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Paper des Monats
- ja (1)
High-entropy alloys (HEAs) and compositionally complex alloys (CCAs) represent new classes of materials containing five or more alloying elements (concentration of each element ranging from 5 to 35 at. %). In the present study, HEAs are defined as single-phase solid solutions; CCAs contain at least two phases. The alloy concept of HEAs/CCAs is fundamentally different from most conventional alloys and promises interesting properties for industrial applications (e.g., to overcome the strength-ductility trade-off). To date, little attention has been paid to the weldability of HEAs/CCAs encompassing effects on the welding metallurgy. It remains open whether welding of HEAs/CCAs may lead to the formation of brittle intermetallics and promote elemental segregation at crystalline defects. The effect on the weld joint properties (strength, corrosion resistance) must be investigated. The weld metal and heat-affected zone in conventional alloys are characterized by non-equilibrium microstructural evolutions that most probably occur in HEAs/CCAs. The corresponding weldability has not yet been studied in detail in the literature, and the existing information is not documented in a comprehensive way. Therefore, this study summarizes the most important results on the welding of HEAs/CCAs and their weld joint properties, classified by HEA/CCA type (focused on CoCrFeMnNi and AlxCoCrCuyFeNi system) and welding process.
The results of analytical measurements performed with solid-sampling techniques are affected by the distribution of the analytes within the matrix. The effect becomes significant in case of determination of trace elements in small subsamples. In this framework we propose a measurement model based on Instrumental Neutron Activation Analysis to determine the relative variability of the amount of an analyte among subsamples of a material. The measurement uncertainty is evaluated and includes the counting statistics, the full-energy gamma peak efficiency and the spatial gradient of the neutron flux at the irradiation position. The data we obtained in a neutron activation experiment and showing the relative variability of As, Au, Ir, Sb and W among subsamples of a highly pure Rh foil are also presented.
Medium and High Entropy Alloys (MEA/HEA) are recently developed material classes, providing manifold applications, e.g., due to extraordinary structural properties. In that connection, the machinability as important issue for the processing of these materials was not in the scientific focus. This study focusses on experimental analysis of milling process conditions including ultrasonic assisted milling (USAM) and their effects on the resulting surface integrity of equiatomic CoCrFeNi-MEA specimens. For that reason, milling parameters (cutting speed, feed per cutting edge) were systematically varied for both conventional milling and USAM. The surface integrity was analyzed in terms of topography, defects, and residual stresses. Especially USAM leads to a decrease of occurring cutting forces and, hence, to an improvement of the surface integrity. Beneficial effects were observed in terms of lower tensile residual stresses at high cutting speed and feed per cutting edge.
The European Union (EU) has included tributyltin (TBT) and its compounds in the list of priority water pollutants. Quality standards demanded by the EU Water Framework Directive (WFD) require determination of TBT at so low concentration level that chemical analysis is still difficult and further research is needed to improve the sensitivity, the accuracy and the precision of existing methodologies. Within the frame of a joint research project “Traceable measurements for monitoring critical pollutants under the European Water Framework Directive” in the European Metrology Research Programme (EMRP), four metrological and designated institutes have developed a primary method to quantify TBT in natural water using liquid–liquid extraction (LLE) and species-specific isotope dilution mass spectrometry (SSIDMS). The procedure has been validated at the Environmental Quality Standard (EQS) level (0.2 ng L−1 as cation) and at the WFD-required limit of quantification (LOQ) (0.06 ng L−1 as cation). The LOQ of the methodology was 0.06 ng L−1 and the average measurement uncertainty at the LOQ was 36%, which agreed with WFD requirements. The analytical difficulties of the method, namely the presence of TBT in blanks and the sources of measurement uncertainties, as well as the interlaboratory comparison results are discussed in detail.
