TY - JOUR A1 - Chyrkin, A. A1 - Epishin, A. A1 - Pillai, R. A1 - Link, T. A1 - Nolze, Gert A1 - Quaddaker, W. J. T1 - Modeling interdiffusion processes in CMSX-10/Ni diffusion couple JF - Journal of Phase Equilibria and Diffusion N2 - A diffusion couple between directionally solidified nickel and the single crystal Ni-base superalloy CMSX-10 was produced by hot pressing in vacuum. The diffusion couples were heat treated at temperatures between 1050 and 1250 °C. The exposed samples were characterized by SEM/EBSD/EPMA. The interdiffusion results in dissolution of the c¢-Ni3 Al in the superalloy and in growth of nickel grains towards CMSX-10. Rapid diffusion of aluminum from the superalloy into pure nickel leads to a significant formation of pores in the superalloy. The interdiffusion processes were modelled using the finite-element simulation software DICTRA with the databases TCNi5 and MobNi2, tailored specially for Ni-base superalloys. The effect of alloying elements on the interdiffusion profiles is discussed in terms of alloy thermodynamics. The calculated element concentration profiles are in good agreement with the EPMA measurements. The interdiffusion modeling correctly predicts the shapes of the concentration profiles, e.g. kinks on the Al and Ti profiles in the vicinity of the original interface in the joint. The calculation predicts with reasonable accuracy the extent and the location of the Kirkendall porosity. KW - Chemical potential KW - Diffusion KW - EBSD KW - Composition profiles KW - DICTRA modeling KW - Electron probe microanalysis KW - EPMA PY - 2016 DO - https://doi.org/10.1007/s11669-015-0444-9 SN - 1547-7037 VL - 37 IS - 2 SP - 201 EP - 211 PB - Springer AN - OPUS4-35776 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan T1 - High-Quality Experimental Data in Electron Microscopy and Microanalysis – What Can, and Should We Jointly Do? JF - Microscopy and Microanalysis N2 - There are different ways how to prove the quality of the analytical results obtained in a laboratory, e.g. use of validated standard operation procedures, participation in proficiency testing exercises, use of certified reference materials, etc. International standards provide requirements, specifications, Guidelines or characteristics of methods, instruments or samples with the final goal that these can be used consistently in accredited laboratories. In the field of electron microscopy and microbeam analysis standardization and metrology are terms which are encountered rather seldom at major conferences and scientific publications. Nevertheless, spectra formats like EMSA/MSA for spectral-data exchange or tagged image file format (TIFF) for SEM, guidelines for performing quality assurance procedures or for the specification of X-ray spectrometers as well as of certified reference materials (CRMs) in EPMA, or measurement of average grain size by electron backscatter diffraction (EBSD), or guidelines for calibrating image magnification in SEM or TEM are ISO standards already published and used successfully by a large part of the electron microscopy and microbeam analysis community. A main and continuous task of ISO/TC 202 and its subcommittees is to identify and evaluate feasible projects/proposals to be developed into new international standards, particularly with respect to recent but established technology, such the silicon drift detector (SDD) EDS. An international platform in the frame of which pre-standardization work can be organized is VAMAS (Versailles Project on Advanced Materials and Standards). International collaborative projects involving aim at providing the technical basis for harmonized measurements, testing, specifications, and standards to be further developed at ISO level. One key point of VAMAS activities is constituted by inter-laboratory comparisons for high-quality data. In the field of microbeam analysis, the technical working area (TWA) 37 Quantitative Microstructural Analysis deals with corresponding projects. Good ideas, e.g. on analysis of low-Z materials/elements and at low energies are particularly encouraged by directly contacting the author. Support and already available guidance will be supplied. KW - Data KW - Electron probe microanalysis KW - Electron microscopy KW - VAMAS KW - Iinter-laboratory comparison PY - 2019 DO - https://doi.org/10.1017/S1431927619009541 VL - 25 SP - 1762 EP - 1763 PB - Cambridge University Press AN - OPUS4-49246 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Boehm, S. A1 - Kim, K. J. T1 - Analysis of elemental composition of Fe1-xNix and Si1-xGex alloy thin films by electron probe microanalysis and micro-focus X-ray fluorescence JF - Surface and Interface Analysis N2 - The present study reports on results of analysis of the elemental composition of thin films by electron probe microanalysis with energy dispersive (ED-EPMA) X-ray spectrometry in conjunction with the dedicated thin-film analysis software package Stratagem and by X-ray fluorescence in its version with a micro-focus X-ray fluorescence (μ-XRF) source attached to a scanning electron microscope (SEM). Two thin-film systems have been analyzed: Fe1-xNix on silicon wafer and Si1-xGex on Al2O3 substrate, in both cases the layers being grown to a thickness of about 200 nm