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Paper des Monats
- ja (25)
The presentation summarizes our recent results on the coupled electrochemical methods for high resolution corrosion studies. The combination of Scanning Electrochemical Microscopy (SECM) and multielectrode (MMA) based real-time corrosion monitoring was presented as a new method for achieving high time resolution in local electrochemical analysis. Correlative imaging by means of Atomic Force Microscopy (AFM) and Scanning Electron Microscopy (SEM) was demonstrated as a tool for the investigation of local corrosion processes initiated by the intermetallic particles (IMPs) on AA2024-T3 aluminium alloy.
The performance of functional coatings and adhesively joined hybrid components relies strongly on the stability of the polymer-metal interface. With the increasing utilization of multi-material structures in the automotive and aerospace industry, it is of great scientific and technical interest to understand the processes leading to interface degradation and to develop novel strategies to increase corrosion and delamination resistance.
The aim of this project is to develop thin epoxy-based films and their carbon nanofiller loaded composites on aluminium alloy AA2024-T3 as a model system and to investigate their interfacial stability under corrosive and coupled corrosive-mechanical load. Spin coating was used for the layer-by-layer deposition of poly[(o-cresyl glycidyl ether)-co-formaldehyde] and poly-(ethylenimine) bi-layers. Atomic force microscopy (AFM) results indicate a very homogeneous and dense film with low surface roughness. Carbon nanofillers were introduced either by mixing into the coating components or in between individual layers to control the separation between the carbon nanofillers and alloy surface. The film chemistry and barrier properties were characterized by means of spectroscopic and electrochemical methods, respectively. The degradation and delamination behavior of the epoxy-based films was characterized by means of in situ AFM corrosion experiments. The quantitative imaging (QI) mode allowed the observation of hydrogen-generation induced blister formation during exposure to corrosive electrolyte and how the local corrosion processes evolved with exposure time. Complementary energy dispersive X-ray spectroscopy (EDX) analysis was performed to correlate the corrosion behavior with the different intermetallic particle chemistries and distributions. The presentation will summarize our results on the effect of interface chemistry and carbon nanofiller – alloy separation on the initiation of local corrosion processes on thin film covered AA2024-T3 aluminium alloys.
Time-dependent in situ measurement of atmospheric corrosion rates of duplex stainless steel wires
(2018)
Corrosion rates of strained grade UNS S32202 (2202) and UNS S32205 (2205) duplex stainless steel wires have been measured, in situ, using time-lapse X-ray computed tomography. Exposures to chloride-containing (MgCl2) atmospheric environments at 50 °C (12–15 M Cl− and pH ~5) with different mechanical elastic and elastic/plastic loads were carried out over a period of 21 months. The corrosion rates for grade 2202 increased over time, showing selective dissolution with shallow corrosion sites, coalescing along the surface of the wire. Corrosion rates of grade 2205 decreased over time, showing both selective and pitting corrosion with more localised attack, growing preferentially in depth. The nucleation of stress corrosion cracking was observed in both wires.
Zänker, Steffen ; Scholz, Gudrun ; Krahl, Thoralf ; Prinz, Carsten ; Emmerling, Franziska ; Kemnitz, E.
Lanthanides doped coordination polymers (CPs) with different binding motifs were synthesized to investigate the influence of the different fluorine positions in the structure on the decay time τ of the excited states. Fluorine can be integrated into the network mechanochemically via a fluorinated organic linker, here barium tetrafluoroterephthalate Ba(p-BDC-F4)2 or directly via a metal-fluorine bond (barium terephthalate fluoride BaF(p-BDC)0.5). The CP with a metal-fluorine bond shows the highest lifetime of the excited states of lanthanides (Eu3+, Tb3+ or Eu3+& Tb3+). The excitation of the lanthanides can be performed directly via the excitation wavelength typical for lanthanides and via the excitation wavelength of the linker. This enabled the simultaneous excitation of Eu3+ and Tb3+ in one CP. In the emission spectra (λem = 393 nm) of the mixed doped CPs (Eu3+ and Tb3+) the bands of both lanthanides can be observed. The integration into the crystal lattice and the homogeneous distribution of the lanthanides in the CPs is shown by X-ray diffraction, TEM, STEM-EDS measurements and the long decay times.
Changes in the global bulk and local structures, of three different barium compounds (BaZrO3, BaF2, and BaFCl),were induced by mechanical milling and followed using X-ray powder diffraction (PXRD), subsequent microstructure analysis, and 137Ba solid state NMR spectroscopy. Harder materials like BaZrO3 experience significantly higher structural changes upon milling than softer materials like BaF2. Moreover, soft materials with layered structures, like BaFCl, show a pronounced structural change during the milling process. By combining PXRD and solid state NMR, detailed information on the changes to the global and local structures were obtained, which are of interest for mechanochemical synthesis, mechanically treated catalysts or ionic conductors.
Per- and polyfluoroalkyl substances (PFAS) are widely used for durable water-repellent finishing of different fabrics and textiles like outdoor clothing, carpets, medical textiles and more. Existing PFAS extraction techniques followed by target analysis are often insufficient in detecting widely used side-chain fluorinated polymers (SFPs) that are barely or non-extractable. SFPs are typically copolymers consisting of a non-fluorinated backbone with perfluoroalkyl side-chains to obtain desired properties. We compared the accessible analytical information and performance of complementary techniques based on oxidation (dTOP assay, PhotoTOP), hydrolysis (THP assay), standard extraction, extractable organic fluorine (EOF), and total fluorine (TF) with five functional textiles and characterized 7 further textiles only by PhotoTOP oxidation. The results show that when applied directly to textile samples, oxidation by dTOP and PhotoTOP and also hydrolysis by the THP are able to capture large fractions of the TF in form of perfluoroalkyl side-chains present in the textiles while methods relying on extracts (EOF, target and non-target analysis) were much lower (e.g., factor ~25-50 lower). The conversion of large fractions of the measured TF into PFCAs or FTOHs from fluorinated side chains is in contrast to previous studies. Concentrations ranged from <LOQ to over ~1000 mg F/kg after oxidation/hydrolysis and <LOQ to over 2000 mg F/kg for TF, while EOF and target PFAS in extracts were detected at much lower concentrations (up to ~ 60 mg F/kg) (amount of fluorine in the order: extraction << EOF << oxidation/hydrolysis ≤ TF). Perfluoroalkyl carboxylic acids (PFCAs) and fluorotelomer alcohols (FTOHs) from THP and PhotoTOP both represented the chain-length distribution in the textiles showing that long-chain SFPs are still used in current textiles. Further advantages and disadvantages of the applied methods are discussed.
