Operando and Ex-Situ Studies of Columbite Electrode Materials

Abstract

Storing and utilising electricity from renewable sources is of growing importance as we move away from our reliance on fossil fuels. Batteries and supercapacitors are becoming ever more present in our day to day lives; in order to improve the next generation of batteries and supercapacitors, we must understand on an atomic scale what happens to electrode materials upon charge and discharge. In order to do this, we must combine structural and electrochemical studies, using techniques which use both different length scales and different timescales. These experiments are known as operando experiments and are a valuable tool in analysing new materials for energy storage.Transition metal niobates of the columbite structure (MNb2O6, M = transition or alkali earth metal) have previously been studied for their photocatalytic and magnetic properties but recently have garnered interest as negative electrode materials for batteries and supercapacitors.1 In this study, a series of columbite materials have been studied using a range of operando and ex-situ techniques. Samples were prepared using both solid-state synthesis2 and solution methods. Ex-situ X-ray diffraction and scanning electron microscopy were used to characterise the columbites prior to electrochemical testing. Operando X-ray absorption spectroscopy and operando Raman studies have been used to probe the changes in oxidation state of the transition metals and local structure upon charge/discharge. References Yang, X. Zhao, F. Liao, Q. Cheng, L. Mao, H. Fa and L. Chen, Sustain. Energy Fuels, 2021, 5, 3039Garía Alvarado, A. Orera, J. Canales-Vázquez, and J. T. S. Irvine, Chem. Mater., 2006, 18, 3827-3834 Figure 1