TY - JOUR A1 - Procop, Mathias A1 - Hodoroaba, Vasile-Dan T1 - Uncertainties in secondary fluorescence correction in EPMA JF - Microscopy and Microanalysis N2 - Secondary fluorescence is an inevitable effect that has to be taken into account in any algorithm for quantitative electron probe microanalysis (EPMA) as an additional correction. Moreover, secondary fluorescence worsens spatial resolution of EPMA. Secondary fluorescence is excited both by characteristic radiation and by the X-ray continuum. In most cases the correction is small. There are, however, cases, e.g. the determination of low heavy metal concentration in a light matrix, where the contribution of secondary fluorescence exceeds 10% of the measured X-ray line intensity. For secondary fluorescence correction the measured X-ray line intensity has to be divided by the correction factor (1+I_flchar/I_p +I_flcont/I_p )≈(1+I_flchar/I_p )(1+I_flcont/I_p ) in order to get those intensity I_p, which is excited only by the primary electrons. I_flchar and I_flcont mean the calculated characteristic and continuums fluorescence intensities. In order to get the intensity of fluorescence radiation, the absorption of the exciting radiation in the specimen, the photoionization probability and the self-absorption of the emitted line must be calculated. The critical quantity is the X-ray yield of the exciting atoms in case of fluorescence by characteristic radiation and the bremsstrahlung yield of the specimen in case of continuum fluorescence. In the former case it is reasonable to apply the same physical model to calculate I_flchar and I_p. KW - EPMA KW - Secondary fluorescence correction KW - Uncertainties KW - Microanalysis PY - 2019 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/uncertainties-in-secondary-fluorescence-correction-in-epma/AA92E973D350A74C574067AAFB2D9044 DO - https://doi.org/10.1017/S1431927619012534 SN - 1431-9276 SN - 1435-8115 VL - 25 IS - Suppl. 2 SP - 2360 EP - 2361 PB - Cambridge University Press AN - OPUS4-48863 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 EPMA and μ-XRF JF - Microscopy and Microanalysis N2 - The present study reports on measurements on thin Fe-Ni films on silicon and first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide Substrate by electron probe microanalysis (EPMA). Standard-based and standardless EPMA (with EDS) results were used in combination with the thin film analysis software Stratagem for the quantification. Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex 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. Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. An excellent agreement has been obtained between the atomic fractions determined by EPMA and µ-XRF with the KRISS certified values.zeige mehr KW - Thin film analysis KW - EPMA KW - XRF KW - Fe-Ni KW - Si-Ge PY - 2019 DO - https://doi.org/10.1017/S1431927619009668 VL - 25 SP - 1786 EP - 1787 PB - Cambridge University Press AN - OPUS4-49245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF 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 EPMA and µ-XRF N2 - The present study reports on measurements on thin Fe-Ni films on silicon and first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide Substrate by electron probe microanalysis (EPMA). Standard-based and standardless EPMA (with EDS) results were used in combination with the thin film analysis software Stratagem for the quantification. Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex 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. Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. An excellent agreement has been obtained between the atomic fractions determined by EPMA and µ-XRF with the KRISS certified values. T2 - Microscopy & Microanalysis 2019 CY - Portland, OR, USA DA - 03.08.2019 KW - Thin films KW - EPMA KW - µ-XRF KW - Elemental composition KW - Atomic fraction KW - Fe-Ni KW - Si-Ge PY - 2019 AN - OPUS4-48709 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Boehm, S. A1 - Kim, K. J. T1 - Measurement of Elemental Composition of FeNi and SiGe Alloy Thin Films by EMPA and µ-XRF N2 - It was demonstrated in the past that the electron probe microanalysis (EPMA) can be applied to determine accurately both elemental composition and thickness of thin films by using the dedicated software package for thin film analysis Stratagem. A relatively small number of film materials such as pure metallic films of platinum and nickel, binary alloys of Fe-Ni, and Pt-Ni-Co ternary alloy films has been reported in literature as working successfully. Further, the software can be applied ‘inversely’, i.e., by feeding it with the thickness of the film and using the determined mass coating, one can easily calculate the film density, which for porous layers leads us to the true film porosity. The present study repeats measurements on an already tested system of Fe-Ni thin films on silicon and reports for the first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide substrate. Standard-based and standardless EPMA (with EDS) results were used in combination with Stratagem for the quantification. Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Compared to EPMA, XRF has a larger information depth and a higher elemental sensitivity because of a generally lower background. Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex 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. Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. The atomic fractions of all the samples including the references have been certified by RBS (Rutherford backscattering spectrometry) and ICP-AES (inductively coupled plasma atomic emission spectroscopy). T2 - EMAS 2019 - 16th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS CY - Trondheim, Norway DA - 19.05.2019 KW - Thin film analysis KW - SEM/EDS KW - EPMA KW - Fe-Ni KW - Si-Ge PY - 2019 AN - OPUS4-48104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Boehm, S. A1 - Kim, K. Y. T1 - Measurement of elemental composition of Fe1-xNix and Si1-xGex alloy thin films by EMPA and µ-XRF N2 - It was demonstrated in the past that the electron probe microanalysis (EPMA) can be applied to determine accurately both elemental composition and thickness of thin films by using the dedicated software package for thin film analysis Stratagem. A relatively small number of film materials such as pure metallic films of platinum and nickel, binary alloys of Fe-Ni, and Pt-Ni-Co ternary alloy films has been reported in literature as working successfully. Further, the software can be applied ‘inversely’, i.e., by feeding it with the thickness of the film and using the determined mass coating, one can easily calculate the film density, which for porous layers leads us to the true film porosity. The present study repeats measurements on an already tested system of Fe-Ni thin films on silicon and reports for the first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide substrate. Standard-based and standardless EPMA (with EDS) results were used in combination with Stratagem for the quantification. Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Compared to EPMA, XRF has a larger information depth and a higher elemental sensitivity because of a generally lower background. Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex 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. Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. The atomic fractions of all the samples including the references have been certified by RBS (Rutherford backscattering spectrometry) and ICP-AES (inductively coupled plasma atomic emission spectroscopy). T2 - EMAS 2019 - 16th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS CY - Trondheim, Norway DA - 19.05.2019 KW - EPMA KW - FeNi KW - SiGe KW - Thin film analysis KW - µ-XRF PY - 2019 AN - OPUS4-48113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Procop, Mathias T1 - Performance of SEM/EDS systems with the Test Material EDS-TM001/002 and Evaluation Software EDS Spectrometer Test – Application and Updates N2 - The test material EDS-TM001 together with an accompanying software package, “EDS spectrometer check”, have been made available in 2009 by BAM to be employed by EDS (energy-dispersive X-ray spectrometer) users to check the performance of an EDS with a SEM. With EDS-TM001/002 test material, this periodical check is simplified to the acquisition of only one 10 kV spectrum. The software “EDS spectrometer check” is destined to evaluate automatically this spectrum and determine the EDS performance in terms of energy resolution and calibration, as well as possible alteration of low-energy efficiency due to detector contamination. Energy resolution can be compared with the specified values according to the international ISO standard ISO 15632:2012. EDS-TM is a synthetic material consisting of a 6 μm thick layer of C, Al, Mn, Cu and Zr deposited on a steel (EDS-TM001) or silicon (EDS-TM002) substrate. The chemical composition of EDS-TM was chosen such as to give nearly equal intensities of the low energy lines in a 10 kV spectrum, thus, making it very sensitive against spectrometer efficiency changes. New results and gained experiences will be presented. When the FWHM of the X-ray lines in the EDS-TM spectrum are determined, the spectrum Background must be subtracted accurately. The applied physical background subtraction procedure is robust and considers the transmission of the detector window. While the previous version considers only Moxtek AP windows, the new software version includes selection of silicon nitride window and the case of windowless detector. T2 - European Conference on Applications of Surface and Interface Analysis ECASIA 2019 CY - Dresden, Germany DA - 15.09.2019 KW - Test material KW - EDS X-ray spectrometer KW - EPMA KW - Performance check PY - 2019 AN - OPUS4-49233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Boehm, S. A1 - Kim, K. J. T1 - Measurement of Elemental Composition of and SiGe Alloy Thin Films by EPMA and µ-XRF N2 - The present study reports on measurements on thin Fe-Ni films on silicon and first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide Substrate by electron probe microanalysis (EPMA). Standard-based and standardless EPMA (with EDS) results were used in combination with the thin film analysis software Stratagem for the quantification. Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex 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. Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. An excellent agreement has been obtained between the atomic fractions determined by EPMA and µ-XRF with the KRISS certified values. T2 - European Conference on Applications of Surface and Interface Analysis ECASIA 2019 CY - Dresden, Germany DA - 15.09.2019 KW - Thin films KW - EPMA KW - XRF KW - FeNi KW - SiGe PY - 2019 AN - OPUS4-49278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Procop, Mathias T1 - Uncertainties in Secondary Fluorescence Correction in EPMA N2 - Secondary fluorescence is an inevitable effect that has to be taken into account in any algorithm for quantitative electron probe microanalysis (EPMA) as an additional correction. Moreover, secondary fluorescence worsens spatial resolution of EPMA, as discussed once more in two recent papers. Secondary fluorescence is excited both by characteristic radiation and by the X-ray continuum. In most cases the correction is small. There are, however, cases, e.g. the determination of low heavy metal concentration in a light matrix, where the contribution of secondary fluorescence exceeds 10% of the measured X-ray line intensity. For secondary fluorescence correction the measured X-ray line intensity has to be divided by the correction factor (1+I_flchar/I_p +I_flcont/I_p )≈(1+I_flchar/I_p )(1+I_flcont/I_p ) in order to get those intensity I_p, which is excited only by the primary electrons and enables the determination of specimen composition. I_flchar and I_flcont mean the calculated characteristic and continuums fluorescence intensities. In order to get the intensity of fluorescence radiation, the absorption of the exciting radiation in the specimen, the photoionization probability and the self-absorption of the emitted line must be calculated. This can be performed in a straightforward way. The critical quantity is the X-ray yield of the exciting atoms in case of fluorescence by characteristic radiation and the bremsstrahlung yield of the specimen in case of continuum fluorescence. In the former case it is reasonable to apply the same physical model to calculate I_flchar and I_p. T2 - Microscopy & Microanalysis 2019 CY - Portland, OR, USA DA - 03.08.2019 KW - EPMA KW - Secondary fluorescence KW - Uncertainties KW - X-ray spectrometry KW - Fluorescence correction PY - 2019 AN - OPUS4-48673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -