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Eingeladener Vortrag
- nein (1030)
This study aims at improving the detection of near-surface defects in magnetizable and conductive specimens by combining the measurements of eddy current, magnetic flux leakage and thermography testing. Different signal processing methods for data normalization are proposed to enable data fusion at the pixel level. These methods are applied to a test specimen which contains 10 variably-sized defects. We quantitatively evaluate the performances of a total of 29 detection methods with respect to false alarm reduction at a fixed level of true positive rate. We report that false positive rate could be reduced from 1.65% down to 0.28% by the best multi-sensor method compared to the best single-sensor performance on the smallest defect, when 50% found flaw pixels are required for successful detection.
In the last years, new approaches for the evaluation of the corrosion resistance of martensitic stainless steels were developed, which allow nearly non-destructive as well as short-term corrosion testing. This work analyzes the sensitive influence of microstructure and surface treatment on the corrosion resistance. The effect of alloy composition and microstructure, which is always present in addition to the influence of various surface treatments will be evaluated and discussed. The corrosion behavior was investigated with conventional evaluation of the pitting potential, electrochemical potentiodynamic reactivation (EPR), electrochemical noise (EN), and the 'KorroPad' (KP) technique. EPR provided information about the passivation ability and the extent of chromium content reduction due to chromium carbide precipitation in the microstructure. The use of EN and KP aims to detect the influence of different surface treatment parameters on the corrosion resistance in a nearly non-destructive way. Furthermore the results shall demonstrate the functionality and convenience of the short-term corrosion test methods EN and KP in order to gain more acceptance within the scientific community. The results will allow the extraction of surface treatment effects on the corrosion behavior of the martensitic stainless steels 1.4116, 1.4034, and 1.4021.
ln den letzten Jahren hat sich gezeigt, dass die Ermittlung des Schwellenwertes DeltaKth nach den bestehenden Standardvorschriften für verschiedene Materialien zu nichtkonservativen Werten führt. Das ergibt sich im Vergleich mit Schwellenwerten, die man mit Anrissen erhält, die hinsichtlich der Ober- und der Unterlast komplett im Druckbereich erzeugt wurden. Dort, wo die Diskrepanz auftritt, verstärkt sie sich mit abnehmendem Spannungsverhältnis. ln der vorliegenden Studie wurden an einem mittel- und einem hochfesten Stahl bei unterschiedlichen Spannungsverhältnissen Schwellenwerte bestimmt. Anwendung fanden die konventionelle Lastabsenkungsmethode nach ASTM-Standard und ein Verfahren, bei dem der Langrissscbwellenwert als Endpunkt der sogenannten Zyklischen R-Kurve erhalten wird. Dieses folgt im Wesentlichen der von Pippan et al. entwickelten Methode, ergänzt diese jedoch durch eine eigene Verfahrensvariante.
In Deutschland fallen aktuell über 5 Mio. Tonnen Hausmüllverbrennungsaschen (HMVA) pro Jahr an. Aus diesen werden nur ca. 8 % Metalle (davon ca. 1 % NE-Metalle) zurückgewonnen. Zur Beurteilung des Wertstoffpotentials werden die HMVA nach standardisierten Vorschriften beprobt, für die Analytik vorbehandelt/vorbereitet/aufgearbeitet und auf ihre Inhaltsstoffe analysiert. Im nachfolgenden Beitrag wird der Schwerpunkt auf die Probenvorbehandlung und -vorbereitung gelegt, wobei der Merkmalstransfer von der Ausgangs-(Feld-)Probe über die Laborprobe und die Prüfprobe bis zur Mess-(Analysen-) Probe am Beispiel von NE-Metallen einer nassaufbereiteten HMVA untersucht wurde. Die Ergebnisse wurden mit Hilfe statistischer Methoden bewertet. Die Ergebnisse zeigen, dass die Verteilung der NE-Metalle in den einzelnen Schritten der Probenbehandlung elementspezifisch ist. Bei Blei ist ein Erhalt der Merkmalsverteilung über alle Behandlungsschritte erkennbar. Bei Kupfer nehmen die Konzentrationen in den aufeinander folgenden Behandlungsschritten deutlich ab. Die Ursache könnte das in der Feinfraktion enthaltene metallische Kupfer mit seinen spezifischen Eigenschaften sein. -------------------------------------------------------------------------------------------------------------------------------------------
More than 5 billion tons of municipal solid waste incineration bottom ashes (MSWI BA) are generated by incineration per year in Germany. Currently only 8 % of metals (of these 1 % are non-ferrous metals) are recovered from MSWI BA. For characterization of recovery potential, MSWI BA samples have to be taken, pre-treated and analyzed according to standardized methods. This manuscript focuses on sample pre-treatment and preparation of a MSWI BA sample aiming to investigate the characteristics transfer over the process of sub-sampling from the original (field) sample to the laboratory sample, test sample until the analytical sample. All results have been evaluated with statistical methods. The results show that influence of each single pre-treatment and preparation step on metal content differs for the individual metals. For lead a conservation of characteristics distribution can be observed, while for copper a continuous decline of solid concentration is observed over all preparation steps. One possible reason may be the fact that copper is mainly contained in the fine fraction as metallic copper with specific properties.
