INVESTIGATION OF THE ANISOTROPIC GROWTH OF OXIDE LAYERS FORMED ON Zr-4 ALLOYS CORRODED IN LiOH AQUEOUS SOLUTION

doi:10.11900/0412.1961.2015.00049

Acta Metall Sin

2015, Vol. 51

Issue (8): 993-1000 DOI: 10.11900/0412.1961.2015.00049

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INVESTIGATION OF THE ANISOTROPIC GROWTH OF OXIDE LAYERS FORMED ON Zr-4 ALLOYS CORRODED IN LiOH AQUEOUS SOLUTION

Shaoqiu GOU¹,Bangxin ZHOU^1,²(

),Shijing XIE¹,Long XU^1,²,Meiyi YAO¹,Qiang LI^1,²

1 Institute of Materials, Shanghai University, Shanghai 200072
2 Laboratory for Microstructures, Shanghai University, Shanghai 200444

Cite this article:

Shaoqiu GOU,Bangxin ZHOU,Shijing XIE,Long XU,Meiyi YAO,Qiang LI. INVESTIGATION OF THE ANISOTROPIC GROWTH OF OXIDE LAYERS FORMED ON Zr-4 ALLOYS CORRODED IN LiOH AQUEOUS SOLUTION. Acta Metall Sin, 2015, 51(8): 993-1000.

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Abstract

Zr-4 coarse-grained specimens were corroded in static autoclave at 360 ℃, 18.6 MPa in 0.01 mol/L LiOH aqueous solution for 70 and 160 d exposure. EBSD, SEM and HRTEM were used to investigate the microstructures and crystal structures of oxide layers, and the relationships between the oxide thickness and the grain orientation of the metal matrix. The results showed that the oxide layers formed on the grain surfaces with the orientations nearby basal plane (0001) were thicker, and exhibited a prominent anisotropic for the oxide growth when Zr-4 specimens were corroded in LiOH aqueous solution for 160 d, but this was not the case for 70 d. The grains with the surface orientation nearby (0001), (1010) and (1120) were selected from the specimens corroded for 70 d to investigate the effect of metal grain orientation on the microstructure of oxide layers. The results showed that the crystal structure and microstructure of oxide layers formed on different metal grains were obviously different, and the scattering of m-ZrO₂ columnar grain orientations in the oxide layers formed on near basal plane (0001) was wider than that on near prismatic plane (1010) and (1120). Besides the majority of m-ZrO₂, c-ZrO₂, t-ZrO₂ and sub-oxide phase Zr₃O were also detected at the oxide/metal interface, and it showed that the microstructure and crystal structure of oxide layers were very complex. The microstructural evolution of oxide layers will affect the diffusion of oxygen and subsequently the growth of oxide. Therefore, the microstructural evolution of oxide layers, which was affected by the different microstructure of oxide layers formed initially on grains and the water chemistry of corrosion tests, resulted in the anisotropic growth of oxide layers when Zr-4 specimens were corroded in LiOH aqueous solution in subsequent corrosion tests.

Key words: Zr-4 corrosion resistance anisotropic growth oxide layer microstructure

Fund: Supported by National Natural Science Foundation of China (Nos.51171102 and 51271104)

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	Shaoqiu GOU
	Bangxin ZHOU
	Shijing XIE
	Long XU
	Meiyi YAO
	Qiang LI

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https://www.ams.org.cn/EN/10.11900/0412.1961.2015.00049 OR https://www.ams.org.cn/EN/Y2015/V51/I8/993

Fig.1 Inverse pole figures (IPFs) of the relationship between the oxide thickness and the surface orientation of metal grains obtained from Zr-4 coarse-grained specimens corroded at 360 ℃ in LiOH aqueous solution for 70 d (a) and 160 d (b)

Fig.2 Surface morphology (a) and cross sectional SEM image (b) of the oxide layer formed on Zr-4 coarse-grained specimens corroded at 360 ℃ in LiOH aqueous solution for 160 d

Fig.3 SAED patterns (a~c) and dark field TEM images (d~f) of m-ZrO₂columnar grains in oxide layers formed on the surface of metal grains near (0001) (a, d), (1010) (b, e) and (1210) (c, f) obtained from Zr-4 coarse-grained specimens corroded for 70 d

Fig.4 HRTEM images and FFT patterns of the oxides at the oxide/metal (O/M) interface (a) and near the O/M interface (b) formed on (1010) plane

Fig.5 IFFT patterns of (200) (a) and (111) (b) for c-ZrO₂ area outlined in Fig.4b and strain fields obtained from the geometric phase images analyzed using Fig.5a (c) and Fig.5b (d) (Arrows in Figs.5a and b show the dislocation cores)

Fig.6 Fracture surface morphologies of the thicker (a, b) and the thinner (c, d) oxide layers formed on Zr-4 coarse-grained specimens corroded at 360 ℃ in LiOH aqueous solution for 160 d (Figs.6b and d show the enlarged images of virtual boxes in Figs.6a and c, respectively)

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