Swiss Light Source Synchrotron Research Articles

Characterization of iLGADs using soft X-rays

Experiments at synchrotron radiation sources and X-ray Free-Electron Lasers in the soft X-ray energy range (250 eV–2 keV) stand to benefit from the adaptation of the hybrid silicon detector technology for low energy photons. Inverse Low Gain Avalanche Diode (iLGAD) sensors provide an internal gain, enhancing the signal-to-noise ratio and allowing single photon detection below 1 keV using hybrid detectors. In addition, an optimization of the entrance window of these sensors enhances their quantum efficiency (QE).In this work, the QE and the gain of a batch of different iLGAD diodes with optimized entrance windows were characterized using soft X-rays at the Surface/Interface:Microscopy beamline of the Swiss Light Source synchrotron. Above 250 eV, the QE is larger than 55% for all sensor variations, while the charge collection efficiency is close to 100%. The average gain depends on the gain layer design of the iLGADs and increases with photon energy. A fitting procedure is introduced to extract the multiplication factor as a function of the absorption depth of X-ray photons inside the sensors. In particular, the multiplication factors for electron- and hole-triggered avalanches are estimated, corresponding to photon absorption beyond or before the gain layer, respectively.

Pulmonary acini exhibit complex changes during postnatal rat lung development.

Pulmonary acini represent the functional gas-exchanging units of the lung. Due to technical limitations, individual acini cannot be identified on microscopic lung sections. To overcome these limitations, we imaged the right lower lobes of instillation-fixed rat lungs from postnatal days P4, P10, P21, and P60 at the TOMCAT beamline of the Swiss Light Source synchrotron facility at a voxel size of 1.48 μm. Individual acini were segmented from the three-dimensional data by closing the airways at the transition from conducting to gas exchanging airways. For a subset of acini (N = 268), we followed the acinar development by stereologically assessing their volume and their number of alveoli. We found that the mean volume of the acini increases 23 times during the observed time-frame. The coefficients of variation dropped from 1.26 to 0.49 and the difference between the mean volumes of the fraction of the 20% smallest to the 20% largest acini decreased from a factor of 27.26 (day 4) to a factor of 4.07 (day 60), i.e. shows a smaller dispersion at later time points. The acinar volumes show a large variation early in lung development and homogenize during maturation of the lung by reducing their size distribution by a factor of 7 until adulthood. The homogenization of the acinar sizes hints at an optimization of the gas-exchange region in the lungs of adult animals and that acini of different size are not evenly distributed in the lungs. This likely leads to more homogeneous ventilation at later stages in lung development.

On-demand droplet loading of ultrasonic acoustic levitator and its application for protein crystallography experiments

Higher throughput has been ever demanded in the state-of-the-art protein crystallography beamlines for applications such as the screening of drug targets in protein-ligand complex structures at room temperature. As a potential method to achieve an order of magnitude higher throughput, we explore capturing of ejected droplets by an acoustic levitator to remotely load single protein crystal samples to an acoustic levitation diffractometer at the Swiss Light Source synchrotron facility. The results from X-ray diffraction experiments support the feasibility of this method as a fully automated sample delivery for high-throughput serial crystallography experiments using the acoustic levitation.

Three‐dimensional visualization of rat retina by X‐ray differential phase contrast tomographic microscopy

The retina is one of the most tiny and sophisticated tissues of the body. Three dimensional (3D) visualization of the whole retina is valuable both in clinical and research arenas. The tissue has been predominantly assessed by time-consuming histopathology and optical coherence tomography (OCT) in research and clinical arenas. However, none of the two methods can provide 3D imaging of the retina. The purpose of this study is to give a volumetric visualization of rat retina at submicron resolution, using an emerging imaging technique-phase-contrast X-ray CT. A Sprague-Dawley (SD) rat eye specimen was scanned with X-ray differential phase contrast tomographic microscopy (DPC-microCT) equipped at the Swiss Light Source synchrotron. After scanning, the specimen was subjected to routine histology procedures and severed as a reference. The morphological characteristics and signal features of the retina in the DPC-microCT images were evaluated. The total retina and its sublayers thicknesses were measured on the DPC-microCT images and compared with those obtained from the histological sections. The retina structures revealed by DPC-microCT were highly consistent with the histological section. In this study, we achieved nondestructive 3D visualization of SD rat retina. In addition to detailed anatomical structures, the objective parameters provided by DPC-microCT make it a useful tool for retinal research and disease diagnosis in the early stage.

