CN105039886A - 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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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, be specifically related to a kind of preparation method with even fine tissue phase Zr-2.5Nb alloy bar material.
Background technology
Zirconium and alloy thereof are widely used in manufacturing the structured material of nuclear reactor owing to having excellent nuclearity energy, comprehensive mechanical property, good machine-shaping property, welding property and high temperature resistance high pressure water and steam corrosion performance.Meanwhile, zirconium alloy and tissue have stronger consistency, and are widely used in the preparation of body implant.At present, the production technique of zirconium and alloy thereof is mainly and is prepared tubing by extruding, prepared sheet material by rolling.And prepare excellent base by open die forging and relate to seldom, because open die forging is relative to extruding and rolling technology, distortion interalloy compression chord direction is less, in addition zirconium and alloy deformation plasticity fine, in distortion, metal easily flows, and causes distortion uneven phenomenon to occur.
Summary of the invention
The object of this invention is to provide a kind of preparation method with even fine tissue phase Zr-2.5Nb alloy bar material, solve the problem of easy uneven phenomenon when existing forging method prepares zirconium and alloy thereof.
The technical solution adopted in the present invention is: a kind of preparation method with even fine tissue phase Zr-2.5Nb alloy bar material, specifically comprises the following steps:
Step 1, cogging:
Adopt Zr-2.5Nb alloy cast ingot, cogging temperature 930-960 DEG C, come out of the stove after heating 100-150min, carry out three upsettings three to ingot casting and pull out, forging ratio controls at 1.9-2.1, abundant broken thick as-cast structure, and after forging, air cooling is to room temperature, obtains blank;
Step 2, middle forging:
Blank after processing through step 1 is carried out time upsetting pull forging of 1 fire at 920-950 DEG C, and during forging, employing is melted down in short-term and is incubated forging process again, and forging ratio controls at 1.8-2.0, and after forging, air cooling is to room temperature;
Step 3, high-temperature water quenching:
Water Quenching immediately after the blank processed through step 2 is incubated 40-50min between 1130-1150 DEG C, ensures that blank completes abundant recrystallize;
Step 4, cryogenic forging:
Blank after processing through step 3 is carried out time forging of 3-5 fire at 730-770 DEG C, adopts to melt down in short-term be incubated forging process again during time forging of every fire, forging ratio controls at 1.7-1.9, and after forging, air cooling is to room temperature;
Step 5, finished product forge:
Forged at 730-770 DEG C by the blank processed through step 4, finished product rod, falling bowlder compared with the blank processed through step 4, requires the deflection being not less than 30%, obtained Zr-2.5Nb alloy bar material.
Feature of the present invention is also,
In step 1, the specification of ingot casting is Ф 340mm, heat insulating coefficient 0.3-0.35.
In step 2, melting down the cold burden heat insulating coefficient being incubated again forging process is in short-term 0.25-0.35, and it is 0.13-0.17 that heat material melts down heat insulating coefficient, and melting down holding temperature is 900-950 DEG C.
In step 4, melting down the cold burden heat insulating coefficient being incubated again forging process is in short-term 0.43-0.47, and it is 0.18-0.22 that heat material melts down heat insulating coefficient, melts down holding temperature 730-770 DEG C.
In step 5, obtained Zr-2.5Nb alloy bar material specification is Ф 70 ~ Ф 150mm.
