Обобщенная нуль-эллипсометрия в схеме "поляризатор-образец-анализатор"

The null-method in generalized ellipsometry with the use of the compensator-free “polarizer ‒ sample ‒ analyzer” scheme is considered for the case of s- and p-polarized incident light on an anisotropic system. Analytical expressions are given that connect the measured angular value — the analyzer azimuth at the detected radiation intensity minimum — with the (2x2) anisotropic Jones matrix elements. To determine the optical and geometric parameters of the studied anisotropic systems, it is proposed to use this value’s dependence on the sample orientation (azimuth). The method sensitivity is estimated. It was found that it is comparable to the sensitivity of the “polarizer‒compensator‒sample‒analyzer” scheme. A comparative analysis of this method and the known photometric method of generalized ellipsometry in the “polarizer-sample-analyzer” scheme based on measuring the dependence of the reflected light intensity on the sample azimuth at the fixed polarizer and analyzer positions is carried out. It is estimated that, to obtain the same sensitivity of these two methods, the one arc minute error in the proposed method corresponds to the 0.05% relative error in determining the energy reflection coefficient in the photometric method.

Maximizing completeness in single-crystal high-pressure diffraction experiments: phase transitions in 2°AP

Sufficiently high completeness of diffraction data is necessary to correctly determine the space group, observe solid-state structural transformations or investigate charge density distribution under pressure. Regrettably, experiments performed at high pressure in a diamond anvil cell (DAC) yield inherently incomplete datasets. The present work systematizes the combined influence of radiation wavelength, DAC opening angle and sample orientation in a DAC on the completeness of diffraction data collected in a single-crystal high-pressure (HP) experiment with the help of dedicated software. In particular, the impact of the sample orientation on the achievable data completeness is quantified and proved to be substantial. Graphical guides for estimating the most beneficial sample orientation depending on the sample Laue class and assuming a few commonly used experimental setups are proposed. The usefulness of these guides has been tested in the case of luminescent 1,3-diacetylpyrene, suspected to undergo transitions from the α phase (Pnma) to the γ phase (Pn21 a) and δ phase (P1121/a) under pressure. Effective sample orientation has ensured over 90% coverage even for the monoclinic system and enabled unrestrained structure refinements and access to complete systematic extinction patterns.

Exploitation of transition temperatures of NiTi- SMA by adjusting SLM parameters

It is well known that the transition temperatures, e.g. the austenite peak temperature Ap, of NiTi Shape Memory Alloys (SMAs) can be adjusted by changing the alloy composition. This topic recently became more interesting due to the possibilities to produce SMA-parts by additive manufacturing, specifically by Selective Laser Melting (SLM). The potential of new designs and smart structures by so-called 4D-printing with locally adjusted transition temperatures Ap potentially opens up new applications and novel temperature-responsive medical devices. This work focuses on the SLM manufacturing parameters exposure time ET (scanning speed) and laser power P and their impact on the transition temperature Ap beyond the commonly used generic process parameter energy density ED. By systematical variation of process- and scan-parameters, the impact of the P, ET, sample orientation and layer height LH as well as interdependencies between them have been studied. A wide range of transition temperatures Ap between -20°C and 70°C has been reached from one starting material by varying ET. These findings potentially allow the manufacturing of smart devices with multi-stage deformation processes in a single 4Dprinted part.

Soft X-ray ARPES for three-dimensional crystals in the micrometre region

An endstation dedicated to angle-resolved photoemission spectroscopy (ARPES) using a soft X-ray microbeam has been developed at the beamline BL25SU of SPring-8. To obtain a high photoemission intensity, this endstation is optimized for measurements under the condition of grazing beam incidence to a sample surface, where the glancing angle is 5° or smaller. A Wolter mirror is used for focusing the soft X-rays. Even at the glancing angle of 5°, the smallest beam spot still having a sufficient photon flux for ARPES is almost round on the sample surface and the FWHM diameter is ∼5 µm. There is no need to change the sample orientation for performing k x − k y mapping by virtue of the electron lens with a deflector of the photoelectron analyzer, which makes it possible to keep the irradiation area unchanged. A partially cleaved surface area as small as ∼20 µm was made on an Si(111) wafer and ARPES measurements were performed. The results are presented.

Evaluating Orientation Effects on the Fire Reaction Properties of Flax-Polypropylene Composites

In this work, the fire reaction properties of flax-polypropylene (PP) composites were investigated at multiple sample angles both experimentally and numerically under two different heat flux conditions (35 and 50 kW/m2) in the cone calorimeter environment. An innovative testing setup which can accommodate a wide range of angles between 0° and 90° for the sample angle frame was developed to perform cone calorimeter tests at different sample angles. An advanced numerical predictive model based on the finite volume method was developed using the fire dynamics simulator (FDS) to quantify the dependency of ignition and combustion properties with sample angles. The numerical model was validated against experimental data from the cone calorimeter tests. The experimental and numerical analyses were conducted to quantify the effects of sample orientation on the different fire reaction properties i.e., ignition time, ignition temperature, burn time, heat release rate (HRR), critical heat flux, etc. The numerical method was utilised to analyse the mechanisms controlling the effect of heat convection and radiation blockage on the heating process. The study establishes that the sample orientation (with respect to the heat flux normal) has a significant influence on the fire reaction properties of natural fibre composites.

Quantitative powder diffraction using a (2 + 3) surface diffractometer and an area detector

X-ray diffractometers primarily designed for surface X-ray diffraction are often used to measure the diffraction from powders, textured materials and fiber-texture samples in 2θ scans. Unlike in high-energy powder diffraction, only a fraction of the powder rings is typically measured, and the data consist of many detector images across the 2θ range. Such diffractometers typically scan in directions not possible on a conventional laboratory diffractometer, which gives enhanced control of the scattering vector relative to the sample orientation. There are, however, very few examples where the measured intensity is directly used, such as for profile/Rietveld refinement, as is common with other powder diffraction data. Although the underlying physics is known, converting the data is time consuming and the appropriate corrections are dispersed across several publications, often not with powder diffraction in mind. This paper presents the angle calculations and correction factors required to calculate meaningful intensities for 2θ scans with a (2 + 3)-type diffractometer and an area detector. Some of the limitations with respect to texture, refraction and instrumental resolution are also discussed, as is the kind of information that one can hope to obtain.

Fusion of Hyperspectral Images. Looking at the structure of vegetal tissues: a case study.

Hyperspectral imaging (HSI) is a useful non-invasive technique that offers spatial and chemical information of samples. Often, different HSI techniques are used to obtain complementary information from the sample by combining different image modalities (Image Fusion). However, issues related to the different spatial resolution, sample orientation or area scanned among platforms need to be properly addressed. Unmixing methods are helpful to analyze and interpret the information of HSI related to each of the components contributing to the signal. Among those, Multivariate Curve Resolution-Alternating Least Squares (MCR-ALS) offers very suitable features for image fusion, since it can easily cope with multiset structures formed by blocks of images coming from different samples and platforms and allows the use of optional and diverse constraints to adapt to the specific features of each HSI employed. In this work, a case study based on the investigation of cross-sections from rice leaves by Raman, synchrotron infrared and fluorescence imaging techniques is presented. HSI of these three different techniques are fused for the first time in a single data structure and analyzed by MCR-ALS. This example is challenging in nature and allows describing clearly the necessary steps required to perform unmixing in an image fusion context.

Laboratory Evaluation of Mechanical Properties of Draupne Shale Relevant for CO2 Seal Integrity

The mechanical integrity of caprocks overlying injection formations is one of the key factors for safe storage of carbon dioxide in geological formations. Undrained effects caused by CO2 injection on strength and elastic parameters should be properly considered in the operational design to avoid fracture creation, fault reactivation and unwanted surface uplift. This study presents results from eleven undrained triaxial compression tests and one oedometer test on the Draupne shale, which is the main caprock of the Smeaheia site in the North Sea, to extract parameters relevant for seal integrity. Tests have been performed on samples oriented perpendicular to and parallel with the horizontal layering of the rock to study the effects of sample orientation relative to the loading direction. Results from undrained triaxial tests showed only minor effects of sample orientation on friction and cohesion. However, when loading during undrained shearing was parallel with layering (horizontal samples), measured Young’s modulus was roughly 1.4 times higher than for the vertical samples. Undrained shearing of vertical samples generated 30–50% more excess pore pressure than for horizontal samples with similar consolidation stress owing to more volume compaction of vertical samples. With apparent pre-consolidation stress determined from a high-stress oedometer test, the normalized undrained shear strength was found to correlate well with the overconsolidation ratio following the SHANSEP (Stress History and Normalized Soil Engineering Properties) procedure.