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 approach was first validated by measurements on powder V₂O₅, used as a commercial standard, and then demonstrated on lithium ion battery materials, that is, LiₓV₂O₅ 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 CVD-grown (400) single crystal diamond and 285 mm for LiₓV₂O₅. Our results demonstrate the inexpensive and straightforward implementation of coupled XPS-Raman spectroscopy for combined surface/bulk analysis.
