CN105039886B - Method for preparing Zr-2.5Nb alloy rod with uniform small structure phase - Google Patents
Method for preparing Zr-2.5Nb alloy rod with uniform small structure phase Download PDFInfo
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- CN105039886B CN105039886B CN201510475479.9A CN201510475479A CN105039886B CN 105039886 B CN105039886 B CN 105039886B CN 201510475479 A CN201510475479 A CN 201510475479A CN 105039886 B CN105039886 B CN 105039886B
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Abstract
The invention discloses a method for preparing a Zr-2.5Nb alloy rod with a uniform small structure phase. The Zr-2.5Nb alloy rod with the uniform small structure phase is obtained through the following steps of carrying out cogging and upsetting and rolling on a Zr-2.5Nb alloy ingot, carrying out intermediate forging and high-temperature water quenching through the short-term melting-down warm-keeping and forging technology, and carrying out low-temperature forging and finished product forging through the short-term melting-down warm-keeping and forging technology; the deformation is required to be not smaller than 30%. The structure evenness of blank can be improved, and the hydrogen absorption phenomenon in high-temperature long-time heat preservation of the blank is restrained; through high-temperature water quenching, the blank structure can be recrystallized, microstructure evolution is achieved, and a wide and thick grain boundary is eliminated; through frequent upsetting, rolling and forging, the blank structure can be made uniform, and therefore the Zr alloy rod with the uniform small structure is prepared, and the method is suitable for large-scale industrial production.
Description
Technical field
The invention belongs to technical field of nonferrous metal processing is and in particular to one kind has uniform fine tissue phase zr-2.5nb
The preparation method of alloy bar material.
Background technology
Zirconium and its alloy are due to having excellent nuclearity energy, comprehensive mechanical property, good machine-shaping property, weldability
Can and high temperature resistance water under high pressure and steam corrosion performance and be widely used in manufacturing the structural material of nuclear reactor.Meanwhile,
Zircaloy and tissue have the stronger compatibility, and are widely used in the preparation of body implant.At present, zirconium and its alloy
Production technology predominantly prepare tubing, sheet material prepared by rolling by extruding.And bar stock is prepared by flat-die forging and is related to
Seldom, because flat-die forging is with respect to extruding and rolling mill practice, in deformation, alloy compression chord direction is less, in addition zirconium and its alloy
Very well, in deformation, metal easily flows deformation plasticity, leads to deform uneven phenomenon generation.
Content of the invention
It is an object of the invention to provide a kind of preparation method with uniform fine tissue phase zr-2.5nb alloy bar material, solution
Existing forging method of having determined prepares the problem that non-uniform phenomenon easily occurs when zirconium and its alloy.
The technical solution adopted in the present invention is: a kind of preparation with uniform fine tissue phase zr-2.5nb alloy bar material
Method, specifically includes following steps:
Step 1, cogging:
Using zr-2.5nb alloy cast ingot, 930-960 DEG C of cogging temperature, come out of the stove after heating 100-150min, ingot casting is entered
Row three upsetting three is pulled out, and forging ratio controls in 1.9-2.1, fully crushes thick as-cast structure, is air cooled to room temperature, obtains blank after forging；
Step 2, middle forging:
Blank after processing through step 1 is carried out 1 fire time upsetting pull forging at 920-950 DEG C, using melting down in short-term during forging
Insulation forging technology again, forging ratio controls and is air cooled to room temperature after 1.8-2.0, forging；
Step 3, high-temperature water quenching:
The blank processing through step 2 is incubated between 1130-1150 DEG C after 40-50min immediately Water Quenching it is ensured that base
Material completes fully to recrystallize；
Step 4, cryogenic forging:
Blank after processing through step 3 is carried out 3-5 fire time forging at 730-770 DEG C, often using in short-term during fire time forging
Melt down insulation forging technology again, forging ratio controls and is air cooled to room temperature after 1.7-1.9, forging；
Step 5, finished product forging:
The blank processing through step 4 is forged at 730-770 DEG C, finished product rod fall bowlder with through step 4 process
Blank is compared it is desirable to there be the deflection not less than 30%, prepared zr-2.5nb alloy bar material.
