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

Abstract

We 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 samplemore » 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. Finally, 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.« less

Authors:
ORCiD logo [1]; ORCiD logo [1];  [1];  [2];  [3]; ORCiD logo [2]; ORCiD logo [4];  [5]; ORCiD logo [6];  [7]; ORCiD logo [8];  [9]; ORCiD logo [10];  [11];  [12];  [13]; ORCiD logo [14]; ORCiD logo [15];  [16];  [17] more »; ORCiD logo [18];  [19];  [20];  [21];  [22]; ORCiD logo [23];  [24];  [20];  [25]; ORCiD logo [26];  [27]; ORCiD logo [16];  [28]; ORCiD logo [4];  [29]; ORCiD logo [30];  [8];  [8]; ORCiD logo [31];  [29];  [2]; ORCiD logo [5];  [29]; ORCiD logo [7]; ORCiD logo [31];  [32];  [33];  [34]; ORCiD logo [4];  [35]; ORCiD logo [1] « less
+ Show Author Affiliations
  1. National Physical Laboratory, Hampton Road, Teddington TW11 0LW, United Kingdom
  2. CINVESTAV-Unidad Queretaro, Queretaro 76230, Mexico
  3. Thermo Fisher Scientific (Surface Analysis), East Grinstead RH19 1XZ, United Kingdom
  4. National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), 1-1-1 Higashi, Tsukuba, Ibaraki 305-8565, Japan
  5. SPECS Surface Nano Analysis GmbH, Voltastraße 5, 13355 Berlin, Germany
  6. School of Materials, Photon Science Institute and Sir Henry Royce Institute, Alan Turing Building, University of Manchester, Oxford Road, Manchester M13 9PL, United Kingdom
  7. Versatile X-ray Spectroscopy Facility, School of Chemical and Process Engineering, University of Leeds, Leeds LS2 9JT, United Kingdom
  8. Academic Centre for Materials and Nanotechnology, AGH University of Science and Technology, 30-059 Kraków, Poland
  9. Robert Bosch GmbH, Robert-Bosch-Campus, 71272 Renningen, Germany
  10. Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, 1 Bethel Valley Road, Oak Ridge, Tennessee 37830
  11. Tascon GmbH, Mendelstr. 17, D-48149 Münster, Germany
  12. Medtronic, 710 Medtronic Parkway, LT240, Fridley, Minnesota 55432
  13. Analysis and Testing Center, Beijing University of Chemical Technology, Beijing 100029, People’s Republic of China
  14. National ESCA and Surface Analysis Center for Biomedical Problems, Department of Bioengineering and Chemical Engineering, University of Washington, Seattle, Washington 98195
  15. Cardiff Catalysis Institute, School of Chemistry, Cardiff University, Main Building, Cardiff CF10 3AT, United Kingdom
  16. Physical Electronics Inc., East Chanhassen, Minnesota 55317
  17. Versatile X-ray Spectroscopy Facility, School of Design, University of Leeds, Leeds LS2 9JT, United Kingdom
  18. Nanoscale and Microscale Research Centre, University of Nottingham, Nottingham NG7 2RD, United Kingdom
  19. CEA-LETI, 17 rue des Martyrs, 38054 Grenoble, France
  20. Instrumental Analysis & Research Center, Sun Yat-sen University, Guangzhou 510275, People’s Republic of China
  21. GE Research, 1 Research Circle, K1 1D7A, Niskayuna, New York 12309
  22. Faculty of Science and Engineering, University of Chester, Thornton Science Park, Chester CH2 4NU, United Kingdom
  23. Materials Analysis Station, National Institute for Materials Science (NIMS), 1-2-1 Sengen, Tsukuba, Ibaraki 305-0044, Japan
  24. Medtronic, 6700 Shingle Creek Parkway, Brooklyn Center, Minnesota 55430
  25. Kratos Analytical Ltd., Wharfside, Trafford Wharf Road, Manchester M17 1GP, United Kingdom
  26. Bundesanstalt für Materialforschung und -prüfung (BAM), Unter den Eichen 44-46, 12203 Berlin, Germany
  27. Department of Chemistry and Biochemistry, University of Maryland, College Park, Maryland 20742
  28. Department of Chemistry, Xi’an Jiaotong-Liverpool University, 111 Ren’ai Road, Suzhou Dushu Lake Science and Education Innovation District, Suzhou Industrial Park, Suzhou 215123, People’s Republic of China
  29. Analysis Department, Materials Characterization Division, Futtsu Unit, Nippon Steel Technology Co. Ltd., 20-1 Shintomi, Futtsu City, Chiba 293-0011, Japan
  30. Department of Physics, University of Warwick, Coventry, West Midlands CV4 7AL, United Kingdom
  31. Department of Chemistry and Biochemistry, Brigham Young University, C100 BNSN, Provo, Utah 84602
  32. Platform Laboratory for Science and Technology, Asahi Kasei Corporation, 2-1 Samejima, Fuji, Shizuoka 416-8501, Japan
  33. Université de Nantes, CNRS, Institut des Matériaux Jean Rouxel, IMN, F-44000 Nantes, France
  34. Atomic Weapons Establishment (AWE), Aldermaston, Reading, Berkshire RG7 4PR, United Kingdom
  35. Material Analysis Department, Yazaki Research and Technology Center, Yazaki Corporation, 1500 Mishuku, Susono-city, Shizuoka 410-1194, Japan
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Sciences (CNMS)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES); National Institutes of Health (NIH); Engineering and Physical Sciences Research Council (EPSRC)
Contributing Org.:
Versailles Project on Advanced Materials and Standards (VAMAS)
OSTI Identifier:
1784150
Grant/Contract Number:  
AC05-00OR22725; EB-002027; EP/K005138/1
Resource Type:
Accepted Manuscript
Journal Name:
Journal of Vacuum Science and Technology A
Additional Journal Information:
Journal Volume: 38; Journal Issue: 6; Journal ID: ISSN 0734-2101
Publisher:
American Vacuum Society / AIP
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; X-ray photoelectron spectroscopy; Electron scattering; Metrology; Surface science; Polymers; Photoelectron spectroscopy

