Research data for article: In-situ Raman spectroscopy of Li+ and Na+ storage in anodic TiO2 nanotubes: implications for battery design

In this study, we present an in-situ Raman spectroscopy investigation under current control to enhance our fundamental comprehension of Li+/Na+ storage in TiO2 nanotubes (TiNTs). We establish connections between the structural characteristics revealed by Raman spectroscopy and the electrochemical data, specifically focusing on the differential capacity plots of d(Q–Q0)/dE–1. A reference electrode (TiNP) was established using commercial TiO2 nano powder (Tronox, 99%). The surface morphology of TiNT and TiNP was examined using a Zeiss Sigma 500 field emission scanning electron microscope (SEM). X-ray diffraction patterns of the TiO2 materials were obtained using a Rigaku RINT-2000 X-ray diffractometer with Cu-Kα radiation (λ = 0.15418 nm). The measurements were conducted in the 2θ range of 10-80 at a scan rate of 0.5 degrees per minute. In the case of TiNT, a grazing incidence mode was employed to reduce signal interference from the Titanium metal substrate. Raman spectra were acquired with a Thermo Scientific DXR3 Raman microscope. This study demonstrates the efficacy of in-situ Raman spectroscopy as a potent tool for real-time monitoring of the structural and chemical changes in battery nanoelectrodes during electrochemical ion insertion, offering exceptional precision.