Filtern
Erscheinungsjahr
Dokumenttyp
- Zeitschriftenartikel (14)
- Posterpräsentation (4)
- Beitrag zu einem Tagungsband (2)
- Sonstiges (1)
Sprache
- Englisch (21)
Schlagworte
- EPMA (7)
- Thin films (6)
- EDX (5)
- Elemental composition (5)
- EDS (4)
- Fe-Ni (3)
- Geometrical collection efficiency (3)
- Si-Ge (3)
- Thin film analysis (3)
- CCQM (2)
- CIGS (2)
- Copper (2)
- Electron probe microanalysis (2)
- FeNi (2)
- Film thickness (2)
- SiGe (2)
- Solid angle (2)
- Tungsten (2)
- X-ray production efficiency (2)
- Zirconium (2)
- (mu-)XRF (1)
- Al2O3 thin films (1)
- Alloy films (1)
- Atomic fraction (1)
- Auger Electron Spectroscopy (AES) (1)
- BADGER film (1)
- BadgerFilm (1)
- Detection efficiency (1)
- ED-EPMA (1)
- EPMA (Electron Probe Microanalysis) (1)
- Effective area (1)
- Effective solid angle (1)
- Electron Probe Microanalysis (EPMA) (1)
- Electron probe microanallysis (EPMA) (1)
- Energy dispersive X-ray spectrometry (1)
- Energy-dispersive X-ray spectrometer (EDS) (1)
- FeNi thin film (1)
- Interlaboratory comparison (1)
- Performance check (1)
- Pilot study (1)
- SEM (1)
- SEM/EDS (1)
- SEM/EDX (1)
- Spectrometer calibration (1)
- Standardless analysis (1)
- Surface analysis (1)
- Test material (1)
- Thickness (1)
- WD-EPMA (1)
- X-ray Fluorescence (1)
- X-ray detectors (1)
- X-ray emission yield (1)
- X-ray spectrometer (1)
- X-rays (1)
- XRF (1)
- k-values (1)
- µ-XRF (1)
Organisationseinheit der BAM
A calibration procedure for the detection efficiency of energy dispersive X-ray spectrometers (EDS) used in combination with scanning electron microscopy (SEM) for standardless electron probe microanalysis (EPMA) is presented. The procedure is based on the comparison of X-ray spectra from a reference material (RM) measured with the EDS to be calibrated and a reference EDS. The RM is certified by the line intensities in the X-ray spectrum recorded with a reference EDS and by its composition. The calibration of the reference EDS is performed using synchrotron radiation at the radiometry laboratory of the Physikalisch-Technische Bundesanstalt. Measurement of RM spectra and comparison of the specified line intensities enables a rapid efficiency calibration on most SEMs. The article reports on studies to prepare such a RM and on EDS calibration and proposes a methodology that could be implemented in current spectrometer software to enable the calibration with a minimum of operator assistance.
A pilot study (PS) has been performed under the Consultative Committee for Amount of Substance (CCQM) / Surface Analysis Working Group (SAWG) with the objective to compare the atomic fractions of Cu, In, Ga and Se in CIGS alloy films. Four polycrystalline CIGS films with different atomic fractions were fabricated by variation of the relative atomic fraction of Ga on 100 mm x 100 mm soda-lime glass (SLG) substrates. Similar to real solar cells the atomic fractions of the four elements (Cu, In, Ga, Se) are not homogeneous with depth. For the analysis of the CIGS layers of about 2 μm thickness depth profiling with surface analysis techniques such as XPS, AES and SIMS was recommended. A CIGS alloy reference sample with atomic fractions certified by isotope dilution ICP-MS at KRISS has been also put at disposal by the coordinator of the comparison. The certified values were close to the atomic fractions of the samples to be analyzed. Hence, the atomic fractions of Cu, In, Ga and Se in the CIGS films could be determined by the relative sensitivity factors (RSF) derived from the reference CIGS film. The total ion intensities of the constituent elements were obtained by the total number counting (TNC) method.
An energy dispersive X-ray spectrometer operating with a semiconductor detector should be specified in compliance with the ISO standard 15632 [1]. Requirements for specification are: a) a general description of the spectrometer to evaluate its performance, b) the energy resolution with corresponding dead time, c) the P/B ratio in the Fe55 spectrum and, finally, d) the L/K intensity Ratio in a Ni or Cu spectrum to estimate spectrometer efficiency at low energies. Items b) to d) can be easily checked by the user. Related procedures are recommended in the annexes of the standard.
