Round Robin exercise: Coated materials for glow discharge spectroscopy

Abstract

A Round Robin (RR) exercise on selected coated materials has been carried out with the aim of finding the optimal conditions for the analysis of nitride layers with GD-OES. Such prenormative work is necessary for the evaluation of parallel development of the production of nitride layers as certified reference materials (CRMs). Two types of samples, Ti-N layer and V-N layer, respectively, with chemical compositions close to stoichiometry and a thickness of B3 mm, deposited on a steel substrate, have been provided to the RR participants. Additionally, another type of sample, a (100 nm CrNi/100 nm Cu) multilayer (ML) stack deposited on silicon wafer has also been included in the RR. This sample can be used as a CRM for checking GD spectrometer conditions and it has been proved helpful in further development of GDS instrumentation and methodology. The RR exercise has been performed in the frame of the EC Thematic Network on Glow Discharge Spectroscopy for Spectrochemical Analysis ('GDS-Net').1. Introduction. State-of-the-art of the analysis of coated/layered materials a Bundesanstalt fu¨r Materialforschung und -pru¨fung (BAM),

Analysis of elemental composition of Fe1‐xNix and Si1‐xGex alloy thin films by electron probe microanalysis and micro‐focus X‐ray fluorescence

“…For this purpose, depth profiling techniques or linescans over cross-sectioned samples should be applied. 9,10 The present study repeats measurements on an already tested system of Fe-Ni thin films on silicon 2,11 and reports for the first-time and Si 1-x Ge x alloy films obtained by different surface analysis techniques, such as X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectrometry (SIMS) applied in the depth-profiling operation mode. 12 In the present paper, only the results obtained by EPMA and microfocus X-ray fluorescence (μ-XRF) are presented in detail.…”

“…It should be noticed that gradients of the elemental composition in the depth of the thin layers cannot be distinguished by EPMA approach. For this purpose, depth profiling techniques or linescans over cross‐sectioned samples should be applied 9,10 …”

In‐depth structural and chemical characterization of engineered TiO2 films

“…In order to attain metrological traceability of the analysis results, it is essential to use suitable certified reference materials (CRM) as well as standard operating procedures for reproducible measurements of the respective TiO 2 film parameter(s). Reference carbide, nitride, oxide or hydrogen containing coatings with certified parameters are of very limited availability or, respectively, completely missing . In this contribution, we have selected two different types of TiO 2 ‐based films to be tested if they are suited as certified reference coating candidates with regard to film parameters mainly relevant to the respective film application: (i) TiO 2 coating synthesized by pulsed d.c. magnetron sputtering (PMS) for photocatalysis applications, where crystallographic information (microstructure, phase, and orientation) at the nanoscale through the ~1 µm depth of the layer is useful and (ii) ruthenium‐dye‐loaded TiO 2 film to be employed as new generation, DSSC, synthesized by screen printing from preformed anatase nanoparticles (NPs) and subsequent dye loading.…”

In-depth profile analysis of oxide films by radiofrequency glow discharge optical emission spectrometry (rf-GD-OES): possibilities of depth-resolved solid-state speciation

“…Nevertheless, several initiatives in the production and certification of layered CRMs (or certified reference coatings, CRCs) are now under development. [14][15][16] Hodoroaba et al 17 have recently carried out a round robin (RR) exercise on coated materials to find the optimal conditions for the analysis of nitride layers with GD-OES as well as to evaluate the development of the production of nitride layers as CRMs (Ti-N layer and V-N layer, respectively, deposited on a steel substrate). In addition, three different coatings (electroplated zinc, carbon-rich coatings and amorphous silicon layers) have also been investigated as potential candidates for CRMs for the determination of hydrogen concentration by GD-OES.…”