CN104492849B - A kind of preparation method of used by nuclear reactor hafnium square rod - Google Patents
A kind of preparation method of used by nuclear reactor hafnium square rod Download PDFInfo
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- CN104492849B CN104492849B CN201410714543.XA CN201410714543A CN104492849B CN 104492849 B CN104492849 B CN 104492849B CN 201410714543 A CN201410714543 A CN 201410714543A CN 104492849 B CN104492849 B CN 104492849B
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Abstract
The invention discloses a kind of preparation method of used by nuclear reactor hafnium square rod, the method is: one, by insulation after the heating of hafnium ingot casting, then carries out first time extruding, is once extruded hafnium pole base; Two, first stage annealing process; Three, be incubated after once extruding the heating of hafnium pole base, then carry out second time extruding, obtain secondary extrusion hafnium pole base; Four, secondary stage annealing process; Five, groove rolling is carried out to secondary extrusion hafnium pole base, obtain semi-finished product hafnium square billet; Six, phase III annealing in process; Seven, stretcher leveling is carried out to semi-finished product hafnium square billet, obtain used by nuclear reactor hafnium square rod.The present invention adopts repeatedly extrusion blooming technique to replace traditional hammer cogging technique, deflection is large, and core die break is abundant, and inside and outside distortion uniformity is good, thus greatly can improve finished product corrosive nature and 320 DEG C of high temperature percentage elongation indexs, and performance uniformity can be improved.
Description
Technical field
The invention belongs to hafnium material processing preparing technical field, be specifically related to a kind of preparation method of used by nuclear reactor hafnium square rod.
Background technology
Metal hafnium has very excellent nuclearity energy, and its thermal-neutron capture cross-section can reach in 100 Palestine and Israels, far away higher than other materials.Meanwhile, the machining property of hafnium and corrosion resistance also very outstanding.Rely on above outstanding characteristic, metal hafnium is one of most important material in atomic energy industry, has irreplaceability, and it is often used as the structure of nuclear reactor, coated and control volume parts.
Along with the development of atomic energy industry, designing and employing side is to the properties of used by nuclear reactor hafnium processing material, especially mechanical behavior under high temperature percentage elongation, corrosive nature desired value and uniformity propose very high request, to ensure that hafnium material can stablely under nuclear reactor high temperature, high pressure, nuclear radiation operating mode be for a long time on active service.
The classical production process of used by nuclear reactor hafnium square rod is mainly forges and is equipped with the process route of vacuum annealing, and classical production process shortcoming is as follows: the first, forging mode comparatively fashion of extrusion, be out of shape poor, single pass working modulus is little, and areal deformation is serious, easily occurs micro-crack defect.Meanwhile, during forging, the distortion of blank core is insufficient, causes finished product mechanical behavior under high temperature percentage elongation, corrosive nature numerical value low, lack of homogeneity; The second, the square rod size inaccuracy that forging mode is produced, does not reach high accuracy dimensional requirement.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of preparation method of used by nuclear reactor hafnium square rod.The method adopts repeatedly extrusion blooming technique to replace traditional hammer cogging technique, extrusion process is large compared with Forging Technology single pass heavy deformation, core die break is abundant, inside and outside distortion uniformity is good, thus greatly can improve finished product corrosive nature and 320 DEG C of high temperature percentage elongation indexs, and performance uniformity can be improved.Compared with hafnium square rod prepared by the used by nuclear reactor hafnium square rod adopting the method to prepare and Conventional processing methods, percentage elongation and corrosive nature index all improve more than 15%, and performance uniformity is good, and product meets designing and employing requirement.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of used by nuclear reactor hafnium square rod, and it is characterized in that, the method comprises the following steps:
