EMRP-IND15: Traceable quantitative surface chemical analysis for industrial applications

• Forschungsstelle: METAS
• Projektnummer: F-5133.30009
• Projekttitel Englisch: EMRP-IND15: Traceable quantitative surface chemical analysis for industrial applications

Schlüsselwörter (Englisch)

Chemical surface analysis, Reference materials, Reference methods

Kurzbeschreibung (Englisch)

Chemical and topographical metrology at surfaces is a horizontal scientific-technical field that underpins almost all subject fields in advanced engineering in industry. The establishment of new traceable measurement methods and reference materials developed for surface chemical analysis will be key for the next generation of instrumentation by European instrument manufactures. Test laboratories will benefit from the development of metrologically underpinned quantitative methodologies of measurements at surfaces which will be developed as industrial standards. Also the development of more efficient, selective and cost-effective catalysts will require a better metrology with focus on surface effects.
The proposed scientific and/or technological methodology is a sound concept because the lack of suitable reference materials and methods in the area of quantitative surface analysis for industrial applications has been highlighted in many key reports. In this project, we address this pressing issue, using materials that are of the highest priority for the most relevant technologies. The majority of techniques and methods that could be reliably used to detect and measure elements and chemical species at surfaces and film thicknesses as well have been identified and are employed within the project. The participation of expert National Metrology Institutes (NMI) within the EC supported by relevant companies as unfunded partners and two partners from academia will ensure that credible recommendations will be made. The provision of well-characterised reference materials and methods through the different partners to costumers in the industry will enable comparability of results between different laboratories, which is currently a limiting factor. There is currently little activity from the NMI community in this area and therefore the project will build new capability and demonstrate responsiveness to the growing concerns of the EC and member states.

This project is part of the European Metrology Research Programme (EMRP, http://www.euramet.org/index.php?id=emrp); it is partly funded by the European Union on the basis of Decision No 912/2009/EC.

Projektziele (Englisch)

The objectives of the joint research project are to provide measurement standards and methods with traceability wherever it is practicable to do so for quantitative surface chemical analysis for industrial applications. This includes:

1. The provision of new Certified Reference Materials with known and stable surface chemistries as well as with defined thickness and lateral structure for instrument development and calibration as well as verification of industry-relevant surface chemical measurements.
2. The provision of new fast non-destructive methods of quantitative surface chemical analysis for industrial in-line quality control. In particular this will include the development of advanced techniques for real time, in-situ measurement of catalyst structure and activity on a localised scale to underpin the development of more efficient, selective and cost-effective catalysts. 
3. The provision of metrological methods including development of new Certified Reference Materials to improve the capability and traceability of technologies widely used in industry for surface analysis such as electron and fluorescence spectroscopy, X-ray reflectrometry, electron probe microanalysis or ion mass spectrometry.
   Each work package is planned considering priority that meets documented industrial needs and that supports transfer into industry by cooperation with relevant companies as unfunded partners and by standardization under ISO TC 201 ”Surface Chemical Analysis” and 202 “Microprobe Analysis".

Abstract (Englisch)

METAS was involved in the

• Fabrication of ultra-thin metal films on SiO2 for the improvement of ARXPS accuracy: Metallic reference samples with different layer thicknesses and structures were ana-lysed by angle-resolved x-ray photoelectron spectroscopy (ARXPS) at METAS. The goal was to calibrate and improve the accuracy of the XPS instrument. The measurements showed that only samples of very high quality were suitable for this purpose. The fabrication of such samples showed to be the limiting factor for the improvement of ARXPS accuracy.
• Methods for quantitative thickness analysis: The goal was to compare and validate different analysis techniques being used for the determination of the layer thicknesses of organic materials. METAS again conducted the ARXPS measurements. By reasons of insufficient surface quality of the reference materials, further investigations could not be continued.
• Traceable calibration of Contact Angle Spectroscopy by XPS for in-line process control: The goal was to establish a traceable correlation between contact angle and XPS measurements. The surface qualities of samples, either marked by laser or electro-chemically polished, were analysed at METAS using XPS and white light interferometry. Correlations between the surface qualities and the manufacturing process could be established and laid the basis future collaborations with industrial partners.

Umsetzung und Anwendungen (Englisch)

Electropolishing is already being used by weight manufacturers around the world to improve the surface quality of mass standards and to enhance stability of mass during dissemination. Through the collaboration between the weight manufacturer and METAS, the electropolishing process could be studied from a scientific point of view.
The study of laser marked samples laid the basis for the next generation of marking weights by laser for a unique identification. Correlations between the manufacturing process and the surface quality could be established.

Publikationen / Ergebnisse (Englisch)

Publishable JRP Summary Report for IND15 SurfChem, Traceable quantitative surface chemical analysis for industrial applications, http://www.euramet.org/fileadmin/docs/EMRP/JRP/JRP_Summaries_2010/IND15_Publishable_JRP_Summary.pdf