The feature of the present invention also resides in,
In step 1, the specification of ingot casting is ф 340mm, heat insulating coefficient 0.3-0.35.
In step 2, the cold burden heat insulating coefficient melting down insulation forging technology more in short-term is 0.25-0.35, and hot material melts down insulation
Coefficient is 0.13-0.17, melts down holding temperature and is 900-950 DEG C.
In step 4, the cold burden heat insulating coefficient melting down insulation forging technology more in short-term is 0.43-0.47, and hot material melts down insulation
Coefficient is 0.18-0.22, melts down holding temperature 730-770 DEG C.
In step 5, prepared zr-2.5nb alloy bar material specification is ф 70～ф 150mm.
The invention has the beneficial effects as follows, a kind of preparation with uniform fine tissue phase zr-2.5nb alloy bar material of the present invention
Method, by using melting down insulation forging technology more in short-term, improving the structural homogenity of blank, and suppress blank high temperature long
Suction hydrogen phenomenon in Shi Baowen；By high-temperature water quenching, blank tissue recrystallization can be made, realize Microstructure evolution, eliminate simultaneously
Generous crystal boundary；Forged by multiple upsetting pull, blank microstructure homogenization can be made, thus preparing the tiny zirconium alloy bar of even tissue
Material, suitable large-scale industrial production.
Brief description
Fig. 1 is the microscopic structure sample position figure of zr-2.5nb alloy bar material of the present invention；
Fig. 2 is the macrostructure figure in the embodiment of the present invention 1；
Fig. 3 is the macrostructure figure in the embodiment of the present invention 2；
Fig. 4 is the micro-organization chart in the embodiment of the present invention 1, and wherein, figure a samples from edge；Figure b samples from 1/4 diameter
Place；Figure c is sampling from center portion；
Fig. 5 is the micro-organization chart in the embodiment of the present invention 2, and wherein, figure a samples from edge；Figure b samples from 1/4 diameter
Place；Figure c is sampling from center portion；
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.
A kind of preparation method with uniform fine tissue phase zr-2.5nb alloy bar material of the present invention, specifically includes following step
Rapid:
Step 1, cogging:
Using the zr-2.5nb alloy cast ingot of ф 340mm, 930-960 DEG C of cogging temperature, come out of the stove after heating 100-150min,
Ingot casting is carried out with three upsettings three pull out, heat insulating coefficient 0.3-0.35 forging ratio controls in 1.9-2.1, fully crush thick as-cast structure, forging
After be air cooled to room temperature, obtain blank；
Step 2, middle forging:
Blank after processing through step 1 is carried out 1 fire time upsetting pull forging at 920-950 DEG C, using melting down in short-term during forging
Insulation forging technology again, cold burden heat insulating coefficient is 0.25-0.35, and it is 0.13-0.17 that hot material melts down heat insulating coefficient, melts down insulation temperature
Spend for 900-950 DEG C, forging ratio controls and is air cooled to room temperature after 1.8-2.0, forging；
Step 3, high-temperature water quenching:
The blank processing through step 2 is incubated between 1130-1150 DEG C after 40-50min immediately Water Quenching it is ensured that base
Material completes fully to recrystallize；
Step 4, cryogenic forging:
Blank after processing through step 3 is carried out 3-5 fire time forging at 730-770 DEG C, often using in short-term during fire time forging
Melt down insulation forging technology again, cold burden heat insulating coefficient is 0.43-0.47, and it is 0.18-0.22 that hot material melts down heat insulating coefficient, melts down guarantor
Temperature 730-770 DEG C, forging ratio controls and is air cooled to room temperature after 1.7-1.9, forging；
Step 5, finished product forging:
The blank processing through step 4 is forged at 730-770 DEG C, finished product rod fall bowlder with through step 4 process
Blank is compared it is desirable to there be the deflection not less than 30%, and prepared specification is the zr-2.5nb alloy bar material of ф 70～ф 150mm.
As shown in Figure 1, the microscopic structure sample position of zr-2.5nb alloy bar material of the present invention respectively be located at bar edge,
At 1/4 diameter and center portion.