Step one, be that to be heated to temperature be incubated 1h ~ 2h after 900 DEG C ~ 1150 DEG C for the hafnium ingot casting of 125mm ~ 145mm by diameter, then carried out to the hafnium ingot casting after insulation first time and extrude, once extruded hafnium pole base; The extrusion ratio of described first time extruding is 3 ~ 4;
Step 2, be placed in vacuum annealing furnace carry out first stage annealing process by once extruding hafnium pole base described in step one;
Step 3, the once extruding hafnium pole base in step 2 after first stage annealing process is heated to be incubated 1h ~ 2h after temperature is 1000 DEG C ~ 1200 DEG C, then second time extruding is carried out to the once extruding hafnium pole base after insulation, obtain secondary extrusion hafnium pole base; The extrusion ratio of described second time extruding is 8 ~ 11;
Step 4, the hafnium of secondary extrusion described in step 3 pole base is placed in vacuum annealing furnace carries out secondary stage annealing process;
Step 5, employing pass milling train carry out groove rolling to the secondary extrusion hafnium pole base in step 4 after secondary stage annealing process, and obtain the semi-finished product hafnium square billet that the length of side is 16mm ~ 20mm, the general working rate of described groove rolling is 20% ~ 50%;
Step 6, the hafnium of semi-finished product described in step 5 square billet is placed in vacuum annealing furnace carries out phase III annealing in process;
Step 7, stretcher leveling is carried out to the semi-finished product hafnium square billet in step 6 after phase III annealing in process, obtain the used by nuclear reactor hafnium square rod that the length of side is 16mm ~ 20mm.
The preparation method of above-mentioned a kind of used by nuclear reactor hafnium square rod, is characterized in that, after having extruded for the first time, adopts roll leveller in step one, utilizes extruding waste heat once will extrude hafnium pole base aligning to linearity < 3mm/m.
The preparation method of above-mentioned a kind of used by nuclear reactor hafnium square rod, it is characterized in that, the temperature of the process of first stage annealing described in step 2 is 750 DEG C ~ 850 DEG C, and the time of first stage annealing process is 1h ~ 2h, and the vacuum of first stage annealing process is not more than 1 × 10
-2pa.
The preparation method of above-mentioned a kind of used by nuclear reactor hafnium square rod, is characterized in that, after second time has extruded in step 3, adopts roll leveller, utilizes extruding waste heat by secondary extrusion hafnium pole base aligning to linearity < 3mm/m.
The preparation method of above-mentioned a kind of used by nuclear reactor hafnium square rod, it is characterized in that, the temperature of the process of secondary stage annealing described in step 4 is 600 DEG C ~ 650 DEG C, and the time of secondary stage annealing process is 1h ~ 2h, and the vacuum of secondary stage annealing process is not more than 1 × 10
-2pa.
The preparation method of above-mentioned a kind of used by nuclear reactor hafnium square rod, it is characterized in that, the temperature of the annealing in process of phase III described in step 6 is 600 DEG C ~ 700 DEG C, and the time of phase III annealing in process is 1h ~ 2h, and the vacuum of phase III annealing in process is not more than 1 × 10
-2pa.
The present invention compared with prior art has the following advantages:
1, the present invention adopts repeatedly extrusion blooming technique to replace traditional hammer cogging technique, extrusion process is large compared with Forging Technology single pass heavy deformation, core die break is abundant, inside and outside distortion uniformity is good, thus greatly can improve finished product corrosive nature and 320 DEG C of high temperature percentage elongation indexs, and performance uniformity can be improved.
2, the present invention adopts square groove rolling mill practice to replace traditional Forging Technology, is conducive to improving square rod dimensional accuracy and surface quality.
3, the hafnium square rod dimensional discrepancy that prepared by conventional forging process is not less than ± 1mm, and the length of side of the used by nuclear reactor hafnium square rod adopting the inventive method to prepare is 16mm ~ 20mm, and precision is high, and dimensional discrepancy is no more than ± 0.5mm.
Compared with hafnium square rod prepared by the used by nuclear reactor hafnium square rod 4, adopting the inventive method to prepare and Conventional processing methods, percentage elongation and corrosive nature index all improve more than 15%, and performance uniformity is good, and product meets designing and employing requirement.
