纳米组织Zr-4合金腐蚀性能研究
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摘要
纳米材料由于其优异的性能具有诱人的应用前景,但目前关于纳米晶结构对耐腐蚀性能影响的研究结果互相矛盾,远没有形成对其腐蚀机制一致的看法。因此,研究表面纳米化后锆合金的腐蚀性能,揭示其腐蚀机理,可以为优化现有合金及开发新型合金提供实验依据,同时也可以丰富核材料领域的研究内容,并有助于深入探索材料耐腐蚀性能的影响因素和作用机理。
本试验采用高速喷丸技术对Zr-4合金板一侧表面纳米化,并将其放入673k/10.3MPa高温过热蒸汽的高压釜中进行腐蚀,利用X射线衍射、扫描电子显微镜、EDS分析、透射电子显微镜对其形成的氧化膜生长情况进行了分析,得到以下结论:
(1)纳米组织Zr-4合金的腐蚀增重明显小于普通组织Zr-4合金的腐蚀增重,但是纳米组织的腐蚀转折时间要滞后于普通组织的腐蚀转折时间。
(2)纳米组织Zr-4合金生成的氧化膜内表面比普通组织Zr-4合金生成的氧化膜内表面平整、光滑,说明纳米组织生成的氧化膜内表面没有出现孔洞簇、或者出现的孔洞簇少于普通组织生成的氧化膜,因此纳米组织生成的氧化膜自身的结合能力和其与金属基体的结合能力均高于普通组织生成的氧化膜。
(3)Zr-4合金经过纳米化的处理,降低了氧化膜/金属界面处氧离子的扩散速度,抑制了氧离子与金属的反应,阻碍了氧化膜的增厚,从而提高了合金的抗腐蚀性能。
(4)纳米组织Zr-4合金生成的氧化膜中四方相等轴晶增多,四方相等轴晶能够延迟氧化膜结构转变,从而使纳米组织Zr-4合金抗腐蚀能力明显提高。
综上所述,在673k/10.3MPa高温过热蒸汽的高压釜中,纳米化Zr-4合金的耐腐蚀性能要比普通Zr-4合金的耐腐蚀性能好,因此我们认为纳米化Zr-4合金耐腐蚀性能的提高与氧化膜内四方氧化锆的含量有直接的关系,而关于纳米化Zr-4合金耐腐蚀性能的机理仍有待进一步的实验研究和分析。
It is certainly that nano-materials will have an attractive application prospects because of their outstanding properties, but the corrosion resistance maybe is the negative factor. At present investigations, the impact of surface nanocrystallined zircaloy on corrosion resistance is contradictory; no coincident opinion can be drawn. Therefore, revealed the corrosion mechanism, by studying the corrosion properties of surface nanocrystallined zircaloy, can provide experimental basis for optimizing of existing alloys and developing of novel alloys.
One side of the simple was subjected to high-speed shot preening treatment in order to achieve a surface nanocrystallization structure in a certain depth. The oxide films of nanocrystallization Zircaloy-4 alloy in autoclave at 673K/10.3MPa steam have been observed by XRD、SEM、EDS、TEM, respectively in this paper. We draw conclusions as following:
(1) Results of 160 days corrosion test under the 673K/10.3MPa condition show that the weight gain of nanostructure Zircaloy-4 is less than that of traditional structure, which indicate that nanostructure Zircaloy-4 has a better corrosion resistance.
(2) The M/O interface of nanostructure Zircaloy-4 is more regular and smoother, which imply that, no or less clusters of pores develop in nanostructure.
(3) The absence of Oxygen-rich area at the M/O interface of nanostructure Zircaloy-4, indicates that the corrosion process is lag of the traditional structure Zircaloy-4
(4) The result of TEM observation indicates that t-ZrO_2 formed as a protected coating at the M/O interface in nanostructure zircaloy-4
Experimental evidences indicated that the nanocrystalline zircaloy-4 could delay the transition of the corrosion. Simultaneously, the metal/oxide interface of nanostructure Zircaloy-4 was more regular and glossy than that of coarse-grain structure Zircaloy-4. Furthermore, many equiaxed grains were discovered in the oxide films formed on the nanostructure basis, which indicated that nanostructure Zircaloy-4 had a better corrosion resistance. This paper showed the corrosion resistance improvement of nanocrystallization Zircaloy-4 alloy had relation with the percentage of tetragonal-Zirconia, the stress of tetragonal-Zirconia and the high compressed stress of oxide film. However about the corrosion resistance mechanism of nanocrystallizaion Zircaloy-4 alloy should be researched and discussed in the further.