From Fig. 2 and Fig. 3, the macrostructure of bar with half fuzzy brilliant as principal character, illustrate bar transformation temperature with
On obtained sufficient deformation.
From Fig. 4 and Fig. 5, microscopic structure is substantially uniformly tiny two-phase structure, from the edge of bar to center portion
Different parts microscopic structure uniformly, illustrates that bar forging deformation is uniformly abundant, finally gives uniformity and preferably organize.
Embodiment 1
Using the zr-2.5nb alloy cast ingot of ф 340mm, 930 DEG C of cogging temperature, come out of the stove after heating 100min, ingot casting is entered
Row three upsetting three is pulled out, heat insulating coefficient 0.3, and forging ratio controls 1.9, fully crushes thick as-cast structure, is air cooled to room temperature, obtains after forging
Blank；Blank after processing is carried out 1 fire time upsetting pull forging at 920 DEG C, using melting down insulation forging technology more in short-term during forging,
Cold burden heat insulating coefficient is 0.25, and it is 0.13 that hot material melts down heat insulating coefficient, melts down holding temperature and is 900 DEG C, forging ratio controls 1.8,
It is air cooled to room temperature after forging；The blank of process is incubated between 1130 DEG C after 40min immediately Water Quenching it is ensured that blank completes to fill
Divide recrystallization；By process after blank 730 DEG C carry out 3 fire time forging, often fire time forging when using melt down in short-term insulation forge again
Make technique, cold burden heat insulating coefficient is 0.43, and it is 0.18 that hot material melts down heat insulating coefficient, melts down 730 DEG C of holding temperature, forging ratio controls
1.7, it is air cooled to room temperature after forging；The blank of process is forged at 730 DEG C, finished product rod is falling bowlder and last process
Blank is compared it is desirable to there be 30% deflection, and prepared specification is the zr-2.5nb alloy bar material of ф 70mm.
Embodiment 2
Using the zr-2.5nb alloy cast ingot of ф 340mm, 940 DEG C of cogging temperature, come out of the stove after heating 110min, ingot casting is entered
Row three upsetting three is pulled out, heat insulating coefficient 0.31, and forging ratio controls 1.9, fully crushes thick as-cast structure, is air cooled to room temperature, obtains after forging
To blank；Blank after processing is carried out 1 fire time upsetting pull forging at 930 DEG C, during forging, forges work again using melting down insulation in short-term
Skill, cold burden heat insulating coefficient is 0.28, and it is 0.14 that hot material melts down heat insulating coefficient, melts down holding temperature and is 910 DEG C, forging ratio controls
1.8, it is air cooled to room temperature after forging；By the blank processing be incubated between 1130 DEG C after 40min immediately Water Quenching it is ensured that blank is complete
Become and fully recrystallize；Blank after processing is carried out 3 fire time forgings at 740 DEG C, often using melting down insulation in short-term during fire time forging
Forging technology again, cold burden heat insulating coefficient is 0.44, and it is 0.18 that hot material melts down heat insulating coefficient, melts down 740 DEG C of holding temperature, forging ratio control
System 1.7, is air cooled to room temperature after forging；The blank of process is forged at 740 DEG C, finished product rod is falling bowlder and last place
The blank of reason is compared it is desirable to there be 32% deflection, and prepared specification is the zr-2.5nb alloy bar material of ф 70mm.
Embodiment 3
Using the zr-2.5nb alloy cast ingot of ф 340mm, 950 DEG C of cogging temperature, come out of the stove after heating 120min, ingot casting is entered
Row three upsetting three is pulled out, and heat insulating coefficient 0.32 forging ratio controls 2.0, fully crushes thick as-cast structure, is air cooled to room temperature, obtains after forging
Blank；Blank after processing is carried out 1 fire time upsetting pull forging at 940 DEG C, using melting down insulation forging technology more in short-term during forging,
Cold burden heat insulating coefficient is 0.30, and it is 0.15 that hot material melts down heat insulating coefficient, melts down holding temperature and is 920 DEG C, forging ratio controls 1.9,
It is air cooled to room temperature after forging；The blank of process is incubated between 1140 DEG C after 45min immediately Water Quenching it is ensured that blank completes to fill
Divide recrystallization；By process after blank 750 DEG C carry out 4 fire time forging, often fire time forging when using melt down in short-term insulation forge again
Make technique, cold burden heat insulating coefficient is 0.45, and it is 0.19 that hot material melts down heat insulating coefficient, melts down 750 DEG C of holding temperature, forging ratio controls
1.8, it is air cooled to room temperature after forging；The blank of process is forged at 750 DEG C, finished product rod is falling bowlder and last process
Blank is compared it is desirable to there be 35% deflection, and prepared specification is the zr-2.5nb alloy bar material of ф 90mm.
