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Samples of Li 4 Ti 5 O 12− y   solid solutions are synthesized by one-step solid-state carbothermal reduction reaction using Li 2 CO 3 , anatase, and carbon black under a nitrogen atmosphere. The underlying formation mechanism that leads to Li 4 Ti 5 O 12− y   solid solutions is proposed. The formation mechanism of the Li 4 Ti 5 O 12−y  solid solution is investigated by  in situ  variable temperature X-Ray diffraction (VT-XRD) and thermogravimetric analysis/differential scanning calorimetry (TGA-DSC). First, some Ti 4+  centers are converted to Ti 3+  (TiO 2 -TiO 2− x  ) because of the presence of carbon black. Secondly, Li 2 CO 3  reacts with TiO 2− x   (anatase) to form Li 2 TiO 3 . Thirdly, Li 2 TiO 3  reacts with TiO 2− x   to form the Li 4 Ti 5 O 12− y   solid solution, while anatase starts to transform into rutile at the same time. Rutile reacts with Li 2 TiO 3  to form Li 4 Ti 5 O 12− y   at higher temperatures. The presence of Ti 3+  not only improves the electrical conductivity but also improves the ionic conductivity. As a result, the as-prepared material exhibits good rate capability and cycling stability with 99.3% capacity retention after 200 cycles.

The formation mechanism of Li4Ti5O12−y solid solutions prepared by carbothermal reduction and the effect of Ti3+ on electrochemical performance