Industrial Radiology is used for volumetric inspection of industrial objects. By penetration of these objects (typically weldments, pipes or castings) with X-ray or Gamma radiation the 3D-volume is projected onto a 2D image detector. The X-ray film is the oldest radiographic image detector and still in wide use in industry. The industrial X-ray film systems used today differ from these used in medicine. Medical film systems are described well in the literature, but industrial film systems not. So we start with a description of the properties and standards for industrial film systems. The requirements on image quality are defined by several standards and can be verified with different image quality indicators (IQIs). They describe the ability of the human being to detect small and low contrast indications in a noisy image background. The essential parameters for digital industrial radiology are described.
Since about 30 years electronic image detectors are gradually replacing the industrial film. These detectors are based on storage phosphor imaging plates in combination with Laser scanners (“Computed Radiography”, CR) or a variety of different digital detector arrays (DDA). Typical applications of CR and DDAs are discussed as well as new possibilities by digital image processing, which is enabled by the computer based image handling, processing and analysis.
X-ray back scatter imaging is rarely applied compared to classical X-ray projection imaging. More than 20 years ago the company Philips developed “COMSCAN”, a first application case for aircraft industry, which allowed even a depth resolution using back scatter imaging. The company AS&E in Boston offers back scatter imaging solutions for the security market. The principle is to scan the object with a highly collimated X-ray needle beam from one side only and to detect the backscattered radiation by a large area detector side by side with the collimation wheel. A new prototype is investigated at BAM for application and optimization in non-destructive testing. As modern industrial application field in-situ inspection in additive manufacturing is targeted. The accessibility of the printed part during the production process is very limited. This prevent the application of a two sided X-ray inspection or Computed Tomography, were an rotation of the object is required to acquire projections from 360 degrees. An important advantage for the X-ray back scatter technique are also the materials used in additive manufacturing (polymers, ceramics, light metals like Aluminum or Titanium). These materials with lower density and lower Z values give better scatter signals than metals with higher densities and Z values. The back scatter intensity decreases with increasing density and Z value of the material. But the requirements on spatial resolution and contrast sensitivity are more stringent for non-destructive testing of additive manufactured parts compared to the security area. In NDT sizes of indications smaller than 1 mm have to be detected clearly. The investigation of these limits on a state-of-the-art prototype for X-ray back scattering using rotating collimated X-ray needle beams is a part of the BAM project “ProMoAM”. The contribution shows first results of the optimization for NDT and the achieved application limits for several example cases.
X-ray back scatter imaging is rarely applied compared to classical X-ray projection imaging. 20 years ago the company Philips developed “COMSCAN”, a first application case in the aircraft industry, which allowed even a depth resolution using back scatter imaging. The company AS&E in Boston offers back scatter imaging solutions for the security market. Their principle is to scan the object with a highly collimated X-ray needle beam from one side only and detect the backscattered radiation by a large area detector side by side with the collimation wheel. A new prototype is investigated at BAM for application and optimization in non-destructive testing. As modern industrial application field in-situ testing in additive manufacturing is targeted. The accessibility of the printed part during the production process is very limited. This prevent the application of a two sided X-ray inspection or Computed Tomography, were an rotation of the object is required to acquire projections from 360 degrees. An important advantage for the X-ray back scatter technique are also the materials used in additive manufacturing (polymers, ceramics, light metals like Aluminum or Titanium). These materials with lower density and lower Z values give better scatter signals than metals with higher densities and Z values. The back scatter intensity decreases with increasing density and Z value of the material. But the requirements on spatial resolution and contrast sensitivity are more stringent for non-destructive testing of additive manufactured parts compared to the security area. In NDT sizes of indications smaller than 1 mm have to be detected clearly. The investigation of these limits on a stateof-the-art prototype for X-ray back scattering using rotating collimated X-ray needle beams is a part of the BAM project “ProMoAM”. The contribution shows first results of the optimization for NDT and the achieved application limits for several example cases.
X-ray back scatter imaging is rarely applied compared to classical X-ray projection imaging. 20 years ago the company Philips developed “COMSCAN”, a first application case in the aircraft industry, which allowed even a depth resolution using back scatter imaging. The company AS&E in Boston offers back scatter imaging solutions for the security market. Their principle is to scan the object with a highly collimated X-ray needle beam from one side only and detect the backscattered radiation by a large area detector side by side with the collimation wheel. A new prototype is investigated at BAM for application and optimization in non-destructive testing. As modern industrial application field in-situ testing in additive manufacturing is targeted. The accessibility of the printed part during the production process is very limited. This prevent the application of a two sided X-ray inspection or Computed Tomography, were an rotation of the object is required to acquire projections from 360 degrees. An important advantage for the X-ray back scatter technique are also the materials used in additive manufacturing (polymers, ceramics, light metals like Aluminum or Titanium). These materials with lower density and lower Z values give better scatter signals than metals with higher densities and Z values. The back scatter intensity decreases with increasing density and Z value of the material. But the requirements on spatial resolution and contrast sensitivity are more stringent for non-destructive testing of additive manufactured parts compared to the security area. In NDT sizes of indications smaller than 1 mm have to be detected clearly. The investigation of these limits on a stateof-the-art prototype for X-ray back scattering using rotating collimated X-ray needle beams is a part of the BAM project “ProMoAM”. The contribution shows first results of the optimization for NDT and the achieved application limits for several example cases.