Embodiment 4
Using the zr-2.5nb alloy cast ingot of ф 340mm, 950 DEG C of cogging temperature, come out of the stove after heating 130min, ingot casting is entered
Row three upsetting three is pulled out, heat insulating coefficient 0.33, and forging ratio controls 2.0, fully crushes thick as-cast structure, is air cooled to room temperature, obtains after forging
To blank；Blank after processing is carried out 1 fire time upsetting pull forging at 940 DEG C, during forging, forges work again using melting down insulation in short-term
Skill, cold burden heat insulating coefficient is 0.30, and it is 0.15 that hot material melts down heat insulating coefficient, melts down holding temperature and is 930 DEG C, forging ratio controls
1.9, it is air cooled to room temperature after forging；By the blank processing be incubated between 1140 DEG C after 45min immediately Water Quenching it is ensured that blank is complete
Become and fully recrystallize；Blank after processing is carried out 4 fire time forgings at 750 DEG C, often using melting down insulation in short-term during fire time forging
Forging technology again, cold burden heat insulating coefficient is 0.45, and it is 0.20 that hot material melts down heat insulating coefficient, melts down 750 DEG C of holding temperature, forging ratio control
System 1.8, is air cooled to room temperature after forging；The blank of process is forged at 750 DEG C, finished product rod is falling bowlder and last place
The blank of reason is compared it is desirable to there be 37% deflection, and prepared specification is the zr-2.5nb alloy bar material of ф 110mm.
Embodiment 5
Using the zr-2.5nb alloy cast ingot of ф 340mm, 960 DEG C of cogging temperature, come out of the stove after heating 140min, ingot casting is entered
Row three upsetting three is pulled out, heat insulating coefficient 0.34, and forging ratio controls 2.1, fully crushes thick as-cast structure, is air cooled to room temperature, obtains after forging
To blank；Blank after processing is carried out 1 fire time upsetting pull forging at 950 DEG C, during forging, forges work again using melting down insulation in short-term
Skill, cold burden heat insulating coefficient is 0.33, and it is 0.16 that hot material melts down heat insulating coefficient, melts down holding temperature and is 950 DEG C, forging ratio controls
2.0, it is air cooled to room temperature after forging；By the blank processing be incubated between 1140 DEG C after 50min immediately Water Quenching it is ensured that blank is complete
Become and fully recrystallize；Blank after processing is carried out 5 fire time forgings at 760 DEG C, often using melting down insulation in short-term during fire time forging
Forging technology again, cold burden heat insulating coefficient is 0.46, and it is 0.21 that hot material melts down heat insulating coefficient, melts down 760 DEG C of holding temperature, forging ratio control
System 1.9, is air cooled to room temperature after forging；The blank of process is forged at 760 DEG C, finished product rod is falling bowlder and last place
The blank of reason is compared it is desirable to there be 40% deflection, and prepared specification is the zr-2.5nb alloy bar material of ф 130mm.
