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Paper des Monats
- ja (1)
Ein wesentlicher Vorteil der Dünnschichtphotovoltaik gegenüber der waferbasierten Photovoltaik liegt in der monolithischen Serienverschaltung. Bei der Herstellung von Chalkopyrit(CIGSe) -Dünnschicht-Solarmodulen erfolgen dafür typischerweise ein Laser-Strukturierungsschritt (P1) und zwei mechanische Strukturierungsschritte (P2, P3). In diesem Beitrag wird gezeigt, dass die Strukturierung von CIGSe-Solarmodulen vollständig mit kurzen Laserpulsen (<10 ns Pulsdauer) und einer einzigen Wellenlänge (532 nm) möglich ist. Der P1- und P3-Schnitt erfolgen durch direkte induzierte Ablation. Für den P2-Schnitt wird gezielt der hohe Wärmeeintrag der ns-Laserpulse genutzt, um die CIGSe-
Absorberschicht lokal aufzuschmelzen und strukturell so zu verändern, dass eine elektrisch gut leitende Verbindung zwischen Front- und Rückkontakt entsteht.
A magnetically stabilized DC arc device, designed for operation with OES spectrometers was used to determine the elements Ag, Al, B, Ba, Be, Ca, Co, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Mo, Na, Nb, Ni, Si, Sn, Sr, Ti, V, Zr at trace levels of some μg kg−1 up to some 10 mg kg−1 in graphite powders. The coil for the generation of the homogeneous magnetic field was placed outside the closed arc chamber. The time programs of variable current strengths of the magnetic coil (up to 6 A) and of the arc (up to 17 A) which was burning in air were computer controlled. Halogenating gases (mainly CCl2F2, alternatively SF6 and NF3) were used as chemical modifiers to allow an effective release of the carbide forming trace elements. The mass flow controlled modifier gas was led through a special carrier electrode near the arc plasma. The emission radiation was guided by an optical fiber alternatively into two different ICP spectrometers in which the ICP torches were removed. The synergistic interaction of the magnetic field with the halogenating modifier gases resulted in a significant improvement in the analytical performance of the optimized analytical method. All our results for 22 trace elements were in good agreement with the means of an inter-laboratory comparison by BAM for certification of a pure graphite powder material; this holds also for our results for two other graphite materials. The optimized method showed an analytical performance suitable for comprehensive trace analysis of pure graphite. The instrumentation could be integrated into modern DC arc emission spectrometers to improve their analytical capabilities substantially.
In this article, we present two Coptic papyri, P 11934 and P 11935 from the Berlin collection excavated in Ashmunein (ancient Hermopolis) by Otto Rubensohn in 1906. We employ a multi-disciplinary approach that takes into account both their materiality – writing support as well as ink – and their content, as has become ‘best practice’. 1 Material aspects of written documents have traditionally been the purview of papyrologists. Recently developed methods of scientific analysis generate sets of archaeometric data with the potential to improve understanding of the materiality of ancient document production, as well as to yield new evidence for genuine papyrological research questions. To achieve this, a large corpus of comparative data needs to be built. Our contribution offers a first step in this direction. We aim at presenting the papyri, which were selected because of the ink corrosion during conservation work at the Berlin collection, in a format that is exhaustive both for material and textual aspects. The inks from both papyri were analysed using a combination of techniques, contributing to our better understanding of the development of ink technology in Late Antiquity.
In many bacteria, the biofilm-promoting second messenger c-di-GMP is produced and degraded by multiple diguanylate cyclases (DGC) and phosphodiesterases (PDE), respectively. High target specificity of some of these enzymes has led to theoretical concepts of "local" c-di-GMP signaling. In Escherichia coli K-12, which has 12 DGCs and 13 PDEs, a single DGC, DgcC, is specifically required for the biosynthesis of the biofilm exopolysaccharide pEtN-cellulose without affecting the cellular c-di-GMP pool, but the mechanistic basis of this target specificity has remained obscure. DGC activity of membrane-associated DgcC, which is demonstrated in vitro in nanodiscs, is shown to be necessary and sufficient to specifically activate cellulose biosynthesis in vivo. DgcC and a particular PDE, PdeK (encoded right next to the cellulose operon), directly interact with cellulose synthase subunit BcsB and with each other, thus establishing physical proximity between cellulose synthase and a local source and sink of c-di-GMP. This arrangement provides a localized, yet open source of c-di-GMP right next to cellulose synthase subunit BcsA, which needs allosteric activation by c-di-GMP. Through mathematical modeling and simulation, we demonstrate that BcsA binding from the low cytosolic c-di-GMP pool in E. coli is negligible, whereas a single c-di-GMP molecule that is produced and released in direct proximity to cellulose synthase increases the probability of c-di-GMP binding to BcsA several hundred-fold. This local c-di-GMP signaling could provide a blueprint for target-specific second messenger signaling also in other bacteria where multiple second messenger producing and degrading enzymes exist.
