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X-ray Compton spectroscopy is one of the few direct probes of the electron momentum distribution of bulk materials in ambient and operando environments. We report high-resolution inelastic x-ray scattering experiments with high momentum and energy transfer performed at a storage-ring-based high-energy x-ray light source facility using an x-ray transition-edge sensor (TES) microcalorimeter detector. The performance was compared with a silicon drift detector (SDD), an energy-resolving semiconductor detector, and Compton profiles were measured for lithium and cobalt oxide powders relevant to lithium-ion battery research. Spectroscopic analysis of the measured Compton profiles demonstrates the high-sensitivity to the low-Z elements and oxidation states. The line shape analysis of the measured Compton profiles in comparison with computed Hartree-Fock profiles is usually limited by the resolution of the semiconductor detector. We have characterized an x-ray TES microcalorimeter detector for high-resolution Compton scattering experiments using a bending magnet source at the Advanced Photon Source with a double crystal monochromator, providing monochromatic photon energies near 27.5 keV. The momentum resolution below 0.16 atomic units (a.u.) was measured, yielding an improvement of more than a factor of 7 over a state-of-the-art SDD for the same scattering geometry. Furthermore, the lineshapes of narrow valence and broad core electron profiles of sealed lithium metal were clearly resolved using an x-ray TES compared to smeared and broadened lineshapes observed when using the SDD. High-resolution Compton scattering using the energy-resolving area detector shown here presents new opportunities for spatial imaging of electron momentum distributions for a wide class of materials with applications ranging from electrochemistry to condensed matter physics.

Electric noise measurements can give useful information on the conduction mechanisms and the dynamic behaviors of the charge carriers in new materials. However, it is well known that not all the electronic fluctuations are originated from the material itself, but some noise sources depend on the experimental procedures used for the measurements. In this article, an experimental technique to reduce "external" noise components, not associated with the bulk system, is presented. The proposed method is based on measurements of the voltage spectral density, using in sequence a four- and a two-probe technique. From the measurements it is possible to evaluate the contact and the background noise contributions and to recover the real spectral trace of the sample. The proposed procedure is demonstrated to be valid in spectral density measurements performed on La(0.7)Sr(0.3)MnO(3) thin films.