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Paper des Monats
- ja (71)
Rhodium(III) octahedral complexes with amine and chloride ligands are the most common starting compounds for preparing catalytically active rhodium(I) and rhodium(III) species. Despite intensive study during the last 100 years, synthesis and crystal structures of rhodium(III) complexes were described only briefly. Some [RhClx(NH3)6-x] compounds are still unknown. In this study, available information about synthetic protocols and the crystal structures of possible [RhClx(NH3)6−x] octahedral species are summarized and critically analyzed. Unknown crystal structuresof(NH4)2[Rh(NH3)Cl5],trans–[Rh(NH3)4Cl2]Cl·H2O,andcis–[Rh(NH3)4Cl2]Clarereported based on high quality single crystal X-ray diffraction data. The crystal structure of [Rh(NH3)5Cl]Cl2 was redetermined. All available crystal structures with octahedral complexes [RhClx(NH3)6-x] were analyzed in terms of their packings and pseudo-translational sublattices. Pseudo-translation lattices suggest face-centered cubic and hexagonal closed-packed sub-cells, where Rh atoms occupy nearly ideal lattices.
In this study, a signal processing approach for heterodyne Փ-OTDR and C-OTDR systems that can obtain external perturbation and its frequency content in a faster way is proposed. We can detect vibrations with the same or better SNR using this processing approach, only with a single step and fast calculation. Fig. 12 shows the comparison of the normalized measurement time for the gamma matrix method and the conventional method throughout the three experiments. The speed of processing using a gamma matrix is ~35%–50% faster compared to a conventional method in high frequency test (PZT), low frequency test (walking) and street monitoring test. The processing speed in low frequency test is normally a bit lower than the similar high frequency one, since we must use higher number of time frames. Also, in street test we have higher speed because we can select wider gauges.
In this study, an approach for mitigation of LSFD in Φ-OTDR systems was proposed. By using one probe pulse as a reference in a system with two or more probe frequencies, we can remove unwanted low frequency noise that is originally caused by the laser source. Although LSFD is problematic issue, it is not the only source of low frequency noise. Change in temperature, humidity, physical surroundings, environment, etc., can result in such noises. The proposed method; however, is expected to highly suppresses all of these effects, regardless of their source, either in the time or frequency domain.
For comparing reference and probe signals, there are sophisticated methods, rather than normal differentiation, available for use. Some of these methods have a close relationship with CPD methods and can further enhance the results. These methods can be further discussed in an independent research or future work.
The proposed method is very helpful for increasing accuracy in passive and active seismic monitoring, reservoir monitoring, underwater monitoring, etc. It also helps using relatively simpler laser sources and make the whole system price-efficient, as well as processing data without lengthy compensation algorithms.
EPDM, HNBR and FKM materials were exposed at 150 ◦C to air under atmospheric pressure and to hydrogen at 50 bar for different ageing times. All measurements after hydrogen exposure were conducted on samples in degassed condition to assess irreversible effects resulting from that exposure and to compare them to those after ageing in air. Density, hardness, tensile properties, compression set, and hydrogen permeability of all samples were analysed. In both ageing environments, HNBR exhibited the most significant changes of material properties.
However, for both EPDM and HNBR, considerably less severe ageing effects were observed under hydrogen in comparison to ageing in air. On the other hand, FKM showed about the same low level of deterioration in both ageing environments but exhibited poor resistance against damage due to rapid gas decompression in hydrogen environment that can lead to seal failure. The obtained results may serve as a guidance toward a better understanding for design and utilisation of elastomeric materials in future hydrogen infrastructure components.
Recovery is an important measure for seal applications representing to which extent the elastomer regains its initial shape after deformation and release of an applied force. Compression set (CS) indicates the degree of recovery. Ethylene propylene diene rubber (EPDM) was aged at 75 ◦C, 100 ◦C, 125 ◦C and 150 ◦C for different ageing times up to five years and compression set measurements were performed at different times after disassembly and after additional tempering. Short- and long-term recovery up to one year after release for samples aged at 125 ◦C and 150 ◦C was also studied. To assess the curvature in the Arrhenius diagram that may occur due to non-sufficiently aged specimens, a degradation-rate based model was fitted to the CS data after tempering. For each ageing temperature, two decay fit functions were proposed, each with an activation energy and a corresponding degradative process. The influence of ageing on the leak-tightness after fast small partial release is investigated and estimated through the analysis of the shift factors from time temperature superposition (TTS) of CS measurements at different times after disassembly. Shift factors of CS measurement after 1 s and after additional tempering are in good agreement.
To improve the predictive capability of long-term stress relaxation of elastomers during thermo-oxidative ageing, a method to separate reversible and irreversible processes was adopted.
The separation is performed through the analysis of compression set after tempering. On the Basis of this separation, a numerical model for long-term stress relaxation during homogeneous ageing is proposed. The model consists of an additive contribution of physical and chemical relaxation.