The invention has the beneficial effects as follows, a kind of preparation method with even fine tissue phase Zr-2.5Nb alloy bar material of the present invention, being incubated forging process again by adopting to melt down in short-term, the homogeneity of structure of blank can be improved, and suction hydrogen phenomenon when suppressing blank high temperature long in insulation; By high-temperature water quenching, blank can be made to organize recrystallize, realize Microstructure evolution, eliminate generous crystal boundary simultaneously; By repeatedly upsetting pull forging, blank microstructure homogenization can be made, thus prepare the tiny Zirconium alloy bar of homogeneous microstructure, be applicable to large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the microstructure 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 sampling is from edge; Figure b sampling is from 1/4 diameter place; Figure c is for sampling is from heart portion;
Fig. 5 is the micro-organization chart in the embodiment of the present invention 2, and wherein, figure a sampling is from edge; Figure b sampling is from 1/4 diameter place; Figure c is for sampling is from heart portion;
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
A kind of preparation method with even fine tissue phase Zr-2.5Nb alloy bar material of the present invention, specifically comprises the following steps:
Step 1, cogging:
Adopt the Zr-2.5Nb alloy cast ingot of Ф 340mm, cogging temperature 930-960 DEG C, come out of the stove after heating 100-150min, carry out three upsettings three to ingot casting to pull out, heat insulating coefficient 0.3-0.35 forging ratio controls at 1.9-2.1, abundant broken thick as-cast structure, after forging, air cooling is to room temperature, obtains blank;
Step 2, middle forging:
Blank after processing through step 1 is carried out time upsetting pull forging of 1 fire at 920-950 DEG C, adopt to melt down in short-term during forging and be incubated forging process again, cold burden heat insulating coefficient is 0.25-0.35, it is 0.13-0.17 that heat material melts down heat insulating coefficient, melting down holding temperature is 900-950 DEG C, forging ratio controls at 1.8-2.0, and after forging, air cooling is to room temperature;
Step 3, high-temperature water quenching:
Water Quenching immediately after the blank processed through step 2 is incubated 40-50min between 1130-1150 DEG C, ensures that blank completes abundant recrystallize;
Step 4, cryogenic forging:
Blank after processing through step 3 is carried out time forging of 3-5 fire at 730-770 DEG C, every fire adopts to melt down in short-term when forging and is incubated forging process again, cold burden heat insulating coefficient is 0.43-0.47, it is 0.18-0.22 that heat material melts down heat insulating coefficient, melt down holding temperature 730-770 DEG C, forging ratio controls at 1.7-1.9, and after forging, air cooling is to room temperature;
Step 5, finished product forge:
Forged at 730-770 DEG C by the blank processed through step 4, finished product rod is falling bowlder compared with the blank processed through step 4, and require the deflection being not less than 30%, obtained specification is the Zr-2.5Nb alloy bar material of Ф 70 ~ Ф 150mm.
As shown in Figure 1, the microstructure sample position of Zr-2.5Nb alloy bar material of the present invention lays respectively at the edge of bar, 1/4 diameter place and heart portion.
From Fig. 2 and Fig. 3, the macrostructure of bar for principal character, illustrates that bar obtains sufficient distortion more than transformation temperature with half fuzzy crystalline substance.
From Fig. 4 and Fig. 5, microstructure is evenly tiny two-phase structure substantially, and the different sites microstructure from the edge of bar to heart portion is even, illustrates that bar forging distortion evenly fully, finally obtains homogeneity and organize preferably.
Embodiment 1
Adopt the Zr-2.5Nb alloy cast ingot of Ф 340mm, cogging temperature 930 DEG C, come out of the stove after heating 100min, carry out three upsettings three to ingot casting and pull out, heat insulating coefficient 0.3, forging ratio controls 1.9, abundant broken thick as-cast structure, and after forging, air cooling is to room temperature, obtains blank; Blank after process is carried out time upsetting pull forging of 1 fire at 920 DEG C, and during forging, employing is melted down in short-term and is incubated forging process again, and cold burden heat insulating coefficient is 0.25, it is 0.13 that heat material melts down heat insulating coefficient, melting down holding temperature is 900 DEG C, and forging ratio controls 1.8, and after forging, air cooling is to room temperature; Water Quenching immediately after the blank of process is incubated 40min between 1130 DEG C, ensures that blank completes abundant recrystallize; Blank after process is carried out time forging of 3 fire at 730 DEG C, adopts to melt down in short-term be incubated forging process again during time forging of every fire, cold burden heat insulating coefficient is 0.43, it is 0.18 that heat material melts down heat insulating coefficient, melt down holding temperature 730 DEG C, forging ratio controls 1.7, and after forging, air cooling is to room temperature; Forged at 730 DEG C by the blank of process, finished product rod is falling bowlder compared with the blank processed for the last time, and require the deflection of 30%, obtained specification is the Zr-2.5Nb alloy bar material of Ф 70mm.
Embodiment 2
Adopt the Zr-2.5Nb alloy cast ingot of Ф 340mm, cogging temperature 940 DEG C, come out of the stove after heating 110min, carry out three upsettings three to ingot casting and pull out, heat insulating coefficient 0.31, forging ratio controls 1.9, abundant broken thick as-cast structure, and after forging, air cooling is to room temperature, obtains blank; Blank after process is carried out time upsetting pull forging of 1 fire at 930 DEG C, and during forging, employing is melted down in short-term and is incubated forging process again, and cold burden heat insulating coefficient is 0.28, it is 0.14 that heat material melts down heat insulating coefficient, melting down holding temperature is 910 DEG C, and forging ratio controls 1.8, and after forging, air cooling is to room temperature; Water Quenching immediately after the blank of process is incubated 40min between 1130 DEG C, ensures that blank completes abundant recrystallize; Blank after process is carried out time forging of 3 fire at 740 DEG C, adopts to melt down in short-term be incubated forging process again during time forging of every fire, cold burden heat insulating coefficient is 0.44, it is 0.18 that heat material melts down heat insulating coefficient, melt down holding temperature 740 DEG C, forging ratio controls 1.7, and after forging, air cooling is to room temperature; Forged at 740 DEG C by the blank of process, finished product rod is falling bowlder compared with the blank processed for the last time, and require the deflection of 32%, obtained specification is the Zr-2.5Nb alloy bar material of Ф 70mm.