Normally, in analytical GD-MS, the doubly charged metallic ion signals from the sample are several orders of magnitude less than the corresponding singly charged signals. However, we have observed that using a neon plasma, the M++ signals of some elements, which have double ionization energies close to the first ionization energy of neon, are of the same order as the M+ signal. Doubly charged ions may be produced directly in the discharge cell by electron ionization (EI), and also by two electron Penning ionization (TEP), but these processes cannot explain the above effect. In this paper, we suggest that an additional process named as ‘Charge Transfer and Ionization’ (CTI) produces such ions either in their ionic ground state or in an excited state. To confirm that this process is typical of the discharges used in GD-MS and not an artefact of any particular form of cell and ion extraction system, we have carried out comprehensive experimental measurements using three different GD-MS instruments, viz., Nu Astrum, VG9000 and ELEMENT GD and our results provide clear evidence for CTI. This is the first time the process has been identified as an ionization process in analytical GD-MS. CTI must be differentiated from Asymmetric Charge Transfer (ACT), which is a “selective” process and requires a close energy match (e.g. ΔE < 0.5 eV for a strong effect). On the other hand, CTI is “non-selective” in the sense that a close energy match is not required (e.g. a strong effect is observed with ΔE ∼ 2 eV), although the process only occurs for a limited number of elements, depending on the plasma gas used and the total energy required to doubly ionize the metallic atom.
After some months of operation, a number of PV modules develop a discolouration defect called 'snail trails', or 'snail traces', which appear as irregular dark stripes across the cells. Whereas these traces were soon identified as discoloured silver contacts along the cell edges or at micro cracks, the chemical and mechanistic reasons for this phenomenon have not yet been resolved in detail. In this work we show that silver nanoparticles accumulating within the encapsulation foil cause the brownish discolouration, and that certain additives of encapsulation and back sheet foils trigger the formation of these nanoparticles.
Selective Catalytic Reduction of Nitric Oxide by Ammonia over Egg-Shell MnOx/NaY Composite Catalysts
(2002)
A novel composite catalyst system for the selective catalytic reduction (SCR) of NOx by NH3 is described operating at temperatures lower than 470 K in the presence of water with NO conversions of 80100% at space velocities of 30,00050,000 h-1. The catalyst is prepared by egg-shell precipitation of MnO2 on the external surface of zeolite NaY. Structural and thermal stability of precipitated MnO2 as well as of the MnO2/NaY composite catalyst were characterized by N2 adsorption, X-ray diffraction, laser Raman spectroscopy, temperature-programmed reduction, and electron microscopy. MnO2 precipitated on zeolite NaY (15 wt% loading) retained its amorphous state up to calcination temperatures of 775 K. The zeolite component remained structurally intact. Calcination at higher temperatures destroyed the zeolite structure and transformed MnO2 into Mn3O4. DRIFT spectroscopic investigations revealed the presence of symmetric O=NON=O species formally corresponding to N2O3 on the composite catalyst after contact with NO. Catalytic measurements under integral flow conditions showed that the catalyst performance is associated with a close coupling of nitrite formation and its drain off from equilibria with NO/NO2 and nitrate by ammonia. Several results are in line with the diazotation mechanism, including NH3 protonation to NH4+, whereas prevailing Lewis acid sites should enable NH3 activation via amide species, thus leading to a parallel amide/nitrosamide SCR reaction route. The activity-temperature profile fulfills the requirements of a low-temperature NOx reduction catalyst for mobile diesel engines if an ammonia supply is implemented on board, e.g., by urea decomposition.
Volatile Organic Compounds (VOC) are ubiquitous in the indoor air since they are emitted from materials used indoors. Investigations of these materials are mostly carried out in emission test chambers under controlled climatic conditions. Reference materials are an important tool for quality assurance/Quality control of emission test chamber measurements but so far they are not commercially available. In this study, a new approach was tested to develop an appropriate reference material with homogenous and reproducible emission of the VOC with well measurable air concentrations in emission test Chambers larger than 20 L at air change rates of 0.5 - 1 /h.
Thermoplastic Polyurethane (TPU) was selected as Matrix material which was impregnated with 2,2,4- trimethyl-1,3-pentanediol monoisobutyrate (texanol) as test VOC using compressed carbon dioxide. An optimization of the impregnation parameters such as temperature, pressure, time, VOC injection volume and TPU sample size was performed until the targeted area specific Emission rate (SERa) value was reached. Further aspects like process control, storage effects and correlation of the sample size to the emission rate were investigated. It was found that the SERa immediately after sample preparation were not reproducible between the batches but became unified 10 days after loading into the test chamber indicating the necessity of aging before use. SERa between 13,000 and 18,000 mg m-2 h-1 were obtained, and the impregnated materials could be well stored in aluminum-coated polyethylene foil for at least seven weeks without significant losses. Furthermore, the impregnation of styrene and the SVOC 2,6-diisopropylnaphthalene was tested.
