck static state high-temperature after the above-mentioned distortion
oC puts into stove with above-mentioned alloy and carries out anneal, takes out behind soaking time 0.5～2 h, and air cooling is to room temperature.
3. a kind of α of having according to claim 2/β bifurcation is organized the preparation method of zirconium-niobium alloy, it is characterized in that: when texturing temperature is higher than 45 ℃, need be incubated 20-30min.
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| CN102816981B (en) * | 2012-08-13 | 2014-01-22 | 燕山大学 | Preparation method for zirconium-niobium alloy having gradient microstructure |
| CN110195199B (en) * | 2019-05-16 | 2020-11-17 | 西安交通大学 | Multi-stage three-dimensional multiphase layered zirconium alloy and preparation method thereof |
| CN113981347B (en) * | 2021-09-29 | 2022-10-25 | 西安交通大学 | High-strength-plasticity heterostructure zirconium alloy and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0085552A3 (en) * | 1982-01-29 | 1983-08-24 | Westinghouse Electric Corporation | Improvements in or relating to zirconium alloys |
| CN1075815A (en) * | 1992-01-17 | 1993-09-01 | 法玛通公司 | Nuclear fuel rod and tectal method for making thereof |
| CN1735706A (en) * | 2003-01-13 | 2006-02-15 | 欧洲塞扎斯“锆”公司 | Method of producing a zirconium alloy semi-finished product for the production of an elongated product and use thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0085552A3 (en) * | 1982-01-29 | 1983-08-24 | Westinghouse Electric Corporation | Improvements in or relating to zirconium alloys |
| CN1075815A (en) * | 1992-01-17 | 1993-09-01 | 法玛通公司 | Nuclear fuel rod and tectal method for making thereof |
| CN1735706A (en) * | 2003-01-13 | 2006-02-15 | 欧洲塞扎斯“锆”公司 | Method of producing a zirconium alloy semi-finished product for the production of an elongated product and use thereof |
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