We report on the formation of polymer-stabilized superparamagnetic single-core and multi-core maghemite nanoparticles. The particle formation was carried out by coprecipitation of Fe(II) and Fe(III) sulfate in a continuous aqueous process using a micromixer system. Aggregates containing 50 primary particles with sizes of 2 nm were formed at a reaction temperature of 30 °C. These particles aggregated further with time and were not stable. In contrast, stable single-core particles with a diameter of 7 nm were formed at 80 °C as revealed by small-angle X-ray scattering (SAXS) coupled in-line with the micromixer for particle characterization. X-ray diffraction and TEM confirmed the SAXS results. X-ray absorption near-edge structure spectroscopy (XANES) identified the iron oxide phase as maghemite.
Particle size modality in bi-modal iron oxide suspensions was resolved by exploiting complex ac-susceptibility (ACS), small angle X-ray scattering (SAXS) and photon cross-correlation spectroscopy. To explain dynamic magnetic response of bi-modal suspensions, the Debye model was expanded to a linear superposition form allowing for the contribution of both particle fractions. This modified and adopted model is able to resolve the bi-modal particle size distributions. The SAXS curves of mono- and bi-modal suspensions were fitted well using a Monte Carlo simulation scheme, allowing the detection of bi-modal particle size distributions with high precision.
Resovist® originally developed as a clinical liver contrast agent for Magnetic Resonance Imaging exhibits also an outstanding performance as a tracer in Magnetic Particle Imaging (MPI). In order to study the physical mechanism of the high MPI performance of Resovist®, we applied asymmetric flow fieldflow fractionation (A4F) and static magnetic fractionation (SMF) to separate Resovist® into a set of fractions with defined size classes. As A4F based on an elution method separates MNP according to their hydrodynamic size, SMF fractionates a particle distribution by its magnetic moment. The obtained fractions of both separation techniques were then magnetically characterized by magnetorelaxometry measurements to extract the corresponding effective magnetic anisotropy and hydrodynamic size distribution parameters. Additionally, the MPI performance of each fraction was assessed using magnetic particle spectroscopy. With both separation techniques fractions (normalized to their iron amount) an MPI signal gain of a factor of two could be obtained, even though the distribution of effective anisotropy and hydrodynamic size were significantly different. Relating these findings to the results from magnetic characterization allows for a better understanding of the underlying mechanisms of MPI performance of Resovist®. This knowledge may help to improve the design of novel MPI tracers and development of separation methods.
Shedding light onto the spectra of lime: Raman and luminescence bands of CaO, Ca(OH)2 and CaCO3
(2015)
In microscopy studies of 19th-century cement stone, we found free lime in the form of darkened spherical structures, as they were described in the literature already. When trying to determine their phase composition by Raman spectroscopy, we encountered contradictive assignments in literature spectra of the lime phases CaO, Ca(OH)2 and CaCO3 and observed strong spectral features that have been ignored or erroneously assigned so far. In this study we present Raman spectra of pure lime phases and of a naturally grown calcite crystal, burnt limestone (quick lime, mainly CaO), aged slaked lime putty (mainly Ca(OH)2), and carbonated lime putty (mainly CaCO3). Based on the results, we shed light mainly onto these two questions: (1) Does CaO have a Raman spectrum? (2) Which features in the spectra are luminescence bands that could be (and already have been) misinterpreted as Raman bands? We proof our assignment of luminescence bands in lime phases by using three different laser wavelengths for excitation, and give hypotheses on the origin of the luminescence as well as practical advices on how to identify these misleading features in Raman spectra. This article is mainly addressed to users of Raman spectroscopy in different fields of material analysis who might not be aware of the presence of interfering bands in their spectra.
