Beitrag zur Prüfung metallischer Werkstoffe im Torsionsversuch

Zusammenfassung Der Torsionsversuch eignet sich zur Untersuchung des plastischen Verhaltens von Metallen bei erhöhten Temperaturen, wenn die Fließspannung stark von der Umformgeschwindigkeit abhängt. Aus der gemessenen Drehmoment-Drehwinkel-Kurve wird die Fließkurvek _f () berechnet. Hierfür wird ein Fließkriterium benötigt, dessen Unsicherheit im allgemeinen größer ist als alle Meßfehler. Diese Unsicherheit geht aber nicht in die berechnete Dehngeschwindigkeitsempfindlichkeit ein, die somit als Hauptergebnis des Versuches anzusehen ist.Um die Bedingungen technischer Warmumformung zu simulieren, wird die Verwendung extrem kurzer Proben (flacher Scheiben) empfohlen, womit sehr hohe Umformgeschwindigkeiten erreicht werden können. Für die Auswertung derartiger Versuche ist die wirksame Länge der kurzen Proben — experimentell oder semiempirisch — zu bestimmen und die Kerbwirkung zu berücksichtigen. Im Gegensatz zur herkömmlichen Vorgehensweise wird empfohlen, die örtliche Spannung und Verzerrung nicht für die Mantelfläche der Probe zu berechnen, sondern für einen kritischen Radialabstand im Innern der Probe, für den die Schiebung von der Kerbwirkung unabhängig ist, so daß sich die zuverlässigsten Werte ergeben.

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Summary The torsion test is often used for studying the plastic deformation of metals at elevated temperatures when stress depends strongly on the strain rate. From the measured torque-twisting angle curve, the stress-strain curvek _f () has to be calculated. For this purpose a yield criterion has to be used the uncertaintly of which normally exceeds all experimental errors. This uncertaintly, however, does not propagate into the calculated strain rate sensitivity which therefore may be considered as the main result of the torsion test.For simulating the conditions of technical hot forming processes, the use of extremely short test pieces (flat discs) by which very high strain rates can be obtained is recommended. For evaluating the test data the efficient lenght of short specimens has to be determined. In opposition to the conventional procedure of test evaluation, it is recommended not to calculate stress and strain for the surface of the specimen but for a critical radius for which strain is independent of the notch effect so that the most reliable values are obtained.

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Fabrication and surface enhanced Raman spectroscopy of single Au@SiO2 dimers linked by benzenedithiol

Metal nanoparticle dimers with controllable gap distance have attracted considerable attention because of their promising application in plasmonics. Generally, gaps with nanometer or subnanometer dimensions generate localized surface plasmon resonance (LSPR) coupling effect, thus contributing to a strong electromagnetic field for improving surface enhanced Raman scattering (SERS) effect. Here, we developed a facile approach to fabricate Au@SiO₂ dimers through the steric hindrance effect, in which the SiO₂ shell functioned as a block and a rigid dithiol molecule was employed as linker. The thickness of the SiO₂ shell played a critical role in improving the yield of dimers. The dimerization efficiency increased significantly as the shell thickness decreased to ~1 nm. When 1,4‐benzenedithiol was used as linker molecule, the yield of dimers was ~30%. Few dimers were obtained when mecaptobenzonic acid was used as linker. A thicker shell is associated with a low yield of dimer, whereas a thinner shell resulted in the formation of multimers and linear structures. The low number of linker molecules on the exposed area of monodisperse single nanoparticles and the lack of LSPR coupling effect (‘hot spots’) resulted in the disappearance of SERS signals of the linkers. The estimated SERS enhancement factor was about eight fold because of the strong coupling effect in the gap of the dimer with the distance of the dithiol molecular length. From the above results, SERS combined with SEM could be developed into powerful tools for monitoring the formation of dimers and positioning of single dimers. It may aid the control of assembly of Au nanoparticles and in probing key issues about SERS enhancements. Copyright © 2015 John Wiley & Sons, Ltd.     

