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We report the results of a Versailles Project on Advanced Materials and Standards (VAMAS) interlaboratory study on the measurement of the shell thickness and chemistry of nanoparticle coatings. Peptide-coated gold particles were supplied to laboratories in two forms: a colloidal suspension in pure water and particles dried onto a silicon wafer. Participants prepared and analyzed these samples using either X-ray photoelectron spectroscopy (XPS) or low energy ion scattering (LEIS). Careful data analysis revealed some significant sources of discrepancy, particularly for XPS. Degradation during transportation, storage, or sample preparation resulted in a variability in thickness of 53%. The calculation method chosen by XPS participants contributed a variability of 67%. However, variability of 12% was achieved for the samples deposited using a single method and by choosing photoelectron peaks that were not adversely affected by instrumental transmission effects. The study identified a need for more consistency in instrumental transmission functions and relative sensitivity factors since this contributed a variability of 33%. The results from the LEIS participants were more consistent, with variability of less than 10% in thickness, and this is mostly due to a common method of data analysis. The calculation was performed using a model developed for uniform, flat films, and some participants employed a correction factor to account for the sample geometry, which appears warranted based upon a simulation of LEIS data from one of the participants and comparison to the XPS results.
This article presents a solid cohesion model for the simulation of bonded granular assemblies in the frame of 3D discrete element approaches (DEM). A simple viscoplastic cohesion model for 2D geometries is extended to 3D conditions, while its yield criterion is generalized as a hyper-surface in the space of bond solicitations to include torsional moments. The model is then calibrated using experimental results of uniaxial traction at both the microscopic and macroscopic scales with an artificial granular cohesive soil. The paper finally presents some simulated results on the macromechanical sample traction application and briefly discusses the model's current limitations and promising prospects for subsequent works.
Redox behaviour of La-Cr compounds formed in CrOX/La2O3 mixed oxides and CrOX/La2O3/ZrO2 catalysts
(2003)
The redox behaviour of chromium oxide in CrOx/La2O3, CrOx/La2O3/ZrO2 and CrOx/ZrO2 mixed oxide systems has been investigated by temperature-programmed reduction (TPR), photoelectron spectroscopy (XPS) and Raman spectroscopy (RS). The formation of La-Cr compounds such as La2CrO6, LaCrO4 was shown to occur by calcination of CrOx/La2O3 and CrOx/La2O3/ZrO2 at 600 °C. With a Cr content of ca. 4 wt.%, it was revealed that, having been reduced to Cr3+-containing compounds, La2CrO6 and/or LaCrO4 in both systems may be restored by reoxidation at 600 °C. In the case of CrOx/La2O3/ZrO2 catalysts, it is suggested that these compounds were real surface species anchored as an overlayer on zirconia. Such a structure may stabilise, on the one hand, the tetragonal modification of zirconia and, on the other hand, highly dispersed state of Cr species in calcined as well as in reduced catalysts.
Nanocrystalline particles of high temperature pretreated titania, zirconia or hafnium oxide, embedded in a carbon matrix, have been found to catalyze the aromatization of n-octane into ethylbenzene (EB) and o-xylene (OX) with high selectivity. The carbon matrix itself is catalytically not active, but seems to co-operate with the transition metal oxides in such a way that the various metal oxide/carbon composite materials exhibit equal selectivity patterns. In detail, the carbon component stabilizes a high dispersion of the oxides during the high temperature pretreatment procedure. This thermal treatment results in a destruction of surface acidity of the oxides, which would otherwise be responsible for undesirable consecutive and parallel reactions. Moreover, the carbon component is involved in the deep dehydrogenation of alkanes to multiple unsaturated alkenes. This is explained by the ability of surface carbon atoms to interact with hydrogen. The bulk and surface structure of the catalysts have been characterized by XRD, specific surface area measurements, XPS, UPS, Raman spectroscopy, in situ ESR and DRIFT spectroscopy.
Patches of white etching layers on rail surfaces were investigated using sophisticated techniques like cross-sectional transmission electron microscopy (XTEM) and synchroton X-ray diffraction. Optical microscopy failed to resolve the microstructure, but in the TEM submicron grains with high dislocation densities and occasional twins, which are characteristic features of high carbon martensite, were observed. The martensitic structure was confirmed by evaluation of synchroton X-ray diffraction line profiles. The latter technique also allowed to determine dislocation densities of the order of 1012 cm-2 and residual compressive stresses of about 200 MPa.
CrOx/La2O3 mixed oxides, prepared by impregnating La2O3 with appropriate aqueous solutions of (NH4)2CrO4 and calcining at 600 °C for 4 h, have been investigated by means of XRD, TPR, XPS, DRIFTS, and Raman spectroscopy (RS). The formation of the compounds La2CrO6, La(OH)CrO4 and LaCrO4 under these conditions was evidenced. Strong peaks at 864, 884, 913, and 921 cm-1, as well as weak peaks at 136, 180, 354, 370, and 388 cm-1 in the RS spectrum of CrOx/La2O3 have been assigned to La2CrO6.
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.