by ion beam sputter deposition. Samples of five different atomic fractions have been produced and analyzed for each thin-film system. Moreover, reference samples with certified elemental composition and thickness have been also available. This study is part of an interlaboratory comparison organized in the frame of standardization technical committee ISO/TC 201 “Surface chemical analysis.” Two laboratories have been analyzed by ED-EPMA (one laboratory standardless and one laboratory using both standardless and with standards variants) and one laboratory by μ-XRF (standardless and with standards). All the elemental compositions obtained with different methods are in very good agreement for the complete two sets of five samples each. KW - Thin films KW - Elemental composition KW - FeNi KW - SiGe KW - Electron probe microanalysis KW - X-ray Fluorescence PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509262 DO - https://doi.org/10.1002/sia.6834 SN - 0142-2421 VL - 52 IS - 12 SP - 929 EP - 932 PB - John Wiley & Sons Ltd AN - OPUS4-50926 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Procop, Mathias T1 - Measurement of X-Ray Emission Efficiencies for K-Lines JF - Microscopy and microanalysis KW - X-ray spectrometry KW - X-ray emission KW - X-ray yield KW - Electron probe microanalysis KW - EMPA KW - Standardless analysis PY - 2004 DO - https://doi.org/10.1017/S1431927604040139 SN - 1431-9276 SN - 1435-8115 VL - 10 IS - 4 SP - 481 EP - 490 PB - Cambridge University Press CY - New York, NY AN - OPUS4-6838 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Procop, Mathias A1 - Hübner, Wolfgang A1 - Wäsche, Rolf A1 - Nieland, S. A1 - Ehrmann, O. T1 - Fast Elemental Mapping in Materials Science JF - European microscopy and analysis KW - Electron probe microanalysis KW - EPMA KW - Energy dispersive X-ray spectroscopy KW - EDS KW - Elemental mapping PY - 2002 UR - http://www.microscopy-analysis.com/sites/default/files/magazine_pdfs/mag%20179_2002_Jan_Procop_1.pdf SN - 0958-1952 IS - January SP - 5 EP - 6 PB - Rolston Gordon Comm. CY - Bookham, Surrey AN - OPUS4-7091 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Procop, Mathias A1 - Radtke, Martin A1 - Krumrey, M. A1 - Hasche, K. A1 - Schädlich, S. A1 - Frank, W. T1 - Electron probe microanalysis (EPMA) measurement of thin-film thickness in the nanometre range JF - Analytical and bioanalytical chemistry N2 - The thickness of thin films of platinum and nickel on fused silica and silicon substrates has been determined by EPMA using the commercial software STRATAGEM for calculation of film thickness. Film thickness ranged in the order 10 nm. An attempt was made to estimate the confidence range of the method by comparison with results from other methods of analysis. The data show that in addition to the uncertainty of the spectral intensity measurement and the complicated fitting routine, systematic deviation caused by the underlying model should be added. The scattering in the results from other methods does not enable specification of a range of uncertainty, but deviations from the real thickness are estimated to be less than 20%. KW - Electron probe microanalysis KW - EPMA KW - Thin films KW - Thickness measurement KW - X-rays PY - 2002 DO - https://doi.org/10.1007/s00216-002-1514-5 SN - 1618-2642 SN - 1618-2650 VL - 374 SP - 631 EP - 634 PB - Springer CY - Berlin AN - OPUS4-7090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Procop, Mathias A1 - Terborg, R. T1 - Measurement and calculation of x-ray production efficiencies for copper, zirconium, and tungsten JF - Microscopy and microanalysis N2 - Electron probe microanalysis (EPMA) is based on physical relations between measured X-ray intensities of characteristic lines and their Xray production efficiency, which depends on the specimen composition. The quality of the analysis results relies on how realistically the physical relations describe the generation and emission of X-rays. Special experiments are necessary to measure X-ray production efficiencies. A challenge in these experiments is the determination of the detection efficiency of the spectrometer as a function of the photon energy. An energy-dispersive spectrometer was used in this work, for which the efficiency was determined at metrological synchrotron beamlines with an accuracy of ±2%. X-ray production efficiencies for the L series and the Kα series of copper and zirconium and for the M and L series of tungsten were determined at energies up to 30 keV in a scanning electron microscope. These experimental values were compared with calculated X-ray production efficiencies using physical relations and material constants applied in EPMA. The objective of the comparison is the further improvement of EPMA algorithms as well as extending the available database for X-ray production efficiencies. Experimental data for the X-ray production efficiency are also useful for the assessment of spectrum simulation software. KW - Copper KW - Electron probe microanalysis KW - Tungsten KW - X-ray production efficiency KW - Zirconium PY - 2022 DO - https://doi.org/10.1017/S1431927622012351 VL - 28 IS - 6 SP - 1865 EP - 1877 PB - Oxford University Press CY - Oxford AN - OPUS4-55711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -