A combined X-ray and scanning tunneling microscopy (STM) instrument is presented that enables the local detection of X-ray absorption on surfaces in a gas environment. To suppress the collection of ion currents generated in the gas phase, coaxially shielded STM tips were used. The conductive outer shield of the coaxial tips can be biased to deflect ions away from the tip core. When tunneling, the X-ray-induced current is separated from the regular, ‘topographic’ tunneling current using a novel high-speed separation scheme. We demonstrate the capabilities of the instrument by measuring the local X-ray-induced current on Au(1 1 1) in 800 mbar Ar.

Within the last three decades Scanning Probe Microscopy has been developed to a powerful tool for measuring surfaces and their properties on an atomic scale such that users can be found nowadays not only in academia but also in industry. This development is still pushed further by researchers, who continuously exploit new possibilities of this technique, as well as companies that focus mainly on the usability. However, although imaging has become significantly easier, the time required for a safe approach (without unwanted tip-sample contact) can be very time consuming, especially if the microscope is not equipped or suited for the observation of the tip-sample distance with an additional optical microscope. Here we show that the measurement of the absolute tip-sample capacitance provides an ideal solution for a fast and reliable pre-approach. The absolute tip-sample capacitance shows a generic behavior as a function of the distance, even though we measured it on several completely different setups. Insight into this behavior is gained via an analytical and computational analysis, from which two additional advantages arise: the capacitance measurement can be applied for observing, analyzing, and fine-tuning of the approach motor, as well as for the determination of the (effective) tip radius. The latter provides important information about the sharpness of the measured tip and can be used not only to characterize new (freshly etched) tips but also for the determination of the degradation after a tip-sample contact/crash.

In situ surface X-ray diffraction and transmission electron microscopy at 1 bar show massive material transport of platinum during high-temperature NO reduction with H₂. A Pt(110) single-crystal surface shows a wide variety of surface reconstructions and extensive faceting of the surface. Pt nanoparticles change their morphology depending on the gas composition: They are faceted in hydrogen-rich environments, but are more spherical in NO-rich environments, indicating the formation of vicinal surfaces. We conclude that high coverage of NO combined with sufficient mobility of platinum surface atoms is the driving force for the formation of steps on both flat surfaces and nanoparticles. Since the steps that are introduced provide strongly coordinating adsorption sites with potential catalytic benefits, this may be of direct practical relevance for the performance of catalytic nanoparticles under high-pressure conditions.