Bacterial biofilms pose serious problems in medical and industrial settings. One of the major societal challenges lies in the increasing resistance of bacteria against biocides used in antimicrobial treatments, e.g., via overabundant use in medicine, industry, and agriculture or cleaning and disinfection in private households. Hence, new efficient bacteria-repellent strategies avoiding the use of biocides are strongly desired. One promising route to achieve bacteria-repellent surfaces lies in the contactless and aseptic large-area laser-processing of technical surfaces. Tailored surface textures, enabled by different laser-processing strategies that result in topographic scales ranging from nanometers to micrometers may provide a solution to this challenge. This article presents a current state-of-the-art review of laser-surface subtractive texturing approaches for controlling the biofilm formation for different bacterial strains and in different environments. Based on specific properties of bacteria and laser-processed surfaces, the challenges of anti-microbial surface designs are discussed, and future directions will be outlined.
Structuring of thin-film photovoltaic modules requires basic knowledge of the laser – thin-film interaction in order to adapt the accessible laser parameters, like wavelength, power, repetition rate and scribing speed whilst taking into account the specific material properties of the layer. We have studied the nanosecond laserablation behavior of corresponding layers (i) of silicon based thin-film solar cells with a-Si/µc-Si tandem absorber type and (ii) of back contact and absorber layer of CIGSe solar cells. The respective ablation threshold fluences were determined as integrative parameters describing the specific laser – material interaction. For the threshold determination we used two different methods and developed a new analytical approach taking into account scribing through the glass substrate as it is preferred for most structuring processes. This was done by analyzing the thin film ablation results by means of optical microscopy, profilometry, scanning electron microscopy (SEM). Moreover, we determined the incubation coefficient of the regarded material layers which allows us to predict quantitatively the influence of the spot overlap on the scribing threshold.
Millions of measurements are performed each year by liquid based analytical atomic spectrometry to support healthcare, diagnostic tests, environmental monitoring, material assay, product development and safety. Despite the effort to develop absolute methods, most methods still depend on calibration solutions, which are gravimetric mixtures of high purity solvents and high purity (source material) metals or compounds. As in the real world ideal purity does not exist, the impurity of the solvent and the purity of the source material needs to be known. The impurity of a solvent with respect to one analyte can be measured rather easily and with low limits of determination. In contrast the measurement of the purity of the source material, i.e., the mass fraction of the main constituent in a high purity metal, is more difficult to determine. It becomes even more difficult when the source material is not a pure metal but a compound since problems regarding stoichiometry arise additionally. Although the major producers of calibration solutions make a special effort to determine the purity of the source material, the actual purity statement is often incomplete or not demonstrated. The main reason for this situation is the complexity and high effort necessary to fully characterize such a material. This problem holds to a very wide extent also for the primary standards for element determination at the National Metrology Institutes and Designated Institutes (NMIs and DIs). It is the task of the NMIs and DIs to realise and disseminate primary standards for providing traceability to the International System of Units (SI). The primary elemental standards at the NMIs should provide the link to secondary standards produced by commercial producers and other independently prepared standards for element determination. Without such primary standards, elemental calibration solutions may vary and, depending on the uncertainty required, comparability of measurement in time and space results cannot be achieved.
It has been successfully demonstrated that ceramic materials can be joined in the green
state without a second phase by using low pressure injection molded parts. The investigation of the
joining interface revealed that a high quality interface can be achieved by carefully adjusting the
different manufacturing steps. The use of monomodal particle size distribution in the used powder
CT3000SG is inferior to a broader particle size distribution obtained by replacing 33% of the finer
alumina powder by coarser CT1200SG. In this way the dewaxing process is significantly improved
when the wall thickness of the part exceeds 3 mm. The investigation of the mechanical properties of
the joined and sintered parts revealed, that the bending strength of the joined specimens achieved
about 80 % of the unjoined, monolithic specimens.
High- and medium-entropy alloys (HEAs) are a quite new class of materials. They have a high potential for applications from low to high temperatures due to the excellent combination of their structural properties.
Concerning their application as components; processing properties, such as machinability, have hardly been investigated so far. Hence, machinability analyses with a focus on the influence of the milling process and its basic parameters (cutting speed, feed per cutting edge) on the resulting surface integrity of specimens from an equiatomic high- (CoCrFeMnNi) and a medium- (CoCrNi) entropy alloy have been carried out. A highly innovative milling process with ultrasonic assistance (USAM) was compared to conventional milling processes.
