http://lib.tkk.fi/Diss/2005/isbn9512278804/article5.pdf

Chemical state quantification of iron and chromium oxides using XPS: the effect of the background subtraction method

The Shirley background revised

Composition and chemical state of the ions of aluminium-oxide films formed by thermal oxidation of aluminium

This guide is intended for both the novice in x-ray photoelectron spectroscopy (XPS) as well as users with some experience. XPS is one of the most widely used methods to characterize surface nanostructured samples, and XPS is now also commonly accessible to most material scientists through XPS facility centers. It is, therefore, increasingly used as a routine analysis technique to complement other techniques. This has led to an increase in the number of users who may not have a full understanding of the details of XPS and consequently must rely on the report provided by the XPS center. The purpose of this practical guide on the aspects of quantitative XPS is first to put the reader in a position to be able to understand and judge the meaning and possible errors in atomic concentrations based on analysis of peak intensities, which is the standard way quantitative XPS is reported. We discuss different ways to improve the analysis. This is attained by giving the reader a good understanding of how the intensities in the peak and the background of inelastically scattered electrons are linked together through the depth distribution of atoms. We then explore how this can be applied to greatly increase the capabilities of XPS to more accurately determine the composition and structure of surfaces on the nanoscale. This is possible at different levels of sophistication. We first see how a visual inspection of the XPS survey spectrum can be applied to get a quick rough indication of the structure. Next, we go through other more quantitative methods that are being used. The practical application of these techniques is illustrated by several examples.

https://avs.scitation.org/doi/pdf/10.1116/6.0000661

Practical guide to the use of backgrounds in quantitative XPS

Photoelectron and Auger peaks are central to most of the important uses of x-ray photoelectron spectroscopy (XPS), and thus, they receive the most attention in many types of analysis. Quantitative chemical analysis using XPS requires the assessment of the intensities of the photoemission peaks of the elements detected. Determination of peak intensities requires separation of the photoelectron peak signals from the background on which the peaks rest. For the determination of peak area intensities, the background is subtracted from overall signal intensity. The spectral background is also critical when peak fitting is used to determine intensities of overlapping peaks, and the model of background used in this process can impact the results. In addition to the impact on quantitative analysis, information about the depth distribution of elements in the near surface region can often be obtained by visual inspection of the background and quantified using appropriate modeling. This introductory guide provides some basic information about backgrounds in the XPS analysis, describes the types of background models that are commonly used, suggests some of their strengths and weaknesses, and provides examples of their use and misuse. Although the fundamental nature of some components of the background signals in XPS is not understood, indicating that none of the models in use are fully correct and the area is subject to active research, appropriate good practices have been established for most routine analysis. The guide describes good practices, identifies errors that frequently appear in the literature, and uses examples to demonstrate the impacts of background selections on determinations of peak intensities.

Introductory guide to backgrounds in XPS spectra and their impact on determining peak intensities

In the present interlaboratory comparison, the consistency and validity of the Shirley, straight-line and Tougaard methods for determination of peak intensities from measured XPS spectra have been studied by analysis of data on Au and Ni taken at eight laboratories. The reproducibility of the individual measuring systems was determined to be 2–6%. The RMS scatter around their mean values of the ratio of the peak intensity to the Au 4d peak intensity was 6% for the Tougaard method, 9–10% for the Shirley method and 8–9% for the straight-line method. The increase in root mean square (RMS) scatter of data due to data being recorded in different laboratories amounts to 3–4%, independent of the method applied for background correction. The RMS deviation from theory of intensity ratios of peaks from Ni and Au to the Au 4d peak intensity is 14% for the Tougaard method, 33% for the Shirley method and 31% for the straight-line method. The absolute accuracy of the methods cannot be established to better than the accuracy on the theoretical peak intensity ratios and the uncertainty in the energy dependence of the analyser response function. It is, however, reasonable to expect the combined uncertainty of these factors to be at least 10–15%. The peak intensity ratios obtained with the Tougaard method then falls within the expected accuracy of the theoretical ratios.

Intercomparison of algorithms for background correction in XPS

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Intercomparison of algorithms for background correction in XPS