Characterization of sub-monolayer coatings as novel calibration samples for X-ray spectroscopy

TL;DR

This paper presents the development and characterization of ultra-thin, sub-monolayer reference samples fabricated via physical vapor deposition for enhanced calibration in X-ray spectroscopy, especially in nanotechnology applications.

Contribution

It introduces novel sub-monolayer reference samples fabricated with PVD techniques and demonstrates their precise characterization using synchrotron radiation, expanding calibration options for XRF methods.

Findings

High precision in manufacturing of sub-monolayer coatings

Versatility of samples for various XRF applications

Confirmed homogeneity and stability of the reference samples

Abstract

With the advent of both modern X-ray fluorescence (XRF) methods and improved analytical reliability requirements the demand for suitable reference samples has increased. Especially in nanotechnology with the very low areal mass depositions, quantification becomes considerably more difficult. However, the availability of suited reference samples is drastically lower than the demand. Physical vapor deposition (PVD) techniques have been enhanced significantly in the last decade driven by the need for extremely precise film parameters in multilayer production. We have applied those techniques for the development of layer-like reference samples with mass depositions in the ng-range and well below. Several types of reference samples were fabricated: multi-elemental layer and extremely low (sub-monolayer) samples for various applications in XRF and total-reflection XRF (TXRF) analysis. Those samples were characterized and compared at three different synchrotron radiation beamlines at the BESSY II electron storage ring employing the reference-free XRF approach based on physically calibrated instrumentation. In addition, the homogeneity of the multi-elemental coatings was checked at the P04 beamline at DESY. The measurements demonstrate the high precision achieved in the manufacturing process as well as the versatility of application fields for the presented reference samples.