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The present work shows results on elemental distribution analyses in Cu(In,Ga)Se2 thin films for solar cells performed by use of wavelength-dispersive and energy-dispersive X-ray spectrometry (EDX) in a scanning electron microscope, EDX in a transmission electron microscope, X-ray photoelectron, angle-dependent soft X-ray emission, secondary ion-mass (SIMS), time-of-flight SIMS, sputtered neutral mass, glow-discharge optical emission and glow-discharge mass, Auger electron, and Rutherford backscattering spectrometry, by use of scanning Auger electron microscopy, Raman depth profiling, and Raman mapping, as well as by use of elastic recoil detection analysis, grazing-incidence X-ray and electron backscatter diffraction, and grazing-incidence X-ray fluorescence analysis. The Cu(In,Ga)Se2 thin films used for the present comparison were produced during the same identical deposition run and exhibit thicknesses of about 2 µm. The analysis techniques were compared with respect to their spatial and depth resolutions, measuring speeds, availabilities, and detection limits.
Glass-ceramics containing Ca2KNa(PO4)2 as the main crystalline phase have a solubility which is 8 times higher than that of alpha-tricalcium phosphate ceramics. When using these compositions in drug delivery systems, especially in bone, it is necessary to create a material with a high open porosity. A Ca2KNa(PO4)2-based glass-ceramic was prepared from a borosilicate glass melt. The processed material includes minor amounts of boron which are low enough for medical application. Tissue response was studied using an animal model. Particles were implanted in rabbit femurs. Bone and soft tissue development occurred at the particle interfaces. In general, most particles were enclosed in the network of trabecular bone. The advantages of using a biomaterial with high porosity (pore size of 1-3 micron), together with rapid biodegradation, bioactivity and biocompatibility, despite traces of boron, were shown. 4 refs.
In vivo test of a high porous rapidly resorbable dicalcium potassium sodium phosphate glass-ceramics
(2002)
Results are reported from a pilot study under the Consultative Committee for Amount of Substance (CCQM) to compare measurements of and resolve any relevant measurement issues in, the amount of thermal SiO2 oxide on (100) and (111) orientation Si wafer substrates in the thickness range 1.5 - 8 nm. As a result of the invitation to participate in this activity, 45 sets of measurements have been made in different laboratories using 10 analytical methods: medium-energy ion scattering spectrometry (MEIS), nuclear reaction analysis (NRA), RBS, elastic backscattering spectrometry (EBS), XPS, SIMS, ellipsometry, grazing-incidence x-ray reflectrometry (GIXRR), neutron reflectometry and transmission electron microscopy (TEM). The measurements are made on separate sets of 10 carefully prepared samples, all of which have been characterised by a combination of ellipsometry and XPS using carefully established reference conditions and reference parameters.
The results have been assessed against the National Physical Laboratory (NPL) data and all show excellent linearity. The remaining data sets correlate with the NPL data with average root-mean-square scatters of 0.15 nm, half being better than 0.1 nm and a few at or better than 0.05 nm. Each set of data allows a relative scaling constant and a zero thickness offset to be determined. Each method has an inherent zero thickness offset between 0 nm and 1 nm and it is these offsets, measured here for the first time, that have caused many problems in the past. There are three basic classes of offset: water and carbonadeous contamination equivalent to ~1 nm as seen by ellipsometry; adsorbed oxygen mainly from water at an equivalent thickness of 0.5 nm as seen by MEIS, NRA, RBS and possibly GIXRR; and no offset as seen by XPS using the Si 2p peaks. Each technique has a different uncertainty for the scaling constant and consistent results have been achieved. X-Ray photoelectron spectroscopy has large uncertainties for the scaling constant but a high precision and, critically, if used correctly, has zero offset. Thus, a combination of XPS and the other methods allows the XPS scaling constant to be determined with low uncertainty, traceable via the other methods. XPS laboratories returning results early were invited to test a new reference procedure. All showed very significant improvements. The reference attenuation lengths thus need scaling by 0.986 ± 0.009 (at an expansion factor of 2) deduced from the data for the other methods. Several other methods have small offsets and, to the extent that these can be shown to be constant or measurable, then these methods will also show low uncertainty. Recommendations are provided for parameters for XPS, MEIS, RBS and NRA to improve their accuracy.