Below by embodiment, technical solution of the present invention is described in further detail.
Detailed description of the invention
Embodiment 1
Step one, be that to be heated to temperature be 900 DEG C for the hafnium ingot casting of 125mm by diameter, insulation 1h, then the hafnium ingot casting after insulation being loaded recipient diameter is carry out first time extruding in the extruder of 130mm, obtain the once extruding hafnium pole base that diameter is 75mm, the extrusion ratio of described first time extruding is 3, after first time has extruded, adopt roll leveller, utilize extruding waste heat once will extrude hafnium pole base aligning to linearity < 3mm/m;
Step 2, the once extruding hafnium pole base after aligning in step one is placed in vacuum annealing furnace and carries out first stage annealing process; The temperature of described first stage annealing process is 850 DEG C, and the time of first stage annealing process is 1.5h, and the vacuum of first stage annealing process is not more than 1 × 10
-2pa;
Step 3, the once extruding hafnium pole base in step 2 after first stage annealing process is heated to temperature is 1150 DEG C, insulation 1h, then the once extruding hafnium pole base after insulation being loaded recipient diameter is carry out second time extruding in the extruder of 80mm, obtain the secondary extrusion hafnium pole base that diameter is 28mm, the extrusion ratio of described second time extruding is 8.16, after second time has extruded, adopt roll leveller, utilize extruding waste heat by secondary extrusion hafnium pole base aligning to linearity < 3mm/m;
Step 4, the hafnium of secondary extrusion described in step 3 pole base is placed in vacuum annealing furnace carries out secondary stage annealing process; The temperature of described secondary stage annealing process is 650 DEG C, and the secondary stage annealing processing time is 1h, and the vacuum of secondary stage annealing process is not more than 1 × 10
-2pa;
Step 5, employing pass milling train carry out square groove rolling to the secondary extrusion hafnium pole base in step 4 after secondary stage annealing process, obtain the semi-finished product hafnium square billet that the length of side is 18mm; Described groove rolling general working rate is 47.4%;
Step 6, the hafnium of semi-finished product described in step 5 square billet is placed in vacuum annealing furnace carries out phase III annealing in process; The temperature of described phase III annealing in process is 600 DEG C, and annealing in process time phase III is 1.5h, and the vacuum of phase III annealing in process is not more than 1 × 10
-2pa;
Step 7, stretcher leveling is carried out to the semi-finished product hafnium square billet in step 6 after phase III annealing in process, finally obtain the used by nuclear reactor hafnium square rod that the length of side is 18mm.
The performance test data of used by nuclear reactor hafnium square rod prepared by the present embodiment is in table 1.
The used by nuclear reactor hafnium square rod performance test data result of table 1 embodiment of the present invention 1
The used by nuclear reactor length of side prepared by the present embodiment is the hafnium square rod of 18mm, and dimensional discrepancy is ± 0.4mm; The hafnium square rod that used by nuclear reactor hafnium square rod prepared by the present embodiment is prepared compared with Conventional processing methods, mechanical behavior under high temperature percentage elongation raising 21.6%, surrosion reduce by 29.1%, and performance uniformity is better.