The revision of ISO 24497:2007 started in 2017 (by decision of Com-V at the IIW annual assembly in Shanghai). After 3 years of discussions and incorporation of many comments from all over the world the working group C-V-E-b headed by Uwe Zscherpel finalized the work with a final draft to be forwarded for final vote at ISO TC 44. The working group C-V-E-b finalised the work and can be resolved. The chair thanks for all the successfully work done, the vote to forward the latest draft to ISO for final vote was done without any negative.
The transition from X-ray film to digital detectors in radiography is accompanied by an increase of unsharpness due to the larger inherent digital detector unsharpness in comparison to film. The basic spatial resolution of digital detectors (see EN ISO 17636-2) is used today to describe this unsharpness. The geometrical unsharpness of the radiographic projection of object structures onto the detector plane is determined by the focal spot size of the X-ray tube and the magnification. The focal spot size is measured today (see ASTM E 1165) from pin hole camera exposures or edge unsharpness (see ASTM E 2903). The final image unsharpness is a result of a convolution of the geometrical and inherent detector unsharpness function, divided by the magnification factor of the object onto the detector plane. Different approximations of this convolution result in ASTM E 1000 and ISO 17636-2 in different optimum values for the magnification factor for a given focal spot size of a X—ray tube and the basic spatial resolution of the detector. The higher contrast sensitivity, an advantage of digital radiography, compared to film radiography is furthermore improved when using higher X-ray voltages as used with film and smaller focal spots of the X-ray tubes. This allows a higher distance between object and detector resulting in reduced object scatter in the image. The interactions between all these parameters will be discussed and simple rules for practitioners will be derived in this contribution.
Heterogeneous Oxysulfide@Fluoride Core/ Shell Nanocrystals for Upconversion-Based Nanothermometry
(2022)
Zou, Q. ; Marcelot, C. ; Ratel-Ramond, N. ; Yi, X. ; Roblin, P. ; Frenzel, Florian ; Resch-Genger, Ute ; Eftekhari, A. ; Bouchet, A. ; Coudret, C. ; Verelst, M. ; Chen, X. ; Mauricot, R. ; Roux, C.
Lanthanide (Ln3+)-doped upconversion nanoparticles (UCNPs) often suffer from weak luminescence, especially when their sizes are ultrasmall (less than 10 nm). Enhancing the upconversion luminescence (UCL) efficiency of ultrasmall UCNPs has remained a challenge that must be undertaken if any practical applications are to be envisaged. Herein, we present a Ln3+-doped oxysulfide@fluoride core/shell heterostructure which shows efficient UCL properties under 980nm excitation and good stability in solution. Through epitaxial heterogeneous growth, a ∼4 nm optically inert β-NaYF4 shell was coated onto ∼5 nm ultrasmall Gd2O2S:20%Yb,1%Tm. These Gd2O2S:20%Yb,1%Tm@NaYF4 core/shell UCNPs exhibit a more than 800-fold increase in UCL intensity compared to the unprotected core, a 180-fold increase in luminescence decay time of the 3H4 → 3H6 Tm3+ transition from 5 to 900 μs, and an upconversion quantum yield (UCQY) of 0.76% at an excitation power density of 155 W/cm2. Likewise, Gd2O2S:20%Yb,2%Er@NaYF4 core/shell UCNPs show a nearly 5000-fold
increase of their UCL intensity compared to the Gd2O2S:20%Yb,2%Er core and a maximum UCQY of 0.61%. In the Yb/Er core−shell UCNP system, the observed variation of luminescence intensity ratio seems to originate from a change in lattice strain as the temperature is elevated. For nanothermometry applications, the thermal sensitivities based on thermally coupled levels are estimated for both Yb/Tm and Yb/Er doped Gd2O2S@NaYF4 core/shell UCNPs.
Zorn, R. ; Yin, Huajie ; Lohstroh, W. ; Harrison, W. ; Budd, P.M. ; Pauw, Brian Richard ; Böhning, Martin ; Schönhals, Andreas
Polymers with intrinsic microporosity are promising candidates for the active separation layer in gas separation membranes. Here, the vibrational density of states (VDOS) for PIM-1, the prototypical polymer with intrinsic microporosity, is investigated by means of inelastic neutron scattering. The results are compared to data measured for a more conventional high-performance polyimide used in gas separation membranes (Matrimid). The measured data show the characteristic low frequency excess contribution to VDOS above the Debye sound wave level, generally known as the Boson peak in glass-forming materials. In comparison to the Boson peak of Matrimid, that of PIM-1 is shifted to lower frequencies. This shift is discussed considering the microporous, sponge-like structure of PIM-1 as providing a higher compressibility at the molecular scale than for conventional polymers. For an annealed PIM-1 sample, the Boson peak shifts to higher frequencies in comparison to the un-annealed sample. These changes in the VDOS of the annealed PIM-1 sample are related to changes in the microporous structure as confirmed by X-ray scattering.
Zorn, R. ; Szymoniak, Paulina ; Kolmangadi, Mohamed Aejaz ; Wolf, M. ; Alentiev, D. ; Bermeshev, M. ; Böhning, Martin ; Schönhals, Andreas
Inelastic incoherent neutron time-of flight scattering was employed to measure the low frequency density of states for a series of addition polynorbornenes with bulky side groups. The rigid main chain in combination with the bulky side groups give rise to a microporosity of these polymers in the solid state. The microporosity characterized by the BET surfaces area varies systematically in the considered series. Such materials have some possible application as active separation layer in gas separation membranes.
All investigated materials show excess contributions to the Debye type density of states characteristic for glasses known as Boson peak. The maximum position of the Boson peak shifts to lower frequency values with increasing microporosity. Data for PIM-1 and Matrimid included for comparison are in good agreement to this dependency. This result supports the sound wave interpretation of the Boson peak.