Recent studies have shown that USAM has a high potential to significantly reduce the mechanical load on the tool and workpiece surface during milling. In this study, the basic machining and ultrasonic parameters were systematically varied. After machining, the surface integrity of the alloys was analyzed in terms of topography, defects, subsurface damage, and residual stresses. It was observed that USAM reduces the cutting forces and increases the surface integrity in terms of lower tensile residual stresses and defect density near the surfaces for the CoCrFeMnNi alloy. It was shown that the cutting forces and the metallurgical influence in the sub surface region are reduced by increasing the cutting speed and reducing the feed rate per cutting edge. With the CoCrNi alloy, the tool revealed severe wear. As a result, for this alloy no influence of the parameters on the machinability could be determined.
Imaging Capability of Terahertz and Millimeter-Wave Instrumentations for NDT of Polymer Materials
(2006)
Pulse thermography is a non-destructive testing method based on infrared imaging of transient thermal patterns. Heating the surface of the structure under test for a short period of time generates a non-stationary temperature distribution and thus a thermal contrast between the defect and the sound material. In modern NDT, a quantitative characterization of hidden imperfections in materials is desired. In particular, defect depth and shape are of interest. The reconstruction of the defect from thermography data is a nonlinear inverse problem, and ill-posed. We propose an algorithm for the identification of subsurface defects based on the travel time of the reflected thermal pulse. Our work extends results by Lugin and Netzelmann, taking lateral thermal flows directly into account while retrieving the defect depth. This requires significantly less computational work. Quantitative information about the defect shape and depth is obtained. Application of our method to both thermography data generated by a finite element simulation and experimental heating of PVC test specimens with different defects yields good reconstruction of the actual defects.
High spatially resolved quantitative bioimaging of CdSe/ZnS Quantum Dots uptake in two kinds of cells is investigated combining laser ablation inductively coupled plasma mass spectrometry and the spatially resolved analysis of dried pL-droplets from a solution with a known concentration of Quantum Dots. Single cells and dried pL-droplets are morphologically characterized by Atomic Force Microscopy. A number concentration of CdSe/ZnS QDs between 3.5 104 and 48 104 is estimated to be uptaken by several selected single cells, after being incubated in the presence of a QDs suspension added to a standard cell culture medium. Mono-elemental bioimaging at subcellular resolution seems to show a higher number concentration of the CdSe/ZnS QDs in the cytosol around the cell nucleus.
In Europe the maximum allowable concentration for tributyltin (TBT) compounds in surface water has been regulated by the water framework directive (WFD) and daughter directive that impose a limit of 0.2 ng L-1 in whole water (as tributyltin cation). Despite the large number of different methodologies for the quantification of organotin species developed in the last two decades, standardised analytical methods at required concentration level do not exist. TBT quantification at picogram level requires efficient and accurate sample preparation and preconcentration, and maximum care to avoid blank contamination. To meet the WFD requirement, a method for the quantification of TBT in mineral water at environmental quality standard (EQS) level, based on solid phase extraction (SPE), was developed and optimised. The quantification was done using species-specific isotope dilution (SSID) followed by gas chromatography (GC) coupled to inductively coupled plasma mass spectrometry (ICP–MS). The analytical process was optimised using a design of experiment (DOE) based on a factorial fractionary plan. The DOE allowed to evaluate 3 qualitative factors (type of stationary phase and eluent, phase mass and eluent volume, pH and analyte ethylation procedure) for a total of 13 levels studied, and a sample volume in the range of 250–1000 mL. Four different models fitting the results were defined and evaluated with statistic tools: one of them was selected and optimised to find the best procedural conditions. C18 phase was found to be the best stationary phase for SPE experiments. The 4 solvents tested with C18, the pH and ethylation conditions, the mass of the phases, the volume of the eluents and the sample volume can all be optimal, but depending on their respective combination. For that reason, the equation of the model conceived in this work is a useful decisional tool for the planning of experiments, because it can be applied to predict the TBT mass fraction recovery when the experimental conditions are drawn. This work shows that SPE is a convenient technique for TBT pre-concentration at pico-trace levels and a robust approach: in fact (i) number of different experimental conditions led to satisfactory results and (ii) the participation of two institutes to the experimental work did not impact the developed model.
