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Acta Metall Sin  2016, Vol. 52 Issue (1): 78-84    DOI: 10.11900/0412.1961.2015.00260
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SECOND PHASE PARTICLES AND THEIR CORROSION BEHAVIOR OF Zr-0.72Sn-0.32Fe-0.15Cr-0.97Nb ALLOY
Zhen WANG1,2,Bangxin ZHOU1,2(),Boyang WANG1,2,Jiao HUANG1,2,Meiyi YAO1,2,Jinlong ZHANG1,2
1 Institute of Materials, Shanghai University, Shanghai 200072, China
2 Laboratory for Microstructures, Shanghai University, Shanghai 200444, China
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Zhen WANG,Bangxin ZHOU,Boyang WANG,Jiao HUANG,Meiyi YAO,Jinlong ZHANG. SECOND PHASE PARTICLES AND THEIR CORROSION BEHAVIOR OF Zr-0.72Sn-0.32Fe-0.15Cr-0.97Nb ALLOY. Acta Metall Sin, 2016, 52(1): 78-84.

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Abstract  

Zr-0.72Sn-0.32Fe-0.15Cr alloy, which has much better corrosion resistance than that of Zr-4 alloy, was alloying by adding 1%Nb (mass fraction). In order to understand the effect of Nb on the corrosion resistance of Zr-0.72Sn-0.32Fe-0.15Cr alloy, the second phase particles (SPPs) and their oxidation behavior in this alloy were investigated using TEM, SEM and EDS techniques. Thin foil specimens for TEM observation were prepared for Zr-0.72Sn-0.32Fe-0.15Cr-0.97Nb alloy after recrystallization annealing. The corrosion tests for these thin foil specimens were conducted in an autoclave at 300 ℃, 8 MPa in deionized water for short time exposure. The results showed that a thin oxide layer in several hundred nanometers mainly consisted of the monoclinic ZrO2 formed on the surface, and SPPs embedded in the thin foil specimens at different corrosion levels were observed after corrosion test. The sizes of SPPs were mainly distributed between 30~150 nm and the maximum size was 230 nm. The size and crystal structure of SPPs have a relationship with Nb/Zr ratio (atomic ratio) of their composition. When Nb/Zr ratio was about zero, the size of SPPs was over 150 nm. When Nb/Zr ratio was in the range of 0.10~0.50, the sizes of SPPs were between 60~150 nm. When Nb/Zr ratio were in the range of 0.50~0.75, the sizes of SPPs were between 30~60 nm. When Nb/Zr ratio was over 0.75, the size of SPPs was smaller than 30 nm. With the increase of Nb/Zr ratio of their composition, three kinds crystal structure of Nb-containing SPPs, fcc (lattice constant a=0.701 nm), hcp (lattice constants a=0.508 nm, c=0.832 nm) and bcc (a=0.325 nm) structures were detected. SPPs without Nb containing have fcc structure (a=0.817 nm) while Fe/Cr ratio was over 5.00 and hcp structure (a=0.492 nm, c=0.788 nm) while Fe/Cr ratio was less than 3.00. The oxidation behavior of SPPs also had a relationship with the Nb/Zr ratio. The SPPs were easy to be oxidized to amorphous when Nb/Zr ratio was over 0.50. However, the SPPs with Nb/Zr ratio less than 0.50 were difficult to be oxidized.

Key words:  Zr alloy      second phase particle      crystal structure      oxidation      Nb/Zr atomic ratio     
Received:  13 May 2015     
Fund: Supported by National Natural Science Foundation of China (Nos.51171102 and 51271104)

URL: 

https://www.ams.org.cn/EN/10.11900/0412.1961.2015.00260     OR     https://www.ams.org.cn/EN/Y2016/V52/I1/78

Fig.1  TEM (a) and SEM (b) images of Zr-0.72Sn-0.32Fe-0.15Cr-0.97Nb alloy (Zr alloy) after annealing at 580 ℃ for 5 h
Fig.2  Size distribution of second phase particles (SPPs) in Zr alloy
Fig.3  Relationship between the size of SPPs and atomic ratios of Nb/Fe and Nb/Zr in the composition of SPPs
Fig.4  TEM images and SAED patterns (below) of SPPs with different Nb/Zr ratios of Nb/Zr=0 (a, b), Nb/Zr=0.42 (c), Nb/Zr=0.67 (d) and Nb/Zr=0.93 (e)
Fig.5  TEM image (a) and SAED pattern (b) of Zr alloy after corrosion test at 300 ℃, 8 MPa in dionized water for short time exposure
Fig.6  TEM images and SAED patterns (insets) of SPPs after corrosion test with Nb/Zr ratios of Nb/Zr=0 (a), Nb/Zr=0.43 (b), Nb/Zr=0.72 (c) and Nb/Zr=0.89 (d)
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