Zorn, R. ; Szymoniak, Paulina ; Kolmangadi, Mohamed Aejaz ; Malpass-Evans, R. ; McKeown, N. ; Tyagi, M. ; Böhning, Martin ; Schönhals, Andreas
The microscopic diffusion and the low frequency density of states (VDOS) of PIM-EATB(CH3) are investigated by inelastic and quasi-elastic neutron scattering where also the demethylated counterpart of PIM-EA-TB(H2) is considered. These intrinsic microporous polymers are characterized by large BET surface area values of several hundred m2/g and pore sizes between 0.5 and 2 nm. Detailed comparison is made to the archetype of polymers of intrinsic microporosity, PIM-1, and polynorbornenes also bearing a microporosity. Due to the wavelength of neutrons, the diffusion and vibrations can be addressed on microscopic length and time scales. From the inelastic neutron scattering experiments the low frequency density of states (VDOS) is estimated which shows excess contributions to the Debye-type VDOS known as Boson peak. It was found that the maximum frequency of the Boson peak decreases with increasing microporosity characterized by the BET surface area. However, besides the BET surface area, additional factors such as the backbone stiffness govern the maximum frequency of the Boson peak. Further the mean squared displacement related to microscopic motions was estimated from elastic fixed window scans. At temperatures above 175 K, the mean squared displacement PIM-EA-TB(CH3) is higher than that for the demethylated counterpart PIM-EA-TB(H2). The additional contribution found for PIM-EATB(CH3) is ascribed to the rotation of the methyl group in this polymer because the only difference between the two structures is that PIM-EA-TB(CH3) has methyl groups where PIM-EA-TB(H2) has none. A detailed comparison of the molecular dynamics is also made to that of PIM-1 and the microporous polynorbornene PTCNSi1. The manuscript focuses on the importance of vibrations and the localized molecular mobility characterized by the microscopic diffusion on the gas Transport in polymeric separation membranes. In the frame of the random gate model localized fluctuations can open or close bottlenecks between pores to enable the diffusion of gas molecules.
Zorn, R. ; Lohstroh, W. ; Zamponi, M. ; Harrison, W. ; Budd, P. ; Böhning, Martin ; Schönhals, Andreas
Quasielastic neutron scattering by employing a combination of time-of-flight and backscattering techniques is carried out to explore the molecular mobility of a polymer of intrinsic microporosity (PIM-1) at microscopic time scales in comparison with a high-performance polyimide. Molecular fluctuations can change the structure of the temporary network of micropores and open or close pathways for gas molecules. Therefore, the investigation might help to understand the selectivity of PIMs in gas separation processes. The performed neutron scattering experiments provide evidence for a low-temperature relaxation process, which was assigned to methyl group rotation. This methyl group rotation was analyzed in terms of jump diffusion in a three-fold potential. The analysis results in a fraction of methyl groups which are immobilized. For PIM-1 it was found that the fraction of immobilized methyl groups decreases with increasing temperature up to 350 K. At higher temperatures the number of immobilized methyl group increases gain due to an underlying relaxation process. This motional process on a somewhat larger length scale might lead to a reversible structural rearrangement which partially hinders the strongly localized methyl group rotation. In addition, it was found that the activation energy for the methyl group rotation for PIM-1 and the polyimide is significantly higher than for conventional polymers.
Zocca, Andrea ; Müller, Bernd R. ; Laquai, René ; Kupsch, Andreas ; Wieder, Frank ; Benemann, Sigrid ; Wilbig, Janka ; Günster, Jens ; Bruno, Giovanni
The microstructure of an apatite-wollastonite (code name AP40) glass-ceramic is analyzed in this study by combining 2D microscopy, phase analysis, X-ray absorption and synchrotron X-ray refraction computed tomography (XCT and SXRCT, respectively). It is shown that this combination provides a useful toolbox to characterize the global microstructure in a wide scale range, from sub-micrometer to millimeter. The material displays a complex microstructure comprising a glassy matrix with embedded fluorapatite and wollastonite small crystals. In this matrix, large (up to 200 μm) spike-shaped structures are distributed. Such microstructural features are oriented around a central sphere, thereby forming a structure resembling a sea urchin. A unique feature of SXRCT, in contrast to XCT, is that internal interfaces are visualized; this allows one to show the 3D distribution of these urchins with exceptionally good contrast. Furthermore, it is revealed that the spike-shaped structures are not single crystals, but rather composed of sub-micrometric crystals, which are identified as fluorapatite and diopside phases by SEM-EDX analysis.
Determination of elemental mass fractions in sediments plays a major role in evaluating the environmental status of aquatic ecosystems. Herewith, the optimization of a new total digestion protocol and the subsequent analysis of 48 elements in different sediment reference materials (NIST SRM 2702, GBW 07313, GBW 07311 and JMC-2) based on ICP-MS/MS detection is presented. The developed method applies microwave acid digestion and utilizes HBF4 as fluoride source for silicate decomposition. Similar to established protocols based on HF, HBF4 ensures the dissolution of the silicate matrix, as well as other refractory oxides. As HBF4 is not acutely toxic; no special precautions have to be made and digests can be directly measured via ICP-MS without specific sample inlet systems, evaporation steps or the addition of e.g. H3BO3, in order to mask excess HF. Different acid mixtures with and without HBF4 were evaluated in terms of digestion efficiency based on the trace metal recovery. The optimized protocol (5 mL HNO3, 2 mL HCL, 1 mL HBF4) allows a complete dissolution of the analyzed reference materials, as well as quantitative recoveries for a wide variety of certified analytes. Low recoveries for e.g. Sr, Ba and rare earth elements due to fluoride precipitation of HF-based digestions protocols, can be avoided by the usage of HBF4 instead. Based on the usage of high purity HBF4 all relevant trace, as well as matrix elements can be analyzed with sufficiently low LOQs (0.002 μg L−1 for U up to 6.7 μg L−1 for Al). In total, 34 elements were within a recovery range of 80%–120% for all three analyzed reference materials GBW 07313, GBW 07311 and JMC-2. 14 elements were outside a recovery range of 80%–120% for at least one of the analyzed reference materials.
