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- Fluorescence (15)
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- 1 Analytische Chemie; Referenzmaterialien (88)
- 6 Materialchemie (76)
- 8 Zerstörungsfreie Prüfung (70)
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- 4 Material und Umwelt (30)
- 6.6 Physik und chemische Analytik der Polymere (27)
- 6.3 Strukturanalytik (22)
- 1.2 Biophotonik (20)
- 7 Bauwerkssicherheit (20)
- 8.1 Sensorik, mess- und prüftechnische Verfahren (20)
Übersicht über die gefahrgutrechtlichen Anforderungen zur Bauartprüfung und dem Qualitätsmanagement für Verpackungen für nicht zulassungspflichtige Versandstücke.
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 X-ray 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 6 μm thick layer of C, Al, Mn, Cu and Zr deposited on a steel (in case of EDS-TM001) or silicon (in case of 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. Meanwhile, about 150 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 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 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.
Windowless detectors have been also tested demonstrating long-term stability after repeated heating and cooling cycles. In this case, the appropriate Background subtraction is decisive for accurate detector characterization. Detailed results will be presented.
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).
Porous materials play an important role in several fields of technology, especially for energy applications like photovoltaics, electrolysis or batteries. The activity of porous films is affected by properties like porosity, film thickness, chemical composition of the material, as well as the crystallinity of the framework. The complex morphology of such porous films constitutes a challenge even for modern analytical techniques and requires new approaches employing the combination/complementation of data of different analytical methods. In this contribution, we characterise thin mesoporous iridium-titanium mixed oxide film properties by electron probe microanalysis (EPMA) with energy-dispersive X-ray spectroscopy (EDS) at an SEM.
Mesoporous iridium oxide - titanium oxide (IrOx-TiOx) films were prepared via dip-coating of a solution containing a triblock-copolymer as structure-directing agent, an iridium precursor as well as a titanium precursor in ethanol. IrOx-TiOx films were synthesized with different amounts of iridium and calcined in air. The SEM micrographs reveal for all films the achievement of a well-ordered mesoporous structure and homogeneous films with thicknesses between 67 nm and 152 nm.
For the determination of film elemental composition and porosity, EPMA can be used as part of a combined SEM/EDS/STRATAGem analysis. Elemental compositions and mass depositions (in μg cm-2) of IrOx-TiOx films were calculated with the thin film analysis Software STRATAGem via k-values measured with SEM/EDS. Pure bulk Ir, TiO2 and Si were measured as references. The average density of the films was obtained from the mass Deposition and the film thickness as measured by cross-section SEM. The porosity was then extracted from the measured average film density divided by a theoretical bulk density. The latter is calculated from the weight fractions of IrOx and TiOx as determined with STRATAGem and the bulk mass densities of IrO2 and TiO2 (rutil) from literature.
The fitting results of the k-values from the STRATAGem software, which are in fair agreement with the measured k-values.
The application of the SEM/EDS/STRATAGem approach for accurate porosity determination on pure mesoporous TiOx films and pure porous IrOx films has been recently demonstrated.
The porosities of pure IrOx, TiOx and mixed IrOx-TiOx films in this study have been determined. The contribution will assess in detail the advantages and limitations of the combined SEM/EDS/STRATAGem analysis for the morphology and porosity of thin metal oxide films. Moreover, the comparison with other measurement techniques and the combination of datasets from multiple measurements will be discussed.
Microbeam analysis data are of continuously improving quality, this owing mainly to developments in instrumentation (hardware and software) and computer performance. The knowledge and skills of the operators must be also kept correspondingly updated. To be deemed as technically competent, the laboratories must be accredited according to an accreditation scheme, mostly following ISO/IEC 17025.