A glass of the composition 37BaO·16CaO·47SiO2 wt% produced on an industrial scale is crystallized at 970 °C for times ranging from 15 min to 2 h. The crystallization at the immediate surface as well as the crystal growth into the bulk are analyzed using scanning electron microscopy (SEM) including energy dispersive X-ray spectroscopy (EDXS) and electron backscatter diffraction (EBSD) as well as X-ray diffraction in the Θ–2Θ setup (XRD). The immediate surface shows the oriented nucleation of walstromite as well as the formation of wollastonite and an unknown phase of the composition BaCaSi3O8. All three phases also grow into the bulk where walstromite ultimately dominates the kinetic selection and grows throughout the bulk due to a lack of bulk nucleation. Walstromite shows systematic orientation changes as well as twinning during growth. A critical analysis of the XRD-patterns acquired from various crystallized samples indicates that their evaluation is problematic and that phases detected by XRD in this system should be verified by another method such as EDXS.
The formation and properties of laser-induced periodic surface structures (LIPSS) were investigated on carbon fibers under irradiation of fs-laser pulses characterized by a pulse duration τ = 300 fs and a laser wavelength λ = 1025 nm. The LIPSS were fabricated in an air environment at normal incidence with different values of the laser peak fluence and number of pulses per spot. The morphology of the generated structures was characterized by using scanning electron microscopy, atomic force microscopy and Fast-Fourier transform analyses. Moreover, the material structure and the surface chemistry of the carbon fibers before and after laser irradiation was analyzed by micro Raman spectroscopy and X-ray photoelectron spectroscopy. Large areas in the cm2 range of carbon fiber arrangements were successfully processed with homogenously distributed high- and low-spatial frequency LIPSS. Beyond those distinct nanostructures, hybrid structures were realized for the very first time by a superposition of both types of LIPSS in a two-step process. The findings facilitate the fabrication of tailored LIPSS-based surface structures on carbon fibers that could be of particular interest for e.g. fiber reinforced polymers and concretes.
Dynamic stall often occurs under conditions of simultaneous unsteady pitching and surging (e.g., rotorcraft and wind turbines), butmanymodels employ a dimensionless time base that implicitly assumes that surging is superimposed, in a quasi-steady manner, on dynamic pitching. An unsteady wind tunnel was used to examine this assumption, where a technique was developed to quantify the unsteady effects of surging on a pitching NACA 0018 airfoil. The technique involved performing multiple harmonic pitching experiments under nominally steady freestream conditions that bracketed a corresponding 50% surging amplitude (1.25 ⋅ 105 ≤ Re ≤ 3.75 ⋅ 105). By interpolating these data, unsteady-pitching/quasi-steady-surging data sets were constructed and compared with de facto synchronous pitch and surging experiments, thereby isolating the unsteady effects of surging on a pitching airfoil. Both large and small poststall maximum angles of attack (αs + 5° and αs + 15°) were considered at multiple pitch-surge phase differences. During deep dynamic stall (αs 15°), with large-scale separation, surging was seen to have a secondary effect on the unsteady aerodynamics. However, at small poststall maximum angles of attack (αs + 5°), either light or deep dynamic stall behavior was observed depending upon the pitch-surge phase difference. This was attributed to Reynolds number history effects, exemplified by boundary-layer transition, and thus it can be referred to as “transitional” dynamic stall.
A combined theoretical and experimental investigation was carried out with the objective of evaluating theoretical predictions relating to a two-dimensional airfoil subjected to high amplitude harmonic oscillation of the free stream at constant angle of attack. Current theoretical approaches were reviewed and extended for the purposes of quantifying the bound, unsteady vortex sheet strength along the airfoil chord. This resulted in a closed form solution that is valid for arbitrary reduced frequencies and amplitudes. In the experiments, the bound, unsteady vortex strength of a symmetric 18 % thick airfoil at low angles of attack was measured in a dedicated unsteady wind tunnel at maximum reduced frequencies of 0.1 and at velocity oscillations less than or equal to 50 %. With the boundary layer tripped near the leading edge and mid-chord, the phase and amplitude variations of the lift coefficient corresponded reasonably well with the theory. Near the maximum lift coefficient overshoot, the data exhibited an additional high-frequency oscillation. Comparisons of the measured and predicted vortex sheet indicated the existence of a recirculation bubble upstream of the trailing edge which sheds into the wake and modifies the Kutta condition.