Embodiment 6
Using the zr-2.5nb alloy cast ingot of ф 340mm, 960 DEG C of cogging temperature, come out of the stove after heating 150min, ingot casting is entered
Row three upsetting three is pulled out, heat insulating coefficient 0.35, and forging ratio controls 2.1, fully crushes thick as-cast structure, is air cooled to room temperature, obtains after forging
To blank；Blank after processing is carried out 1 fire time upsetting pull forging at 950 DEG C, during forging, forges work again using melting down insulation in short-term
Skill, cold burden heat insulating coefficient is 0.35, and it is 0.17 that hot material melts down heat insulating coefficient, melts down holding temperature and is 950 DEG C, forging ratio controls
2.0, it is air cooled to room temperature after forging；By the blank processing be incubated between 1150 DEG C after 50min immediately Water Quenching it is ensured that blank is complete
Become and fully recrystallize；Blank after processing is carried out 5 fire time forgings at 770 DEG C, often using melting down insulation in short-term during fire time forging
Forging technology again, cold burden heat insulating coefficient is 0.47, and it is 0.22 that hot material melts down heat insulating coefficient, melts down 770 DEG C of holding temperature, forging ratio control
System 1.9, is air cooled to room temperature after forging；The blank of process is forged at 770 DEG C, finished product rod is falling bowlder and last place
The blank of reason is compared it is desirable to there be 40% deflection, and prepared specification is the zr-2.5nb alloy bar material of ф 150mm.
Claims (2)
1. a kind of preparation method with uniform fine tissue phase zr-2.5nb alloy bar material it is characterised in that specifically include with
Lower step:
Step 1, cogging:
Using the zr-2.5nb alloy cast ingot for ф 340mm for the specification, 930-960 DEG C of cogging temperature, go out after heating 100-150min
Stove, carries out three upsettings three and pulls out to ingot casting, heat insulating coefficient 0.3-0.35, and forging ratio controls in 1.9-2.1, fully crushes thick as cast condition group
Knit, after forging, be air cooled to room temperature, obtain blank；
Step 2, middle forging:
Blank after processing through step 1 is carried out 1 fire time upsetting pull forging at 920-950 DEG C, using melting down insulation in short-term during forging
Forging technology again, cold burden heat insulating coefficient is 0.25-0.35, and it is 0.13-0.17 that hot material melts down heat insulating coefficient, and melting down holding temperature is
900-950 DEG C, forging ratio controls and is air cooled to room temperature after 1.8-2.0, forging；
Step 3, high-temperature water quenching:
The blank processing through step 2 is incubated between 1130-1150 DEG C after 40-50min immediately Water Quenching it is ensured that blank is complete
Become and fully recrystallize；
Step 4, cryogenic forging:
Blank after processing through step 3 is carried out 3-5 fire time forging at 730-770 DEG C, often using melting down in short-term during fire time forging
Insulation forging technology again, cold burden heat insulating coefficient is 0.43-0.47, and it is 0.18-0.22 that hot material melts down heat insulating coefficient, melts down insulation temperature
730-770 DEG C of degree, forging ratio controls and is air cooled to room temperature after 1.7-1.9, forging；
Step 5, finished product forging:
The blank processing through step 4 is forged at 730-770 DEG C, finished product rod is falling bowlder and the blank processing through step 4
Compare it is desirable to there be the deflection not less than 30%, prepared zr-2.5nb alloy bar material.
2. a kind of preparation method with uniform fine tissue phase zr-2.5nb alloy bar material according to claim 1, its
It is characterised by, in described step 5, prepared zr-2.5nb alloy bar material specification is ф 70～ф 150mm.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113462998B (en) * | 2020-03-30 | 2023-05-02 | 国核宝钛锆业股份公司 | Preparation method of Zr-Nb alloy bar |
| CN112662973B (en) * | 2020-12-14 | 2021-11-16 | 西部新锆核材料科技有限公司 | Method for manufacturing zirconium alloy pressure pipe of fuel channel of nuclear reactor |
| CN112775202B (en) * | 2020-12-23 | 2023-07-21 | 西部新锆核材料科技有限公司 | Preparation method of zirconium or zirconium alloy rolled section bar |
| CN112775203B (en) * | 2020-12-23 | 2024-01-19 | 西部新锆核材料科技有限公司 | Preparation method of zirconium or zirconium alloy extrusion profile |
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| US5620536A (en) * | 1992-12-18 | 1997-04-15 | Abb Atom Ab | Manufacture of zirconium cladding tube with internal liner |
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| EP1813691A1 (en) * | 2006-01-27 | 2007-08-01 | Rolls-Royce plc | A method of heat treating titanium aluminide |
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