A systematic structural investigation of R-phenyl-substituted 2,2':6',2"-terpyridines, a family of mono- and bifunctional charge transfer (CT)-operated fluorescent reporters for protons and metal ions, is presented. These molecules are equipped with non-binding and analyte coordinating donor substituents R (R = CF3, H, OMe, OH, DMA, A15C5 equaling monoaza-15-crown-5) of various donor strength and display CT-controlled spectroscopic properties and communication of analytereceptor interactions. The crystal structures of the neutral fluorescent probes are compared to the structures of their terpyridine-alkylated or -protonated counterparts that represent model systems for acceptor protonation or cation coordination. The aim is here a better understanding of the complexation-induced structural and spectroscopic changes and the identification of common packing motifs of bpb-R thereby taking into account the importance of terpyridine building blocks for the construction of supramolecular systems and coordination arrays revealing ππ interactions.
A novel synthetic strategy toward highly fluorinated BODIPY dyes with exceptional photostabilities relying on sustainable gold catalysis has been developed. A key to the tailored pyrrole precursors is the gold catalysis performed in ionic liquids as the reaction medium, allowing a facile recycling of the catalysts. The dyes prepared are well-matching with the spectral windows of popular rhodamine dyes and possess high brightness while showing a distinctly higher photostability than the rhodamines especially in aprotic solvents.
A liver biopsy specimen from a Wilson’s disease (WD) patient was analyzed by means of micro-X-ray fluorescence (mXRF) spectroscopy to determine the elemental distribution. First, bench-top mXRF was utilized for a coarse scan of the sample under laboratory conditions. The resulting distribution maps of copper and iron enabled the determination of a region of interest (ROI) for further analysis. In order to obtain more detailed elemental information, this ROI was analyzed by synchrotron radiation (SR)-based mXRF with a beam size of 4 mm offering a resolution at the cellular level. Distribution maps of additional elements to copper and iron like zinc and manganese were obtained due to a higher sensitivity of SR-mXRF. In addition to this, X-ray absorption near edge structure spectroscopy (XANES) was performed to identify the oxidation states of copper in WD. This speciation analysis indicated a mixture of copper(I) and copper(II) within the WD liver tissue.
For the last decades vibration based identification of damage on civil Engineering structures has become an important issue for maintenance operations on transport infrastructure.
Research in that field has been rapidly expanding from classic modal Parameter estimation using measured excitation to modern operational monitoring. Here the difficulty is to regard to the specific environmental and operational influence to the structure under observation. In this paper, two methods accounting for statistical and/or operational uncertainties are applied to measurement data of a progressive damage test on a prestressed concrete bridge. On the base of covariance driven Stochastic Subspace Identification (SSI) an algorithm is developed to monitor and automatically compute confidence intervals of the obtained modal parameters. Furthermore, a null space based non-parametric damage detection method, utilizing a statistical χ2 type test is applied to the measurement data. It can be shown that for concrete bridges the proposed methodology is able to clearly indicate the presence of structural damage, if the damage leads to a change of the structural system.
In Operational Modal Analysis, the modal parameters (natural frequencies, damping ratios and mode shapes) obtained from Stochastic Subspace Identification (SSI) of a structure, are afflicted with statistical uncertainty. For evaluating the quality of the obtained results it is essential to know the respective confidence intervals of these figures. In this paper we present algorithms that automatically compute the confidence intervals of modal parameters obtained from covarianceand data-driven SSI of a structure based on vibration measurements. They are applied to the monitoring of the modal parameters of a prestressed concrete highway bridge during a progressive damage test that was accomplished within the European research project IRIS. Results of the covariance- and data-driven SSI are compared.
For the last decades vibration based damage detection of engineering structures has become an important issue for maintenance operations on transport infrastructure. Research in vibration based structural damage detection has been rapidly expanding from classic modal parameter estimation to modern operational monitoring. Methodologies from control Engineering especially of aerospace applications have been adopted and converted for the application on civil structures. Here the difficulty is to regard to the specific environmental and operational influence to the structure under observation. A null space based damage detection algorithm is tested for its sensitivity to structural damage of a prestressed concrete road bridge. Specific techniques and extensions of the algorithm are used to overcome difficulties from the size of the structure which is associated with the number of recorded sensor channels as well as from the operational disturbances by a nearby construction site. It can be shown that for concrete bridges the proposed damage detection methodology is able to clearly indicate the presence of structural damage, if the damage leads to a significant change of the structural system. Small damage which do not result in a System change when not activated by loading, do not lead to a modification of the dynamic response behavior and for that cannot be detected with the proposed global monitoring method.
