Prospect of making XPS a high-throughput analytical method illustrated for a CuxNi1-xOy combinatorial material library

Combinatorial material science crucially depends on robust, high-throughput characterization methods. While X-ray photoelectron spectroscopy (XPS) may provide detailed information about chemical and electronic properties, it is a time-consuming technique and, therefore, is not viewed as a high-throughput method. Here we present preliminary XPS data of 169 measurement spots on a combinatorial 72 x 72 cm(2) CuxNi1-xOy compositional library to explore how characterization and evaluation routines can be optimized to improve throughput in XPS for combinatorial studies. In particular, two quantification approaches are compared. We find that a simple integration (of XPS peak regions) approach is suited for fast evaluation of, in the example system, the [Cu]/([Cu] + [Ni]) ratio. Complementary to that, the time-consuming (XPS peak-) fit approach provides additional insights into chemical speciation and oxidation state changes, without a large deviation of the [Cu]/([Cu] + [Ni]) ratio. This insight suggests exploiting the fast integration approach for 'real time' analysis during XPS data collection, paving the way for an 'on-the-fly' selection of points of interest (i.e., areas on the sample where sudden composition changes have been identified) for detailed XPS characterization. Together with the envisioned improvements when going from laboratory to synchrotron-based excitation sources, this will shorten the analysis time sufficiently for XPS to become a realistic characterization option for combinatorial material science.

Automated summary

Combinatorial material science relies heavily on high-throughput characterization methods. X-ray photoelectron spectroscopy (XPS) is evaluated as a potential method for combinatorial studies. It is found that a simple integration approach is suitable for fast evaluation of the [Cu]/([Cu]+[Ni]) ratio, while the time-consuming peak fit approach provides additional insights into chemical speciation and oxidation state changes. These findings suggest the use of the integration approach for real-time analysis and pave the way for detailed XPS characterization.