Embodiment 2
Step one, be that to be heated to temperature be 900 DEG C for the hafnium ingot casting of 125mm by diameter, insulation 2h, then the hafnium ingot casting after insulation being loaded recipient diameter is carry out first time extruding in the extruder of 130mm, obtain the once extruding hafnium pole base that diameter is 65mm, the extrusion ratio of described first time extruding is 4, after first time has extruded, adopt roll leveller, utilize extruding waste heat once will extrude hafnium pole base aligning to linearity < 3mm/m;
Step 2, the once extruding hafnium pole base after aligning in step one is placed in vacuum annealing furnace and carries out first stage annealing process; The temperature of described first stage annealing process is 800 DEG C, and the time of first stage annealing process is 1h, and the vacuum of first stage annealing process is not more than 1 × 10
-2pa;
Step 3, the once extruding hafnium pole base in step 2 after first stage annealing process is heated to temperature is 1120 DEG C, insulation 1h, then the once extruding hafnium pole base after insulation being loaded recipient diameter is carry out second time extruding in the extruder of 70mm, obtain the secondary extrusion hafnium pole base that diameter is 23mm, the extrusion ratio of described second time extruding is 9.26, after second time has extruded, adopt roll leveller, utilize extruding waste heat by secondary extrusion hafnium pole base aligning to linearity < 3mm/m;
Step 4, the hafnium of secondary extrusion described in step 3 pole base is placed in vacuum annealing furnace carries out secondary stage annealing process; The temperature of described secondary stage annealing process is 620 DEG C, and the secondary stage annealing processing time is 1.5h, and the vacuum of secondary stage annealing process is not more than 1 × 10
-2pa;
Step 5, employing pass milling train carry out square groove rolling to the secondary extrusion hafnium pole base in step 4 after secondary stage annealing process, obtain the semi-finished product hafnium square billet that the length of side is 16mm; Described groove rolling general working rate is 38.4%;
Step 6, the hafnium of semi-finished product described in step 5 square billet is placed in vacuum annealing furnace carries out phase III annealing in process; The temperature of described phase III annealing in process is 630 DEG C, and annealing in process time phase III is 1h, and the vacuum of phase III annealing in process is not more than 1 × 10
-2pa;
Step 7, stretcher leveling is carried out to the semi-finished product hafnium square billet in step 6 after phase III annealing in process, finally obtain the used by nuclear reactor hafnium square rod that the length of side is 16mm.
The performance test data of used by nuclear reactor hafnium square rod prepared by the present embodiment is in table 2.
The used by nuclear reactor hafnium square rod performance test data result of table 2 embodiment of the present invention 2
The used by nuclear reactor length of side prepared by the present embodiment is the hafnium square rod of 16mm, and dimensional discrepancy is ± 0.3mm; The hafnium square rod that used by nuclear reactor hafnium square rod prepared by the present embodiment is prepared compared with Conventional processing methods, mechanical behavior under high temperature percentage elongation raising 17.1%, surrosion reduce by 32.4%, and performance uniformity is better.
Embodiment 3
Step one, be that to be heated to temperature be 1000 DEG C for the hafnium ingot casting of 135mm by diameter, insulation 1h, then the hafnium ingot casting after insulation being loaded recipient diameter is carry out first time extruding in the extruder of 140mm, obtain the once extruding hafnium pole base that diameter is 74mm, the extrusion ratio of described first time extruding is 3.58, after first time has extruded, adopt roll leveller, utilize extruding waste heat once will extrude hafnium pole base aligning to linearity < 3mm/m;
Step 2, the once extruding hafnium pole base after aligning in step one is placed in vacuum annealing furnace and carries out first stage annealing process; The temperature of described first stage annealing process is 800 DEG C, and the time of first stage annealing process is 1h, and the vacuum of first stage annealing process is not more than 1 × 10
-2pa;
Step 3, the once extruding hafnium pole base in step 2 after first stage annealing process is heated to temperature is 1150 DEG C, insulation 1h, then the once extruding hafnium pole base after insulation being loaded recipient diameter is carry out second time extruding in the extruder of 80mm, obtain the secondary extrusion hafnium pole base that diameter is 24mm, the extrusion ratio of described second time extruding is 11, after second time has extruded, adopt roll leveller, utilize extruding waste heat by secondary extrusion hafnium pole base aligning to linearity < 3mm/m;
Step 4, the hafnium of secondary extrusion described in step 3 pole base is placed in vacuum annealing furnace carries out secondary stage annealing process; The temperature of described secondary stage annealing process is 630 DEG C, and the secondary stage annealing processing time is 1.5h, and the vacuum of secondary stage annealing process is not more than 1 × 10
-2pa;
Step 5, employing pass milling train carry out square groove rolling to the secondary extrusion hafnium pole base in step 4 after secondary stage annealing process, obtain the semi-finished product hafnium square billet that the length of side is 19mm; Described groove rolling general working rate is 20%;
Step 6, the hafnium of semi-finished product described in step 5 square billet is placed in vacuum annealing furnace carries out phase III annealing in process; The temperature of described phase III annealing in process is 700 DEG C, and annealing in process time phase III is 1.5h, and the vacuum of phase III annealing in process is not more than 1 × 10
-2pa;
Step 7, stretcher leveling is carried out to the semi-finished product hafnium square billet in step 6 after phase III annealing in process, finally obtain the used by nuclear reactor hafnium square rod that the length of side is 19mm.