International standards are able to 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 standardisation and metrology are terms that are encountered rather seldom at major conferences and scientific publications. Several ISO standards already published and used successfully by a large part of the electron microscopy and microbeam analysis community. For example, file formats such as EMSA/MSA for spectral-data exchange or tagged image file format (TIFF) for SEM images; procedures for the specification of X-ray spectrometers, the specification of certified reference materials (CRMs), and for measurement of average grain size by electron backscatter diffraction (EBSD); and guidelines for calibrating image magnification in SEM or TEM. A main task of ISO technical committee TC 202 ‘Microbeam Analysis’ is to identify feasible projects/proposals needed to be developed into new international standards, particularly in respect to recent technology, such the silicon drift detector (SDD).
As far as the metrological aspects are regarded, The International Bureau of Weights and Measures (BIPM) through the Consultative Committee for the Amount of Substance (CCQM) is concerned with the metrological aspect in Chemistry and Biology. In particular, the Surface Analysis Working Group (SAWG) assists in identifying and establishing inter-laboratory work to test the consistency as well as to improve the traceability of spatially resolved chemical surface analysis at the micro and nanoscale. Examples of recent projects on quantitative microbeam analysis at low energies, such as the quantification of light elements such as carbon and nitrogen will be presented.
The significant sources of measurement uncertainty will be emphasized. These are: quality of the unknown and the reference materials used, the quantification model, instrumental parameters like take-off-angle, spectrometer efficiency, and particularly the beam current. The crucial importance of working with uniform and well-defined measurement and data evaluation protocols will be discussed in compliance with the ISO document “Guide to the expression of uncertainty in measurement (GUM)”.
Another international platform where pre-standardisation work can be organised is VAMAS (Versailles Project on Advanced Materials and Standards). International collaborative Projects aim at providing the technical basis for harmonised 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 at low energies, are particularly encouraged by directly contacting the author. Support and guidance will be supplied.
Virtual-lab-based determination of a macroscopic yield function for additively manufactured parts
(2019)
This work aims for a yield function description of additively manufactured parts of S316L steel at the continuum-mechanical macro-scale by means of so-called virtual experiments using a crystal plasticity (CP) model at meso-scale. Additively manufactured parts require the consideration of the specific process-related microstructure, which prevents this material to be macroscopically treated as isotropic, because of crystallographic as well as topological textures. From virtual experiments, yield loci under various loading conditions are simulated. The scale bridging from meso- to macro-scale is realised by the identification of the simulated yield loci as a modified anisotropic Barlat-type yield model representation.
The simultaneous detection of different analytes has gained increasing importance in recent years, especially in the fields of environmental and health monitoring. Particularly suitable formats for multiplexing are bead-based assays. The beads employed need to fulfil size and density requirements important for instance for flow cytometry and shall exhibit an as high as possible surface area for anchoring capture probes to allow for low limits of detection. Core/shell particles are ideally suited in this sense because of their modularity in design and adaptability for various (bio)analytical assays. Here, polystyrene particles coated with different kinds of mesoporous silica shells are presented, possessing distinctly higher surface areas in comparison to non-porous core/shell particles. Different factors such as pH and amount and type of mediator salt used during shell preparation were evaluated with shell inspection by scanning/transmission scanning electron microscopy (SEM/tSEM) being key to architecture control of the monodisperse particles.
For a cytometric model assay, the optimized core/shell particles were functionalized with capture oligonucleotides for DNA detection. After covalent attachment of single-stranded DNA to the silane-modified silica surface, a hybridisation assay using labelled t-DNA complementary strands was carried out to demonstrate particle performance, showing how tailoring of the shell’s surface area controls sensitivity and dynamic range of the assay. Finally, a multiplex assay for the determination of DNA from different human papilloma virus (HPV) lines was developed. Using our optimized particles, we were able to detect down to 10 amolμl‒1, which is an improvement of one order of magnitude compared to assays using non-porous particles reported in the literature. In addition, multiplexed detection could successfully be demonstrated.