In the field of optically excited thermography, flash lamps (impulse shaped planar heating) and halogen lamps (modulated planar heating) have become established for the specific regimes of impulse and lock-in thermography. Flying-spot laser thermography is implemented by means of a rasterized focused laser, e. g. for crack detection (continuous wave operation) and photothermal material characterization (high-frequency modulated). The availability of novel technologies, i. e. fast and high-resolution IR cameras, brilliant innovative light sources and high-performance data acquisition and processing technology will enable a paradigm shift from stand-alone photothermal and thermographic techniques to uniform quantitative measurement and testing technology that is faster and more precise. Similar to an LED array, but with irradiance two orders of magnitude higher, a new type of brilliant laser source, i. e. the VCSEL array (vertical-cavity surface-emitting laser), is now available. This novel optical energy source eliminates the strong limitation to the temporal dynamics of established light sources and at the same time is spectrally clearly separated from the detection wavelength. It combines the fast temporal behavior of a diode laser with the high optical irradiance and the wide illumination area of flash lamps. In addition, heating can also be carried out in a structured manner, because individual areas of the VCSEL array can be controlled independently of each other. This new degree of freedom enables the development of completely new thermographic NDT methods.
Optical lock-in thermography is a completely contactless and very sensitive NDT technique. As an optical source of energy, incandescent lamps are most commonly used because they are relatively inexpensive and offer high irradiances at the test specimen. However, they are strongly restricted by their low modulation bandwidth with a maximum modulation frequency of only about 1 Hz. The use of high-power kilowattclass laser sources, e.g. diode laser arrays, pushes this constraint beyond 100 Hz. This allows for the exploration of the near-surface region of metals and layer systems with better and more accurate penetration depth and depth resolution. Moreover, these lasers are virtually free of any additional thermal radiation that could interfere with the “true” thermal response emitted from the heated sample. In turn, they can be easily used in a one-sided test configuration. We present current activities with kilowatt-class highpower laser sources for advanced lock-in thermography and focus on the application of laser arrays that offer a very high irradiation strength over a large sample area beyond the mentioned advantages.
Impact damages and delaminations in fibre-reinforced composites (FRC) might not be visible at the surface, but could have an influence on the resistance and on the long-term behaviour of the component. Therefore, and especially for safety relevant structures, non-destructive methods are required for the assessment of such damages.
Active thermography methods are suitable to characterize damages after loading using different kind of excitation techniques and various configurations of infrared (IR) camera and heating sources. Here, flash lamps, impulse excitation with infrared radiator and lock-in technique with halogen lamps or widened laser beams are suited. In addition, non-optical sources like sonotrodes (requiring direct contact to the structure) or induction generators (only suited for carbon fibre reinforced polymer (CFRP) structures) could be applied as well. For the investigation of the evolution of the damage during the impact, passive thermography can be applied in-situ. Elastic and plastic deformations alter the temperature of the structure and thus the temperature on the surface.
In this contribution, at first the general principles of quantitative defect characterisation in FRC using active thermography with flash, impulse and lock-in excitation are described. Optical and thermal properties of the FRC material and its anisotropy are considered. Results of phase differences obtained at flat bottom holes with flash and lock-in thermography are compared for qualifying both methods for quantitative defect characterization. Secondly, the damage evolution of CFRP and GFRP structures under impact load and static tensile loading is described. The spatial and temporal evolution of the surface temperature enables us to distinguish matrix cracks or fibre-matrix separation from delaminations between the layers. Afterwards, all results for loading defects, obtained by passive and active thermography, are compared with each other. Fig. 1 and 2 show the difference of passive and flash thermography obtained at impact and tensile loaded CFRP plates, respectively. As one purpose of these investigations is the development of standards within national (DIN) and European (CEN) standardisation bodies, new draft and final standards are presented and further needs are discussed at the end of the presentation.
Using spatial and temporal shaping of laser-induced diffuse thermal wave fields in thermography
(2020)
Ziegler, Mathias ; Ahmadi, Samim ; Hirsch, Philipp Daniel ; Lecompagnon, Julien ; Hassenstein, Christian ; Thiel, Erik ; Pech May, Nelson Wilbur
The diffuse nature of thermal waves is a fun-damental limitation in thermographic nonde-structive testing. In our studies we investigated different approaches by shaping the thermal wave fields which result from heating. We have used high-power laser sources to heat metallic samples. Using these spatial and temporal shaping techniques leads to a higher detection sensitivity in our measurements with the infra-red camera. In this contribution we show our implementation of shaping laser-induced diffuse thermal wave fields and the effect on the defect reconstruction quality.
Optical lock-in thermography is a completely contactless and very sensitive NDT technique. As an optical source of energy, incandescent lamps are most commonly used because they are relatively inexpensive and offer high irradiances at the test specimen. However, they are strongly restricted by their low modulation bandwidth with a maximum modulation frequency of only about 1 Hz. The use of high-power kilowatt-class laser sources, e.g. diode laser arrays, pushes this constraint beyond 100 Hz. This allows for the exploration of the near-surface region of metals and layer systems with better and more accurate penetration depth and depth resolution. Moreover, these lasers are virtually free of any additional thermal radiation that could interfere with the “true” thermal response emitted from the heated sample. In turn, they can be easily used in a one-sided test configuration.
We present current activities with kilowatt-class high-power laser sources for advanced lock-in thermography and focus on the application of laser arrays that offer a very high irradiation strength over a large sample area beyond the mentioned advantages.
