Oxide Layers on (0001) Plane of Zircaloy-4 After Corrosion at 360 °C in Lithiated Aqueous Solution

doi:10.1007/s40195-015-0256-2

摘要/Abstract

Abstract:

The microstructures of the oxide layers formed on near (0001) plane of Zircaloy-4 were investigated by autoclave tests at 360 °C in lithiated aqueous solution. Oxygen-rich regions with hcp structure were observed at the undulating O/M interface, and the inner surface morphology of the oxide layers formed on (0001) was only concave-convex. Monoclinic, tetragonal and cubic phases and a kind of zirconium sub-oxide with bcc structure were detected in the oxide layer near the metal matrix. This zirconium sub-oxide layer had a coherent relationship with α-Zr matrix, and the growth direction of the zirconium sub-oxide layer was nearly parallel to the [0001] direction of α-Zr regardless of the orientation of metal matrix. The orientations scattering of columnar grains formed on near (0001) plane differ from that formed on near () plane.

Key words: Zircaloy-4, (0001), plane, Oxide/metal, interfaces, Microstructure, Oxygen-rich, regions, Zirconium, sub-oxide

. [J]. 金属学报英文版, 2015, 28(6): 748-757.

Shao-Qiu Gou, Bang-Xin Zhou, Mei-Yi Yao, Jian-Chao Peng, Chuan-Ming Chen, Qiang Li, Jin-Long Zhang. Oxide Layers on (0001) Plane of Zircaloy-4 After Corrosion at 360 °C in Lithiated Aqueous Solution[J]. Acta Metallurgica Sinica (English Letters), 2015, 28(6): 748-757.

图/表 10

Fig. 1 TEM image of the whole thin foil sample showing the oxide layer and O/M interface

Fig. 2 a Bright-field image of metal matrix; b SAED pattern of the metal matrix; c bright-field image of the oxygen-rich region; d SAED pattern of the oxygen-rich region

Table 1 EDS results of the positions in Fig. 2a marked by the numbers

Position	Zr content (at%)	O content (at%)	Zr/O ratio
1	96.04	3.96	24.3
2	96.30	3.70	26.0
3	97.15	2.85	34.1
4	85.15	14.85	5.7
5	83.16	16.84	4.9
6	59.79	40.21	1.5
7	61.56	38.44	1.6
8	56.75	43.25	1.3

Fig. 3 Inner surface morphologies of the oxide layers formed on the grain surface with near (0001) plane: a the inner surface was concave-convex; b there were some relatively small concave-convex on the ridge strips observed at higher magnification

Fig. 4 HRTEM image of the type 1 O/M interface and FFT patterns for the areas marked by the letters (A α-Zr matrix, B bcc-ZrOx, C m-ZrO2, D c-ZrO2, E undefined structure)

Fig. 5 HRTEM image of the type 2 O/M interface and FFT patterns for the areas marked by the letters (A oxygen-rich region, B t-ZrO2, C m-ZrO2, D m-ZrO2)

Fig. 6 Reconstruction of the phase-contrast image of the area marked by “B” in Fig. 5

Fig. 7 HRTEM images of bcc-ZrO x that formed on metal grain with an orientation near ()

Fig. 8 HRTEM images of bcc-ZrO x that formed on metal grain with an orientation near (0001)

Fig. 9 SAED patterns of the oxide layers formed on near (0001) plane a, near () plane b, the corresponding dark-field TEM images obtained from the oxide layers on near (0001) plane c, near () plane d

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