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摘要: 在一次氢化-脱氢法的基础上探索锆-2合金粉末制备的循环氢化-脱氢法新工艺。研究了氢化温度和氢化压力对氢化相转变过程的影响，并在此基础上研究了循环次数对氢化脱氢实验过程、氢化锆组织、锆组织及出粉率的影响，结合工艺组织性能研究，探讨了氢化脱氢过程对裂纹扩展的影响机理。研究结果表明：较优的氢化温度为600 ℃，氢化压力为0.3 MPa，循环次数为2次；循环氢化脱氢是两个过程的动态平衡过程，2次循环可以达到一个较优点；循环氢化脱氢的杂质含量控制可以满足要求。Abstract: Based on the single process of hydrogenation-dehydrogenation, a new cyclical hydrogenation-dehydrogenation technology of Zr-2 alloy powder preparation was studied. The effects of hydrogenation temperature and pressure on hydride phase transition were investigated, and the effects of cycle number on hydrogenation-dehydrogenation process, ZrH and Zr structure, and powder productivity were investigated. The influence mechanism of hydrogenation-dehydrogenation process on crack propagation was discussed. In the results, the optimum hydrogenation temperature is 600 ℃, the optimum hydrogenation pressure is 0.3 MPa, and the optimum cycle number is 2 times. Cyclical hydrogenation-dehydrogenation is a dynamic equilibrium process between two hydrogenation-dehydrogenation processes, twice cycle can reach an optimum point. In addition, the impurity controlling can meet the requirement.
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Key words:
- hydrogenation /
- dehydrogenation /
- Zr-2 /
- cycle number /
- crack propagation
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图 2 氢化温度对氢化相转变过程的影响
Figure 2. Influence of hydrogenation temperature on hydride phase transition
图 3 氢化压力对氢化相转变过程的影响
Figure 3. Influence of hydrogenation pressure on hydride phase transition
图 6 不同循环次数下循环氢化脱氢实验后氢化锆显微组织：（a）1次；（b）2次；（c）3次
Figure 6. Microstructures of ZrH after cyclical hydrogenation-dehydrogenation in different cycle numbers: (a) 1 time; (b) 2 times; (c) 3 times
图 7 不同循环次数下循环氢化脱氢实验后锆块显微组织：（a）1次；（b）2次；（c）3次
Figure 7. Microstructures of Zr after cyclical hydrogenation-dehydrogenation in different cycle numbers: (a) 1 time; (b) 2 times; (c) 3 times
图 8 2次循环氢化脱氢后氢化锆块及锆块裂纹扫描电子显微形貌：（a），（b）氢化锆；（c），（d）锆
Figure 8. SEM morphology of ZrH and Zr crack after twice cycle hydrogenation-dehydrogenation: (a), (b) ZrH; (c), (d) Zr
表 1 氢化温度对氢化锆中氢质量分数的影响
Table 1. Influence of hydrogenation temperature on hydrogen content by mass
氢化温度/℃ 500 600 700 氢质量分数/% 1.78 1.72 1.61 
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表 2 氢化压力对氢质量分数的影响
Table 2. Influence of hydrogenation pressure on hydrogen content by mass
氢化压力/MPa 0.2 0.3 氢质量分数/% 1.71 1.72
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表 3 循环次数对氢质量分数影响
Table 3. Influence of cycle number on hydrogen content by mass
循环次数/次 1 2 3 氢质量分数/% 1.72 1.72 1.69
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表 4 循环次数对出粉率影响
Table 4. Influence of cycle number on powder productivity
循环次数/次 出粉率/% 140目 325目 1 10.61 1.32 2 15.44 1.28 3 12.27 1.19
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表 5 杂质含量分析
Table 5. Analysis of impurity content
杂质元素 O H N 循环氢化脱氢工艺中杂质含量要求/(μg·g-1) ＜2500 ＜25 ＜120 2次循环样品中杂质含量/(μg·g-1) 2100 22 106
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