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Organisationseinheit der BAM
- 6 Materialchemie (339)
- 1 Analytische Chemie; Referenzmaterialien (336)
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- 8.2 Zerstörungsfreie Prüfmethoden für das Bauwesen (88)
- 8.0 Abteilungsleitung und andere (87)
- 6.3 Strukturanalytik (84)
- 4 Material und Umwelt (70)
- 1.4 Prozessanalytik (61)
Austenitic stainless steel welds as well as dissimilar metal welds with nickel alloy filler material, used in safety relevant parts of nuclear power plants, still challenge the ultrasonic inspection. The weld material forms large oriented grains which lead on the one hand to high sound scattering and on the other hand – to inhomogeneity and to the acoustic anisotropy of the weld structure. The ultrasonic wave fronts propagate not linearly, as in ferritic weld joints, but along the curves, which depend on the specific grain structure of the weld. Due the influence of these phenomena, it is difficult to analyze the inspection results and to classify the ultrasonic indications, which could be both from the weld geometry and from the material defects. A correct flaw sizing is not possible.
In an ongoing research project, different techniques to improve the reliability of ultrasonic testing at these kinds of welds are investigated. In a first step (in the previous research project) two ultrasonic inspection techniques were developed and validated on plane test specimens with artificial and realistic flaws. In the ongoing project, these techniques are applied to circumferential pipe welds with longitudinal and transverse flaws.
The technique developed at the Federal Institute for Materials Research and Testing (BAM) in Germany uses a combination of ray tracing and synthetic aperture focusing technique (SAFT). To investigate the unknown grain structure, the velocity distribution of weld-transmitting ultrasound waves is measured and used to model the weld by ray tracing.
The second technique, developed at the Fraunhofer Institute for Nondestructive Testing (IZFP) in Germany, uses Sampling Phased Array (Full Matrix Capture) combined with the reverse phase matching (RPM) and the gradient elastic constant descent algorithm (GECDM). This inspection method is able to estimate the elastic constants of the columnar grains in the weld and offers an improvement of the reliability of ultrasonic testing through the correction of the sound field distortion. The unknown inhomogeneity and anisotropy are investigated using a reference indication and the special optimization algorithm.
Both reconstruction techniques give quantitative inspection results and allow the defect sizing. They have been compared to conventional ultrasonic testing with techniques, which are state of the art for components in nuclear power plants. The improvement will be quantified by the comparison of the probability of detection (POD) of each technique.
The paper addresses “WHITE LIGHT INTERFERENCE MICROSCOPY, ELLIPSOMETRY, AND INSTRUMENTED INDENTATION TESTING AS REFERENCE PROCEDURES“ and is subdivided in the following sections: 1. Measurement vs. testing vs. reference procedures, 2. White light interference microscopy (WLIM) for determination of step height h, 3. Spectroscopic ellipsometry (SE) for determination of layer thickness d and 4. Instrumented indentation testing (IIT) for determination of indentation hardness HIT. The following points are discussed in more detail: methodology of measurement and testing, uncertainty budgets for direct (WLIM), model-based (SE) and formula-based (IIT) reference procedures by means of specific examples. It is shown that standardization efforts are connected to reference procedures.
The overall interest in nanotoxicity, triggered by the increasing use of nanomaterials in the material and life sciences, and the synthesis of an ever increasing number of new functional nanoparticles calls for standardized test procedures1,2 and for efficient approaches to screen the potential genotoxicity of these materials. Aiming at the development of fast and easy to use, automated microscopic methods for the determination of the genotoxicity of different types of nanoparticles, we assess the potential of the fluorometric γH2AX assay for this purpose. This assay, which can be run on an automated microscopic detection system, relies on the detection of DNA double strand breaks as a sign for genotoxicity3. Here, we provide first results obtained with broadly used nanomaterials like CdSe/CdS and InP/ZnS quantum dots as well as iron oxide, gold, and polymer particles of different surface chemistry with previously tested colloidal stability and different cell lines like Hep-2 and 8E11 cells, which reveal a dependence of the genotoxicity on the chemical composition as well as the surface chemistry of these nanomaterials. These studies will be also used to establish nanomaterials as positive and negative genotoxicity controls or standards for assay performance validation for users of this fluorometric genotoxicity assay. In the future, after proper validation, this microscopic platform technology will be expanded to other typical toxicity assays.
