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Nanocomposites based on poly(L-lactide) (PLA) and organically modified Ni/Al layered double hydroxides (NiAl/LDHs) are prepared by melt blending and investigated by a combination of size exclusion chromatography, differential scanning calorimetry (DSC), small-angle X-ray scattering (SAXS), wide-angle X-ray scattering, and broadband dielectric spectroscopy. A detailed comparison to the behavior of the corresponding MgAl/LDH–PLA nanocomposites is made. SAXS investigations show that the morphology of the NiAl/LDH–PLA nanocomposites is more intercalated compared to the MgAl/LDH based PLA nanocomposite, which is more exfoliated. The DSC investigation gives a different dependence of the degree of crystallization on the concentration of LDH for NiAl/LDH–PLA than for MgAl/LDH–PLA nanocomposite system. These differences are discussed taking the differences of the morphologies of both systems into account. Broadband dielectric spectroscopy reveals information about the molecular dynamics where essential differences are observed for all relaxation processes taking place in both systems which were related to the different morphologies.
The quantum yield is a critically important parameter in the development of lanthanide-based upconverting nanoparticles (UCNPs) for use as novel contrast agents in biological imaging and optical reporters in assays. The present work focuses on the influence of the beam Profile in measuring the quantum yield (f) of nonscattering dispersions of nonlinear upconverting probes, by establishing a relation between f and excitation light power density from a rate equation analysis. A resulting 60% correction in the measured f due to the beam profile utilized for excitation underlines the significance of the beam profile in such measurements, and its impact when comparing results from different Setups and groups across the world.
In concrete elements, simultaneously subjected to cyclic loadings and external alkalis, the risk for damage caused by or under participation of an alkali-silica reaction (ASR) is particularly high. This is of particular concern for concrete pavements due to the increasing heavy vehicle traffic and the application of sodium chloride (NaCl) de-icer during winter. Since 2004, the climate simulation concrete prism test (CS-CPT) has been used successfully to evaluate job mixtures for pavements by considering the impact of alkali-containing de-icers. However, the role of mechanical predamage on ASR is largely unclear. In a joint research project, the CS-CPT has been used to investigate the influence of preexisting microcracks on ASR. It was evident that an ASR initiated earlier in the predamaged concrete prisms due to the more rapid ingress of NaCl solution through the microcracks.
Approximation of the crack driving force for cracks at notches under static and cyclic loading
(2017)
The work deals with the efficient calculation of the elastic-plastic crack driving force (J-integral for monotonic loading andΔJ-integral under cyclic loading) for short cracks at notches as essential parameter for the reliable static and fatigue assessment of notched structures. The J- or ΔJ-integral is calculated based on analytical solutions for stress intensity factors, estimated by means of well-known weight function solutions in the case of cracks under power-law stress distributions. A plasticity-correction function is applied to the stress intensity factors to obtain the final expression of the crack driving force. The comparison between analytical solutions and finite element calculations in case of cracks at the weld toe in welded joints shows good agreement.
One of the great strengths of X-ray computed tomography over conventional inspection methods (ultrasound, thermography, radiography) is that it can image damage in 3D. However for curved ordeformed composite panels it can be difficult to automatically ascribe the damage to specific plies or inter-ply interfaces. An X-ray computed tomography (CT) data processing methodology is developed to extract the through-thickness distribution of damage in curved or deformed composite panels. The method is applied to [(0°/90°)2]s carbon fibre reinforced polymer (CFRP) panels subjected low velocity impact damage (5 J up to 20 J) providing 3D ply-by-ply damage visualisation and analysis. Our distance transform approach allows slices to be taken that approximately follow the composite curvature allowing the impact damage to be separated, visualised and quantified in 3D on a ply-by-ply basis. In this way the interply delaminations have been mapped, showing characteristic peanut shaped delaminations with the major axis oriented with the fibres in the ply below the interface. This registry to the profile of the panel constitutes a significant improvement in our ability to characterise impact damage in composite laminates and extract relevant measurements from X-ray CT datasets.
The 7th International Conference on Spectroscopic Ellipsometry (ICSE-7) was held in Berlin in June 2016, jointly organised by ICSE and BAM. The publication of the proceedings special issue in Applied Surface Science follows this event. In the special issue, about 100 articles on current topics of optics and surface science related to ellipsometry, polarimetry, and similar techniques are presented, underpinning the high significance of these techniques for many fields of materials science.
