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Traceable morphological and chemical characterization of nanomaterials with respect to the various possible sizes, size distributions, shapes, and concentrations of real-world nanoparticles (NPs) is a challenging task. Particularly for the nonspherical, non-monodisperse nanoparticles – as typically for most of the commercial particles, including their strong tendency to agglomerate, there is a lack of standard operation procedures providing accurate nanoparticle characterisation.
In the framework of the pre-standardisation framework of VAMAS (Versailles Project on Advanced Materials and Standards, www.vamas.org) two interlaboratory comparison (ILC) studies are being carried out under the Technical Working Area (TWA) 34 “Nanoparticle Populations”:i) Project #15 addresses the analysis of the size and shape distribution of TiO2 bipyramidal NPs by traceable imaging methods such as TEM, SEM, STEM-in-SEM, AFM as well as with SAXS as an ensemble method. This ILC is thought as the next level development of the case studies exemplified in the published ISO standards ISO 21363 and ISO 19749. It was agreed to complete the first ILC with the NPs already prepared according to the same procedure on a TEM grid, and, at a later stage, to carry out second ILCs with the same NPs distributed to the participants as liquid suspensions together with protocols for the uniform NP deposition on suited substrates - as developed and optimized within the European project nPSize. Once having good deposition protocols available, the door for automated image analysis gets opened. Corresponding image analysis protocols and reporting templates have been distributed to the ILC participants, too.
ii) Project #16: two spherical SiO2 NP samples with bi-modal size distributions in two nominal relative number concentrations were prepared and distributed also as liquid suspensions accompanied by sample preparation, measurement, and image analysis protocols and reporting templates. Here, the NP concentration is the primary parameter to be measured. For the imaging methods it is targeted to
measure the relative nanoparticle concentrations (relative populations of the two modes).
The results of all the participating laboratories, in both ILCs, compiled in comparative representations will be shown and discussed for the first time. The reduction of the measurement uncertainties associated to the size, shape and number-concentration results induced by the significant improvement of the sample preparation on substrates (as single particles with a high-density coverage), combined with welldefined image analysis procedures will be highlighted.
The consideration of ageing mechanisms is with integration into the IAEA-requirements now obligatory for the design of transport packages. For packages intended to be used for shipment after storage the consideration of the effects of ageing mechanisms during storage in safety analyses and the implementation of corresponding instructions for operation and maintenance are required. Therefore, these packages have been maintained during storage in a manner that all requirements specified in the IAEA-requirements and in the applicable certificates of approval have been fulfilled.
BAM is the competent authority in Germany for evaluating the thermal and mechanical design of packages for the transport of radioactive materials. In this context, BAM also evaluates the aging mechanisms and aging effects occurring during the long-term storage period of such transport packages. BAM has developed a guideline for the implementation of ageing assessment and of the measures for ageing management into the approval procedure based on IAEA-requirements.
The goal of the presented paper is to introduce this guideline and the general approach for ageing management requirements and to describe the application to a specific package design. The type and amount of the ageing management not only depend on the use of the packaging, but also on the accessibility of the components that are considered in the ageing assessment. The different operating phases of a packaging are considered for the ageing assessment, such as loading, interim storage or transport.
The implementation of measures for ageing management is divided into three levels – systemic measures, package design related measures and documentation. The systemic measures are attributed to the general management system and define the whole activities for organization of ageing management like structure, responsibilities, documentation, reports and evaluation. The package design related measures are defined in an ageing management plan. These measures shall ensure that the anticipated changes of the package design under consideration of ageing effects still complies with the design approval specification. Therefore, an ageing surveillance program and, if necessary, a gap analysis program shall be developed. The ageing management documentation ensures the continuous documentation of the compliance of a specific package to the approved package design, comprising mainly records resulting from operation and surveillance.
Use/distribution of cost-effective and biocompatible pieces of cellulose paper as passive optical chemosensors and readout by the camera system.
Modification of the paper surface using various chemically sensitive dyes (indicators) provides an optically detectable reaction and conclusions about the target substances and precise location.
In infrared thermography, the interaction of the heat flow with the internal geometry or inhomogeneities in a sample and their effect on the transient temperature distribution is used, e.g., to detect defects non-destructively. An equivalent way of describing this is the propagation of thermal waves inside the sample. Although thermography is suitable for a wide range of inhomogeneities and materials, the fundamental limitation is the diffuse nature of thermal waves and the need to measure their effect radiometrically at the sample surface only. The crucial difference between diffuse thermal waves and propagating waves, as they occur, e.g., in ultrasound, is the rapid degradation of spatial resolution with increasing defect depth. This degradation usually limits the applicability of thermography for finding small defects on and below the surface.
A promising approach to improve the spatial resolution and thus the detection sensitivity and reconstruction quality of the thermographic technique lies in the shaping of these diffuse thermal wave fields using structured laser thermography.
Some examples are:
• Narrow crack-like defects below the surface can be detected with high sensitivity by superimposing several interfering thermal wave fields,
• Defects very close to each other can be separated by multiple measurements with varying heating structures,
• Defects at different depths can be distinguished by an optimized temporal shaping of the thermal excitation function,
• Narrow cracks on the surface can be found by robotic scanning with focused laser spots.
We present the latest results of this technology obtained with high-power laser systems and modern numerical methods.
Thermographic NDT is based on the interaction of thermal waves with inhomogeneities. The propagation of thermal waves from the heat source to the inhomogeneity and to the detection surface according to the thermal diffusion equation leads to the fact that two closely spaced defects can be incorrectly detected as one defect in the measured thermogram. In order to break this spatial resolution limit (super resolution), the combination of spatially structured heating and numerical methods of compressed sensing can be used.