本试验采用高速喷丸技术对Zr-4合金板一侧表面纳米化,并将其放入673k/10.3MPa高温过热蒸汽的高压釜中进行腐蚀,利用X射线衍射、扫描电子显微镜、EDS分析、透射电子显微镜对其形成的氧化膜生长情况进行了分析,得到以下结论:
(1)纳米组织Zr-4合金的腐蚀增重明显小于普通组织Zr-4合金的腐蚀增重,但是纳米组织的腐蚀转折时间要滞后于普通组织的腐蚀转折时间。
(2)纳米组织Zr-4合金生成的氧化膜内表面比普通组织Zr-4合金生成的氧化膜内表面平整、光滑,说明纳米组织生成的氧化膜内表面没有出现孔洞簇、或者出现的孔洞簇少于普通组织生成的氧化膜,因此纳米组织生成的氧化膜自身的结合能力和其与金属基体的结合能力均高于普通组织生成的氧化膜。
(3)Zr-4合金经过纳米化的处理,降低了氧化膜/金属界面处氧离子的扩散速度,抑制了氧离子与金属的反应,阻碍了氧化膜的增厚,从而提高了合金的抗腐蚀性能。
(4)纳米组织Zr-4合金生成的氧化膜中四方相等轴晶增多,四方相等轴晶能够延迟氧化膜结构转变,从而使纳米组织Zr-4合金抗腐蚀能力明显提高。
综上所述,在673k/10.3MPa高温过热蒸汽的高压釜中,纳米化Zr-4合金的耐腐蚀性能要比普通Zr-4合金的耐腐蚀性能好,因此我们认为纳米化Zr-4合金耐腐蚀性能的提高与氧化膜内四方氧化锆的含量有直接的关系,而关于纳米化Zr-4合金耐腐蚀性能的机理仍有待进一步的实验研究和分析。
It is certainly that nano-materials will have an attractive application prospects because of their outstanding properties, but the corrosion resistance maybe is the negative factor. At present investigations, the impact of surface nanocrystallined zircaloy on corrosion resistance is contradictory; no coincident opinion can be drawn. Therefore, revealed the corrosion mechanism, by studying the corrosion properties of surface nanocrystallined zircaloy, can provide experimental basis for optimizing of existing alloys and developing of novel alloys.
One side of the simple was subjected to high-speed shot preening treatment in order to achieve a surface nanocrystallization structure in a certain depth. The oxide films of nanocrystallization Zircaloy-4 alloy in autoclave at 673K/10.3MPa steam have been observed by XRD、SEM、EDS、TEM, respectively in this paper. We draw conclusions as following:
(1) Results of 160 days corrosion test under the 673K/10.3MPa condition show that the weight gain of nanostructure Zircaloy-4 is less than that of traditional structure, which indicate that nanostructure Zircaloy-4 has a better corrosion resistance.
(2) The M/O interface of nanostructure Zircaloy-4 is more regular and smoother, which imply that, no or less clusters of pores develop in nanostructure.
(3) The absence of Oxygen-rich area at the M/O interface of nanostructure Zircaloy-4, indicates that the corrosion process is lag of the traditional structure Zircaloy-4
(4) The result of TEM observation indicates that t-ZrO_2 formed as a protected coating at the M/O interface in nanostructure zircaloy-4
Experimental evidences indicated that the nanocrystalline zircaloy-4 could delay the transition of the corrosion. Simultaneously, the metal/oxide interface of nanostructure Zircaloy-4 was more regular and glossy than that of coarse-grain structure Zircaloy-4. Furthermore, many equiaxed grains were discovered in the oxide films formed on the nanostructure basis, which indicated that nanostructure Zircaloy-4 had a better corrosion resistance. This paper showed the corrosion resistance improvement of nanocrystallization Zircaloy-4 alloy had relation with the percentage of tetragonal-Zirconia, the stress of tetragonal-Zirconia and the high compressed stress of oxide film. However about the corrosion resistance mechanism of nanocrystallizaion Zircaloy-4 alloy should be researched and discussed in the further.
引文
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