Feuchte, insbesondere in Form von Flüssigwasser, stellt in Baustoffen ein hohes Schadenspotential dar. Um mit zerstörungsfreier Prüfung mögliche Risikostellen zu lokalisieren und Präventionsmaßnahmen zu ergreifen, sind Kenntnisse über das Porengefüge und Feuchtetransportmechanismen im Baustoff erforderlich. Eine wesentliche Problematik besteht derzeit in der Erfassung und Quantifizierung von Feuchteverteilungen bei Teilsättigung.
Wir verfolgen derzeit einen Ansatz, mittels Nuklear Magnetischer Resonanz (NMR) in Korrelation mit relativen Luftfeuchtmessungen den Flüssigwasseranteil bei Teilsättigung zu ermitteln. Mit Protonen-NMR lassen sich Relaxationszeiten von Wasserstoffprotonen in Abhängigkeit von ihrer Bindungsart und ihrer Umgebung - z. B. Porenstruktur und -größe - erfassen. Allerdings lässt sich bei Materialien mit sehr breiten Porengrößenverteilungen nicht klar differenzieren, ob kurze Relaxationszeiten durch größere teilgesättigte oder kleinere vollgesättigte Poren verursacht werden. Für die Korrelation mit der relativen Luftfeuchte im Baustoff erfolgt zunächst eine künstliche Regulierung im Klimaschrank. Durch einen neuentwickelten Ansatz von Hillerborg lassen sich dann bei jeder Luftfeuchte die adsorbierten Wasserschichtdicken und der Porensättigungsgrad für die vorhandenen Porengrößen berechnen. Mithilfe des berechneten Porensättigungsgrades lässt sich eine genauere Analyse der zeitlichen Entwicklung von Relaxationszeitenverteilungen (insbesondere bei Trocknungs- und Aufsättigungsprozessen) vornehmen. Somit sollen erstmals Aussagen zu kürzeren Relaxationszeiten bei teilgesättigten Porensystemen, die beispielsweise auch eine multimodale Porengrößenverteilung aufweisen, getroffen werden können.
In dieser Arbeit wird die Kombination aus NMR und der relativen Luftfeuchte an sehr porösen Dämmplatten aus Kalziumsilikat, die zur Wärmedämmung sowie der Entgegenwirkung von Schimmelbildung eingesetzt werden, angewendet. Untersucht werden 28 Proben à 6 Gruppen, die von unterschiedlichen Herstellern stammen bzw. unterschiedlich hergestellt wurden.
Ultraschallmessverfahren werden seit Langem erfolgreich für Prüfaufgaben im Bauwesen eingesetzt. Die dauerhafte Überwachung und frühzeitige Erkennung von Schäden an komplexen Neubauten und alternder Infrastruktur kann mittels Ultraschall-Transmissionsmessungen und speziellen Auswertemethoden, wie z. B. Korrelationverfahren und Codawelleninterferometrie, realisiert werden. Für die Dauerüberwachung wurde ein kompaktes System entwickelt, das Ultraschall-Messdaten erfassen und ins Internet auf einen FTP-Server übertragen kann. Es können hierbei alle angeschlossenen Prüfköpfe für jede Messung wahlweise als Sender oder Empfänger geschaltet werden. Es wurden Vorverstärker entwickelt, bei denen die Versorgung mit Strom über die Messleitung erfolgt. Dadurch können die Verstärker nahe am Prüfkopf positioniert werden. Durch Änderungen in den Ultraschall-Signalen können Schädigungen des Bauteils, wie z.B. Risse, in Echtzeit erkannt werden.