Optical lock-in thermography is a completely contactless and very sensitive NDT technique. As an optical source of energy, incandescent (i.e. halogen) lamps are most commonly used because they are relatively inexpensive and offer high irradiances at the test site. However, they are strongly restricted by their low modulation bandwidth with a maximum modulation frequency of only about 1 Hz. The use of high-power kilowatt-class laser sources, e.g. diode laser arrays, pushes this constraint beyond 100 Hz, see Fig.1. This allows for the exploration of the near-surface region of metals and layer systems with better and more accurate penetration depth and depth resolution. Moreover, these lasers are virtually free of any additional thermal radiation that could interfere with the “true” thermal response emitted from the heated sample. In turn, they can be easily used in a one-sided test configuration.
Using the one-dimensional solution to the thermal heat diffusion equation together with the absorptance of the material which is illuminated with a harmonically modulated light source, we can calculate the temperature oscillation at the surface of a solid. As a second step, we calculate the corresponding oscillation of the total thermal emission using Stefan-Boltzmann law as a first order approximation and taking into account the emissivity of the material. Within this framework we can calculate the minimal irradiance of a light source necessary to provoke a measurable signal within a thermographic camera at a noise equivalent temperature difference (NETD) of 30 mK. In Fig. 2 this relationship is displayed for a wide spectrum of modulation frequencies and for a number of different light sources scaled to the same electrical input power and illumination area. Using this figure, it is now easily possible to analyze the range of materials to be tested using lock-in thermography, since only the materials (dotted lines) below the irradiance-vs-frequency curves (solid lines) are heated in excess of the camera’s NETD. This figure clearly shows that laser sources considerably increase the application range of lock-in thermography, since especially for metals with a high reflectance and high thermal diffusivity a high irradiance is vitally important to allow for lock-in texting.
We present current activities with kilowatt-class high-power laser sources for advanced lock-in thermography and focus on the application of laser arrays that offer a very high irradiation strength over a large sample area beyond the mentioned advantages.
Optical lock-in thermography is a completely contactless and very sensitive NDE technique. As an optical source of energy, incandescent (i.e. halogen) lamps are most commonly used because they are relatively inexpensive, do not need any work safety measures and offer high irradiances at the test site. However, they are strongly restricted by their low modulation bandwidth with a maximum modulation frequency of only about 1 Hz. The use of high-power kilowatt-class laser sources, e.g. diode laser arrays, pushes this constraint beyond 100 Hz. This allows for the exploration of the near-surface region of metals and layer systems with better and more accurate penetration depth and depth resolution. Moreover, these lasers are virtually free of any additional thermal radiation that could interfere with the “true” thermal response emitted from the heated sample. In turn, they can be easily used in a one-sided test configuration. Altogether using lasers considerably increases the application range of lock-in thermography, since especially for metals with a high reflectance and high thermal diffusivity a high irradiance is vitally important to allow for lock-in testing [1, 2]. We report on the mentioned benefits of using such high-power lasers and analyze the range of materials to be tested using lock-in thermography in dependence on the laser irradiance, the modulation frequency, the infrared camera as well as the optical and thermal material parameters. In this context, we also address a number of systematic errors caused by the use of ideal and non-ideal heat sources. For example, the measured phase angle in lock-in thermography depends on the irradiance and the modulation bandwidth of the source. This in turn has a decisive influence on the uncertainty in the quantification of, e.g. layer thicknesses.
Due to their high irradiance and wide modulation bandwidth, high-power lasers open up a wide field of application. For example, the classical methods of pulse and lock-in thermography can be realized in high quality. In addition, structured heating is also possible by using arrays of such lasers. This makes it possible to implement new thermographic methods, such as interference-based detection of cracks or super resolution.
Thermographic non-destructive testing 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.
Ziegler, K. ; Kunert, A. T. ; Reinmuth-Selzle, K. ; Leifke, A. L. ; Widera, D. ; Weller, Michael G. ; Schuppan, D. ; Fröhlich-Nowoisky, J. ; Lucas, K. ; Pöschl, U.
Environmental pollutants like fine particulate matter can cause adverse health effects through oxidative stress and inflammation. Reactive oxygen and nitrogen species (ROS/RNS) such as peroxynitrite can chemically modify proteins, but the effects of such modifications on the immune system and human health are not well understood. In the course of inflammatory processes, the Toll-like receptor 4 (TLR4) can sense damage-associated molecular patterns (DAMPs). Here, we investigate how the TLR4 response and pro-inflammatory potential of the proteinous DAMPs α-Synuclein (α-Syn), heat shock protein 60 (HSP60), and high-mobility-group box 1 protein (HMGB1), which are relevant in neurodegenerative and cardiovascular diseases, changes upon chemical modification with peroxynitrite.
For the peroxynitrite-modified proteins, we found a strongly enhanced activation of TLR4 and the pro-inflammatory transcription factor NF-κB in stable reporter cell lines as well as increased mRNA expression and secretion of the pro-inflammatory cytokines TNF-α, IL-1β, and IL-8 in human monocytes (THP-1). This enhanced activation of innate immunity via TLR4 is mediated by covalent chemical modifications of the studied DAMPs.
Our results show that proteinous DAMPs modified by peroxynitrite more potently amplify inflammation via TLR4 activation than the native DAMPs, and provide first evidence that such modifications can directly enhance innate immune responses via a defined receptor. These findings suggest that environmental pollutants and related ROS/RNS may play a role in promoting acute and chronic inflammatory disorders by structurally modifying the body's own DAMPs. This may have important consequences for chronic neurodegenerative, cardiovascular or gastrointestinal diseases that are prevalent in modern societies, and calls for action, to improve air quality and climate in the Anthropocene.