Thermal ionisation, also known as surface ionisation, was one of the first ionisation techniques developed for mass spectrometry, having been invented as early as 1918. The ionization process, described by the empirically derived “fractionation laws”, is widely understood. Isotope ratio measurements can be achieved with high precision and accuracy. Due to this, thermal ionisation has paved the way for great scientific achievements including: the discovery of new isotopes, the determination of radioactive half-lives and atomic weights of the elements, the accurate determination of the age of the earth and investigations on human society in the past such as mobility and trade. TIMS is still regarded as ‘golden standard’ in isotope ratio measurements. Thus the method is a reference technique that remains at the forefront of isotopic analysis particularly in the fields of metrology. A concise overview is given here of the technical background of thermal ionisation as well as the numerous applications of this technique in earth sciences, industry, metrology, and nuclear forensics.
This paper indicates that the tribological behavior under dry sliding of a Fe3Al-niobium carbide (NbC) composite prepared by pyrometallurgical synthesis was compared to NbC-based hard metals bonded by cobalt or Fe3Al. The dry sliding wear resistance (0,1-7/10 m/s) of the present Fe3Al-NbC with ∼60% NbC was close to those known of NbC-based hard metals. No grain pull-outs or fragmentations of the NbC grains were seen in the wear tracks, as a metallurgical interphase was formed between matrix and NbC grains.
Measurement strategies
(2015)
Designing an appropriate measurement strategy for a particular analytical question is not always obvious, since a number of factors have to be considered, whereby some of them might be difficult to define. A set of key questions generally precede the experimental design in analytical measurements and help to choose the measurement strategy, which is fit for the intended use – in the particular case of the content of this book – either for quantification, elemental ratio or isotope ratio analyses, accordingly.
Maintenance, Repair and Overhaul (MRO) is acquiring increasing commercial and socio-economic significance. For products and goods with high investment costs and a long lifespan, especially in the sectors of energy and transportation, a considerable portion of commercial profits are generated by after-sales services. In the field of research and development, not enough attention has been paid so far to tasks and approaches involving MRO. The field thus has a limited scientific background, despite a high potential in the business sector for technological and scientific optimization. The challenges and chances of MRO for sustainable enterprises will be explained with reference to the Fraunhofer Innovation Cluster Maintenance, Repair and Overhaul in Energy and Transport. The developments and project results of the four fields of innovation »Cleaning«, »Repair and Overhaul«, »Condition Monitoring and Diagnosis«, as well as »MRO Planning and Digital Assistance« will be explained.
In- and quasielastic neutron scattering is employed to investigate both the vibrational density of states and the molecular dynamics of two homologous discotic liquid crystals (DLC) with different length of the alkyl side chain based on a triphenylene derivate. For both compounds characteristic low frequency excess contributions to the vibrational density of states are found. Therefore it is concluded that these liquid crystals show a glass-like behaviour. Elastic scans further show that in these materials a rich molecular dynamics takes place.
The application of high-strength fine-grained structural steels with yield strengths greater than or equal to 690 MPa expands because of present light weight design trends. The requirements regarding the welded components safety increased due to high loading capacity. This determines a sustainable and economic application as well. However, high welding residual stresses could diminish the components safety, especially due to high restraint conditions in component or repair welds. Therefore, this work is concerned with global and local welding stresses, especially crack-critical welding stresses in the HAZ and while root welding due to the restraint conditions. Restraint intensities of real components were analysed and realised with two different weld tests, alongside two different plate dimensions and steel grades. A comparison of the test results showed several significant effects for heat control and restraint intensity regarding restraint forces and local welding stresses. Among these effects, substantial influences were found for the filler metal selection with partially altered results for root and filler beads. Local stresses of weld seam and HAZ were affected differently.
