Reporting the methodology of your data acquisition and analysis is highly important in any publication, be it a research paper, thesis or internal report.
The inclusion of experimental parameters and conditions allow the reader to make an informed decision to the data presented and highlight any possible issues which may have been overlooked (e.g. analysis induced damage).
An example of a poor description can be seen in the righthand panel.
X-ray photoelectron spectroscopy (XPS) analysis was conducted on a <insert system name> with a monochromatized Al X-ray source.
Such a description is far to commonly encountered in journal articles. Here we know nothing about X-ray power, the data step size, pass energy for analysis, was charge compensation used, how the data was calibrated or how analysed – what software, sensitivity factors employed etc.
A better example would be something more comprehensive such as that to the right written for a Kratos Axis Ultra DLD spectrometer.
It is evident from the this experimental that a lot more information is provided. The reader can now make an informed decision on the data based on having knowledge of the acquisition parameters, the pass energy which would affect any peak fitting performed for example. Additionally, we have an idea of the software and methods used for quantification also.
X-ray Photoelectron Spectroscopy (XPS) analysis was performed using a Kratos Axis Ultra DLD (Kratos, Manchester, UK) using a monochromatic Al Ka X-ray source (10 mA x 12 kV = 120 W). The samples were mounted using double sided scotch tape placed on glass slide and attached using copper clips to the sample bar, the glass slide ensured the samples were floated from the spectrometer. The base pressure of the spectrometer was 5×10-10 Torr, rising to ca. 1×10-9 Torr during analysis.
High resolution spectra were collected at a pass energy of 40 eV, with a step size of 0.1 eV over a typical energy window of 20 – 30 eV, depending on the element. Survey spectra were recoded at a pass energy of 150 eV, using a step size of 1 eV over the energy range -5 – 1350 eV. All data was collected in the Hybrid mode using a slot aperture resulting in an analysis area of 700 x 300 microns. The system resolution at 40 eV pass energy is 0.68 eV, as measured by the FWHM of the Ag(3d5/2) peak for sputter cleaned metallic silver.
Charge compensation was performed using low energy electrons coupled with a magnetic immersion lens. The spectra were then subsequently calibrated to their corresponding C(1s) line of adventitious carbon taken to be 284.8 eV.
Data was analysed using CasaXPS (v2.3.25) using Kratos RSF’s which are modified Wagner factors. All data was transmission corrected in the analysis software and analysed using a Shirley type background. Where performed, fitting was acheived using lineshapes derived from bulk standards recorded on the same spectrometer using the LA peak shape in CasaXPS,