Microstructural analysis and XPS investigation of nodular oxides formed on Zircaloy-4

Park, Jeong Yong; Jeong, Yong Hwan

doi:10.1016/j.jnucmat.2011.03.010

Cited by 21 publications

(5 citation statements)

References 11 publications

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“…The XPS peaks located at 183 and 185 eV can be assigned to Zr3d 5/2 and Zr3d 3/2 respectively, exhibiting the fully oxidized state of Zr 4+ . These results are in good agreement with the reported literature [ 21 , 37 ]. The high-resolution spectra of oxygen in the as-prepared and the annealed Zr-4 oxide nanotubes are depicted in Figure 6 d. It shows a single dominant peak located at 530.0 eV which can be attributed to the lattice oxygen of ZrO 2 .…”

Section: Resultssupporting

confidence: 94%

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Formation of self-organized Zircaloy-4 oxide nanotubes in organic viscous electrolyte via anodization

et al. 2014

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This work reports the formation of self-organized Zircaloy-4 (Zr-4) oxide nanotubes in viscous organic ethylene glycol (EG) electrolyte containing a small amount of fluoride salt and deionized (DI) water via an electrochemical anodization. The structure, morphology, and composition of the Zr-4 oxide nanotubes were studied using X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), EDX, and XPS. SEM results showed that the length of the nanotubes is approximately 13 μm, and TEM results showed that the inner diameter of the Zr-4 oxide nanotubes is approximately 20 nm with average wall thickness of approximately 7 nm. XRD and selected area electron diffraction pattern (SAED) results confirmed that the as-anodized Zr-4 oxide nanotubes have cubic crystalline structure. Both cubic and monoclinic phases were found after annealing of Zr-4 oxide nanotubes. The tubular structure morphology of Zr-4 oxide nanotubes did not remain intact after annealing which is attributed to the elimination of F species from the annealed nanotubes.

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Section: Resultssupporting

confidence: 94%

“…In addition, a broad shoulder peak in the energy range of 533 eV can be seen in the annealed Zr-4 oxide nanotubes. This peak can be attributed to the presence of hydroxyl species bond [ 35 , 37 ]. Figure 6 e gives the high-resolution XPS spectra of Sn in the as-anodized and the annealed Zr-4 oxide nanotubes.…”

Section: Resultsmentioning

confidence: 99%

Formation of self-organized Zircaloy-4 oxide nanotubes in organic viscous electrolyte via anodization

et al. 2014

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“…Thus, this zirconium sub-oxide (bcc-ZrO x ) was the same as reported in Ref. [17], and the same coherent relationship of (1 " O/M interface would appear to be of the order of 1-1.3 GPa [23,24]. The metastable oxide phase can be stabilized under high compressive stress at O/M interface [25].…”

Section: Microstructure Of Oxide Layers Adjacent To the Oxide/metal Isupporting

confidence: 66%

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

Shaoqiu

Zhou

Yao

et al. 2015

Acta Metall. Sin. (Engl. Lett.)

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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 concaveconvex. 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 a-Zr matrix, and the growth direction of the zirconium sub-oxide layer was nearly parallel to the [0001] direction of a-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 (10 " 10) plane.

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“…1b. The non-uniformity of the Zircaloy-4 composition, in particular the Sn distribution, is known to give rise to a non-uniform stoichiometry of the surface as well as to the plasticity [8][9][10] within the same sample, as shown in sample #5.…”

Section: Resultsmentioning

confidence: 99%

Effect of Zr Oxide on the Electrochemical Dissolution of Zircaloy-4 Cladding Tubes

Lee

Jeon

Heo

et al. 2012

J. Electrochem. Soc.

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The effect of the Zr oxide layer on the electrochemical dissolution of Zircaloy-4 cladding tubes is examined in LiCl-KCl-ZrCl 4 molten salts at 500 • C. The cyclic voltammetry of Zircaloy-4 cladding tubes oxidized at 400 • C reveals an evident oxidation peak associated with an immediate dissolution of Zr, as also observed in the current transient. In contrast, the Zr oxide layer formed on Zircaloy-4 tubes at 500 • C and 600 • C significantly inhibits both Zr reduction/oxidation processes on the voltammetric scans in a given potential range. However, the current transients at a constant potential of −0.78 V, where the oxidation of Zr is involved, reveal a dissolution process that is strongly suppressed for an initial period of time proportional to the oxidation temperature, followed by a gradual increase in the dissolution current over time. After the dissolution at −0.78 V for 1 hr, metallic Zr is exposed on a Zircaloy-4 tube oxidized at 500 • C, which leads to a recovered current response for Zr reduction/oxidation in the subsequent voltammetric experiments. The XPS results show that the oxide passivation layer is found to be dissolved or removed under high-temperature molten salts.

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Microstructural analysis and XPS investigation of nodular oxides formed on Zircaloy-4

Cited by 21 publications

References 11 publications

Formation of self-organized Zircaloy-4 oxide nanotubes in organic viscous electrolyte via anodization

Formation of self-organized Zircaloy-4 oxide nanotubes in organic viscous electrolyte via anodization

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

Effect of Zr Oxide on the Electrochemical Dissolution of Zircaloy-4 Cladding Tubes

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