# The Effect of TiO2 on the Electrochemical Performance of Sb2O3 Anodes for Li-Ion Batteries
## 3 Results and Discussion
### Characterization
The \(\chi^{2}\) values being below 5 showed good agreement between the literature and the collected data. More importantly, the structure and morphology of the TiO\({}_{2}\)/Sb\({}_{2}\)O\({}_{3}\) composite are very different from what has been reported on similar systems [37; 49]. The synthesis method used in this work is very simple, which can result in the implementation of this method by industry to mass-produce the Sb\({}_{2}\)O\({}_{3}\)/TiO\({}_{2}\) composite anode. In addition, the simplicity of the methodology ensures that the studies are reproducible and thus that the results are reliable. Figure 6A shows the XPS for the hydrothermally synthesized TiO\({}_{2}\) nanoparticles at 175 \({}^{\circ}\)C. The XPS spectrum shows the presence of three peaks, located at 458.6, 464.3 and 472.0 eV, which corresponds to the Ti 2P\({}_{3/2}\). Ti2P\({}_{1/2}\) and the Ti 2P satellite peaks, respectively. The XPS peaks were determined to consist of individual peaks and no further deconvolution was necessary for the fitting. The observed peak energies were consistent with those observed on a rutile phase of TiO\({}_{2}\)[56; 57]. Figure 6B shows the Ti 2P for the synthesized TiO\({}_{2}\)@Sb\({}_{2}\)O\({}_{3}\) (3:1) composite. The data show three peaks in the Ti 2P region, located at 458.6, 464.3 and 472.0 eV. The Ti peaks corresponded to the Ti 2P\({}_{3/2}\), Ti2P\({}_{1/2}\) and the Ti 2P satellite peaks, respectively. The energies for the Ti correspond to Ti in the 4+ oxidation state bound to oxygen as would be present in TiO\({}_{2}\)[56; 57]. \begin{table}
\begin{tabular}{c c c c c c c c c} \hline \hline
**Sample** & **Phase** & **Space Group** & **a (Å)** & **b (Å)** & **c (Å)** & \(\alpha\) (\({}^{\circ}\))** & \(\beta\) (\({}^{\circ}\)) & \(\gamma\) (\({}^{\circ}\)) & \(\chi^{2}\) \\ \hline TiO\({}_{2}\) & Rutile & P4\({}_{2}\)/mmm & 4.59 (8) & 4.59 (8) & 2.95 (9) & 90.0 & 90.0 & 90.0 & 2.41 \\ Sb\({}_{2}\)O\({}_{3}\) & Cubic & Fm-3m & 11.15 (3) & 11.15 (3) & 11.15 (3) & 90.0 & 90.0 & 90.0 & 3.15 \\  & Orthorhombic & Pccn & 4.91 (0) & 12.46 (5) & 5.40 (5) & 90.0 & 90.0 & 90.0 & \\ TiO\({}_{2}\)@Sb\({}_{2}\)O\({}_{3}\) 3:1 & Sb\({}_{5}\)O\({}_{4}\)Cl\({}_{2}\) & P2\({}_{1}\)/C & 6.21 (9) & 5.11 (6) & 13.49 (9) & 90.0 & 97.3 & 90.0 & 1.28 \\  & TiO\({}_{2}\) & P4\({}_{2}\)/mmm & 4.59 (6) & 4.59 (6) & 2.95 (8) & 90.0 & 90.0 & 90.0 & \\ \hline \hline \end{tabular}
\end{table} 
Table 1: Results of the LeBail fitting procedure for the TiO\({}_{2}\) synthesized at 175 \({}^{\circ}\)C, the Sb\({}_{2}\)O\({}_{3}\) starting material and the TiO\({}_{2}\)@Sb\({}_{2}\)O\({}_{3}\) composites synthesized at different ratios. Figure 6: Ti 2P XPS spectrum for hydrothermally synthesized TiO\({}_{2}\) nanoparticles at 175 \({}^{\circ}\)C (**A**) and the (3:1) TiO\({}_{2}\)@Sb\({}_{2}\)O\({}_{3}\) (**B**). The bleu, green and cyan lines are the fitting curves of the XPS results of TiO2 and (3:1) TiO\({}_{2}\)@Sb\({}_{2}\)O\({}_{3}\). Figure 7A shows the XPS spectrum of O1S for the hydrothermally synthesized TiO\({}_{2}\). It was deconvolved into two peaks at 529.8 and 531.1 eV, representing the Ti-O bond and OH bound to the surface, respectively. Figure 7B shows the XPS of the Sb3d for the 3:1 TiO\({}_{2}\)@Sb\({}_{2}\)O\({}_{3}\) sample indicating the presence of four peaks, which were further deconvolved into five peaks. The fifth peak was determined to be from the O 1S spectrum, which overlapped with the Sb 3d. The binding energies of the individual peaks were located at 528.3, 530.7, 531.4, 537.7 and 540.3 eV, corresponding to the Sb (0) 3d\({}_{5/2}\), Sb (III) 3d\({}_{5/2}\), O 1S, Sb (0) 3d\({}_{3/2}\) and the Sb(III)3d\({}_{3/2}\), respectively [56; 58; 59; 60; 61; 62]. The binding energies for the Ti2P, O1S and Sb 3d XPS fittings are summarized in Table 2.