If fracture mechanics shall be applied to the total lifetime respectively the fatigue limit of components (within the meaning of the S-N curve approach) it has to address four challenges:
(a) It has to adequately describe so-called short crack propagation, which cannot be based on the common long crack concepts for principle reasons. Since the crack size is in the order of the plastic zone size, the modelling of short crack propagation cannot be based on the common linear elastic Delta K concept. Instead, an elastic-plastic parameter such as the cyclic J integral has to be applied. A second point is that the crack closure concept has to be modified in that the crack opening stress is not a constant, crack size- independent parameter but shows a transient behaviour with increasing short crack size.
(b) It has to provide a meaningful definition of the initial crack dimensions as the starting point for an S-N curve relevant (residual) lifetime analysis. This can be based either on the (statistical) size of material defects which can be treated as cracks or by the size of the crack which would arrest subsequent to early crack propagation, whatever is larger.
(c) It has to cope with the problem of multiple cracks for load levels higher than the fatigue limit such as it occurs in many applications in the absence of very large initial defects.
(d) This requires consequent statistical treatment taking into account variations in the local geometry of the area where crack initiation has to be expected as well as the scatter in the initial crack size and in the material data used for the analyses.
The unparalleled excited-state potential-energy landscape of the chromium(III)-based dye [1]3+ ([Cr(ddpd)2]3+; ddpd=N,N’-dimethyl-N,N’-dipyridin-2-ylpyridin-2,6-diamine) enables a strong dual emission in the near infrared region. The temperature dependence of this dual emission allows the use of [1]3+ as an unprecedented molecular ratiometric thermometer in the 210–373 K temperature range in organic and in aqueous media. Incorporation of [1]3+ in biocompatible nanocarriers, such as 100 nm-sized polystyrene nanoparticles and solutol micelles, provides nanodimensional thermometers operating under physiological conditions.
The mechanochemical Knoevenagel condensation of malononitrile with p-nitrobenzaldehyde was studied in situ using a tandem approach. X-ray diffraction and Raman spectroscopy were combined to yield time-resolved information on the milling process. Under solvent-free conditions, the reaction leads to a quantitative conversion to p-nitrobenzylidenemalononitrile within 50 minutes. The in situ data indicate that the process is fast and proceeds under a direct conversion. After stopping the milling process, the reaction continues until complete conversion. The continuous and the stopped milling process both result in crystalline products suitable for single crystal X-ray diffraction.
The practical performance of surface coatings in applications like catalysis, water splitting or batteries depends critically on the coating materials’ porosity. Determining the porosity in a fast and nondestructive way is still an unsolved problem for industrial thin-films technology. As a contribution to calibrated, non-destructive, optical layer characterisation, we present a multi-method comparison study on porous TiO2 films deposited by sol-gel synthesis on Si wafers. The ellipsometric data were collected on a range of samples with different TiO2 layer thickness and different porosity values. These samples were produced by templated sol-gel synthesis resulting in layers with a well-defined pore size and pore density. The ellipsometry measurement data were analysed by means of a Bruggeman effective medium approximation (BEMA), with the aim to determine the mixture ratio of void and matrix material by a multi-sample analysis strategy. This analysis yielded porosities and layer thicknesses for all samples as well as the dielectric function for the matrix material. Following the idea of multi-method techniques in metrology, the data was referenced to imaging by electron microscopy (SEM) and to a new EPMA (electron probe microanalysis) porosity approach for thin film analysis. This work might lead to a better metrological understanding of optical porosimetry and also to better-qualified characterisation methods for nano-porous layer systems.
1. IntroductionPorous materials, especially porous thin films play an importantrole in chemical and physical technology in every case where thecontact area between two media has to be maximised. From cataly-sis to photochemistry and photovoltaics, the applications of porouslayer materials are diverse and numerous [1–6].The accurate and non-destructive characterisation of porousfilms for layered systems poses a challenge. This applies especiallyfor the key parameter of porous films, their porosity, i.e. the mix-ing ratio between the Matrix of the film (host material) and thepore volume which is empty or filled with a fluid medium (inclu-sions). This parameter influences most of the physical and chemicalproperties of a porous thin film and is therefore essential for theunderstanding as well as the optimisation of this class of materials.