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. 2014 Oct 4;9(1):553.
doi: 10.1186/1556-276X-9-553. eCollection 2014.

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

Ghafar Ali  1 , Yang Jeong Park  2 , Hyun Jin Kim  2 , Sung Oh Cho  2
Affiliations

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

Ghafar Ali et al. Nanoscale Res Lett. .

Abstract

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.

Keywords: Anodization; Nanotubes; SEM; TEM; XPS; Zircaloy.

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Figures

Figure 1
Figure 1
FESEM images of the as-anodized Zr-4 oxide nanotubes. The nanotubes were prepared in ethylene glycol (EG) electrolyte containing a small amount of NH4F and DI water showing the top (a) and cross-sectional (b)-(c) surface morphology. Digital photo of Zr-4 oxide nanotubes along with Zr-4 substrate (d).
Figure 2
Figure 2
TEM images and EDX spectrum of Zr-4 oxide nanotubes. TEM images (a)-(c) showing the formation of Zr-4 oxide nanotubes in EG electrolyte containing a small amount of NH4F and DI water. EDX spectrum of Zr-4 oxide nanotubes (d).
Figure 3
Figure 3
TEM images of annealed Zr-4 oxide nanotubes. The disintegration of tubular morphology (a) and increase in crystallinity (b) after annealing are shown.
Figure 4
Figure 4
Wide-scan XPS spectra of the as-anodized and annealed Zr-4 oxide nanotubes.
Figure 5
Figure 5
XRD patterns. As-received Zr-4 sheet (a). As-anodized (b) and annealed (c) Zr-4 oxide nanotubes. XRD patterns of the Zr-4 oxide nanotubes clearly show that the as-anodized nanotubes were crystalline in cubic phase which is transformed into monoclinic after annealing.
Figure 6
Figure 6
High-resolution XPS spectra. (a) F, (b) C, (c) Zr, (d) O, (e) Sn, (f) Fe, and (g) Cr of the as-anodized and annealed Zr-4 oxide nanotubes.
See this image and copyright information in PMC

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