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Register a new userSimultaneous ambient pressure X-ray photoelectron spectroscopy and grazing incidence X-ray scattering in gas environments
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We have developed an experimental system to simultaneously observe surface structure, morphology, composition, chemical state, and chemical activity for samples in gas phase environments. This is accomplished by simultaneously measuring X-ray photoelectron spectroscopy (XPS) and grazing incidence X-ray scattering (GIXS) in gas pressures as high as the multi-Torr regime, while also recording mass spectrometry. Scattering patterns reflect near-surface sample structures from the nano- to the meso-scale. The grazing incidence geometry provides tunable depth sensitivity while scattered X-rays are detected across a broad range of angles using a newly designed pivoting-UHV-manipulator for detector positioning. At the same time, XPS and mass spectrometry can be measured, all from the same sample spot and in ambient conditions. To demonstrate the capabilities of this system, we measured the chemical state, composition, and structure of Ag-behenate on a Si(001) wafer in vacuum and in O$_2$ atmosphere at various temperatures. These simultaneous structural, chemical, and gas phase product probes enable detailed insights into the interplay between structure and chemical state for samples in gas phase environments. The compact size of our pivoting-UHV-manipulator makes it possible to retrofit this technique into existing spectroscopic instruments installed at synchrotron beamlines. Because many synchrotron facilities are planning or undergoing upgrades to diffraction limited storage rings with transversely coherent beams, a newly emerging set of coherent X-ray scattering experiments can greatly benefit from the concepts we present here.
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Photoelectron spectroscopy (PES) and microscopy are highly demanded for exploring morphologically complex solid-gas and solid-liquid interfaces under realistic conditions, but the very small electron mean free path inside the dense media imposes serious experimental challenges. Currently, near ambient pressure PES is conducted using sophisticated and expensive electron energy analyzers coupled with differentially pumped electron lenses. An alternative economical approach proposed in this report uses ultrathin graphene membranes to isolate the ambient sample environment from the PES detection system. We demonstrate that the graphene membrane separating windows are both mechanically robust and sufficiently transparent for electrons in a wide energy range to allow PES of liquid and gaseous water. The reported proof-of-principle experiments also open a principal possibility to probe vacuum-incompatible toxic or reactive samples enclosed inside the hermetic environmental cells.
The GALAXIES beamline at the SOLEIL synchrotron is dedicated to inelastic x-ray scattering (IXS) and photoelectron spectroscopy (HAXPES) in the 2.3-12 keV hard x-ray range. These two techniques offer powerful, complementary methods of characterization of materials with bulk sensitivity, chemical and orbital selectivity, resonant enhancement and high resolving power. After a description of the beamline components and endstations, we address the beamline performances through a selection of recent works both in the solid and gas phases and using either IXS or HAXPES approaches. Prospects for studies on liquids are discussed.
We present here an experimental set-up to perform simultaneously measurements of surface plasmon resonance (SPR) and X-ray absorption spectroscopy (XAS) in a synchrotron beamline. The system allows measuring in situ and in real time the effect of X-ray irradiation on the SPR curves to explore the interaction of X-rays with matter. It is also possible to record XAS spectra while exciting SPR in order to detect the changes in the electronic configuration of thin films induced by the excitation of surface plasmons. Combined experiments recording simultaneously SPR and XAS curves while scanning different parameters can be carried out. The relative variations in the SPR and XAS spectra that can be detected with this set-up ranges from 10-3 to 10-5, depending on the particular experiment.
We describe the concepts and technical realization of the high-resolution soft-X-ray beamline ADRESS operating in the energy range from 300 to 1600 eV and intended for Resonant Inelastic X-ray Scattering (RIXS) and Angle-Resolved Photoelectron Spectroscopy (ARPES). The photon source is an undulator of novel fixed-gap design where longitudinal movement of permanent magnetic arrays controls not only the light polarization (including circular and 0-180 deg rotatable linear polarizations) but also the energy without changing the gap. The beamline optics is based on the well-established scheme of plane grating monochromator (PGM) operating in collimated light. The ultimate resolving power E/dE is above 33000 at 1 keV photon energy. The choice of blazed vs lamellar gratings and optimization of their profile parameters is described. Due to glancing angles on the mirrors as well as optimized groove densities and profiles of the gratings, high photon flux is achieved up to 1.0e13 photons/s/0.01%BW at 1 keV. Ellipsoidal refocusing optics used for the RIXS endstation demagnifies the vertical spot size down to 4 um, which allows slitless operation and thus maximal transmission of the high-resolution RIXS spectrometer delivering E/dE better than 11000 at 1 keV photon energy. Apart from the beamline optics, we give an overview of the control system, describe diagnostics and software tools, and discuss strategies used for the optical alignment. An introduction to the concepts and instrumental realization of the ARPES and RIXS endstations is given.
The optics of a number of future X-ray telescopes will have very long focal lengths (10 - 20 m), and will consist of a number of nested/stacked thin, grazing-incidence mirrors. The optical quality characterization of a real mirror can be obtained via profile metrology, and the Point Spread Function of the mirror can be derived via one of the standard computation methods. However, in practical cases it can be difficult to access the optical surfaces of densely stacked mirror shells, after they have been assembled, using the widespread metrological tools. For this reason, the assessment of the imaging resolution of a system of mirrors is better obtained via a direct, full-illumination test in X-rays. If the focus cannot be reached, an intra-focus test can be performed, and the image can be compared with the simulation results based on the metrology, if available. However, until today no quantitative information was extracted from a full-illumination, intra-focal exposure. In this work we show that, if the detector is located at an optimal distance from the mirror, the intensity variations of the intra-focal, full-illumination image in single reflection can be used to reconstruct the profile of the mirror surface, without the need of a wavefront sensor. The Point Spread Function can be subsequently computed from the reconstructed mirror shape. We show the application of this method to an intra-focal (8 m distance from mirror) test performed at PANTER on an optical module prototype made of hot-slumped glass foils with a 20 m focal length, from which we could derive an expected imaging quality near 16 arcsec HEW.
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