The improvement of the spatial resolution for defect detection then depends in the classical sense directly on the number of measurements. Current practical implementations of this super resolution detection still suffer from long measurement times, since not only the achievable resolution depends on performing multiple measurements, but due to the use of single spot laser sources or laser arrays with low pixel count, also the scanning process itself is quite slow. With the application of most recent high-power digital micromirror device (DMD) based laser projector technology this issue can now be overcome.
Our studies deal with the application of fully 2D-structured DMD-based excitation and subsequent super-resolution-based defect reconstruction. We analyze the influence of different testing parameters, like the number of measurements or the white content of the excitation pattern. Furthermore, we have dealt with the choice of parameters in the reconstruction that have an influence on the underlying minimization problem in terms of compressed sensing. Finally, the results of the super resolution reconstruction are compared with the results based on conventional thermographic testing methods.
Die zunehmende Bedeutung der luftgekoppelten Ultraschallprüfung (ACUT) in der zerstörungsfreien Prüfung (ZfP) unterstreicht die Notwendigkeit von standardisierten Abläufen und Methoden. Bei der ACUT bestehen grundlegende Unterschiede zur manuell durchgeführten Ultraschallprüfung mit Kontakttechnik oder zur automatisierten Tauchtechnik. Die Unterschiede bei der Bestimmung von Prüfkopfparametern für ACUT wurde von Herstellern, Forschungseinrichtungen und Anwendern bereits als wichtig erkannt, was sie veranlasst hat, im Rahmen des Unterausschusses Luftgekoppelte Ultraschallprüfung der DGZfP die Richtlinie US08 zur standardisierten Charakterisierung von luftgekoppelten Ultraschallwandlern zu erarbeiten. Darüber hinaus bestehen auch bei der Durchführung einer Messung grundlegende Unterschiede, die aktuell in einem Leitfaden zusammengetragen und definiert werden.
In diesem Beitrag wird ein Überblick über die geplanten Inhalte dieses Leitfadens gegeben. Insbesondere wird die Auswahl von Prüfparametern in Form von Frequenzen, Abständen und Positionierung sowie die Auswertung behandelt. Darüber hinaus werden die Ergebnisse eines Ringversuchs vorgestellt, welcher an einem eigens hierfür entwickelten und mit Defekten versehenem Prüfkörper, der sog. ACUT-Prüfplatte, durchgeführt wurde. In diesem Ringversuch werden unterschiedliche Messanordnungen, die mittels luftgekoppeltem Ultraschall möglich sind, anhand des erreichbaren Signal-Rausch-Verhältnisses sowie der messbaren Defektgröße quantifiziert. Zudem findet eine Abgrenzung zu weiteren gängigen Verfahren der ZfP statt. Anhand der hier vorgestellten Ergebnisse ist es möglich, die Anwendbarkeit des luftgekoppelten Ultraschalls unter Berücksichtigung unterschiedlicher Messanordnungen besser einzuschätzen.
Die größten Vorteile der luftgekoppelten Ultraschallprüfung sind: die berührungslose Prüfung und der Verzicht auf ein flüssiges Koppelmittel. Allerdings weisen die meisten luftgekoppelten Prüfszenarien ein sehr geringes Signal-zu-Rausch-Verhältnis (SNR) auf und die Pegel, die von luftgekoppelten Ultraschallwandlern realisiert werden, sind um mehrere Größenordnungen kleiner.
Da diese Herausforderung auch in anderen Disziplinen wie bspw. der Radartechnik existiert und dort ebenfalls eine entscheidende Rolle spielt, wurde die dort eingesetzte Pulskompression auf die physikalischen Gegebenheiten der luftgekoppelten Ultraschallprüfung angepasst und angewandt.
Dieser Beitrag präsentiert die Ergebnisse von zwei Versuchsaufbauten: 1) ein thermoakustischer Sender und ein optisches Mikrofon und 2) ein Paar Ferroelektret-Wandler als Sender und Empfänger. Aufgrund der physikalischen Randbedingungen wurden unipolare Kodierungen verwendet. Die Verwendung von unipolaren Kodes zur Modulation der Anregungssignale stellt dabei eine neue Methode dar, die so die Pulskompression für Ferroelektret- und thermoakustische Wandler ermöglichen soll. Die Anwendung der Pulskompression auf die Kombination aus thermoakustischem Sender und optischem Mikrofon konnte das Signal-zu-Rausch-Verhältnis um bis zu 15 dB und für die Ferroelektret-Wandler um bis zu 23 dB erhöhen.
In this paper, we investigate the influence of different heat source pulse shapes by Infrared impulse thermography (IRT) on the results of the thermal shock response spectrum (TSRS) methodology. TSRS is a new alternative approach for evaluating impulse thermography (IRT) data based on an analogy to Shock Response Spectrum (SRS) analysis (ISO 18431) for mechanical systems. It allows processing the entire recorded signal without truncating the saturated thermogram, as in pulse-phase thermography (PPT) or thermal signal reconstruction (TSR). For this purpose, we use a widespread halogen lamp as heat source as well as laser spot. The laser source enables not only to generate a precise shape of the pulse, but also to heat a specific area of the sample uniformly. This makes it possible to suppress influences of lateral fluxes due to uneven distribution of the excitation source on the surface of the specimen and leads to improved results. In order to quantitatively compare the results and to investigate the possible influence of the source shape on the TSRS, the Tanimoto criterion and the signal-to-noise ratio (SNR) were applied to the region of interest (ROI) of the carbon fiber reinforced polymer (CFRP) laminate with artificial defects as defect detectability criterion.