Verlag des Forschungszentrums Jülich

JUEL-3431
Westheide, Jochen
Aufbau einer Apparatur zur laserinduzierten Verdampfung und Untersuchungen zur LA ICP-MS für die Analyse keramischer Schichten
107 S., 1997



The starting point for this work was the question of whether laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) can be used for the analysis of refractory materials, in particular ceramics. This was examined with the example of the two materials La0,65Sr0,3MnO3 and YSZ, which are both receiving considerable attention in connection with the solid oxide fuel cell (SOFC). The results ofthis work show that LA-ICP-MS fulfils expectations and is of great benefit for a fast and sensitive analysis of compact ceramics and ceramic coatings.

For these studies preparation rules were defined concerning synthetic standards for calibration and blank sampIes to determine detection limits owing to the lack of suitable standard reference materials (SRMs) for both materials, La0,65Sr0,3MnO3 and YSZ. Therefor elements dissolved in nitric acid were added to the powdered starting materials, which are also used for the preparation of SOFC coatings.

A comparison of the results with those obtained by other methods -the only possibility of verifying the results due to the lack of SRMs -showed good agreement, both for Lao,65Sro,3MnO3 and YSZ. Aspects studied included the concentrations of trace elements in single layers and in coating systems and the homogeneity of major elements in coatings, which were in part prepared by methods used for the first time for La0,65Sr0,3MnO3 and YSZ. Furthermore, the origin of microlocal contaminations was clarified and the attempt made to record depth profiles.

LA-ICP-MS was also used for SOFC process control. The concentrations of trace elements were determined both in the starting powder and in the sintered coatings prepared from it to trace the cause of the inadequate electrochemical properties of the SOFC in question. Some sources of contamination were revealed. In general it was found that La0,65Sr0,3MnO3 coatings have a distinctly higher purity than YSZ coatings.

In addition, in some basic studies important insights were obtained into the interaction of laser radiation with matter under an argon atmosphere. Amongst other aspects, experimentally measured crater depths were compared with theoretical predictions and the loss of laser radiation through the plasma formed in the interaction process on the surface was determined.

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Letzte Änderung: 07.06.2022