A method is proposed to determine the effective detector area for energy-dispersive X-ray spectrometers (EDS). Nowadays, detectors are available for a wide range of nominal areas ranging from 10 up to 150mm2. However, it remains in most cases unknown whether this nominal area coincides with the “net active sensor area” that should be given according to the related standard ISO 15632, or with any other area of the detector device. Moreover, the specific geometry of EDS installation may further reduce a given detector area. The proposed method can be applied to most scanning electron microscope/EDS configurations. The basic idea consists in a comparison of the measured count rate with the count rate resulting from known X-ray yields of copper, titanium, or silicon. The method was successfully tested on three detectors with known effective area and applied further to seven spectrometers from different manufacturers. In most cases the method gave an effective area smaller than the area given in the detector description.
Quantitative analysis of a bulk sample requires that the
composition of the sample is homogeneous over the analyzed
volume. For inhomogenous samples the calculation of
the matrix effects is not correct and this can lead to wrong results in the element concentrations. For samples containing a layer structure a different quantitative evaluation has to be applied. This can be provided with the standard-based analysis in ESPRIT in combination with the STRATAGem software.
The test material EDS-TM001 together with an accompanying software package, “EDX spectrometer check”, have been made available in 2009 by BAM to be employed by EDS (energy dispersive spectrometer) users to check the performance of an EDS attached to the SEM. Particularly for test laboratories operating under accreditation schemes like ISO/IEC 17025, a periodical control of the critical instrumental parameters in end-user laboratories is required. With EDS-TM001 or EDS-TM002 (second generation) test material, this periodical check is simplified to the acquisition of only one 10 kV spectrum. The software “EDX spectrometer check” is destined to evaluate automatically this spectrum and determine the performance of the EDS 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 thick layer of C, Al, Mn, Cu and Zr in a well-defined composition, deposited on a steel (in case of EDS-TM001) or silicon (in case of EDS-TM002) substrate. Meanwhile, more than one hundred laboratories use the EDS-TM001 or EDS-TM002 test material for the periodical check of their EDS. A detailed description of the test material and software together with examples of application was published recently. New results and gained experiences will be presented as well.
When the FWHM of lines appearing in the EDS-TM spectrum are determined, the spectrum background must be subtracted accurately. The applied physical background subtraction procedure is robust and takes into account the transmission of the detector window. While the previous version considers only Moxtek AP windows, the new version includes selection of silicon nitride window and the case of windowless detector. Moreover, the new version allows importing of spectra in Bruker spx format and EMSA/MSA files from EDAX TEAM software.
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).
To compare the performance of different energy dispersive X-ray spectrometers (EDS), it is important to define characteristic spectrometer parameters. The ISO 15632 standard defines parameters like energy resolution as FWHM for the Kα lines of carbon, fluorine and manganese. The quantum efficiency, which is the ratio of the detected photons divided by the number of incoming photons for different energies, is another significant spectrometer property. It is important for the light element and low energy line detection sensitivity as well as for higher photon energies above 10 keV. A striking EDS feature, provided and marketed by many manufactures, is the active area of the detector, although actually, the solid angle available for photon collection is the more relevant geometrical parameter. It is defined as: Ω = A /r2 with A being the active area of a spherical detector and r being the distance between the point of the radiation origin and the center of the surface of the active detector chip. A more accurate calculation should be used for large flat detector areas. One should note that the solid angle Ω is not an intrinsic spectrometer property. It can only be defined for a specific detector in combination with a specific system (e.g. SEM, EPMA or TEM). Thus, the minimal possible distance r is determined by the particular geometry e.g. a possible interference with the pole piece or other detectors/components in the chamber of a microscope. New EDS technologies use e.g. integrated SDD chips or inclined chips in thinner detector fingers which can be placed closer to the sample with the final result of larger real solid angles. Therefore, the knowledge of the real solid angle is one of the crucial parameters of an EDS microscope combination. A straightforward way to estimate the real solid angle is to simply determine A and r. If respective data are not provided by the manufacturer, this approach can be difficult.