Practical guides for x-ray photoelectron spectroscopy: First steps in planning, conducting, and reporting XPS measurements
Environmental Molecular Sciences Laboratory1, University of Surrey2, University of Maryland, College Park3, University of Illinois at Urbana–Champaign4, Brigham Young University5, National Institute of Standards and Technology6, National Physical Laboratory7, University of Washington8, General Electric9
08 Apr 2019-Journal of Vacuum Science and Technology (J Vac Sci Technol A)-Vol. 37, Iss: 3, pp 031401
TL;DR: This first guide outlines steps appropriate for determining whether XPS is capable of obtaining the desired information, identifies issues relevant to planning, conducting and reporting an XPS measurement, and identifies sources of practical information for conducting XPS measurements.
Abstract: Over the past three decades, the widespread utility and applicability of X-ray photoelectron spectroscopy (XPS) in research and applications has made it the most popular and widely used method of surface analysis. Associated with this increased use has been an increase in the number of new or inexperienced users which has led to erroneous uses and misapplications of the method. This article is the first in a series of guides assembled by a committee of experienced XPS practitioners that are intended to assist inexperienced users by providing information about good practices in the use of XPS. This first guide outlines steps appropriate for determining whether XPS is capable of obtaining the desired information, identifies issues relevant to planning, conducting and reporting an XPS measurement, and identifies sources of practical information for conducting XPS measurements. Many of the topics and questions addressed in this article also apply to other surface-analysis techniques.
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TL;DR: X-ray photoelectron spectroscopy is an indispensable technique in modern materials science for the determination of chemical bonding as evidenced by more than 10000 XPS papers published annually.
Abstract: X-ray photoelectron spectroscopy (XPS) is an indispensable technique in modern materials science for the determination of chemical bonding as evidenced by more than 10 000 XPS papers published annually. A literature survey reveals that in the vast majority of cases an incorrect referencing of the binding energy scale is used, neglecting warnings that have been formulated from the early days of the technique. Consequences for the data reliability are disastrous and decades of XPS work require revisiting. The purpose of this Viewpoint is to highlight the existing problems, review the criticism and suggest ways forward.
458 citations
01 Sep 2021
TL;DR: The methodology presented within this work is a result of years of interactions between many junior and senior X-ray Photoelectron Spectroscopy (XPS) users operating within the CasaXPS spectral processing and interpretation program framework.
Abstract: The methodology presented within this work is a result of years of interactions between many junior and senior X-ray Photoelectron Spectroscopy (XPS) users operating within the CasaXPS spectral processing and interpretation program framework. In particular, discussions arising from a series of workshops have been a significant source for developing the overall XPS data processing concept and are the motivation for creating this work. These workshops organized by the Institut des Materiaux Jean Rouxel (IMN), Nantes gather both experienced and novice users of XPS for a week of discourse in conceptual experiment design and the resulting data processing. However, the framework constructed and utilized within these workshops encouraged the dissemination of knowledge beyond XPS data analysis and emphasized the importance of a multi-disciplinary collaborative approach to surface analysis problem-solving. The material presented here embodies data treatment originating from data made available to the first CNRS Thematic Workshop presented at Roscoff 2013. The methodology described here has evolved over the subsequent workshops in 2016 and 2019 and currently represents the philosophy used in CasaXPS spectral data processing paradigm.
290 citations
TL;DR: In this paper, a review of the use of X-ray diffraction, Raman spectroscopy, electron microscopy/spectroscopy and a number of other techniques to understand if the precursor is suitable for MXene synthesis, confirm successful synthesis of MXene, and finally determine its composition, structure and properties.
193 citations
TL;DR: In this paper , the authors present a comprehensive tutorial written in the form of a step-by-step guide starting from experimental planning, through sample selection and handling, instrument setup, data acquisition, spectra analysis, and results presentation.
Abstract: There is a growing concern within the surface science community that the massive increase in the number of XPS articles over the last few decades is accompanied by a decrease in work quality including in many cases meaningless chemical bond assignment. Should this trend continue, it would have disastrous consequences for scientific research. While there are many factors responsible for this situation, the lack of insight of physical principles combined with seeming ease of XPS operation and insufficient training are certainly the major ones. To counter that, we offer a comprehensive tutorial written in the form of a step-by-step guide starting from experimental planning, through sample selection and handling, instrument setup, data acquisition, spectra analysis, and results presentation. Six application examples highlight the broad range of research questions that can be answered by XPS. The topic selection and the discussion level are intended to be accessible for novices yet challenging possible preconceptions of experienced practitioners. The analyses of thin film samples are chosen for model cases as this is from where the bulk of XPS reports presently emanate and also where the author's key expertise lies. At the same time, the majority of discussed topics is applicable to surface science in general and is, thus, of relevance for the analyses of any type of sample and material class. The tutorial contains ca. 160 original spectra and over 290 references for further reading. Particular attention is paid to the correct workflow, development of good research practices, and solid knowledge of factors that impact the quality and reliability of the obtained information. What matters in the end is that the conclusions from the analysis can be trusted. Our aspiration is that after reading this tutorial each practitioner will be able to perform error-free data analysis and draw meaningful insights from the rich well of XPS.
143 citations
TL;DR: In this paper, the conditions for reliable X-ray photoelectron spectroscopy (XPS) analysis were checked by studying ion irradiation effects for single-phase Group IVB transition metal (IVB-TM) boride, carbide, nitride, and oxide thin film specimens.
88 citations
References
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Book•
01 Jan 1983
4,689 citations
2,609 citations
Book•
25 Apr 2003
TL;DR: In this article, the authors present a comparison of XPS and AES with other analytical techniques. But they do not discuss the application of the XPS in the field of materials science.
Abstract: Preface. Acknowledgements. Electron Spectroscopy: Some Basic Concepts. Electron Spectrometer Design. The Electron Spectrum: Qualitative and Quantitative Interpretation. Compositional Depth Profiling. Applications of Electron Spectroscopy in Materials Science. Comparison of XPS and AES with Other Analytical Techniques. Glossary. Bibliography.
890 citations
Book•
01 Jan 1983
849 citations
"Practical guides for x-ray photoele..." refers background in this paper
...8 extended volumes, 36 and journal articles covering specific topics such as sample preparation,(37) quantification,(38) data analysis,(39) curve fitting,(40-42) spectra interpretation(43) and information available from XPS valence-band spectra.(29,19) Books and journal articles also focus on specific applications of XPS that include materials science,(43-45) nanoparticles, 46 corrosion,(47) biological samples, 10 and environmental surfaces....
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Book•
20 Dec 2011
Abstract: This book introduces readers interested in the field of X-ray Photoelectron Spectroscopy (XPS) to the practical concepts in this field. The book first introduces the reader to the language and concepts used in this field and then demonstrates how these concepts are applied. Including how the spectra are produced, factors that can influence the spectra (all initial and final state effects are discussed), how to derive speciation, volume analysed and how one controls this (includes depth profiling), and quantification along with background substraction and curve fitting methodologies.
323 citations