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Versailles Project on Advanced Materials and Standards interlaboratory study on intensity calibration for x-ray photoelectron spectroscopy instruments using low-density polyethylene

Reed, B P; Cant, D J H; Spencer, S J; Carmona-Carmona, A J; Bushell, A; Herrera-Gómez, A; Kurokawa, A; Thissen, A; Thomas, A G; Britton, A J; Bernasik, A; Fuchs, A; Baddorf, A P; Bock, B; Theilacker, B; Cheng, B; Castner, D G; Morgan, D J; Valley, D; Willneff, E A; Smith, E F; Nolot, E; Xie, F; Zorn, G; Smith, G C; Yasufuku, H; Fenton, J L; Chen, J; Counsell, J D P; Radnik, J; Gaskell, K J; Artyushkova, K; Yang, L; Zhang, L; Eguchi, M; Walker, M; Hajdyła, M; Marzec, M M; Linford, M R; Kubota, N; Cortazar-Martínez, O; Dietrich, P; Satoh, R; Schroeder, S L M; Avval, T G; Nagatomi, T; Fernandez, V; Lake, W; Azuma, Y; Yoshikawa, Y; Shard, A G (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 ISSN 0734-2101

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Abstract

We report the results of a VAMAS (Versailles Project on Advanced Materials and Standards) inter-laboratory 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 which are corrected for different instrument geometries were developed using data provided by participants in this study. The equations to generate these geometry-corrected LDPE reference spectra are also reported. Using these new reference spectra, an LDPE 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 ~3.4% and a systematic deviation of ±7.6% on average across all participants. For spectra recorded at high pass energies (¿ 90 eV), values of absolute offset and systematic deviation are ~5.9 % and ± 5.8 % respectively, whereas for spectra collected at lower pass energies (< 90 eV), values of absolute offset and systematic deviation are ~3.1 % and ± 12.1 % respectively; low pass energy spectra perform worse than the global average due to diminished count rates and signal-to-noise. 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 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.

Item Type: Article
Keywords: X-ray photoelectron spectroscopy, VAMAS, intensity calibration, transmission function
Subjects: Nanoscience > Surface and Nanoanalysis
Divisions: Chemical & Biological Sciences
Identification number/DOI: 10.1116/6.0000577
Last Modified: 04 May 2021 14:38
URI: http://eprintspublications.npl.co.uk/id/eprint/9117

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