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. 2016 Dec 13:6:38933.
doi: 10.1038/srep38933.

Preparation of Hollow Fe2O3 Nanorods and Nanospheres by Nanoscale Kirkendall Diffusion, and Their Electrochemical Properties for Use in Lithium-Ion Batteries

Jung Sang Cho  1   2 , Jin-Sung Park  1 , Yun Chan Kang  1
Affiliations

Preparation of Hollow Fe2O3 Nanorods and Nanospheres by Nanoscale Kirkendall Diffusion, and Their Electrochemical Properties for Use in Lithium-Ion Batteries

Jung Sang Cho et al. Sci Rep. .

Abstract

A novel process for the preparation of aggregate-free metal oxide nanopowders with spherical (0D) and non-spherical (1D) hollow nanostructures was introduced. Carbon nanofibers embedded with iron selenide (FeSe) nanopowders with various nanostructures are prepared via the selenization of electrospun nanofibers. Ostwald ripening occurs during the selenization process, resulting in the formation of a FeSe-C composite nanofiber exhibiting a hierarchical structure. These nanofibers transform into aggregate-free hollow Fe2O3 powders via the complete oxidation of FeSe and combustion of carbon. Indeed, the zero- (0D) and one-dimensional (1D) FeSe nanocrystals transform into the hollow-structured Fe2O3 nanopowders via a nanoscale Kirkendall diffusion process, thus conserving their overall morphology. The discharge capacities for the 1000th cycle of the hollow-structured Fe2O3 nanopowders obtained from the FeSe-C composite nanofibers prepared at selenization temperatures of 500, 800, and 1000 °C at a current density of 1 A g-1 are 932, 767, and 544 mA h g-1, respectively; and their capacity retentions from the second cycle are 88, 92, and 78%, respectively. The high structural stabilities of these hollow Fe2O3 nanopowders during repeated lithium insertion/desertion processes result in superior lithium-ion storage performances.

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Figures

Figure 1
Figure 1. Formation mechanism of the hollow-structured Fe2O3 nanopowders with 0D and 1D structure.
Figure 2
Figure 2. Conversion reaction of the FeSe filled structure into Fe2O3 hollow structure by nanoscale Kirkendall diffusion effect.
(a) hollow-structured Fe2O3 nanopowder with 1D and (b) hollow-structured Fe2O3 nanopowder with 0D.
Figure 3
Figure 3. Morphologies of the FeSe-carbon composite nanofibers obtained after different selenization temperatures.
(a) selenization at 500 °C, (b) selenization at 800 °C, and (c) selenization at 1000 °C.
Figure 4
Figure 4. XPS spectra of the FeSe-C composite nanofibers obtained after selenization at 800 °C.
(a) Fe 2p spectrum, (b) Se 3d spectrum, and (c) C 1 s spectrum.
Figure 5
Figure 5
Morphologies, SAED pattern, and elemental mapping images of the hollow-structured Fe2O3 nanopowders after oxidation at 600 °C, from the FeSe-C composite nanofibers selenized at (a–g) 500 °C, (h–n) 800 °C, and (o–u) 1000 °C: (a,h,o) SEM images, (b–d,i–k,p–r) TEM images, (e,l,s) HR-TEM images, (f,m,t) SAED patterns, and (g,n,u) elemental mapping images.
Figure 6
Figure 6. XPS spectra and TG curve of the hollow-structured Fe2O3 nanopowders after oxidation at 600 °C from the FeSe-C nanofibers selenized at 800 °C.
(a) XPS Fe 2p spectrum, (b) XPS O 1 s spectrum, and (c) TG curve.
Figure 7
Figure 7. Electrochemical properties of the hollow-structured Fe2O3 nanopowders.
(a) CV curves of the Sel.500-Oxi.600, (b) first discharge-charge profiles at a current density of 1.0 A g−1, (c) cycling performances at a current density of 1.0 A g−1, and (d) rate performances.
Figure 8
Figure 8. Nyquist impedance plots of the hollow-structured Fe2O3 nanopowders before and after cycling.
(a) before cycle, (b) after 1st cycle, and (c) after 200th cycle.
Figure 9
Figure 9. Morphologies of the hollow Fe2O3 powders obtained after 200 cycles at a current density of 1.0 A g−1.
(a) Sel.500-Oxi.600, (b) Sel.800-Oxi.600, and (c) Sel.1000-Oxi.600.
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