Without boundary layer tripping, a mid-chord bubble is present that strengthens during flow deceleration and its shedding produces a dramatically different effect.
Instead of a lift coefficient overshoot, as per the theory, the data exhibit a significant undershoot. This undershoot is also accompanied by high-frequency oscillations that are characterized by the bubble shedding. In summary, the location of bubble and ist subsequent shedding play decisive roles in the resulting temporal aerodynamic loads.
The impact of femtosecond (fs) laser-induced periodic surface structures (LIPSS) on tribological properties was investigated for metal-reinforced ceramic composites (Al2O3-ZrO2-Nb). For this purpose, the metallic niobium (Nb) phase was selectively structured with LIPSS in an air environment with different values of the fs-laser peak fluence by near-infrared fs-laser radiation (λ = 1025 nm, τ = 300 fs, frep = 1 kHz), taking advantage of the different light absorption behavior of ceramic and metal. The tribological performance was evaluated by reciprocating sliding tests in a ball-on-disc configuration using Ringer's solution as lubricant. The surfaces were characterized before and after laser irradiation by optical microscopy, scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, energy dispersive X-ray spectroscopy and by measuring the contact angle with Ringer's solution. The LIPSS formation resulted in an increased wetting of the surface with the lubricant. Moreover, the selectively structured composite surfaces revealed a coefficient of friction significantly reduced by a factor of ~3 when compared to the non-irradiated surface. Furthermore, the formation of a laser-induced oxidation layer was detected with NbO as the most prominent oxidation state. Selectively structured composites with outstanding mechanical properties and enhanced tribological performance are of particular interest for biomedical applications.
Germination induces the glucosylation of the Fusarium mycotoxin deoxynivalenol in various grains
(2012)
In food, the mycotoxin deoxynivalenol (DON) often occurs in conjunction with its 3-β-D-glucopyranoside (D3G). The transformation of DON to D3G through glucosylation is catalysed by plant enzymes, however, the exact circumstances are not well understood. In order to investigate the role of enzymatic glucosylation in germinating grains, DON treated kernels were steeped and germinated under laboratory conditions. Furthermore, the effect of malting on the DON content of the contaminated barley was investigated. In all cases, DON and its derivatives were quantified by HPLC-MS/MS before, during and after the experiments. Amongst the six tested cereals; wheat, rye, barley, spelt, and millet transformed DON to D3G during germination whilst the oats were inactive. For wheat, barley, and spelt the initial DON content was reduced by 50%, with the loss being almost entirely accounted for by D3G formation. As D3G might be cleaved during digestion, the elevated D3G concentration may obscure the toxicologically relevant DON content in processed food and beer. The germination process has a major influence on the 'masking' of DON, leading to high quantities of D3G that may be missed in common mycotoxin analyses.