The performance test data of used by nuclear reactor hafnium square rod prepared by the present embodiment is in table 3.
The used by nuclear reactor hafnium square rod performance test data result of table 3 embodiment of the present invention 3
The used by nuclear reactor length of side prepared by the present embodiment is the hafnium square rod of 19mm, and dimensional discrepancy is ± 0.5mm; The hafnium square rod that used by nuclear reactor hafnium square rod prepared by the present embodiment is prepared compared with Conventional processing methods, mechanical behavior under high temperature percentage elongation raising 16.2%, surrosion reduce by 28.1%, and performance uniformity is better.
Embodiment 4
Step one, be that to be heated to temperature be 1050 DEG C for the hafnium ingot casting of 135mm by diameter, insulation 1h, then the hafnium ingot casting after insulation being loaded recipient diameter is carry out first time extruding in the extruder of 140mm, obtain the once extruding hafnium pole base that diameter is 70mm, the extrusion ratio of described first time extruding is 4, after first time has extruded, adopt roll leveller, utilize extruding waste heat once will extrude hafnium pole base aligning to linearity < 3mm/m;
Step 2, the once extruding hafnium pole base after aligning in step one is placed in vacuum annealing furnace and carries out first stage annealing process; The temperature of described first stage annealing process is 750 DEG C, and the time of first stage annealing process is 2h, and the vacuum of first stage annealing process is not more than 1 × 10
-2pa;
Step 3, the once extruding hafnium pole base in step 2 after first stage annealing process is heated to temperature is 1000 DEG C, insulation 1h, then the once extruding hafnium pole base after insulation being loaded recipient diameter is carry out second time extruding in the extruder of 75mm, obtain the secondary extrusion hafnium pole base that diameter is 23mm, the extrusion ratio of described second time extruding is about 10.63, after second time has extruded, adopt roll leveller, utilize extruding waste heat by secondary extrusion hafnium pole base aligning to linearity < 3mm/m;
Step 4, the hafnium of secondary extrusion described in step 3 pole base is placed in vacuum annealing furnace carries out secondary stage annealing process; The temperature of described secondary stage annealing process is 600 DEG C, and the secondary stage annealing processing time is 1h, and the vacuum of secondary stage annealing process is not more than 1 × 10
-2pa;
Step 5, employing pass milling train carry out square groove rolling to the secondary extrusion hafnium pole base in step 4 after secondary stage annealing process, obtain the semi-finished product hafnium square billet that the length of side is 17mm; Described groove rolling general working rate is 30.4%;
Step 6, the hafnium of semi-finished product described in step 5 square billet is placed in vacuum annealing furnace carries out phase III annealing in process; The temperature of described phase III annealing in process is 670 DEG C, and annealing in process time phase III is 1h, and the vacuum of phase III annealing in process is not more than 1 × 10
-2pa;
Step 7, stretcher leveling is carried out to the semi-finished product hafnium square billet in step 6 after phase III annealing in process, finally obtain the used by nuclear reactor hafnium square rod that the length of side is 17mm.
The performance test data of used by nuclear reactor hafnium square rod prepared by the present embodiment is in table 4.