Leitungswasserschäden nahmen im Jahr 2016 mit rund 2,6 Milliarden Euro den größten Posten bei Gebäudeversicherungen ein. Die Bestimmung und Lokalisierung des Schadensausmaßes ist dabei ein erster wichtiger Schritt, um die erforderlichen Sanierungsarbeiten abschätzen und effizient vornehmen zu können. Hierfür sind Radar und Neutronensonden bereits etablierte Verfahren. Für verlässliche Aussagen zum quantitativen Feuchtegehalt eines Baustoffes werden jedoch zerstörende Sondierungsbohrungen zur Kalibrierung der aufgenommenen Daten benötigt. Dieser hohe zeitliche und finanzielle Aufwand soll zukünftig durch den parallelen Einsatz der genannten Messverfahren verhindert werden. In der durchgeführten Studie wurden Estrichprobekörper auf Zement- und Anhydritbasis mit variablen Dicken und Festigkeiten hergestellt und deren Austrocknung mit Radar und Neutronensonde über einen Zeitraum von 90 Tagen beobachtet. Als Referenzverfahren zur Ermittlung des Feuchteverlaufs dienten die gravimetrische Darr- und chemische Calcium-Carbid-Methode, welche an kleineren Schwesterproben der gleichen Charge angewendet wurden. Kontinuierliche Wägungen der größeren Probekörper gaben hierbei Aufschluss über den durch Austrocknung schwindende Wasseranteil. Aus dem aufgenommen Radardatensatz konnten anschließend markante Signalmerkmale im Zeit- und Frequenzbereich extrahiert und deren Zusammenhang zum Feuchtegehalt der Estrichtypen untersucht werden. Hierbei wurden gängige Methoden aus der Literatur zur Feuchtemessung mit Radar angewandt, wobei die Kombination dieser und das Hinzuziehen der Neutronensonde mittels Datenfusion zu einem höheren Informationsgehalt beiträgt. Somit kann eine zerstörungsfreie Quantifizierung des Feuchteschadens an schwimmenden Fußbodenaufbauten vorgenommen werden
As part of the BonaRes research initiative, funded by the BMBF, strategies are being developed to use soil as a sustainable resource in the bio economy. The interdisciplinary subproject I4S - “Intelligence for soil” - is responsible for the development of an integrated system for site-specific management of soil fertility. For this purpose, a platform is constructed and various sensors are installed. Real-time data will be summarised in models and decision-making algorithms will be used to control fertilisation and accordingly improve soil functions. Aim of the BAM in the frame of I4S is the characterisation of an energy-dispersive X-ray fluorescence (EDXRF) based sensor for robust determination of plant essential nutrients in soil.
First a principal component analysis (PCA) was used to identify outliers and to observe the largest variance within the German soil samples. It could be monitored that splitting of the samples was due to their iron content. Given that clay samples contain high amounts of iron and sandy samples low amounts, a classification of the samples by their soil texture according to VD LUFA was possible. Considering the complex composition of soil, a matrix-specific calibration was carried out by univariate and multivariate data analysis. The figures of merit demonstrated that a more robust calibration model with negligible matrix effects can be obtained by a multivariate approach using partial least squares regression (PLSR). A better correlation between predicted values compared to reference values for German soil samples was observed for the chemometric calibration model than for the univariate one.
Different factors can affect the received calibration models such as moisture and particle size distribution which is especially important due to later online analysis.
In first studies the influence of moisture on the detection of plant essential nutrients was investigated. With increasing water content, the characteristic fluorescence peaks decrease and start to increase again at a water content of 15 %. With lower moisture content the soil agglomerates which leads to lower packing of the sample, resulting in a rougher surface which negatively influence the signals. Whereas, agglomerates are not formed at higher water content. This allows the sample to be packed more tightly thus a smoother surface and a better homogeneity is obtained.
Furthermore, particle size distribution leads to significantly higher uncertainties and lower signals when comparing grounded (< 500 μm) and not grounded (< 2 mm) samples. This can be explained by amplifying of the already known inhomogeneity of soils.
Both factors must be included in the chemometric PLSR to obtain robust calibration models for each macro and micro nutrient.
