A kind of preparation method of zirconium and zirconium alloy coarse grain
A zirconium alloy and coarse crystal technology, which is applied in the field of coarse crystal and single crystal material research, can solve the problems that do not involve the preparation method of zirconium and zirconium alloy coarse crystal or single crystal, and achieves easy operation, wide applicability and simple process. Effect
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Embodiment 1
[0030] (1) Vacuum arc melting of pure zirconium (purity mass fraction>99.9%) sponge zirconium to obtain a button ingot with a mass of 65g. For the microstructure of the button ingot, see image 3 ;
[0031] (2) Seal the button ingot into the quartz tube and vacuumize it (vacuum degree-3 Pa), then filled with argon (0.5Mpa);
[0032] (3) The vacuum-protected sample was subjected to solid solution treatment at 1200°C in an ultra-high temperature resistance furnace, kept for 8 hours, and the cooling method was furnace cooling;
[0033] (4) Repeat the above-mentioned solution treatment process at 1200° C. for 5 times.
[0034] (5) The sample treated in step (4) is subjected to solution treatment for a long time below the α transformation point. The specific solution treatment temperature is 860° C., the solution time is 100 h, and the cooling method is furnace cooling.
[0035] Pure zirconium samples were pre-ground and mechanically polished, and then treated with a volume ratio...
Embodiment 2
[0037] (1) Cut a block sample of 10*10*10mm on a Zircaloy-4(Zr-1.5Sn-0.2Fe-0.1Cr)(Zr-4) alloy plate with a thickness of 10mm, and its original structure can be found in Figure 5 ;
[0038] (2) Seal the bulk sample in a quartz tube and vacuumize it (vacuum degree-3 Pa), then filled with argon (0.5Mpa);
[0039] (3) The vacuum-protected sample was subjected to solution treatment at 1300°C in an ultra-high temperature resistance furnace, kept for 10 hours, and the cooling method was furnace cooling;
[0040] (4) Repeat the above-mentioned solution treatment process at 1300° C. for 3 times.
[0041] (5) The sample treated in step (4) was subjected to solution treatment for a long time below the α phase transformation point. The specific solution treatment temperature was 880° C., the solution time was 200 h, and the cooling method was furnace cooling.
[0042] The Zr-4 alloy sample was pre-ground and mechanically polished, and then the volume ratio was 9(H 2 O): 9 (HNO 3 ): 2...
Embodiment 3
[0044] (1) Cut a block sample of 5*10*10mm on a Zirlo (Zr-1.0Nb-1.0Sn-0.1Fe) alloy plate with a thickness of 5mm, and see the original structure Figure 7 ;
[0045] (2) Seal the bulk sample in a quartz tube and vacuumize it (vacuum degree-3 Pa), then filled with argon (0.5Mpa);
[0046] (3) The vacuum-protected sample was subjected to solution treatment at 1250°C in an ultra-high temperature resistance furnace, kept for 12 hours, and the cooling method was furnace cooling;
[0047] (4) Repeat the above-mentioned solution treatment process at 1250° C. for 5 times.
[0048] (5) The sample treated in step (4) is subjected to solution treatment for a long time below the α transformation point. The specific solution treatment temperature is 870° C., the solution time is 150 h, and the cooling method is furnace cooling.
[0049]Zirlo alloy samples were pre-ground and mechanically polished, and then treated with a volume ratio of 9(H 2 O): 9 (HNO 3 ): 2 (HF) etchant to wipe the ...
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