Structural health monitoring with statistical methods during progressive damage test of S101 Bridge
(2014)
For the last decades vibration based damage detection of engineering structures has become an important issue for maintenance operations on transport infrastructure. Research in vibration based structural damage detection has been rapidly expanding from classic modal parameter estimation to modern operational monitoring. Since structures are subject to unknown ambient excitation in operation conditions, all estimates from the finite data measurements are of statistical nature. The intrinsic uncertainty due to finite data length, colored noise, non-stationary excitations, model order reduction or other operational influences needs to be considered for robust and automated structural health monitoring methods. In this paper, two subspace-based methods are considered that take these statistical uncertainties into account, first modal parameter and their confidence interval estimation for a direct comparison of the structural states, and second a statistical null space based damage detection test that completely avoids the identification step. The performance of both methods is evaluated on a large scale progressive damage test of a prestressed concrete road bridge, the S101 Bridge in Austria. In an on-site test, ambient vibration data of the S101 Bridge was recorded while different damage scenarios were introduced on the bridge as a benchmark for damage identification. It is shown that the proposed damage detection methodology is able to clearly indicate the presence of structural damage, if the damage leads to a change of the structural system.
This article presents a solid cohesion model for the simulation of bonded granular assemblies in the frame of 3D discrete element approaches (DEM). A simple viscoplastic cohesion model for 2D geometries is extended to 3D conditions, while its yield criterion is generalized as a hyper-surface in the space of bond solicitations to include torsional moments. The model is then calibrated using experimental results of uniaxial traction at both the microscopic and macroscopic scales with an artificial granular cohesive soil. The paper finally presents some simulated results on the macromechanical sample traction application and briefly discusses the model's current limitations and promising prospects for subsequent works.
The cyclic R-curve describes the resistance of a material to fatigue crack propagation fromthe short to the long crack regimes and it is therefore an essential ingredient in any fracturemechanics-based fatigue assessment procedure. This work presents different testing proceduresemployed in the experimental determination of the cyclic R-curve, especially focusing onthe comparison with long fatigue crack propagation thresholds obtained by means of thecompression precracking load reduction (CPLR) procedure. The tests were performed on theEA4T steel considering different stress ratios. The results show a good reproducibility of thecyclic R-curves at every stress ratio and for any testing procedure. In addition, the cyclicR-curves were used in a fracture mechanics-based assessment to predict the fatigue limits ofspecimens containing micro-notches.
High quality tubular products are essential to the oil and gas industry. Quality control during their production focuses on the non-destructive detection of surface defects. The structured light technique is a candidate for the challenge to detect, monitor and evaluate such defects in real-time.
In the present study the automatic processing of structured light measurements is performed and validated. The algorithm for the automatic Analysis of inspection data has an advantage over current data evaluation methods based on individual assessments of operators.
Nitrogen-rich noble metal nitrides possess unique mechanical and catalytic properties, therefore their synthesis and characterization is of interest for fundamental solid state chemistry and materials science. In this study we have synthesized a singlesource precursor [Rh(NH3)6]3(N3)5Cl4 (Rh:N ratio 1:11). Its controlled decomposition in a laser-heated diamond anvil cell at 39 GPa resulted in a formation of rhodium pernitride, RhN2. According to the results of single-crystal X-ray diffraction RhN2 has arsenopyrite structure type crystal structure previously unknown for this compound (P21/c (no. 14).
A new type of test sample for the determination of lateral resolution in surface analysis is presented. The certified reference material BAM-L002 Nanoscale strip pattern for length calibration and testing of lateral resolution is an embedded cross-section of epitaxially grown layers of AlxGa1-xAs and InxGa1-xAs on GaAs substrate. The surface of the sample provides a flat pattern with strip widths of 0.4-500 nm. The combination of gratings, isolated narrow strips and sharp edges of wide strips offers improved possibilities for the calibration of a length scale, the determination of lateral resolution and the optimization of instrument settings. The feasibility of the reference material for an analysis of lateral resolution is demonstrated for SIMS.
Heat accumulation induced by a succession of railway brakings leads to changes of the friction conditions occurring in pad-disc contact. Infrared thermography observations show a progressive increase of surface temperature over the succession, as well as a modification of the hot band migration phenomenon. From a tribological point of view, the heat accumulation, accompanied by a wear increase, progressively modifies the friction behaviour from one braking to the next. Post-mortem observations of pads are performed on surface by scanning electron microscopy and in depth after Focus Ion Beam cut by scanning ion microscopy. Observations show that, with heat accumulation, the third body quantity rises inside the contact, in accordance with wear increase. It is concluded that source flows of third body, which increase with temperature, feed aplenty the contact and modify its load-bearing capacity.
In the paper the method of discrete modeling (movable cellular automata method) and combined discrete-continuous description of the simulated medium are used to analyze processes occurring in the local contact of the automotive brake system. The characteristic size of the considered region is 1.5 ?m. The following contact situation is simulated: steel fiber coated by an iron oxide film as the brake pad and pearlitic steel also coated by an iron oxide layer as the disc. On the assumption of oxide layer wearing we simulate the iron oxide - iron oxide, iron oxide - metal and metal - metal contacts.
The calculation results for the friction coefficient for various contact situations give quite adequate values. For example, for the oxide - oxide system the calculated coefficient is approximately equal to 0.4, while for the metal - metal contact the obtained value varies from 0.7 to 0.9. Analysis of a set of the obtained results allows concluding that oxide is formed more rapidly than the sliding layer, which in turn makes the friction coefficient value stabilized.