Citation Formats

Reed, Benjamen P., Cant, David H., Spencer, Steve J., Carmona-Carmona, Abraham Jorge, Bushell, Adam, Herrera-Gómez, Alberto, Kurokawa, Akira, Thissen, Andreas, Thomas, Andrew G., Britton, Andrew J., Bernasik, Andrzej, Fuchs, Anne, Baddorf, Arthur P., Bock, Bernd, Theilacker, Bill, Cheng, Bin, Castner, David G., Morgan, David J., Valley, David, Willneff, Elizabeth A., Smith, Emily F., Nolot, Emmanuel, Xie, Fangyan, Zorn, Gilad, Smith, Graham C., Yasufuku, Hideyuki, Fenton, Jeffery L., Chen, Jian, Counsell, Jonathan P., Radnik, Jörg, Gaskell, Karen J., Artyushkova, Kateryna, Yang, Li, Zhang, Lulu, Eguchi, Makiho, Walker, Marc, Hajdyła, Mariusz, Marzec, Mateusz M., Linford, Matthew R., Kubota, Naoyoshi, Cortazar-Martínez, Orlando, Dietrich, Paul, Satoh, Riki, Schroeder, Sven M., Avval, Tahereh G., Nagatomi, Takaharu, Fernandez, Vincent, Lake, Wayne, Azuma, Yasushi, Yoshikawa, Yusuke, and Shard, Alexander G. Versailles Project on Advanced Materials and Standards interlaboratory study on intensity calibration for x-ray photoelectron spectroscopy instruments using low-density polyethylene. United States: N. p., 2020. Web. doi:10.1116/6.0000577.
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Reed, Benjamen P., Cant, David H., Spencer, Steve J., Carmona-Carmona, Abraham Jorge, Bushell, Adam, Herrera-Gómez, Alberto, Kurokawa, Akira, Thissen, Andreas, Thomas, Andrew G., Britton, Andrew J., Bernasik, Andrzej, Fuchs, Anne, Baddorf, Arthur P., Bock, Bernd, Theilacker, Bill, Cheng, Bin, Castner, David G., Morgan, David J., Valley, David, Willneff, Elizabeth A., Smith, Emily F., Nolot, Emmanuel, Xie, Fangyan, Zorn, Gilad, Smith, Graham C., Yasufuku, Hideyuki, Fenton, Jeffery L., Chen, Jian, Counsell, Jonathan P., Radnik, Jörg, Gaskell, Karen J., Artyushkova, Kateryna, Yang, Li, Zhang, Lulu, Eguchi, Makiho, Walker, Marc, Hajdyła, Mariusz, Marzec, Mateusz M., Linford, Matthew R., Kubota, Naoyoshi, Cortazar-Martínez, Orlando, Dietrich, Paul, Satoh, Riki, Schroeder, Sven M., Avval, Tahereh G., Nagatomi, Takaharu, Fernandez, Vincent, Lake, Wayne, Azuma, Yasushi, Yoshikawa, Yusuke, & Shard, Alexander G. Versailles Project on Advanced Materials and Standards interlaboratory study on intensity calibration for x-ray photoelectron spectroscopy instruments using low-density polyethylene. United States. https://doi.org/10.1116/6.0000577
