Simultaneous ambient pressure x-ray photoelectron spectroscopy and grazing incidence x-ray scattering in gas environments

• Published in: Review of scientific instruments 2021-04, Vol.92 (4)
• Main Authors: Kersell, Heath, Chen, Pengyuan, Martins, Henrique, Lu, Qiyang, Brausse, Felix, Liu, Bo-Hong, Blum, Monika, Roy, Sujoy, Rude, Bruce, Kilcoyne, Arthur, Bluhm, Hendrik, Nemšák, Slavomír
• Format: Article
• Language: English
• Subjects: gas phase; goniometers; incidence geometry; mass spectrometry; OTHER INSTRUMENTATION; synchrotrons; ultra-high vacuum; x-ray photoelectron spectroscopy; x-ray scattering
• ISSN: 0034-6748; 1089-7623

We have developed an experimental system to simultaneously measure 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 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-scale to the meso-scale, and the grazing incidence geometry provides tunable depth sensitivity of structural measurements. 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 under 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 O2 atmosphere at various temperatures. These simultaneous structural, chemical, and gas phase product probes enable detailed insights into the interplay between the 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.