AbstractHigh-strength aluminum alloys used in aerospace and automotive applications obtain their strength through precipitation hardening. Achieving the desired mechanical properties requires precise control over the nanometer-sized precipitates. However, the microstructure of these alloys changes over time due to aging, leading to a deterioration in strength. Typically, the size, number, and distribution of precipitates for a quantitative assessment of microstructural changes are determined by manual analysis, which is subjective and time-consuming. In our work, we introduce a progressive and automatable approach that enables a more efficient, objective, and reproducible analysis of precipitates. The method involves several sequential steps using an image repository containing dark-field transmission electron microscopy (DF-TEM) images depicting various aging states of an aluminum alloy. During the process, precipitation contours are generated and quantitatively evaluated, and the results are comprehensibly transferred into semantic data structures. The use and deployment of Jupyter Notebooks, along with the beneficial implementation of Semantic Web technologies, significantly enhances the reproducibility and comparability of the findings. This work serves as an exemplar of FAIR image and research data management.
Tri-structural Isotropic (TRISO)-coated particle is the fission energy source and the first safety barrier in high temperature gas-cooled reactors (HTGRs). The integrity of TRISO particle should be carefully tested before operation because the shape may affect the failure possibility of the particles, leading to increased risk of fission product release. Due to the large difference in density between the kernel and the coating layers in TRISO particles, traditional X-ray radiography cannot achieve a good image quality in terms of identifying coating layers reliably, while phase-contrast CThas the advantageof being sensitive to boundaries. This paperpresents a non-destructive test and evaluation (NDT&E) method to facilitate 3-dimensional (3D) measurement of a TRISO particle's structure, using a synchrotron phase-contrast CT. After reconstructed, the TRISO particle was rendered in a 3D space and the thickness and asphericity of the TRISO particle's layers were measured. It was found that the thickness of coating layers of the tested particle obeys Gaussian distribution. The deviation of thicknesses of the kernel and the other four layers is −2.42%, −16.32%, 26.51%, 0.98% and 7.49% compared with the design parameters. The deviation of asphericity of the kernel, IPyC and OPyC layers is −11.51%, −0.41% and 3.39%, respectively. The effect of the deviations on the temperature distribution and failure probability calculation of the particle will be investigated in the future.
In this study, an Impulse Response Function analysis of pile response to sine-sweep excitation by a low cost, portable Shaker was used to identify defects in piles. In straightforward impact-echo methods, echoes from the pile toe and defects are visible in the time domain measurements. However, these echoes are not present in the time domain records of piles subjected to sine-sweep excitations, due to interactions between the input and output signals. For this reason, the impulse response function in the time domain has been calculated and is able to identify the echoes from pile impedance changes. The proposed methodology has been evaluated both numerically and experimentally. A one-dimensional pile-soil interaction system was developed, and a finite difference method used to calculate the pile response to sine-sweep excitation. The numerical simulations indicate that impulse response measurements with a synthesized logarithmic, sine-sweep excitation could be an effective tool for detecting defects in piles. The methodology was further tested with field trials on 6 cast in situ concrete test piles including 1 intact pile and 5 defective piles subjected to sine-sweep excitations by a shaker. In 5 of the 6 cases the echoes from the pile toe could be identified in the deconvoluted waveforms—the impulse Response functions. Damage detection is more difficult and dependent on the selection of the optimal regularization parameter. Further research and optimization of the deconvolution process is needed to evaluate the effectiveness compared to standard pile integrity testing methods.
Hot carriers (electrons and holes) generated from the decay of localized surface plasmon resonances can take a major role in catalytic reactions on metal nanoparticles. By obtaining surface enhanced Raman scattering (SERS) spectra of p-aminothiophenol as product of the reduction of p-nitrothiophenol by hot electrons, different catalytic activity is revealed here for nanoparticles of silver, gold, and copper. As a main finding, a series of different ligands, comprising halide and non-halide species, are found to enhance product formation in the reduction reaction on nanoparticles of all three metals. A comparison with the standard electrode potentials of the metals with and without the ligands and SERS data obtained at different electrode potential indicate that the higher catalytic activity can be associated with a higher Fermi level, thereby resulting in an improved efficiency of hot carrier generation. The concept of such a ligand-enhanced hot electron reduction provides a way to make light-to-chemical energy conversion more efficient due to improved electron harvesting.
Self-assembled monolayers (SAMs) on plasmonic substrates play a significant role applications of surface-enhanced Raman scattering (SERS). At the same time, localized surface plasmon resonances (LSPRs) can be employed for a broad range of plasmon-supported chemical modifications. Here, micropatterning using the derivatization of SAMs on gold nanosubstrates for rewritable SERS-based security labels or as the basis for sensing arrays functionalized with biomolecules is demonstrated using different plasmon-catalyzed reactions. The formation of 4,4′-dimercaptoazobenzene (DMAB) from p-aminothiophenol (PATP) as well as from p-nitrothiophenol (PNTP) and the reduction of PNTP to PATP are used to change the functionality of the substrate in specified positions. Employing LSPR, the reactions are started by illumination using visible laser light at a high intensity in a focal spot of a microscope objective and yield microscopic patterns of the reaction product. The obtained molecular patterns can be erased by other reactions, enabling different strategies for rewriting, encryption, or stepwise functionalization.
The spectroscopic characterization by surface-enhanced Raman scattering (SERS) has shown great potential in studies of heterogeneous catalysis. We describe a plug-in multifunctional optofluidic platform that can be tailored to serve both as a variable catalyst material and for sensitive optical characterization of the respective reactions using SERS in microfluidic systems. The platform enables the characterization of reactions under a controlled gas atmosphere and does not present with limitations due to nanoparticle adsorption or memory effects. Spectra of the gold-catalyzed reduction of p-nitrothiophenol by sodium borohydride using the plug-in probe provide evidence that the borohydride is the direct source of hydrogen on the gold surface, and that a radical anion is formed as an intermediate. The in situ monitoring of the photoinduced dimerization of p-aminothiophenol indicates that the activation of oxygen is essential for the plasmon-catalyzed oxidation on gold nanoparticles and strongly supports the central role of metal oxide species.
