A Laboratory-based Hard X-ray Monochromator for High-Resolution X-ray Emission Spectroscopy and X-ray Absorption Near Edge Structure Measurements

Abstract

We report the development of a laboratory-based Rowland-circle monochromator that incorporates a low poer x-ray (bremsstrahlung) tube source, a spherically-bent crystal analyzer (SBCA), and an energy-resolving solid-state detector. This relatively inexpensive, introductory level instrument achieves 1-eV energy resolution for photon energies of 5 keV to 10 keV while also dmeonstrating a net efficiency previously seen only in laboratory monochromators having much coarser energy resolution. Despite the use of only a compact, air-cooled 10 W x-ray tube, we find count rates for nonresonant x-ray emission spectroscopy (XES) comparable to those achived at monochromatized spectroscopy beamlines at synchrotron light sources. For x-ray absorption near edge structure (XANES), the monochromatized flux is small (due to the use of a low-powered x-ray generator) but still useful for routine transmission-mode studies of concentrated samples. These results indicate that upgrading to a standard commercial high-powered line-focused x-ray tube or rotating anode x-ray generator would result in monochromatized fluxes of order 10^6 to 10^7 photons/s with no loss in energy resolution. This work establishes core technical capabilities for a rejuvenation of laboratory-based x-ray spectroscopies that could have special relevance for contemporary research on catalytic or electrical energy storage systems using transition-metal, lanthanide, or noble-metal active species.

arXiv commentSubmitted to the Review of Scientific Instruments

Cited by in corpus (10)

• An Improved Laboratory-Based XAFS and XES Spectrometer for Analytical Applications in Materials Chemistry Research
• Laboratory von Hámos X-ray Spectroscopy for Routine Sample Characterization
• High energy-resolution x-ray spectroscopy at ultra-high dilution with spherically bent crystal analyzers of 0.5 m radius
• Johann-type laboratory-scale X-ray absorption spectrometer with versatile detection modes
• Benchmark Results and Theoretical Treatments for Valence-to-Core X-ray Emission Spectroscopy in Transition Metal Compounds
• A Compact Dispersive Refocusing Rowland Circle X-ray Emission Spectrometer for Laboratory, Synchrotron, and XFEL Applications
• A Modern Laboratory XAFS Cookbook
• Benchtop Nonresonant X-ray Emission Spectroscopy: Coming Soon to Laboratories and XAS Beamlines Near You?
• Double-Ionization Satellites in the X-ray Emission Spectrum of Ni Metal
• In situ and operando laboratory X-ray absorption spectroscopy at high temperature and controlled gas atmosphere with a plug-flow fixed-bed cell