Defects band enhanced by resonance Raman effect in praseodymium doped CeO2

In this work, the origin of the Raman defects band at 570 cm⁻¹ of praseodymium‐doped ceria was revisited from in situ spectra using six different exciting lines between 458 and 785 nm at low temperatures after oxidizing or reducing treatment. The observation of overtones and the fast change of relative intensity with excitation wavelength were explained by a resonance effect around 514 nm, which involved a Pr⁴⁺ containing defect stabilized at the oxidized state leading to an absorption band around 530 nm. The reduction of Pr⁴⁺ cations contained in such defects modifies the electronic properties of praseodymium doped ceria inhibiting the resonance effect. Additionally, the number of D1 defects that involved Pr³⁺ cations and oxygen vacancies increased allowing them to be distinguished. Copyright © 2016 John Wiley & Sons, Ltd.     

Two polymorphs of 5‐cyclohexyl‐5‐ethylbarbituric acid and their packing relationships with other barbiturates

Polymorph (Ia) (m.p. 474 K) of the title compound, C₁₂H₁₈N₂O₃, displays an N—H...O=C hydrogen‐bonded layer structure which contains R₆⁶(28) rings connecting six molecules, as well as R₂²(8) rings linking two molecules. The 3‐connected hydrogen‐bonded net resulting from these interactions has the hcb topology. Form (Ib) (m.p. 471 K) displays N—H...O=C hydrogen‐bonded looped chains in which neighbouring molecules are linked to one another by two different R₂²(8) rings. Polymorph (Ia) is isostructural with the previously reported form II of 5‐(2‐bromoallyl)‐5‐isopropylbarbituric acid (noctal) and polymorph (Ib) is isostructural with the known crystal structures of four other barbiturates.     

Capillary isoelectric focusing immunoassay as a new nanoscale approach for the detection of oligoclonal bands

The detection of oligoclonal bands (OCBs) in cerebrospinal fluid is an indicator of intrathecal synthesis of immunoglobulins which is a neurochemical sign of chronic inflammatory brain diseases. Intrathecally synthesized IgGs are typically observed in patients with multiple sclerosis. The current standard protocol for the detection of OCBs is IEF on agarose or polyacrylamide gels followed by immunoblotting or silver staining. These methods are time consuming, show substantial interlaboratory variation and cannot be used in a high throughput‐approach. We have developed a new nanoscale method for the detection of OCBs based on automated capillary IEF followed by immunological detection. Evidence for intrathecal IgG synthesis was found in all tested patients (n = 27) with multiple sclerosis, even in two subjects who did not have oligoclonal bands according to standard methods. The test specificity was at 97.5% (n = 19). Our findings indicate that the novel OCB‐CIEF‐immunoassay is suitable for the rapid and highly sensitive detection of OCBs in clinical samples. Furthermore, the method allows for a higher sample throughput than the current standard methods.     

Water revealed as molecular mirror when measuring low concentrations of sugar with near infrared light

Near infrared spectroscopy is an overtone spectroscopy regarded as a quick and non-destructive method that provides analytical solutions for components that represent approximately 1% or more of the total mass of the investigated composite samples. Aquaphotomics offers the possibility for disentanglement of information remaining hidden in the spectra when conventional data evaluation methods are used, since this concept utilizes changes of the water structure induced by the measured solute as specific molecular vibrations at water bands. Here, near infrared technique and aquaphotomics are applied for non-destructive identification and quantification of mono- and di-saccharide solutes at 100–0.02 mM concentration that is accepted as unachievable with near infrared spectroscopy. The results presented in this study support the aquaphotomics' water molecular mirror concept that explores spectral changes related to water molecular rearrangements caused by minute changes of the solutes in the aqueous systems. The method provides quick and accurate alternative for classical analytical measurements of saccharides even at millimolar concentration levels.     

