Quantification via X‐ray fluorescence analysis of oxygen in the surface layer of a Si‐sphere used as a new mass standard

• Published in: X-ray spectrometry 2022-03, Vol.51 (2), p.122-128
• Main Authors: Wu, Yu‐Hsin, Tsao, Lin, Chiu, Jeng‐Yu, Chen, Sheng‐Jui, Fliegauf, Rolf, Müller, Matthias, Beyer, Edyta, Kolbe, Michael
• Format: Article
• Language: English
• Subjects: Calibration; Deposition; Fluorescence; Industrial applications; Oxygen; Photoelectrons; Raman spectra; Silicon; Si‐sphere; Surface analysis (chemical); surface characterization; Surface layers; X ray photoelectron spectroscopy; XRCD; XRF
• ISSN: 0049-8246; 1097-4539
• DOI: 10.1002/xrs.3265

The distribution of oxygen present in the surface layer of the Si‐sphere used as new mass standard is measured and quantified using the combined X‐ray fluorescence (XRF)/X‐ray photoelectron spectroscopy (XPS) surface analysis system in the Center for Measurement Standards, Industrial Technology Research Institute (CMS/ITRI). A radiometric calibration of the X‐ray source is not possible because the spectral distribution of the X‐ray tube used is complex and not stable over the long term. Hence, the quantification of oxygen on the Si‐sphere is based on a calibration curve that establishes a correlation between the mass deposition of oxygen from the calibration samples qualified by PTB and the ratio of the oxygen fluorescence to silicon RRS (resonant Raman scattering) intensities in the in‐house system. This paper presents the methodology for and the results of an oxygen quantification performed using the combined XRF/XPS surface analysis system. With a relative uncertainty of less than 10%, the average mass deposition of oxygen on the Si‐sphere was 133 ± 12 ng/cm2. The oxygen quantified via XRF is treated as a reference for the quantification of other elements on the surface layer. The quantification of carbon mass deposition in the surface layer in relation to the oxygen mass deposition is also described in this paper. The surface analysis system is part of our contribution to the realization and dissemination of the unit of the kilogram (based on its new definition) via the XRCD method.