Coupling Long‐Range Raman with X‐Ray Photoelectron Spectroscopy for Complementary Bulk and Surface Characterization of Battery Materials

Abstract

For the combined surface and bulk characterization of functional powder materials, we report on the direct coupling of Raman spectroscopy with X-ray photoelectron spectroscopy (XPS) within one setup, avoiding the influence of different sample states and measurement environments. Our approach is based on the Raman integration into the XPS analysis chamber, employing a long-range camera objective connected to a portable 532 nm Raman spectrometer. For optimization of the measurement geometry, a (400) single crystal (SC), chemical vaper deposition (CVD)-grown diamond was employed. The applicability of the combined XPS-Raman spectroscopy ap-proach was first validated by measurements on powder V 2 O 5 , used as a commercial standard, and then demonstrated on lithium ion battery materials, that is, Li x V 2 O 5 lithium pentoxides. The transferability to other XPS systems is strongly facilitated by the long-range Raman-spectroscopic approach, which allowed for Raman analysis over a distance of 320 mm for the CVDgrown (400) single crystal diamond and 285 mm for Li x V 2 O 5 . Our results demonstrate the inexpensive and straightforward implementation of coupled XPS-Raman spectroscopy for combined surface/bulk analysis.

Understanding Nanoscale Interactions between Minerals and Microbes: Opportunities for Green Remediation of Contaminated Sites

“…50 Structured line illumination Raman microscopy combined with X-ray photoelectron spectroscopy, and synchrotron-based X-ray fluorescence spectroscopy combined with X-ray absorption spectroscopy, are capable of showing the mapping of chemical components and valencestate of metals at the microbe−mineral interfaces. 51,52 In situ attenuated total reflection Fourier transform infrared spectroscopy with two-dimensional correlation analysis allows the identification of the specific functional groups of cell membrane or biomolecules forming complexes with minerals. 53,54 The charge transfer and mass transfer at microbe−mineral interfaces are key processes to be characterized and modulated for enhanced remediation.…”

“…Atomic force microscopy gains insights on the intensity of the hydrodynamic forces, and super-resolution microscopy such as correlated light and electron microscopy directly visualizes the physical contact between microbes and minerals at nanoscale resolutions. , The specific biotic moieties (e.g., proteins in cell membranes) binding to mineral surfaces can be identified with super or high-resolution fluorescence microscopy using fluorophores to stain targeted structures or sites . Structured line illumination Raman microscopy combined with X-ray photoelectron spectroscopy, and synchrotron-based X-ray fluorescence spectroscopy combined with X-ray absorption spectroscopy, are capable of showing the mapping of chemical components and valence-state of metals at the microbe–mineral interfaces. , In situ attenuated total reflection Fourier transform infrared spectroscopy with two-dimensional correlation analysis allows the identification of the specific functional groups of cell membrane or biomolecules forming complexes with minerals. , …”