Computer simulations of compression stress relaxation were performed for long ageing times and the results were validated with the Arrhenius treatment, the kinetic study and the time-temperature superposition technique based on experimental data. For chemical relaxation, two decay functions are introduced each with an activation energy and a degradative process. The first process with the lower activation energy dominates at lower ageing times, while the second one with the higher activation energy at longer ageing times. A degradation-rate based model for the evolution of each process and ist contribution to the total system during homogeneous ageing is proposed. The main advantage of the model is the possibility to quickly validate the interpolation at lower temperatures within the range of slower chemical processes without forcing a straight-line extrapolation.
During an extensive test programme at the Bundesanstalt für Materialforschung und prüfung, material property changes of EPDM O-rings were investigated at different ageing times and two ageing temperatures of 125∘C and 150∘C. To exclude possible diffusion-limited oxidation (DLO) effects that can distort the data, IRHD microhardness measurements were taken over the cross section of compressed O-rings. Continuous stress relaxation measurements were taken on samples free of DLO effects. The additional effect of physical processes to irreversible chemical ones during a long-term thermal exposure is quantified by the analysis of compression set measurements under various test conditions. By combining the different experimental methods, characteristic times relative to the degradation processes were determined. On the basis of experimental data, a microphysically motivated model that takes into account reversible and irreversible processes was developed. The parameter identification strategy of the material model is based on our experimental investigations on homogeneously aged elastomer O-rings. The simulated results are in good agreement with the experiments.
Elastomers are susceptible to chemical ageing, i.e., scission and cross-linking, at high temperatures. This thermally driven ageing process affects their mechanical properties and leads to limited operating time. Continuous and intermittent stress Relaxation measurements were conducted on ethylene propylene diene rubber (EPDM) and hydrogenated nitrile butadiene rubber (HNBR) samples for different ageing times and an ageing temperature of 125 °C. The contributions of chain scission and cross-linking were analysed for both materials at different ageing states, elucidating the respective ageing mechanisms. Furthermore, compression set experiments were performed under various test conditions. Adopting the two-network model, compression set values were calculated and compared to the measured data. The additional effect of physical processes to scission and cross-linking during a long-term thermal exposure is quantified through the compression set analysis. The characteristic times relative to the degradation processes are also determined.
Understanding the mechanical behavior of silicon nanowires is essential for the implementation of advanced nanoscale devices. Although bending tests are predominantly used for this purpose, their findings should be properly interpreted through modeling. Various modeling approaches tend to ignore parts of the effective parameter set involved in the rather complex bending response. This oversimplification is the main reason behind the spread of the modulus of elasticity and strength data in the literature. Addressing this challenge, a surface-based nanomechanical model is introduced in this study. The proposed model considers two important factors that have so far remained neglected despite their significance: (i) intrinsic stresses composed of the initial residual stress and surface-induced residual stress and (ii) anisotropic implementation of surface stress and elasticity. The modeling study is consolidated with molecular dynamics-based study of the native oxide surface through reactive force fields and a series of nanoscale characterization work through in situ threepoint bending test and Raman spectroscopy. The treatment of the test data through a series of models with increasing complexity demonstrates a spread of 85 GPa for the modulus of elasticity and points to the origins of ambiguity regarding silicon nanowire properties, which are some of the most commonly employed nanoscale building blocks. A similar conclusion is reached for strength with variations of up to 3 GPa estimated by the aforementioned nanomechanical models. Precise consideration of the nanowire surface state is thus critical to comprehending the mechanical behavior of silicon nanowires accurately. Overall, this study highlights the need for a multiscale theoretical framework to fully understand the size-dependent mechanical behavior of silicon nanowires, with fortifying effects on the design and reliability assessment of future nanoelectromechanical systems.
An observation of the fracture process in front of the crack tip inside a dentin sample by means of ex-situ X-ray computed tomography after uniaxial compression at different deformation values was carried out in this work. This ex-situ approach allowed the microstructure and fracturing process of human dentin to be observed during loading. No cracks are observed up to the middle part of the irreversible deformation in the samples at least visible at 0.4μm resolution. First cracks appeared before the mechanical stress reached the compression strength. The growth of the cracks is realized by connecting the main cracks with satellite cracks that lie ahead of the main crack tip and parallel its trajectory. When under the stress load the deformation in the sample exceeds the deformation at the compression strength of dentin, an appearance of micro-cracks in front of the main cracks is observed. The micro-cracks are inclined (~60°) to the trajectory of the main cracks. The further growth of the main cracks is not realized due to the junction with the micro-cracks; we assume that the micro-cracks dissipate the energy of the main crack and suppressed its growth. These micro-cracks serve as additional stress accommodations, therefore the samples do not break apart after the compression test, as it is usually observed under bending and tension tests.