Motivation:
- Reduktion der CO 2 Emissionen von Verbrennungsmotoren durch den Einsatz von LNG als alternativer Kraftstoff
- Aktuell werden doppelwandige Edelstahltanks mit Vakuumisolation für den Transport eingesetzt
- Reduktion des Tankgewichts und Vereinfachung der Konstruktion soll durch die Substitution mit GFK inklusive einer Isolationsschicht erreicht werden
- Leichtere Überprüfung von einwandigen Tankkonstruktionen
- Günstiges Versagensverhalten von GFK im Brandfall
Zusammenfassung:
- Thermische Performance kann mit Isolation aus PU Schaum erreicht werden
- Messung der Abdampfrate bildet einfache Möglichkeit zur Bestimmung der thermischen Performance
- Mikrorisse in der Matrix führen zur Leckage -> Liner notwendig
- Biegemodul bis 30 MPa vergleichbar, danach Abfall um ca. 50 % bei tiefen Temperaturen
Ausblick:
- Prüfung von GFK Proben mit Fasern in 0°-Orientierung
- Prüfung der thermischen Performance mit Demonstratoreinheiten verschiedene Größen
- Entwicklung einer Skalierungsfunktion, um Ergebnisse von druckloser Prüfung auf Druckanstieg zu übertragen
The introduction of the 5G technology and automotive radar applications moving into higher frequency ranges trigger further miniaturization of LTCC technology (low temperature co-fired ceramics). To assess dimensional tolerances of inner metal structures of an industrially produced LTCC multilayer, computer tomography (CT) scans were evaluated by machine learning segmentation.
The tested multilayer consists of several layers of a glass ceramic substrate with low resistance silver-based vertical interconnect access (VIA). The VIAs are punched into the LTCC green tape and then filled with silver-based pastes before stacking and sintering. These geometries must abide by strict tolerance requirements to ensure the high frequency properties.
This poster presents a method to extract shape and size specific data from these VIAs. For this purpose, 4 measurements, each containing 3 to 4 samples, were segmented using the trainable WEKA segmentation, a non-commercial machine learning tool. The dimensional stability of the VIA can be evaluated regarding the edge-displacement as well as the cross-sectional area. Deviation from the ideal tubular shape is best measured by aspect ratio of each individual layer. The herein described method allows for a fast and semi-automatic analysis of considerable amount of structural data. This data can then be quantified by shape descriptors to illustrate 3-dimensional information in a concise manner. Inter alia, a 45 % periodical change of cross-sectional area is demonstrated.
Homogeneous introduction of organic additives is a key of ceramic powder processing. Addition of organics to ceramic slurries holds advantages compared to dry processing like organic content reduction and a more homogeneous additive distribution on the particle surface.
Investigations of the alumina slurries were primarily based on zeta potential measurements and sedimentation analysis by optical centrifugation. Both methods were combined to determine a suitable additive type, amount and composition, whereas the spray drying suitability has been ensured by viscosity measurements. Granules, yielded by spray drying of such ideally dispersed alumina slurries, are mostly hollow and possess a hard shell. Those granules cannot easily be processed and can only hardly be destroyed in the following shaping step, leading to sinter bodies with many defects and poor strength and density.
The precise slurry destabilization, carried out after ideally dispersing the ceramic powder, shows a strong influence on the drying behavior of the granules and hence on the granule properties. A promising degree of destabilization and partial flocculation was quantified by optical centrifugation and resulted in improved granule properties. Spray drying the destabilized alumina slurries yielded homogeneous “non-hollow” granules without the above mentioned hard shell. Sample bodies produced of these granules exhibited a reduction of defect size and number, leading to better results for sinter body density and strength.
The positive effect of the slurry destabilization has been further improved, by exchanging the atomizing unit from a two-fluid one to an ultrasound atomizer with only minor slurry adjustments necessary. The controlled destabilization and ultrasound atomization of the ceramic slurry show excellent transferability for zirconia and even ZTA (zirconia toughened alumina) composite materials.