X-RAY SPECTROMETRY, cilt.51, sa.5-6, ss.422-443, 2022 (SCI-Expanded)
X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS) and X-ray Raman scattering (XRS) spectroscopy are the element-specific tools providing local electronic and chemical structure insights. XPS is widely used for qualitative/quantitative surface analysis of solids and replaced by synchrotron-based ambient pressure-XPS and hard-XPS to benefit from the advantages of near-ambient pressures and hard X-rays to study complex sample environments. XAS is a well-established soft and hard X-ray probe to examine the coordination, spin and oxidation states in solids, liquids and gases with high resolutions and short data acquisition time. XRS, using the hard X-rays of similar to 10 keV, is preferred to conventional XAS and XPS in the study of soft X-ray absorption edges such as C, O, Li Kedges bulk-sensitively in vacuum-free medium for energy storage systems during working operations, inner Earth elements under realistic conditions, probing chemical and biological reactions in the liquid phase, C speciation in archeological and paleontological samples and direct tomography. In this study, first the basics of XPS, XAS, and XRS techniques with their advantages and limitations are introduced to provide a general overview. In the Results and Discussion, the particular emphasis is given to the comparison of XPS, XAS, and XRS with the interpretation of the spectroscopic signatures for organic carbonate-based electrolytes. The computed C 1 s binding energy shifts for ethylene carbonate (EC), propylene carbonate (PC), dimethyl carbonate (DMC), and diethyl carbonate (DEC) are presented to discuss the XPS peak assignments and the performed C K-edge XRS measurements of 1 M LiPF6 in DMC and EC are given for a detailed discussion of the XRS spectra. C 1 s XPS, C K-edge XAS, and XRS of PC from the literature are discussed to interpret the spectra of each technique comparatively.