Im Zuge der Anwendung des Schadens-Toleranz-Prinzips wird ein adäquates zerstörungsfreies Prüfsystem benötigt um strukturelle Integrität sicher zu stellen. Wenn ein zerstörungsfreies Prüfsystem jedoch bis zu den Grenzen der Detektionsfähigkeit beansprucht wird, liefert es keine übereinstimmende Indikationen der Defektentdeckung (Hit/Miss). Deshalb wird dessen Fähigkeit Defekte zu entdecken als Entdeckungswahrscheinlichkeit (POD Probability of Detection) ausgedrückt. In der herkömmlichen 'Signal Response' Signal-Antwort-Zuverlässigkeitsanalyse wird die Entdeckungswahrscheinlichkeit als eine Funktion der Defektgröße angegeben. Die Eignung des Prüfsystems wird durch den Vergleich der Größe des Defektes, der zuverlässig entdeckt wird, mit der des größten zulässigen Defektes, der die strukturelle Integrität nicht gefährdet, verifiziert. Analysen moderner Strukturen zeigen aber, dass auch andere Parameter den Schweregrad des Defektes bzgl. der Integrität der Struktur bestimmen können. Im Rahmen der Multi-Parameter-Zuverlässigkeitsanalyse kann die Entdeckungswahrscheinlichkeit als eine Funktion verschiedener Einflussparameter ausgedrückt werden. Wenn die Eignung des zerstörungsfreien Prüfsystems bestimmt wird, muss die Fähigkeit des Systems Defekte zu entdecken gegenüber dem kritischen Wert genau des Parameters ausgedrückt und geprüft werden, der den Schweregrad des Defektes für die Integrität der Struktur bestimmt. Die Nichterfüllung dieser Forderung kann zur Ablehnung von intakten Teilen oder der Akzeptanz von schlechten Teilen führen. Das Prinzip wird anhand von longitudinalen Ultraschall-Sende-Empfangs-Prüfdaten der Gußeisenmatrix mit oberflächenoffenen, semi-elliptischen, rißartigen Defekten demonstriert.
The analysis of biomolecules requires highly sensitive and selective detection methods capable of tolerating a complex, biological matrix. First applications of biomolecule detection by ICP-MS relied on the use of heteroelements as a label for quantification. However, the combination of immunoassays and ICP-MS facilitates multiparametric analyses through elemental tagging, and provides a powerful alternative to common bioanalytical methods. This approach extends the detection of biomarkers in clinical diagnosis, and has the potential to provide a deeper understanding of the investigated biological system. The results might lead to the detection of diseases at an early stage, or guide treatment plans. Immunoassays are well accepted and established for diagnostic purposes, albeit ICP-MS is scarcely applied for the detection of immune-based assays. However, the screening of biomarkers demands high throughput and multiplex/multiparametric techniques, considering the variety of analytes to be queried. Finally, quantitative information on the expression level of biomarkers is highly desirable to identify abnormalities in a given organism. Thus, it is the aim of this review to introduce the fundamentals, and to discuss the enormous strength of ICP-MS for the detection of different immunoassays on the basis of selected applications, with a special focus on LA-ICP-MS.
We have developed lanthanide labeling strategies for antibodies to adapt conventional biochemical workflows like Western blot immunoassays for detection by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) analysis with a special interest to apply the multi-element capabilities of ICP-MS for the design of multiplexed immunoassays. In this paper the lanthanide labeling of antibodies with MeCAT was investigated and the reaction conditions were optimized for application in a Western blot immunoassay analyzed by LA-ICP-MS. Furthermore, the MeCAT labeling strategy was compared with two other commercially available labeling reagents, MAXPAR and SCN-DOTA. As a proof-of-principle experiment chemically induced alterations of cytochrome P450 protein expression were investigated and the suitability of the differentially labeled antibodies for Western blot immunoassays of a complex liver microsomal protein fraction was tested. Limits of detection (LODs) in the lower fmol range were reached in the Western blot application using MeCAT and MAXPAR as element labeling reagents, whereas even sub-fmol LODs can be achieved in a dot blot experiment for the pure antibodies.
Synchrotron X-ray radiography and tomography investigations of a custom-made polymer electrolyte membrane fuel cell optimised for visualisation purposes are presented. The 3D water distribution and transport pathways in the porous carbon fibre gas diffusion layers (GDLs) were investigated. The authors found that water is not only moving from the GDL into the channel, but can also take the opposite way, that is, from the channel into free pore space of the GDL. Such movement of water into the opposite direction has been subject of speculations but has so far not yet been reported and might bring new insights into the general water transport behaviour, which might give new aspects to the general description of water transport processes and influence modelling assumptions to describe the process taking place in the GDL.
Zur genaueren Kenntnis des Einflusses der Ermüdungsbelastung auf das Versagen von Beton wurde das Ermüdungsverhalten von gekerbten Betonbalken in kraft- und verformungsgeregelten Dreipunktbiegezugversuchen untersucht. Für die verformungsgeregelten Versuche wurde eine neuentwickelte Versuchstechnik angewendet, mit der auch unter hochzyklischer Beanspruchung mit Lastspielzahlen von bis zu einer Million Zyklen sowohl der ansteigende als auch der abfallende Ast in einem Kraft-Verformungsdiagramm aufgezeichnet werden kann.
