GISAXS and TOF-GISANS studies on surface and depth morphology of self-organized TiO2 nanotube arrays: Model anode material in Li-ion batteries

Neelima Paul*, Jassen Brumbarov, Amitesh Paul, Ying Chen, Jean Francois Moulin, Peter Müller-Buschbaum, Julia Kunze-Liebhaüser, Ralph Gilles

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

13 Scopus citations

Abstract

Self-organized anodic titania (TiO2) nanotube arrays are an interesting model anode material for use in Li-ion batteries owing to their excellent rate capability, their cycling stability and their enhanced safety compared to graphite. A composite material where carbothermally treated conductive TiO2 nanotubes are used as support for a thin silicon film has been shown to have the additional advantage of high lithium storage capacity. This article presents a detailed comparison of the structure, surface and bulk morphology of self-organized conductive TiO2 nanotube arrays, with and without silicon coating, using a combination of X-ray diffraction, X-ray reflectivity, grazing-incidence small-angle X-ray scattering (GISAXS) and time-of-flight grazing-incidence small-angle neutron scattering (TOF-GISANS) techniques. X-ray diffraction shows that the nanotubes crystallize in the anatase structure with a preferred (004) orientation. GISAXS and TOF-GISANS are used to study the morphology of the nanotube arrays, delivering values for the inner nanotube radius and intertubular distances with high statistical relevance because of the large probed volume. The analyses reveal the distinct signatures of a prominent lateral correlation of the TiO2 nanotubes of ∼9414nm and a nanotube radius of ∼4614nm. The porosity averaged over the entire film using TOF-GISANS is 46%. The inner nanotube radius is reduced to half (∼2314nm) through the silicon coating, but the prominent lateral structure is preserved. Such in-depth morphological investigations over large sample volumes are useful towards development of more efficient battery electrode morphologies.

Original languageEnglish
Pages (from-to)444-454
Number of pages11
JournalJournal of Applied Crystallography
Volume48
DOIs
StatePublished - 1 Apr 2015
Externally publishedYes

Keywords

  • grazing-incidence small-angle X-ray scattering
  • lithium-ion batteries
  • nanotube arrays
  • time of flight grazing-incidence small-angle neutron scattering

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