The used by nuclear reactor hafnium square rod performance test data result of table 4 embodiment of the present invention 4
The used by nuclear reactor length of side prepared by the present embodiment is the hafnium square rod of 17mm, and dimensional discrepancy is ± 0.3mm; The hafnium square rod that used by nuclear reactor hafnium square rod prepared by the present embodiment is prepared compared with Conventional processing methods, mechanical behavior under high temperature percentage elongation raising 19.4%, surrosion reduce by 27.35%, and performance uniformity is better.
Embodiment 5
Step one, be that to be heated to temperature be 1150 DEG C for the hafnium ingot casting of 145mm by diameter, insulation 1.5h, then the hafnium ingot casting after insulation being loaded recipient diameter is carry out first time extruding in the extruder of 150mm, obtain the once extruding hafnium pole base that diameter is 85mm, the extrusion ratio of described first time extruding is 3.11, after first time has extruded, adopt roll leveller, utilize extruding waste heat once will extrude hafnium pole base aligning to linearity < 3mm/m;
Step 2, the once extruding hafnium pole base after aligning in step one is placed in vacuum annealing furnace and carries out first stage annealing process; The temperature of described first stage annealing process is 780 DEG C, and the time of first stage annealing process is 1.5h, and the vacuum of first stage annealing process is not more than 1 × 10
-2pa;
Step 3, the once extruding hafnium pole base in step 2 after first stage annealing process is heated to temperature is 1150 DEG C, insulation 2h, then the once extruding hafnium pole base after insulation being loaded recipient diameter is carry out second time extruding in the extruder of 90mm, obtain the secondary extrusion hafnium pole base that diameter is 31mm, the extrusion ratio of described second time extruding is 8.43, after second time has extruded, adopt roll leveller, utilize extruding waste heat by secondary extrusion hafnium pole base aligning to linearity < 3mm/m;
Step 4, the hafnium of secondary extrusion described in step 3 pole base is placed in vacuum annealing furnace carries out secondary stage annealing process; The temperature of described secondary stage annealing process is 650 DEG C, and the secondary stage annealing processing time is 2h, and the vacuum of secondary stage annealing process is not more than 1 × 10
-2pa;
Step 5, employing pass milling train carry out square groove rolling to the secondary extrusion hafnium pole base in step 4 after secondary stage annealing process, obtain the semi-finished product hafnium square billet that the length of side is 20mm; Described groove rolling general working rate is 46.98%;
Step 6, the hafnium of semi-finished product described in step 5 square billet is placed in vacuum annealing furnace carries out phase III annealing in process; The temperature of described phase III annealing in process is 630 DEG C, and annealing in process time phase III is 1.5h, and the vacuum of phase III annealing in process is not more than 1 × 10
-2pa;
Step 7, stretcher leveling is carried out to the semi-finished product hafnium square billet in step 6 after phase III annealing in process, finally obtain the used by nuclear reactor hafnium square rod that the length of side is 20mm.
The performance test data of used by nuclear reactor hafnium square rod prepared by the present embodiment is in table 5.
The used by nuclear reactor hafnium square rod performance test data result of table 5 embodiment of the present invention 5
The used by nuclear reactor length of side prepared by the present embodiment is the hafnium square rod of 20mm, and dimensional discrepancy is ± 0.3mm; The hafnium square rod that used by nuclear reactor hafnium square rod prepared by the present embodiment is prepared compared with Conventional processing methods, mechanical behavior under high temperature percentage elongation raising 27.78%, surrosion reduce by 22.37%, and performance uniformity is better.