Embodiment 3
Adopt the Zr-2.5Nb alloy cast ingot of Ф 340mm, cogging temperature 950 DEG C, come out of the stove after heating 120min, carry out three upsettings three to ingot casting and pull out, heat insulating coefficient 0.32 forging ratio controls 2.0, abundant broken thick as-cast structure, and after forging, air cooling is to room temperature, obtains blank; Blank after process is carried out time upsetting pull forging of 1 fire at 940 DEG C, and during forging, employing is melted down in short-term and is incubated forging process again, and cold burden heat insulating coefficient is 0.30, it is 0.15 that heat material melts down heat insulating coefficient, melting down holding temperature is 920 DEG C, and forging ratio controls 1.9, and after forging, air cooling is to room temperature; Water Quenching immediately after the blank of process is incubated 45min between 1140 DEG C, ensures that blank completes abundant recrystallize; Blank after process is carried out time forging of 4 fire at 750 DEG C, adopts to melt down in short-term be incubated forging process again during time forging of every fire, cold burden heat insulating coefficient is 0.45, it is 0.19 that heat material melts down heat insulating coefficient, melt down holding temperature 750 DEG C, forging ratio controls 1.8, and after forging, air cooling is to room temperature; Forged at 750 DEG C by the blank of process, finished product rod is falling bowlder compared with the blank processed for the last time, and require the deflection of 35%, obtained specification is the Zr-2.5Nb alloy bar material of Ф 90mm.
Embodiment 4
Adopt the Zr-2.5Nb alloy cast ingot of Ф 340mm, cogging temperature 950 DEG C, come out of the stove after heating 130min, carry out three upsettings three to ingot casting and pull out, heat insulating coefficient 0.33, forging ratio controls 2.0, abundant broken thick as-cast structure, and after forging, air cooling is to room temperature, obtains blank; Blank after process is carried out time upsetting pull forging of 1 fire at 940 DEG C, and during forging, employing is melted down in short-term and is incubated forging process again, and cold burden heat insulating coefficient is 0.30, it is 0.15 that heat material melts down heat insulating coefficient, melting down holding temperature is 930 DEG C, and forging ratio controls 1.9, and after forging, air cooling is to room temperature; Water Quenching immediately after the blank of process is incubated 45min between 1140 DEG C, ensures that blank completes abundant recrystallize; Blank after process is carried out time forging of 4 fire at 750 DEG C, adopts to melt down in short-term be incubated forging process again during time forging of every fire, cold burden heat insulating coefficient is 0.45, it is 0.20 that heat material melts down heat insulating coefficient, melt down holding temperature 750 DEG C, forging ratio controls 1.8, and after forging, air cooling is to room temperature; Forged at 750 DEG C by the blank of process, finished product rod is falling bowlder compared with the blank processed for the last time, and require the deflection of 37%, obtained specification is the Zr-2.5Nb alloy bar material of Ф 110mm.
Embodiment 5
Adopt the Zr-2.5Nb alloy cast ingot of Ф 340mm, cogging temperature 960 DEG C, come out of the stove after heating 140min, carry out three upsettings three to ingot casting and pull out, heat insulating coefficient 0.34, forging ratio controls 2.1, abundant broken thick as-cast structure, and after forging, air cooling is to room temperature, obtains blank; Blank after process is carried out time upsetting pull forging of 1 fire at 950 DEG C, and during forging, employing is melted down in short-term and is incubated forging process again, and cold burden heat insulating coefficient is 0.33, it is 0.16 that heat material melts down heat insulating coefficient, melting down holding temperature is 950 DEG C, and forging ratio controls 2.0, and after forging, air cooling is to room temperature; Water Quenching immediately after the blank of process is incubated 50min between 1140 DEG C, ensures that blank completes abundant recrystallize; Blank after process is carried out time forging of 5 fire at 760 DEG C, adopts to melt down in short-term be incubated forging process again during time forging of every fire, cold burden heat insulating coefficient is 0.46, it is 0.21 that heat material melts down heat insulating coefficient, melt down holding temperature 760 DEG C, forging ratio controls 1.9, and after forging, air cooling is to room temperature; Forged at 760 DEG C by the blank of process, finished product rod is falling bowlder compared with the blank processed for the last time, and require the deflection of 40%, obtained specification is the Zr-2.5Nb alloy bar material of Ф 130mm.