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Reed, Benjamen P., Cant, David H., Spencer, Steve J., Carmona-Carmona, Abraham Jorge, Bushell, Adam, Herrera-Gómez, Alberto, Kurokawa, Akira, Thissen, Andreas, Thomas, Andrew G., Britton, Andrew J., Bernasik, Andrzej, Fuchs, Anne, Baddorf, Arthur P., Bock, Bernd, Theilacker, Bill, Cheng, Bin, Castner, David G., Morgan, David J., Valley, David, Willneff, Elizabeth A., Smith, Emily F., Nolot, Emmanuel, Xie, Fangyan, Zorn, Gilad, Smith, Graham C., Yasufuku, Hideyuki, Fenton, Jeffery L., Chen, Jian, Counsell, Jonathan P., Radnik, Jörg, Gaskell, Karen J., Artyushkova, Kateryna, Yang, Li, Zhang, Lulu, Eguchi, Makiho, Walker, Marc, Hajdyła, Mariusz, Marzec, Mateusz M., Linford, Matthew R., Kubota, Naoyoshi, Cortazar-Martínez, Orlando, Dietrich, Paul, Satoh, Riki, Schroeder, Sven M., Avval, Tahereh G., Nagatomi, Takaharu, Fernandez, Vincent, Lake, Wayne, Azuma, Yasushi, Yoshikawa, Yusuke, and Shard, Alexander G. Mon . "Versailles Project on Advanced Materials and Standards interlaboratory study on intensity calibration for x-ray photoelectron spectroscopy instruments using low-density polyethylene". United States. https://doi.org/10.1116/6.0000577. https://www.osti.gov/servlets/purl/1784150.
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@article{osti_1784150,
title = {Versailles Project on Advanced Materials and Standards interlaboratory study on intensity calibration for x-ray photoelectron spectroscopy instruments using low-density polyethylene},
author = {Reed, Benjamen P. and Cant, David H. and Spencer, Steve J. and Carmona-Carmona, Abraham Jorge and Bushell, Adam and Herrera-Gómez, Alberto and Kurokawa, Akira and Thissen, Andreas and Thomas, Andrew G. and Britton, Andrew J. and Bernasik, Andrzej and Fuchs, Anne and Baddorf, Arthur P. and Bock, Bernd and Theilacker, Bill and Cheng, Bin and Castner, David G. and Morgan, David J. and Valley, David and Willneff, Elizabeth A. and Smith, Emily F. and Nolot, Emmanuel and Xie, Fangyan and Zorn, Gilad and Smith, Graham C. and Yasufuku, Hideyuki and Fenton, Jeffery L. and Chen, Jian and Counsell, Jonathan P. and Radnik, Jörg and Gaskell, Karen J. and Artyushkova, Kateryna and Yang, Li and Zhang, Lulu and Eguchi, Makiho and Walker, Marc and Hajdyła, Mariusz and Marzec, Mateusz M. and Linford, Matthew R. and Kubota, Naoyoshi and Cortazar-Martínez, Orlando and Dietrich, Paul and Satoh, Riki and Schroeder, Sven M. and Avval, Tahereh G. and Nagatomi, Takaharu and Fernandez, Vincent and Lake, Wayne and Azuma, Yasushi and Yoshikawa, Yusuke and Shard, Alexander G.},
abstractNote = {We 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. Finally, 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.},
doi = {10.1116/6.0000577},
journal = {Journal of Vacuum Science and Technology A},
number = 6,
volume = 38,
place = {United States},
year = {Mon Nov 23 00:00:00 EST 2020},
month = {Mon Nov 23 00:00:00 EST 2020}
}
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https://doi.org/10.1116/6.0000577
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