Versailles Project on Advanced Materials and Standards interlaboratory study on intensity calibration for x-ray photoelectron spectroscopy instruments using low-density polyethylene
Smith, Graham C.
AffiliationNational Physical Laboratory; CINVESTAV-Unidad Queretaro; Thermo Fisher Scientific (Surface Analysis); National Institute of Advanced Industrial Science and Technology; SPECS Surface Nano Analysis GmbH; University of Manchester; University of Leeds; AGH University of Science and Technology; Robert Bosch GmbH; Oak Ridge National Laboratory; Tascon GmbH; Medtronic; University of Chemical Technology; University of Washington; Cardiff University; Physical Electronics Inc.; University of Leeds; University of Nottingham; CEA-LETI; Sun Yat-sen University; GE Research; University of Chester; National Institute for Materials Science, Japan; Medtronic; Kratos Analytical Ltd; Bundesanstalt für Materialforschung und -prüfung; University of Maryland; Physical Electronics Inc.; Xi’an Jiaotong-Liverpool University; Nippon Steel Technology Co. Ltd; University of Warwick; Brigham Young University; SPECS Surface Nano Analysis GmbH; Asahi Kasei Corporation; Université de Nantes; Atomic Weapons Establishment, Aldermaston; Yazaki Corporation
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AbstractWe report the results of a Versailles Project on Advanced Materials and Standards interlaboratory study on the intensity scale calibration of x-ray photoelectron spectrometers using low-density polyethylene (LDPE) as an alternative material to gold, silver, and copper. An improved set of LDPE reference spectra, corrected for different instrument geometries using a quartz-monochromated Al Kα x-ray source, was developed using data provided by participants in this study. Using these new reference spectra, a transmission function was calculated for each dataset that participants provided. When compared to a similar calibration procedure using the NPL reference spectra for gold, the LDPE intensity calibration method achieves an absolute offset of ∼3.0% and a systematic deviation of ±6.5% on average across all participants. For spectra recorded at high pass energies (≥90 eV), values of absolute offset and systematic deviation are ∼5.8% and ±5.7%, respectively, whereas for spectra collected at lower pass energies (<90 eV), values of absolute offset and systematic deviation are ∼4.9% and ±8.8%, respectively; low pass energy spectra perform worse than the global average, in terms of systematic deviations, due to diminished count rates and signal-to-noise ratio. Differences in absolute offset are attributed to the surface roughness of the LDPE induced by sample preparation. We further assess the usability of LDPE as a secondary reference material and comment on its performance in the presence of issues such as variable dark noise, x-ray warm up times, inaccuracy at low count rates, and underlying spectrometer problems. In response to participant feedback and the results of the study, we provide an updated LDPE intensity calibration protocol to address the issues highlighted in the interlaboratory study. We also comment on the lack of implementation of a consistent and traceable intensity calibration method across the community of x-ray photoelectron spectroscopy (XPS) users and, therefore, propose a route to achieving this with the assistance of instrument manufacturers, metrology laboratories, and experts leading to an international standard for XPS intensity scale calibration.
CitationReed, B., Cant, D., Spencer, S., Carmona-Carmona, A., Bushell, A. ... Shard, A. (2020). Versailles Project on Advanced Materials and Standards interlaboratory study on intensity calibration for x-ray photoelectron spectroscopy instruments using low-density polyethylene. Journal of Vacuum Science & Technology A, 38(6), 063208. https://doi.org/10.1116/6.0000577
PublisherAmerican Vacuum Society
DescriptionThe following article appeared in Reed, B., Cant, D., Spencer, S., Carmona-Carmona, A., Bushell, A. ... Shard, A. (2020). Versailles Project on Advanced Materials and Standards interlaboratory study on intensity calibration for x-ray photoelectron spectroscopy instruments using low-density polyethylene. Journal of Vacuum Science & Technology A, 38, 063208 and may be found at https://doi.org/10.1116/6.0000577. This article may be downloaded for personal use only. Any other use requires prior permission of the author and AIP Publishing.
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