Embodiment 6
Adopt the Zr-2.5Nb alloy cast ingot of Ф 340mm, cogging temperature 960 DEG C, come out of the stove after heating 150min, carry out three upsettings three to ingot casting and pull out, heat insulating coefficient 0.35, forging ratio controls 2.1, abundant broken thick as-cast structure, and after forging, air cooling is to room temperature, obtains blank; Blank after process is carried out time upsetting pull forging of 1 fire at 950 DEG C, and during forging, employing is melted down in short-term and is incubated forging process again, and cold burden heat insulating coefficient is 0.35, it is 0.17 that heat material melts down heat insulating coefficient, melting down holding temperature is 950 DEG C, and forging ratio controls 2.0, and after forging, air cooling is to room temperature; Water Quenching immediately after the blank of process is incubated 50min between 1150 DEG C, ensures that blank completes abundant recrystallize; Blank after process is carried out time forging of 5 fire at 770 DEG C, adopts to melt down in short-term be incubated forging process again during time forging of every fire, cold burden heat insulating coefficient is 0.47, it is 0.22 that heat material melts down heat insulating coefficient, melt down holding temperature 770 DEG C, forging ratio controls 1.9, and after forging, air cooling is to room temperature; Forged at 770 DEG C by the blank of process, finished product rod is falling bowlder compared with the blank processed for the last time, and require the deflection of 40%, obtained specification is the Zr-2.5Nb alloy bar material of Ф 150mm.
Claims (5)
1. there is a preparation method for even fine tissue phase Zr-2.5Nb alloy bar material, it is characterized in that, specifically comprise the following steps:
Step 1, cogging:
Adopt Zr-2.5Nb alloy cast ingot, cogging temperature 930-960 DEG C, come out of the stove after heating 100-150min, carry out three upsettings three to ingot casting and pull out, forging ratio controls at 1.9-2.1, abundant broken thick as-cast structure, and after forging, air cooling is to room temperature, obtains blank;
Step 2, middle forging:
Blank after processing through step 1 is carried out time upsetting pull forging of 1 fire at 920-950 DEG C, and during forging, employing is melted down in short-term and is incubated forging process again, and forging ratio controls at 1.8-2.0, and after forging, air cooling is to room temperature;
Step 3, high-temperature water quenching:
Water Quenching immediately after the blank processed through step 2 is incubated 40-50min between 1130-1150 DEG C, ensures that blank completes abundant recrystallize;
Step 4, cryogenic forging:
Blank after processing through step 3 is carried out time forging of 3-5 fire at 730-770 DEG C, adopts to melt down in short-term be incubated forging process again during time forging of every fire, forging ratio controls at 1.7-1.9, and after forging, air cooling is to room temperature;
Step 5, finished product forge:
Forged at 730-770 DEG C by the blank processed through step 4, finished product rod, falling bowlder compared with the blank processed through step 4, requires the deflection being not less than 30%, obtained Zr-2.5Nb alloy bar material.
2. a kind of preparation method with even fine tissue phase Zr-2.5Nb alloy bar material according to claim 1, is characterized in that, in described step 1, the specification of ingot casting is Ф 340mm, heat insulating coefficient 0.3-0.35.
3. a kind of preparation method with even fine tissue phase Zr-2.5Nb alloy bar material according to claim 1, it is characterized in that, in true step 2, melting down the cold burden heat insulating coefficient being incubated again forging process is in short-term 0.25-0.35, it is 0.13-0.17 that heat material melts down heat insulating coefficient, and melting down holding temperature is 900-950 DEG C.
4. a kind of preparation method with even fine tissue phase Zr-2.5Nb alloy bar material according to claim 1, it is characterized in that, in described step 4, melting down the cold burden heat insulating coefficient being incubated again forging process is in short-term 0.43-0.47, it is 0.18-0.22 that heat material melts down heat insulating coefficient, melts down holding temperature 730-770 DEG C.
5. a kind of preparation method with even fine tissue phase Zr-2.5Nb alloy bar material according to claim 1, is characterized in that, in described step 5, obtained Zr-2.5Nb alloy bar material specification is Ф 70 ~ Ф 150mm.
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| CN112662973A (en) * | 2020-12-14 | 2021-04-16 | 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 |
| CN112775202A (en) * | 2020-12-23 | 2021-05-11 | 西部新锆核材料科技有限公司 | Preparation method of zirconium or zirconium alloy rolled section |
| CN112775203A (en) * | 2020-12-23 | 2021-05-11 | 西部新锆核材料科技有限公司 | Preparation method of zirconium or zirconium alloy extruded section |
| CN113462998A (en) * | 2020-03-30 | 2021-10-01 | 国核宝钛锆业股份公司 | Preparation method of Zr-Nb alloy bar |
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| Publication number | Priority date | Publication date | Assignee | Title |
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