The representations of nested composition algebras

In this paper, we investigate the basis graph of the monoid algebra of a submonoid of the monoid of mappings from N = {1,…,n} to itself, defined by a nested sequence of compositions of N. Each such monoid is a left regular band (LRB), that is, a semigroup S satisfying x² = x and xyx = xy for all x,y∈S. This class is su?ciently rich that every path algebra of an acyclic quiver can be embedded in such a monoid algebra. The multiplication in the monoid algebra has a particularly simple quasi-multiplicative form, allowing definition over the integers. Combining this with a formula for Ext-groups for LRBs due to Margolis et al. [6 Margolis, S., Saliola, F., Steinberg, B. (2015). Combinatorial topology and the global dimension of algebras arising in combinatorics. J. Eur. Math Soc. 17(12):3037–3080.[Crossref], [Web of Science ®] , [Google Scholar]], we get a simple criterion for the nested composition algebras to be hereditary.     

On shapes of body waves in periodically inhomogeneous, magnetostrictive, dielectric materials

The shapes of shear body waves in periodically inhomogeneous, magnetostrictive, dielectric media are studied with emphasis on the partial (elastic and magnetostrictive) wave motions coupled to produce magnetoelastic waves __________ Translated from Prikladnaya Mekhanika, Vol. 42, No. 7, pp. 57–63, July 2006.     

Effect of Isochronous Annealing on the Formation of Shear Bands in the Vicinity of a Stress Concentrator on the Surface of Iron-Based Amorphous Alloys

The effect of isochronous annealing on the formation of shear bands in the vicinity of a stress concentrator on the surface of an amorphous material is studied. Using the local deformation method, a parameter is introduced to determine the temperature interval in which amorphous and crystal phases coexist.     

Hollow fiber liquid phase microextraction as a preconcentration and clean-up step after pressurized hot water extraction for the determination of non-steroidal anti-inflammatory drugs in sewage sludge

A method for the quantitative determination of non-steroidal anti-inflammatory drugs (NSAIDs) in sewage sludge was developed and validated. The target compounds were extracted using pressurized hot water extraction (PHWE) and then purified and preconcentrated by three-phase hollow fiber liquid phase microextraction (HF-LPME) followed by LC–ESI-MS analysis. The PHWE was optimized with regard to the pH of solvent as well as other operational parameters. The optimum conditions were 0.01 M NaOH as the extraction solvent, temperature of 120 °C, pressure of 100 bar, static time 5 min, 5 cycles, flush volume 90% and purge time 60 s. Spike recoveries for sludge samples spiked at 200 ng g⁻¹ were in the range of 101–109% but for the native drugs in non-spiked sludge samples, recoveries were 38.9%, 59.8%, 90.3% and 47.8% for ketoprofen, naproxen, diclofenac and ibuprofen, respectively. Donor phase pH, ionic strength and extraction time were optimized for HF-LPME after PHWE. The optimum conditions were 2 h extraction at pH 1.5 without salt addition. Enrichment factors in the range of 947–1213 times were achieved (extraction recoveries were 23.6–30.3%) for HF-LPME after PHWE. The matrix effect on the ionization of drugs in LC–ESI-MS was also investigated. The results show that there is a smaller matrix effect (−8.9% to +14.6%) in comparison with other published values obtained using solid phase extraction (SPE) for clean-up after pressurized liquid extraction (PLE). Method detection limits (MDLs) and method quantification limits (MQLs) for different drugs were in the range of 0.4–3.7 ng g⁻¹ and 1.5–12.2 ng g⁻¹ in dried sludge samples, respectively. The characteristics of the proposed method were compared with those of other published works. The considerably lower ion suppression/enhancement and minimum use of organic solvents (a few microliters of di-n-hexyl ether) in the sample preparation step are two highlighted advantages of the proposed method in comparison with previously published works. The method was applied to determine NSAIDs in sewage sludge from Källby wastewater treatment plant (Lund, Sweden) in April, June, August and October 2010. The highest concentration level was recorded for ibuprofen in the April sewage sludge sample (588 ng g⁻¹) and all of the selected NSAIDs were detected in all the samples analyzed.