For the description of (single) crystal orientations, e.g. as measured by electron backscatter diffraction (EBSD) & X-ray diffraction (XRD), Euler angles are still generally used to import and export data. However, because of the lack of standard definitions for the unit cell reference settings and specimen axes, several transformation descriptions exist which produce different sets of Euler angles for the same orientation. There is also no recommended region within the minimal Euler orientation space into which orientations should be placed. This is the reason why different sets of Euler angles for the same orientation are generated by the available software packages for indexing EBSD patterns. These issues are reviewed and addressed.
The influence of crystal symmetry in form of chiral (enantiomorphic) groups is discussed, as well as how multiple, but symmetry-equivalent sets of Euler angles can be reduced in order to deliver a unique orientation description. The Euler coloring algorithms applied to EBSD map data is critically discussed. The specific case of cubic symmetry, especially the effect of the three-fold rotation on the Euler space is investigated in more detail for the highest-symmetric chiral group 432. Recommendations for standard settings of the unit cell to orthogonal coordinate system transformation are given which exploit inherent symmetry.
The formation of laser-induced periodic surface structures (LIPSS) on different materials (silicon, fused silica, quartz) with linearly polarized fs-laser irradiation is studied experimentally. In dielectrics, the importance of transient excitation stages in the LIPSS formation is demonstrated by using (multiple) cross-polarized double-fs-laser-pulse irradiation sequences. A characteristic decrease of the spatial LIPSS periods is observed for double-pulse delays of less than 2 ps along with a characteristic 90°-rotation of the LIPSS orientation.
Polyglycerol (PG) coated polypropylene (PP) films were synthesized in a two-step approach that involved plasma bromination and subsequently grafting hyperbranched polyglycerols with very few amino functionalities. The influence of different molecular weights and density of reactive linkers were investigated for the grafted PGs. Longer bromination times and higher amounts of linkers on the surface afforded long-term stability. The protein adsorption and bacteria attachment of the PP-PG films were studied. Their extremely low amine content proved to be beneficial for preventing bacteria attachment.
A two-step separation procedure for the quantification of Pd and Pt in automotive exhaust emissions using isotope dilution mass spectrometry was established using a combination of cation and anion exchange chemistry. AG 50W-X12 was used as cation exchange resin and DGA as weakly basic anion exchange resin. This procedure enabled the effective separation of Pd and Pt from the matrix and from interfering elements. Additionally Pd and Pt were collected in separate chromatographic fractions, which increased the precision of the isotope ratio determination by separate measurements using single collector sector field ICPMS. The analytical procedure was validated by analysing the synthetically prepared samples and the certified reference materials BCR-723 (road dust) and IAEA-450 (algae). For the SI-traceable results complete uncertainty budgets were calculated yielding relatively expanded uncertainties (k = 2) of ≈1% for analyte masses in the ng range. Procedure blanks of 55 pg Pd and 3 pg Pt were obtained. The detection limits were calculated as 12 pg for Pd and 7 pg for Pt. Additionally, Pd and Pt blank levels of different filter materials are presented as well as the first results for automotive exhaust particles collected on cellulose filters.
Beim Abreißen von Flaschenventilen an Atemluftflaschen wird schlagartig sehr viel Energie frei. Im Beitrag wird auf Unfälle im Zusammenhang mit Atemschutzgeräten, welche gerade nicht im Einsatz verwendet werden, eingegangen. Es wird beschrieben, welche die häufigsten Fehler bei der Handhabung solcher Geräte sind, was im schlimmsten Fall passieren kann und an welchen Stellen welche Maßnahmen ergriffen werden sollten, um die Unfallfolgen zu begrenzen bzw. den Unfall zu vermeiden.
Effective cleanup of groundwater contaminated with radionuclides using permeable reactive barriers
(2015)
The mining of natural resources always causes environmental impacts such as land use, large quantities of waste, destruction of habitat, impairment of groundwater regime, and quite possibly contamination of soil, water, or air (Dudka and Adriano 1997). The environmental impact of mining cannot be estimated easily. The concept of total material requirement (TMR) is an attempt to quantify the environmental impact of materials. TMR is the sum of domestic and imported primary natural resources and their hidden flows (Adriaanse et al. 1997). Hidden flows are often not considered in environmental analyses because they are attributed with no cost. However, overburden from mining, earth moving for construction, and soil erosion are major sources of ecological damage. From the mining of minerals to the final products, a number of process steps take place (exploration, mine site development, extraction, milling, washing, concentration, smelting, refining, fabrication), each step being connected to other input flows such as energy or other resources. The hidden flows for metals related to metal ore mining have been investigated by Halada et al. (2001). Table 9.1 lists the data for some metals, together with the data for some other minerals and fuels. The TMR in the United States in the 1990s was between 80 and 100 tonnes per capita; in the European Union (EU-15) approximately 50 tonnes per capita (Bringezu 2002).