Embodiment 6
Step one, be that to be heated to temperature be 1150 DEG C for the hafnium ingot casting of 145mm by diameter, insulation 1.5h, then the hafnium ingot casting after insulation being loaded recipient diameter is carry out first time extruding in the extruder of 150mm, obtain the once extruding hafnium pole base that diameter is 75mm, the extrusion ratio of described first time extruding is 4, after first time has extruded, adopt roll leveller, utilize extruding waste heat once will extrude hafnium pole base aligning to linearity < 3mm/m;
Step 2, the once extruding hafnium pole base after aligning in step one is placed in vacuum annealing furnace and carries out first stage annealing process; The temperature of described first stage annealing process is 800 DEG C, and the time of first stage annealing process is 1h, and the vacuum of first stage annealing process is not more than 1 × 10
-2pa;
Step 3, the once extruding hafnium pole base in step 2 after first stage annealing process is heated to temperature is 1200 DEG C, insulation 1.5h, then the once extruding hafnium pole base after insulation being loaded recipient diameter is carry out second time extruding in the extruder of 79mm, obtain the secondary extrusion hafnium pole base that diameter is 28mm, the extrusion ratio of described second time extruding is 8, after second time has extruded, adopt roll leveller, utilize extruding waste heat by secondary extrusion hafnium pole base aligning to linearity < 3mm/m;
Step 4, the hafnium of secondary extrusion described in step 3 pole base is placed in vacuum annealing furnace carries out secondary stage annealing process; The temperature of described secondary stage annealing process is 650 DEG C, and the secondary stage annealing processing time is 1h, and the vacuum of secondary stage annealing process is not more than 1 × 10
-2pa;
Step 5, employing pass milling train carry out square groove rolling to the secondary extrusion hafnium pole base in step 4 after secondary stage annealing process, obtain the semi-finished product hafnium square billet that the length of side is 17.5mm; Described groove rolling general working rate is 50%;
Step 6, the hafnium of semi-finished product described in step 5 square billet is placed in vacuum annealing furnace carries out phase III annealing in process; The temperature of described phase III annealing in process is 600 DEG C, and annealing in process time phase III is 2h, and the vacuum of phase III annealing in process is not more than 1 × 10
-2pa;
Step 7, stretcher leveling is carried out to the semi-finished product hafnium square billet in step 6 after phase III annealing in process, finally obtain the used by nuclear reactor hafnium square rod that the length of side is 17.5mm.
The performance test data of used by nuclear reactor hafnium square rod prepared by the present embodiment is in table 6.
The used by nuclear reactor hafnium square rod performance test data result of table 6 embodiment of the present invention 6
The used by nuclear reactor length of side prepared by the present embodiment is the hafnium square rod of 17.5mm, and dimensional discrepancy is ± 0.4mm; The hafnium square rod that used by nuclear reactor hafnium square rod prepared by the present embodiment is prepared compared with Conventional processing methods, mechanical behavior under high temperature percentage elongation raising 18.92%, surrosion reduce by 28%, and performance uniformity is better.
The above; it is only preferred embodiment of the present invention; not any restriction is done to the present invention, every above embodiment is done according to invention technical spirit any simple modification, change and equivalent structure change, all still belong in the protection domain of technical solution of the present invention.
Claims (6)
1. a preparation method for used by nuclear reactor hafnium square rod, is characterized in that, the method comprises the following steps:
Step one, be that to be heated to temperature be incubated 1h ~ 2h after 900 DEG C ~ 1150 DEG C for the hafnium ingot casting of 125mm ~ 145mm by diameter, then carried out to the hafnium ingot casting after insulation first time and extrude, once extruded hafnium pole base; The extrusion ratio of described first time extruding is 3 ~ 4;
Step 2, be placed in vacuum annealing furnace carry out first stage annealing process by once extruding hafnium pole base described in step one;
Step 3, the once extruding hafnium pole base in step 2 after first stage annealing process is heated to be incubated 1h ~ 2h after temperature is 1000 DEG C ~ 1200 DEG C, then second time extruding is carried out to the once extruding hafnium pole base after insulation, obtain secondary extrusion hafnium pole base; The extrusion ratio of described second time extruding is 8 ~ 11;
Step 4, the hafnium of secondary extrusion described in step 3 pole base is placed in vacuum annealing furnace carries out secondary stage annealing process;
Step 5, employing pass milling train carry out groove rolling to the secondary extrusion hafnium pole base in step 4 after secondary stage annealing process, and obtain the semi-finished product hafnium square billet that the length of side is 16mm ~ 20mm, the general working rate of described groove rolling is 20% ~ 50%;
Step 6, the hafnium of semi-finished product described in step 5 square billet is placed in vacuum annealing furnace carries out phase III annealing in process;
Step 7, stretcher leveling is carried out to the semi-finished product hafnium square billet in step 6 after phase III annealing in process, obtain the used by nuclear reactor hafnium square rod that the length of side is 16mm ~ 20mm.