Mechanically interlocked molecules (MIMs) such as rotaxanes and catenanes are capable of mechanical motion on the nanoscale and are therefore promising prototypes for molecular machines in recent nanotechnology. However, most of the existing examples are isotropically distributed in solution, which prohibits concerted movement and with it the generation of macroscopic effects. Thus, arranging them in ordered arrays is of huge interest in recent research. We report the deposition of quite densely packed multilayers of tetralactam macrocycles on gold surfaces by metal-coordinated layer-by-layer self-assembly. Linear dichroism effects in angle-resolved NEXAFS spectra indicate a preferential orientation of the macrocycles. The sequence of the metal ions can be programmed by the use of different transition metal ions at each deposition step. Additionally, reversible on-surface pseudorotaxane formation was successfully realized by repeated uptake and release of axle molecules inside the macrocycles cavities.
Mechanically interlocked molecules (MIMs) such as rotaxanes and catenanes are capable of mechanical motion on the nanoscale and are therefore promising prototypes for molecular machines in recent nanotechnology. However, most of the existing examples are isotropically distributed in solution, which prohibits concerted movement and with it the generation of macroscopic effects. Thus, arranging them in ordered arrays is of huge interest in recent research. We report the deposition of quite densely packed multilayers of tetralactam macrocycles on gold surfaces by metal-coordinated layer-by-layer self-assembly. Linear dichroism effects in angle-resolved NEXAFS spectra indicate a preferential orientation of the macrocycles. The sequence of the metal ions can be programmed by the use of different transition metal ions at each deposition step. Additionally, reversible on-surface pseudorotaxane formation was successfully realized by repeated uptake and release of axle molecules inside the macrocycles cavities.
The development of two metallizations based on the solid-phase regrowth principle is presented, namely Pd/Sb(Zn) and Pd/Ge(Zn) on moderately doped In0.53Ga0.47As (p=4×1018 cm-3). Contact resistivities of 23×10-7 and 67×10-7 ?cm2, respectively, have been achieved, where both systems exhibit an effective contact reaction depth of zero and a Zn diffusion depth below 50 nm. Exhibiting resistivities equivalent to the lowest values of Au-based systems in this doping range, especially Pd/Sb(Zn) contacts are superior to them concerning metallurgical stability and contact penetration. Both metallizations have been successfully applied for contacting the base layer of InP/In0.53Ga0.47As heterojunction bipolar transistors.
One wavelength fits all
(2011)
Structuring of Thin-film Solar Cells with a Single Laser Wavelength Structuring of a PV module into a number of cells is necessary to lower the current and to increase the voltage, and is typically accomplished with nanosecond laser pulses of different wavelengths. Duetothe many available laser sources, complex and expensive scribing Setups are necessary. To overcome this a concept for laser structuring of thin-film PV modules using a single wavelength allows prediction ofthe ablation behaviourfor a given laser pulse energy.
Copolyesters with an alternating sequence of terephthalic acid and aliphatic dicarboxylic acids were prepared with three different methods. First, dicarboxylic acid dichlorides were reacted with bis(2-hydroxyethyl)terephthalate (BHET) in refluxing 1,2-dichlorobenzene. Second, the same monomers were polycondensed at 0-20 °C in the presence of pyridine. Third, dicarboxylic acid dichlorides and silylated BHET were polycondensed in bulk. Only this third method gave satisfactory molecular weights. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry revealed that the copolyesters prepared by the pyridine and silyl methods might have contained considerable fractions of cyclic oligoesters and polyesters despite the absence of transesterification and backbiting processes. The alternating sequences and thermal properties were characterized with 1H NMR spectroscopy and differential scanning calorimetry measurements, respectively. In agreement with the alternating sequence, all copolyesters proved to be crystalline, but the crystallization was extremely slow [slower than that of poly(ethylene terephthalate)]. A second series of alternating copolyesters was prepared by the polycondensation of silylated bis(4-hydroxybut- yl)terephthalate with various aliphatic dicarboxylic acid dichlorides. The resulting copolyesters showed significantly higher rates of crystallization, and the melting temperatures were higher than those of the BHET-based copolyesters. © 2001 John Wiley & Sons, Inc. J Polym Sci Part A: Polym Chem 39: 3371-3382, 2001
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.
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.