From simple molar mass disperse homopolymers over copolymers to functionalized, 3-dimensional structures containing various distributions, the complexity of polymeric materials has become more and more sophisticated in recent years. With applications in medicine, pharmacy, smart materials or for the semiconductor industry the requirements for the characterization have risen with the complexity of the used polymers. For each additional distribution, an additional dimension in analysis is needed. Small, often isobaric heterogeneities in topology or microstructure can usually not be simply separated chromatographically or distinguished by any common detector. Instead of a complicated, time consuming and/or expensive 2d-chromatography or ion mobility spectrometry (IMS) method, that also has its limitations, here a simple approach using size exclusion chromatography (SEC) coupled with electrospray ionization mass spectrometry (ESI) is proposed. We used SEC for the separation because unlike other separation modes the separation in this mode solely should occur due to the hydrodynamic volume with no interference of other interactions. This simplifies the interpretation and the above mentioned heterogeneities should show a slight difference in hydrodynamic volume. ESI mass spectrometry can offer more than an access to mass dependent information like MMD, end group masses or CCD in polymer analysis. The online coupling to SEC allows the analysis of reconstructed ion chromatograms (RIC) of each degree of polymerization. While a complete separation often cannot be achieved, the derived retention times and peak widths lead to information on the existence and dispersity of heterogeneities in microstructure or topology, that are otherwise inaccessible or accessible only by time consuming or expensive methods. Because these heterogeneities might vary with the molar mass, analysis of the whole MMD-Peak (here the total ion current (TIC)) would not lead to the desired information. The broadening of the chromatographic peaks in this case does not origin from the already well known band broadening factors in chromatography from diffusion. This band broadening is attributed to the nature and composition of the analyte itself. Surprisingly there is very little investigation into the peak width or peak shape due to analyte structure itself found in literature. It is also shown, that with proper calibration even quantitative information could be obtained. This method is suitable to detect small differences in e. g. branching, topology, monomer sequence or tacticity and could potentially be used in production control of oligomeric products or other routinely done analyses to quickly indicate deviations from set parameters. Based on a variety of examples we demonstrate the possibilities and limitations of this approach.
We show both theoretically and experimentally how the encapsulation of the active region by additional guard layers can be used to achieve a significant reduction of the built-in electric fields in polar nitride heterostructures. This reduction of the QCSE results in a strongly enhanced emission intensity and faster recombination dynamics in the active region. In particular we are able to shift the emission energy of 4-nm-thick GaN nano-discs up to 3.32 eV, which is just 150 meV below the bulk GaN bandgap as compared to a red-shift of about 1 eV in a conventional heterostructure with the same thickness.
This is the first time that PE frits were used to quantify sulfur in copper and its alloys by isotope dilution combined with LA-ICP-MS: an alternative approach for sample preparation. The following properties of the PE frit meet the requirements for isotope dilution LA-ICPMS: porous material, thermo plastic (melting point >100°C), chemical resistance (nitric acid >70%) and high adsorption efficiency. The breakthrough, however, as a support material, especially when comparing the PE frit with other materials such gelatin or sodium silicate is the low blank, which is only two times of the gas flow blank (2.3-4.0 x 10⁴ cps). Additionally, the porosity of the frit was considered, as it directly affects the adsorption efficiency for the sample solution, which is present in the cavities of the frit.
Adsorption efficiency was studied by depositing sulfur standards with varying sulfur amounts (0, 2, 5, 10, 20, 40 and 80 µg S) on the frits. The remaining sulfur which was not absorbed by the frit was rinsed off and was measured by ICP-MS. This indirect method shows that more than 99.5 % of the loaded sulfur was absorbed by the frit. Such high absorption efficiency is completely sufficient for a support material to be used in LA-ICP-IDMS. The so prepared frits with increasing sulfur amount were measured by LA-ICP-MS showing a good linearity between 0 µg S and 40 µg S with a correlation coefficient r2 of 0.9987 and sensitivity of 3.4x10⁴ cps µgˉ¹ for 32S.
Three copper reference materials produced by BAM were selected to develop and validate the LA-ICP-IDMS procedure. The IDMS technique was applied to these samples as follows: the samples were spiked, dissolved, digested and then the digest was adsorbed on the frits.
In situ laser-induced breakdown spectroscopy measurements in stainless steels during TIG welding
(2018)
Chemical composition of the welding seam and HAZ has significant effect on weld quality. Current inspection methods for weld seams measure and investigate post factum and cannot prevent weld defects. Element burn-off may significantly affect solidification leading to embrittlement or cracking Control of weld chemical compositions insures a controlled solidification and resistance to related weld defects. A prototype of a LIBS controlled welding process is presented.
Photoelectron spectroscopy
(2018)
Grundkenntnisse zum besseren Verständnis der Funktionsweise der Elektronenstrahl-Mikroanalyse (ESMA) werden präsentiert und anhand Beispielen diskutiert.
Das physikalische Messprinzip von ESMA am REM, das Wechselwirkungs- und Informationsvolum und die Anregung der charakteristischen Röntgenlinien werden erklärt. Verschiedene potentielle Artefakte, wie z.B. Heterogenität der Probenzusammensetzung, Oberflächenbeschaffenheit der Probe und Linienüberlagerung werden eingeführt.
Die physikalischen Grenzen der analytischen Methode werden spezifiziert.