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We have developed an experimental system to simultaneously observe surfacestructure, morphology, composition, chemical state, and chemical activity forsamples in gas phase environments. This is accomplished by simultaneouslymeasuring X-ray photoelectron spectroscopy (XPS) and grazing incidence X-rayscattering (GIXS) in gas pressures as high as the multi-Torr regime, while alsorecording mass spectrometry. Scattering patterns reflect near-surface samplestructures from the nano- to the meso-scale. The grazing incidence geometryprovides tunable depth sensitivity while scattered X-rays are detected across abroad range of angles using a newly designed pivoting-UHV-manipulator fordetector positioning. At the same time, XPS and mass spectrometry can bemeasured, all from the same sample spot and in ambient conditions. Todemonstrate the capabilities of this system, we measured the chemical state,composition, and structure of Ag-behenate on a Si(001) wafer in vacuum and inO$_2$ atmosphere at various temperatures. These simultaneous structural,chemical, and gas phase product probes enable detailed insights into theinterplay between structure and chemical state for samples in gas phaseenvironments. The compact size of our pivoting-UHV-manipulator makes itpossible to retrofit this technique into existing spectroscopic instrumentsinstalled at synchrotron beamlines. Because many synchrotron facilities areplanning or undergoing upgrades to diffraction limited storage rings withtransversely coherent beams, a newly emerging set of coherent X-ray scatteringexperiments can greatly benefit from the concepts we present here.

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