In order to assess the anisotropy-related uncertainties of relatively determined photoluminescence quantum yields (ΦPL) of molecular emitters and luminescent nanomaterials, we compared ΦPL values measured without and with polarizers using magic angle conditions and studied systematically the dependence of the detected emission intensity on the polarizer settings for samples of varying anisotropy. This includes a dispersion of a spherical quantum dot (QD) with an ideally isotropic emission, a solution of a common small organic dye in a fluid solvent as well as dispersions of elongated quantum dot rods (QDR) with an anisotropic luminescence and a small organic dye in a rigid polymeric matrix, as ideally anisotropic emitter. Our results show that for instruments lacking polarizers, anisotropy-related measurement uncertainties of relative photoluminescence quantum yields can amount to more than 40%, with the size of these systematic errors depending on the difference in emission anisotropy between the sample and the standard.
Mit einer neuartigen analytischen Zentrifuge können Klebverbindungen, Beschichtungen und Kompositwerkstoffe untersucht werden. Die Idee der Wissenschaftler an der BAM Bundesanstalt für Materialforschung und -prüfung: Die Proben müssen nicht mehr eingespannt, sondern nur noch eingesteckt werden. Durch das einfache Einstecken der Prüfkörper ist eine sehr schnelle Beladung möglich. Zudem können bis zu acht Proben gleichzeitig unter identischen Bedingungen geprüft werden. Konventionelle Zugprüfmaschinen waren und sind nur in der Lage, einen (eingespannten) Probekörper zu testen. Das von BAM-Forschern bereits 2004 zum Patent angemeldete Funktionsprinzip wurde seitdem von der Berliner LUM GmbH als Lizenznehmer zum marktreifen Produkt weiterentwickelt.
Radiologic evaluation techniques are nondestructive testing (NDT) used to detect the bulk of explosives and contraband materials in large objects. As compared to conventional low-energy (<450 key) X-ray imaging, high-energy (>1 MeV) digital X-ray radiography is required for the NOT of large containers because of the need for high penetration through thick materials, sensitivity, and the ability to distinguish between low-and high-Z materials. Mobile, high-energy, and high-resolution radiologic techniques are useful to detect contraband and threat materials in digital radiographic images of containers with complex packing. This paper presents a mobile, high-energy X-ray radiographic technique for the in-field nondestructive inspection of cargo containers. The developed experimental technique consisted of a betatron as a high-energy (7.5 MeV) X-ray source and a high-resolution (400 mu m) matrix detector for the digital X-ray imaging. In order to evaluate the detection efficiency and image quality of the measurement technique, a test specimen was proposed that was made of a 3 mm thick steel container with an inner dimension of 60 x 30 x 40 cm(3) comprising different low-and high-Z materials. Image quality indicators were used to assess the essential image quality parameters such as image basic spatial resolution, effective attenuation coefficient, and signal-to-noise ratio (SNR). Experimental investigations were performed on a 6.1 m sea freight container with mockup dangerous materials in complex packing. Preliminary experimental results showed that the proposed technique was able to distinguish between liquids and solids, as well as detect contraband materials. Furthermore, a remarkable SNR of 400 was achieved in the measured digital X-ray images. The influence of temperature on X-ray radiation dose rate at different X-ray energies was also investigated. Finally, important applications of the proposed technique in the context of maritime security are discussed.
In den Untersuchungen zum Zündvermögen von Filmeffektzündern wurde nachgewiesen, dass diese einen Plastiksprengstoff auf Basis von PETN nicht zu einer detonativen Umsetzung anregen können. Die Erfüllung der grundlegenden Sicherheitsanforderung (ESR) des Anhanges 1 der Richtlinie 2013/29/EG und die Kategorisierung als pyrotechnischer Gegenstand für Theater (T2) kann somit als gegeben angesehen werden, da der verwendete Explosivstoff zur Gruppe der sensibelsten Sprengstoffe (Initiierung mit geringen Zündenergien) gehört. Es wurde weiterhin nachgewiesen, dass der Untemassertest nach DIN EN 13763 Teil 15 aussagekräftige Ergebnisse liefert, welche die Fähigkeit von Filmeffektzündern und vergleichbaren pyrotechnischen Gegenständen bestätigen respektive widerlegen, einen Sekundärsprengstoff zu zünden (eine Detonation zu initiieren).