For the first time, an international comparison was conducted on the determination of the purity of a high purity element. Participants were free to choose any analytical approach appropriate for their institute’s applications and services. The material tested was a high purity zinc, which had earlier been assessed for homogeneity and previously used in CCQM-K72 for the determination of six defined metallic impurities. Either a direct metal assay of the Zn mass fraction was undertaken by EDTA titrimetry, or an indirect approach was used wherein all impurities, or at least the major ones, were determined and their sum subtracted from ideal purity of 100 %, or 1 kg/kg. Impurity assessment techniques included glow discharge mass spectrometry, inductively coupled plasma mass spectrometry and carrier gas hot extraction/combustion analysis. Up to 91 elemental impurities covering metals, non-metals and semi-metals/metalloids were quantified. Due to the lack of internal experience or experimental capabilities, some participants contracted external laboratories for specific analytical tasks, mainly for the analysis of non-metals. The reported purity, expressed as zinc mass fraction in the high purity zinc material, showed excellent agreement for all participants, with a relative standard deviation of 0.011 %. The calculated reference value, w(Zn) = 0.999 873 kg/kg, was assigned an asymmetric combined uncertainty of + 0.000025 kg/kg and – 0.000028 kg/kg. Comparability amongst participating metrology institutes is thus demonstrated for the purity determination of high purity metals which have no particular difficulties with their decomposition / dissolution process when solution-based analytical methods are used, or which do not have specific difficulties when direct analysis approaches are used. Nevertheless, further development is required in terms of uncertainty assessment, quantification of non-metals and the determination of purity of less pure elements and/or for those elements suffering difficulties with the decomposition process.
In this article we present inelastic neutron scattering (INS) experiments on different systems of confined glass-formers. The aim of these experiments is to study the influence of spatial restriction on the microscopic dynamics related to the glass transition. Such results could be helpful for the detection of a currently speculated cooperativity length of the glass transition. The glass-forming component is either a molecular liquid or a polymer. The confining matrices are `hard' (silica glass, silicon) or `soft' (microemulsion droplets). For some experiments the confining structure could be spatially oriented. Except for the soft confinement the naïvely expected acceleration effect could only be found at low temperatures where INS experiments are difficult because of the long relaxation times. A clear effect of confinement could be observed for the glass-typical low energy vibrations (boson peak). This effect seems to be completely different for soft and hard confinement. Surprisingly, the experiments on oriented nanopores did not show any signs of an anisotropy of the dynamics.
Aiming for a round-robin test, a new method for the direct determination of fluorine in niobium oxide has been developed. It is based on the use of high-resolution molecular absorption spectra of calcium mono-fluoride (CaF) generated in the graphite tube, combined with the slurry sampling technique. The absorption measurement was performed at the 606.44 nm CaF rotational line. By using graphite tubes with zirconium carbide (ZrC) modified platform, the molecular absorption sensitivity of CaF has been improved by a factor of 20, and no additional chemical modifier was necessary. Generally, non-spectral interferences were observed in the presence of HCl, H2SO4, and H3PO4. For HCl, additional spectral interference occurred due to an overlap of the absorption spectra of CaF and CaCl. However, due to the absence of these mentioned substances in the current material, such interferences do not exist for this application. The characteristic mass found for the CaF 606.44 nm line was 0.1 ng; the limit of detection was 5 mg fluorine per kg solid sample (3σ criterion). The results obtained by the method were within the range of certified values. Comparing to the classical method such as the pyrohydrolysis-photometric method, the developed new method showed clear advantages regarding sensitivity and specificity. The time requirement for one sample analysis was strongly shortened from several hours to only some minutes.
The analytical potential of a nanosecond laser ablation inductively coupled plasma mass spectrometer (ns-LA-ICP-SFMS) system, equipped with an ultra-fast wash-out ablation chamber, is critically investigated for fast and highly spatially resolved (∼μm) qualitative elemental distribution within single cells. Initially, a low surface roughness (< 10 nm) thin In–SnO2 layer (total coating thickness ∼200 nm) deposited on glass is employed to investigate the size, morphology and overlapping of laser-induced craters obtained at different laser repetition rates, making use of Atomic Force Microscopy (AFM). Conical craters with a surface diameter of about 2 µm and depths of about 100 nm were measured after a single laser shot. Furthermore, the influence of the sampling distance (i.e. distance between the sample surface and the inner sniffer of the ablation chamber) on the LA-ICP-MS ion signal wash-out time is evaluated. A significant decrease of the transient 120Sn+ ion signal is noticed after slight variations (±200 μm) around the optimum sampling position. Ultra-fast wash-outs (< 10 ms) are achieved reducing the aerosol mixing from consecutive laser shots even when operating the laser at high repetition rates (25 – 100 Hz). Fast and highly spatially resolved images of elemental distribution within mouse embryonic fibroblast cells (NIH/3T3 fibroblast cells) and human cervical carcinoma cells (HeLa cells), incubated with gold nanoparticles (Au NPs) and Cd-based quantum dots (QDs), respectively, are determined at the optimized operating conditions. Elemental distribution of Au and Cd in single cells is achieved using a high scanning speed (50 µm/s) and high repetition rate (100 Hz). The results obtained for the distribution of fluorescent Cd-based QDs within the HeLa cells are in good agreement with those obtained by confocal microscopy. The size, morphology and overlapping of laser-induced craters in the fixed cells are also investigated using AFM, observing conical craters with a surface diameter of about 2.5 µm and depths of about 800 nm after a single laser shot.