We investigate the pore space of rock samples with respect to different petrophysical parameters using various methods, which provide data on pore size distributions, including micro computed tomography (µ-CT), mercury Intrusion porosimetry (MIP), nuclear magnetic resonance (NMR), and spectral-induced polarization (SIP). The resulting cumulative distributions of pore volume as a function of pore size are compared. Considering that the methods differ with
regard to their limits of resolution, a multiple-length-scale characterization of the pore space is proposed, that is based on a combination of the results from all of these methods.
The approach is demonstrated using samples of Bentheimer and Röttbacher sandstone. Additionally, we compare the potential of SIP to provide a pore size distribution with other commonly used methods (MIP, NMR). The limits of Resolution of SIP depend on the usable frequency range (between 0.002 and 100 Hz). The methods with similar Resolution show a similar behavior of the cumulative pore volume distribution in the verlapping pore size range. We assume that µ-CT and NMR provide the pore body size while MIP and SIP characterize the pore throat size. Our study Shows that a good agreement between the pore radius distributions can only be achieved if the curves are adjusted considering the resolution and pore volume in the relevant range of pore radii. The MIP curve with the widest range in Resolution should be used as reference.
The discussion of the surface-enhanced Raman scattering (SERS) spectra of p-aminothiophenol (PATP) and of ist photocatalytic reaction product 4,4′-dimercaptoazobenzene (DMAB) is important for understanding plasmon-supported spectroscopy and catalysis. Here, SERS spectra indicate that DMAB forms also in a nonphotocatalytic reaction on silver nanoparticles. Spectra measured at low pH, in the presence of the acids HCl, H2SO4, HNO3, and H3PO4, show that DMAB is reduced to PATP when both protons and chloride ions are present. Moreover, the successful reduction of DMAB in the presence of other, halide and nonhalide, ligands suggests a central role of these species in the reduction. As discussed, the ligands increase the efficiency of hot-electron harvesting. The pH-associated reversibility of the SERS spectrum of PATP is established as an Observation of the DMAB dimer at high pH and of PATP as a product of its hot-electron reduction at low pH, in the presence of the appropriate ligand.
To complement the information provided by deterministic seismic imaging at length scales above a certain resolution limit we present the first application of adjoint envelope tomography (AET) to experimental data. AET uses the full envelopes of seismic records including scattered coda waves to obtain information about the distribution of absorption and small-scale heterogeneity which provide complementary information about the investigated medium. Being below the resolution limit this small-scale structure cannot be resolved by conventional tomography but still affects wave propagation by attenuating ballistic waves and generating scattered waves. Using ultrasound data from embedded sensors in a meter-sized concrete specimen we image the distribution of absorption and heterogeneity expressed by the intrinsic quality factor Q−1 and the fluctuation strength ɛ that characterizes the strength of the heterogeneity. The forward problem is solved by modeling the 2-D multiple nonisotropic scattering in an acoustic medium with spatially variable heterogeneity and attenuation using the Monte-Carlo method. Gradients for the model updates are obtained by convolution with the back-propagated envelope misfit using the adjoint formalism in analogy to full waveform inversion.
We use a late coda time window to invert for absorption and an earlier time window to infer the distribution of heterogeneity. The results successfully locate an area of salt oncrete with increased scattering and concentric anomalies of intrinsic attenuation. The resolution test shows that the recovered anomalies constitute reasonable representations of internal structure of the specimen.
Raman microspectra combine information on chemical composition of plant tissues with spatial information. The contributions from the building blocks of the cell walls in the Raman spectra of plant tissues can vary in the microscopic sub-structures of the tissue. Here, we discuss the analysis of 55 Raman maps of root, stem, and leaf tissues of Cucumis sativus, using different spectral contributions from cellulose and lignin in both univariate and multivariate imaging methods. Imaging based on hierarchical cluster analysis (HCA) and principal component analysis (PCA) indicates different substructures in the xylem cell walls of the different tissues. Using specific signals from the cell wall spectra, analysis of the whole set of different tissue sections based on the Raman images reveals differences in xylem tissue morphology. Due to the specifics of excitation of the Raman spectra in the visible wavelength range (532 nm), which is, e.g., in resonance with carotenoid species, effects of photobleaching and the possibility of exploiting depletion difference spectra for molecular characterization in Raman imaging of plants are discussed. The reported results provide both, specific information on the molecular composition of cucumber tissue Raman spectra, and general directions for future imaging studies in plant tissues.
Zeipert, H. ; Johannesmann, S. ; Nicolai, Marcel ; Lugovtsova, Yevgeniya ; Prager, Jens ; Henning, B.
In the field of non-destructive testing, Lamb waves are often used for material characterisation. The increasing computational capabilities further enable complex and detailed simulations to predict the material behaviour in reality. Since adhesive bonding of different materials is a widely used method in modern applications, a reliable measurement system to determine the quality of these adhesive bonds is needed. Investigations of the dispersive behaviour of acoustic waves in adhesively bonded multi-layered waveguides show mode repulsions in the dispersion diagrams in regions where the modes of the single materials would otherwise intersect. In previous works, changes of the distance between those modes with respect to the bonding quality are observed. The experimental data for this investigation is generated using pulsed laser radiation to excite broadband acoustic waves in plate like specimens which are detected by a piezoelectric ultrasonic transducer. Numerical data is generated using simulations via a semi-analytical finite element method. Using a combination of experimental and numerical data, the present work introduces an approach to determine a parameter which indicates the bonding quality in relation
to an ideal material coupling.
Zeipert, H. ; Claes, L. ; Johannesmann, S. ; Webersen, M. ; Lugovtsova, Yevgeniya ; Prager, Jens ; Henning, B.
Lamb waves are a common tool in the field of non-destructive testing and are widely used for materialcharacterisation. Further, the increasing computational capability of modern systems enables the Simulation of complex and detailed material models. This work demonstrates the possibility of simulating an adhesive-bonded multilayer system by characterising each layer individually, and introduces an Approach for determining the dispersive behaviour of acoustic waves in a multilayer system via real measurements.