Für eine allgemeine Einschätzung des Zündvermögens von Filmeffektzündern und vergleichbaren pyrotechnischen Gegenständen ist ein Grenzbereich für ein äquivalentes Zündvermögen in g PETN auf Basis der Experimente mit dem o. g. Unterwassertest bestimmt worden. Filmeffektzünder und vergleichbare pyrotechnische Gegenstände sind nicht in der Lage, einen Sekundärsprengstoff zur Detonation anzuregen, wenn das aus dem Unterwassertest ermittelte äquivalente Zündvermögen unter 0,25 g PETN liegt.
Auswirkungen von Ermüdungsbeanspruchungen auf Struktur und Eigenschaften von Fahrbahndeckenbeton
(2015)
Ausgehend von der Zielsetzung der DFG-Forschergruppe 1498, die Einflüsse auf den AKR-Schädigungsprozess in Fahrbahndecken aus Beton grundlegend zu klären, sind zwei aufeinander aufbauende Untersuchungsschwerpunkte Gegenstand dieses Beitrags. Im ersten Schwerpunkt wurden die prüftechnischen Voraussetzungen für die Charakterisierung der Degradation und damit der Rissbildung im Fahrbahndeckenbeton durch die Vorschädigung infolge von Ermüdungsbeanspruchungen geschaffen. Realisiert wurde dies durch die Implementierung und Optimierung eines Monitoringsystems im zyklischen 4-Punkt-Biegeversuch zur simultanen Erfassung der Rissbildung im großformatigen Schwingbalken. Zusätzlich wurde die Röntgen-3D-Computertomografie für die hochauflösende räumliche quantitative Rissanalyse in den Bohrkernen aus den Schwingbalken ohne und mit Vorschädigung weiterentwickelt. Im zweiten Untersuchungsschwerpunkt wurde mittels vielfältiger Experimente an kleinformatigen Probekörpern aus dem Schwingbalken gezeigt, dass durch die Ermüdungsbeanspruchung die bruchmechanischen Materialkennwerte des Betons zum Teil eine signifikante Veränderung erfahren. Based on the objective of the DFG (German research foundation) funded research group 1498 to clarify the influences on the ASR damage process, this paper deals with two focuses of investigation. In the first focus the technical requirements for the characterisation concerning the degradation and the formation of cracks in concrete pavements by the pre-damage as a result of fatigue loading were created. This was realized by the implementation and the optimisation of a monitoring system in the cyclic four point bending test to capture simultaneously the formation of cracks in the beam under sinusoidal bending load. In addition, the X-ray 3D-computed tomography was enhanced for the high-resolution quantitative spatial crack analysis in the drilling cores extracted of the beam under sinusoidal bending load without and with a pre-damage. Building on the first focus, in the second focus of investigation a significant change of the fracture-mechanical properties of the concrete as a result of fatigue loading has been demonstrated in numerous experiments using small specimens extracted from the beam under sinusoidal bending load.
This paper presents a new X-ray backscatter technique (XBT) for non-destructive imaging of aerospace materials with only a single-sided access. It uses a special twisted slit collimator to inspect the whole object by changing the viewing direction of the X-ray backscatter camera. For the first time, the X-ray backscatter measurements were conducted using high-energy (>500 keV) X-ray sources. Experiments were performed on thick complex structured aluminium components, stringers and honeycomb structures to validate the applicability of the present technique to image small changes in the material properties and also to detect low-density material inclusions. In order to reduce the inspection time from hours to several seconds and to improve the image quality of the X-ray backscatter image, the backscattered signals were measured using a digital detector array with high spatial resolution (200 µm). The influence of the energy of the X-ray source and the slit width of the camera on the X-ray backscatter image were also investigated. In the proposed technique, the whole object is irradiated by an un-collimated X-ray beam resulting in a low image acquisition time of 3 min that facilitates the use of XBT for the real time NDT&E of aerospace materials.