Ein effektives Wassermanagement ist ein wichtiger Aspekt in der Entwicklung von Brennstoffzellen hinsichtlich Langzeitstabilität und Optimierung der Leistungsfähigkeit. Eine zentrale Rolle spielt dabei die Gasdiffusionslage, die für die gleichmäßige Verteilung der Reaktionsgase auf die elektrochemisch aktive Schicht (Katalysator) sorgen soll. In diesem Beitrag werden gemeinsame Forschungsaktivitäten des Helmholtz-Zentrums Berlin für Materialien und Energie (Entwicklung bildgebender Verfahren) sowie des Zentrums für Sonnenenergie- und Wasserstoff-Forschung (ZSW, Entwicklung von Brennstoffzellen) vorgestellt. Im Rahmen dieser Kooperation werden die Entstehung, die Verteilung und der Transport von flüssigem Wasser, kurz das Wassermanagement, unter Betriebsbedingungen untersucht. Mittels Synchrotronradiografie und -tomografie werden kleinste Wassercluster in der Gasdiffusionslage detektiert. Die gewonnenen Erkenntnisse dienen der Modifikation und einer gezielten Auswahl der eingesetzten Materialien.
We present a synchrotron X-ray tomographic study on the morphology of carbon fiber-based gas diffusion layer (GDL) material under compression. A dedicated compression device is used to provide well-defined compression conditions. A flat compression punch is employed to study the fiber geometry at different degrees of compression. Transport relevant geometrical parameters such as porosity, pore size and tortuosity distributions are calculated. The geometric properties notably change upon compression which has direct impact on transport conditions for gas and fluid flow. The availability of broad 3D paths, which are most important for the transport of liquid water from the catalyst layer through the GDL, is markedly reduced after compression. In a second experiment, we study the influence of the channel-land-pattern of the flow-field on shape and microstructure of the GDL. A flow-field compression punch is employed to reproduce the inhomogeneous compression conditions found during fuel cell assembly. While homogenously compressed underneath the land the GDL is much less and inhomogeneously compressed under the channel. The GDL material extends far into the channel volume where it can considerably influence gas and fluid flow. Loose fiber endings penetrate deeply into the channel and form obstacles for the discharge of liquid water droplets.
Microplastics are small plastic fragments that are widely distributed in marine and terrestrial environments. While the soil ecosystem represents a large reservoir for plastic, research so far has focused mainly on the impact on aquatic ecosystems and there is a lack of information on the potentially adverse effects of microplastics on soil biota. Earthworms are key organisms of the soil ecosystem and are due to their crucial role in soil quality and fertility a suitable and popular model organism in soil ecotoxicology.
Therefore, the aim of this study was to gain insight into the effects of environmentally relevant concentrations of microplastics on the earthworm Eisenia andrei on multiple levels of biological organization after different exposure periods. Earthworms were exposed to two types of microplastics: (1) polystyrene-HBCD and (2) car tire abrasion in natural soil for 2, 7, 14 and 28 d. Acute and chronic toxicity and all subcellular investigations were conducted for all exposure times, avoidance behavior assessed after 48 h and reproduction after 28 d. Subcellular endpoints included enzymatic biomarker responses, namely, carboxylesterase, glutathione peroxidase, acetylcholinesterase, glutathione reductase, glutathione S-transferase and catalase activities, as well as fluorescence-based measurements of oxidative stress-related markers and multixenobiotic resistance activity. Multiple biomarkers showed significant changes in activity, but a recovery of most enzymatic activities could be observed after 28 d. Overall, only minor effects could be observed on a subcellular level, showing that in this exposure scenario with environmentally relevant concentrations based on German pollution levels the threat to soil biota is minimal. However, in areas with higher concentrations of microplastics in the environment, these results can be interpreted as an early warning signal for more adverse effects. In conclusion, these findings provide new insights regarding the ecotoxicological effects of environmentally relevant concentrations of microplastics on soil organisms.