Sample handling, preparation and mounting for XPS and other surface analytical techniques

Abstract

Sample preparation and mounting are important aspects of x-ray photoelectron spectroscopy (XPS) analysis. New users do not know many techniques that are familiar to analysts with years of experience, and these observations and "tricks of the trade" are typically not published. This article is intended to convey the experience of the authors in this field who have creatively analyzed a wide range of samples. Samples can include solids, powders, fibers, porous solids, and even liquids. This information is also important to anyone submitting samples for analysis, since the preparation of the sample may influence the usefulness of the data collected. These techniques are also applicable to other surface analysis methods.

Imaging of nitrogen fixation at lithium solid electrolyte interphases via cryo-electron microscopy

“…Then, the XPS sample holder was stored inside an air-free transfer vessel that enables direct transfer to the XPS sample introduction chamber without air exposure. 47 XPS spectra were collected using a Physical Electronics Versaprobe II X-ray Photoelectron Spectrometer.…”

Silica: ubiquitous poison of metal oxide interfaces

“…Near ambient pressure XPS promises studies under more realistic operation conditions. 70,71 A large number of operando methods have been developed to examine SOFC/SMOX. [72][73][74] In the field of SMOX based gas sensing, operando x-ray adsorption spectroscopy is used to study the oxidations state and structural parameters of surface additives on the interaction with the surrounding atmosphere.…”

Advances in studying interfacial reactions in rechargeable batteries by photoelectron spectroscopy

“…For example, many plastics or adhesive tapes contain silicones, which can easily migrate to the sample surface. 61 However, sometimes it is necessary to prepare samples days in advance of a synchrotron beamtime or to ship samples to a collaborator's lab for analysis, in which case it is difficult to avoid the necessity to disassemble batteries beforehand and package the samples. One particularly important study, though, demonstrated that the best method to preserve the SEI chemistry is to transport the unopened cells and perform the measurements as soon as possible after opening them.…”