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Nano-sized particles of rutile TiO 2 is a promising material for cheap high-capacity anodes for Li-ion batteries. It is well-known that rutile undergoes an irreversible order-disorder transition upon deep discharge. However, in the disordered state, the Li x TiO 2 material retains a high reversible ion-storage capacity of &gt;200 mA h g -1 . Despite the promising properties of the material, the structural transition and evolution during the repeated battery operation has so far been studied only by diffraction-based methods, which only provide insight into the part that retains some long-range order. Here, we utilize a combination of ex situ and operando total scattering with pair distribution function analysis and transmission electron microscopy to investigate the atomic-scale structures of the disordered Li x TiO 2 forming upon the discharge of nano-rutile TiO 2 as well as to elucidate the phase behavior in the material during the repeated charge-discharge process. Our investigation reveals that nano-rutile upon Li-intercalation transforms into a composite of ∼5 nm domains of a layered Li x TiO 2 α-NaFeO 2 -type structure with ∼1 nm Li x TiO 2 grain boundaries with a columbite-like structural motif. During repeated charge-discharge cycling, the structure of this composite is retained and stores Li through a complete solid-solution transition with a remarkably small volume change of only 1 vol%.

Order–disorder transition in nano-rutile TiO2 anodes: a high capacity low-volume change Li-ion battery material

Order–disorder transition in nano-rutile TiO₂ anodes: a high capacity low-volume change Li-ion battery material