2. the preparation method of a kind of used by nuclear reactor hafnium square rod according to claim 1, it is characterized in that, after having extruded for the first time in step one, adopt roll leveller, utilize extruding waste heat once will extrude hafnium pole base aligning to linearity < 3mm/m.
3. the preparation method of a kind of used by nuclear reactor hafnium square rod according to claim 1, it is characterized in that, the temperature of the process of first stage annealing described in step 2 is 750 DEG C ~ 850 DEG C, and the time of first stage annealing process is 1h ~ 2h, and the vacuum of first stage annealing process is not more than 1 × 10
-2pa.
4. the preparation method of a kind of used by nuclear reactor hafnium square rod according to claim 1, it is characterized in that, after second time has extruded in step 3, adopt roll leveller, utilize extruding waste heat by secondary extrusion hafnium pole base aligning to linearity < 3mm/m.
5. the preparation method of a kind of used by nuclear reactor hafnium square rod according to claim 1, it is characterized in that, the temperature of the process of secondary stage annealing described in step 4 is 600 DEG C ~ 650 DEG C, and the time of secondary stage annealing process is 1h ~ 2h, and the vacuum of secondary stage annealing process is not more than 1 × 10
-2pa.
6. the preparation method of a kind of used by nuclear reactor hafnium square rod according to claim 1, it is characterized in that, the temperature of the annealing in process of phase III described in step 6 is 600 DEG C ~ 700 DEG C, and the time of phase III annealing in process is 1h ~ 2h, and the vacuum of phase III annealing in process is not more than 1 × 10
-2pa.
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| CN105436232B (en) * | 2015-12-08 | 2017-05-24 | 西安诺博尔稀贵金属材料有限公司 | High-quantity hafnium rod manufacturing method |
| CN105478521B (en) * | 2016-01-21 | 2017-11-21 | 南京佑天金属科技有限公司 | The process that hafnium filament is drawn |
| CN106378591A (en) * | 2016-11-28 | 2017-02-08 | 西安诺博尔稀贵金属材料有限公司 | Processing method for small-size and high-strength niobium-hafnium alloy bar |
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| JPS59208044A (en) * | 1983-05-13 | 1984-11-26 | Toshiba Corp | Corrosion-resistant hafnium alloy |
| JPS6199519A (en) * | 1984-10-22 | 1986-05-17 | Kobe Steel Ltd | Manufacture of hafnium control-bar covered with zirconium alloy |
| FR2841368B1 (en) * | 2002-06-25 | 2004-09-24 | Framatome Anp | ARRANGEMENT FOR ADJUSTING THE REACTIVITY OF THE HEART OF A NUCLEAR REACTOR, ARRAY ABSORBING THE ARRANGEMENT AND METHOD FOR PROTECTING AGAINST THE WEAR OF THE ABSORBENT ARRAY |
| CN103611757B (en) * | 2013-12-10 | 2015-08-19 | 西部新锆核材料科技有限公司 | A kind of preparation method of zirconium metal fiber wire |
| CN103849803B (en) * | 2014-03-26 | 2017-01-11 | 宁夏东方钽业股份有限公司 | Tantalum alloy and method for preparing tantalum alloy tube |
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