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- Dehngeschwindigkeit (4)
- Steifigkeit (3)
- Zugversuch (3)
- Surface click chemistry (2)
- XANES (2)
- 1,2,3-Triazole (1)
- Assessment (1)
- Azide (1)
- Density functional theory (1)
- Double-quantum NMR (1)
Organisationseinheit der BAM
Evaluation of an interlaboratory comparison of the chemical assay of U, Th oxide coated particles
(1981)
An ethynylterpyridine was 'clicked' to an azide-terminated self-assembled monolayer on gold and characterized by synchrotron radiation based surface analysis as NEXAFS and XPS. The detection of azide and terpyridine signatures confirmed a partial click reaction at room temperature. The absence of the azides after reaction at 50 °C indicates an almost complete conversion. For the latter case successful Pd(II) coordination has been proven. The Au–S interface of the SAMs has been characterized by S 1s and S 2p XPS.
Neutron tomography was applied to study the 3D water distribution in full polymer electrolyte membrane fuel cell (PEMFC) stacks. The water distribution after switch-off of the fuel cell was analyzed over a period of 36 h. We found a slowly increasing water amount in the fuel cell, but only few changes within a time period of 5 h, which is about the time necessary for neutron tomography. In this way, the requirement for successful tomography was obtained. It is demonstrated how the quasi in-situ tomography technique enables us to study the water content in individual flow field channels of three-fold stacks. Flow field as well as stack design issues are addressed by this visualization method showing weak points due to a non-uniform water distribution that can be identified by means of neutron imaging.
With the publication of EN ISO 6892-1:2009, the harmonisation of tensile testing at room temperature in Europe was achieved by combining EN 10002-1:2001 with ISO 6892:1998. Essential changes are the introduction of the strain rate and the strain rate control as the significant testing rate or control mode, respectively, referred to as “Method A”. By using this method in the correct way it is guaranteed that in the moment of determination of properties comparable resulting strain rates at the test piece in smaller ranges of specified strain rates are adopted — also if different stiffnesses of the testing equipment are present. This leads especially for strain rate sensitive materials to better comparable results. In this paper it is documented the need for the implementation of method A, methods for the realisation — also by the use of older testing systems — and an example of the comparability of results of the methods for a strain-rate-sensitive-steel.
Mit der Veröffentlichung der DIN EN ISO 6892-1:2009 wurde für den Zugversuch bei Raumtemperatur eine Harmonisierung der in Europa verbindlichen EN 10002-1:2001 mit der ISO 6892:1998 erreicht. Wesentliche Änderungen sind die Einführung der Dehngeschwindigkeit und der Dehngeschwindigkeitsregelung als maßgebliche Prüfgeschwindigkeit bzw. Regelungsart, als Verfahren A bezeichnet. Mit der korrekten Anwendung dieses Verfahrens wird gewährleistet, dass im Moment der Kennwerteermittlung bei enger spezifizierten zulässigen Dehngeschwindigkeitsbereichen vergleichbare resultierende Dehngeschwindigkeiten an der Probe auch bei unterschiedlichen Steifigkeiten der Prüfaufbauten vorliegen. Dieses führt besonders bei dehngeschwindigkeitssensitiven Werkstoffen zu deutlich vergleichbareren Ergebnissen. In diesem Beitrag wird auf die Notwendigkeit der Einführung des Verfahrens A, der möglichen Umsetzungen auch bei Verwendung von älteren Prüfsystemen sowie exemplarisch auf vergleichende Ergebnisse der Verfahren an einem dehngeschwindigkeitssensitivem Stahlwerkstoff eingegangen.
Die im Mai 2011 veröffentlichte Internationale Norm ISO 6892-2 "Metallische Werkstoffe — Zugversuch - Teil 2: Prüfverfahren bei erhöhter Temperatur" ersetzt die Europäische Norm EN 10002-5 und die Internationale Norm ISO 783.
Technische Änderungen/Ergänzungen im Vergleich zu den Vorgängernormen beziehen sich im Wesentlichen auf die Prüfgeschwindigkeiten und die Dehnungsmessung. In Anlehnung an Teil 1 der ISO 6892 (Prüfung bei Raumtemperatur) wird die Dehngeschwindigkeit als maßgebliche Prüfgeschwindigkeit mit eingeengten Bereichen (Verfahren A) empfohlen. Zum Ansetzen des Dehnungsaufnehmers und zur Festlegung der Messlänge sind nun verschiedene Verfahren möglich.
In dem Beitrag wird auch anhand von Beispielen auf mögliche Auswirkungen auf die zu bestimmenden Kennwerte eingegangen.
Experimental N K-edge NEXAFS data of surface immobilized azide, 1,2,3-triazole and terpyridyl groups are interpreted with the help of DFT spectrum simulations. Assignments of π* resonances in experimental N K-edge NEXAFS spectra to nitrogen atoms within these functional groups have been made. The azide was immobilized on gold as the head group of a thiol SAM, 1,2,3-triazole was formed on this SAM by click reaction and terpyridyl groups were introduced as substituents of the acetylene used for the click reaction. For azide-terminated molecules, DFT spectrum simulations are found to be useful to find measurement conditions delivering experimental N K-edge NEXAFS data with negligible X-ray damage. The 1,2,3-triazole group is found to be rather stable under X-ray irradiation.
Thermo-mechanical fatigue (TMF) testing plays an increasingly important role in the design, the reliability assessment and the lifecycle management of safety critical components used, for instance, for power generation, in the process industry and in aeronautical and automotive applications, with a view to increasing the fuel efficiency, safety and service intervals, while reducing production (and material) costs. In a European Commission funded research project (acronym: TMF-Standard) of the 5th Framework Programme, 20 European laboratories have undertaken a joint research effort to establish a validated code-of-practice (CoP) for strain-controlled TMF testing. Starting from a survey of the testing protocols and procedures previously used by the partners, a comprehensive pre-normative research activity into various issues has been completed, addressing the dynamic temperature control, the effects of deviations in nominal temperatures and phase angles, the influences of temperature gradients, as well as the practicalities of test interruption and restart procedures. Meaningful allowable tolerances for the various test parameters were identified and practical recommendations as to the test techniques were formulated. From this a preliminary CoP was compiled and used to guide an extensive round robin exercise among the project partners. From the statistical analysis of that exercise, a validated CoP was derived dealing with strain-controlled constant amplitude TMF of nominally homogeneous metallic materials subjected to spatially uniform temperature fields and uniaxial mechanical loading. It is intended to give advice and guidance on the appropriate test setup, testing procedures and the analysis of results, in particular for newcomers in the field of strain-controlled TMF. This paper highlights some of the results of the TMF-Standard project. Moreover, commonalities and differences of the present CoP with respect to the standard documents for strain-controlled TMF, which have been developed at ISO and ASTM levels, are presented in this paper.