Characterization of Liquid Water Invasion in Gdls Using X-Ray Tomographic Microscopy

The accumulation of liquid water in the gas diffusion layer (GDL) of low temperature polymer electrolyte fuel cells (PEFC) results in increased mass transport limitations [1] and eventually in a significant potential and efficiency penalty. To achieve efficient water removal and maintain high performance, it is necessary to understand the morphological (porosity, pore and throat sizes) and chemical (surface tension) properties of the GDL, which control the water transport [2]. An ex-situ capillary pressure (pc) – saturation setup was developed in the framework of the IMPALA project [3] for imaging experiments using X-ray tomographic microscopy (XTM) at the Swiss Light Source synchrotron facility as it offers the advantage of well defined capillary pressure boundary conditions. This approach allows a quantitative analysis of the water transport through the GDL by linking the local saturation at the achieved pc levels with the microstructure of the invaded pores and throats.Within the setup, a hydrophilic membrane implements a homogeneous boundary condition at the bottom of the GDL. At the top of the GDL either a hydrophobic membrane or a flow field was placed. While the hydrophobic membrane setup allows to study complete liquid wetting of the pore space, the flow field structure allows to implement an anisotropic compression simulating PEFC conditions and to study its consequences on water transport. GDL samples of different suppliers have been tested. The breakthrough pressure, which corresponds to the capillary pressure when water reaches the opposite side of the injection surface, is a function of the materials. Correlation with the dry GDL microstructure shows that pore (and throat) size is the major controlling parameter. SGL 24BA shows a lower breakthrough pressure than Toray TGP-H060 due to larger throats and exhibits a stronger channel rib deviation of pore and throat sizes as well as of saturation.

The ionisation energy of cyclopentadienone: a photoelectron–photoion coincidence study

Imaging photoelectron photoion coincidence (iPEPICO) spectra of cyclopentadienone (C5H4=O and C5D4=O) have been measured at the Swiss Light Source Synchrotron (Paul Scherrer Institute, Villigen, Switzerland) at the Vacuum Ultraviolet (VUV) Beamline. Complementary to the photoelectron spectra, photoionisation efficiency curves were measured with tunable VUV radiation at the Chemical Dynamics Beamline at the Advanced Light Source Synchrotron (Lawrence Berkeley National Laboratory, Berkeley, CA, USA). For both experiments, molecular beams diluted in argon and helium were generated from the vacuum flash pyrolysis of o-phenylene sulphite in a resistively heated microtubular SiC flow reactor. The Franck–Condon profiles and ionisation energies were calculated at the CCSD(T) level of theory, and are in excellent agreement with the observed iPEPICO spectra. The ionisation energies of both cyclopentadienone-d0, IE(C5H4=O), and cyclopentadienone-d4, IE(C5D4=O), were observed to be the same: 9.41 ± 0.01 eV. The mass-selected threshold photoelectron spectrum (ms-TPES) of cyclopentadienone reveals that the C=C stretch in the ground state of the cation is excited upon ionisation, supporting computational evidence that the ground state of the cation is 2A2, and is in agreement with previous studies. However, the previously reported ionisation potential has been improved considerably in this work. In addition, since o-benzoquinone (o-O=C6H4=O and o-O=C6D4=O) is also produced in this process, its ms-TPES has been recorded. From the iPEPICO and photoionisation efficiency spectra, we infer an adiabatic ionisation energy of IE(o-O=C6H4=O) = 9.3 ± 0.1 eV, but the rather structureless spectrum indicates a strong change in geometry upon ionisation making this value less reliable.

In situ oxidation kinetics of magnetite nanoparticles by total scattering

Iron oxide nanoparticles (NPs) show different structures as a function of oxidation state. In particular, magnetite (Fe3O4) NPs are easily oxidized in air at moderate temperatures, eventually yielding maghemite (Fe2O3). Oxidation proceeds via the creation of iron vacancies. While the vacancies may be created with a random distribution throughout the octahedral Fe sites, they eventually order over a specific subset of these sites, lowering the symmetry from F-centered (magnetite) to P-centered (cubic maghemite). By ex situ X-ray Total Scattering studies of magnetite-maghemite NPs in different oxidation states[1] we have recently studied, by the DFA method[2], the correlation between particle diameter, stoichiometry and lattice parameter in polydisperse NP samples unraveling also the size dependence of lattice parameter and composition. Moreover, we have shown indirect evidence of the formation of a polycrystalline surface layer of maghemite on a magnetite core in the intermediate oxidation states. Motivated by the excellent ex-situ results, we have also performed in-situ studies where magnetite NPs were oxidised in air at moderate temperatures (50-200 C). We present here an in-situ study performed at the X04SA-Materials Science beamline of the Swiss Light Source synchrotron[3]. Total Scattering X-ray diffraction patterns were collected every few minutes, while the oxidation was completed within several hours. The mechanism of NPs oxidation - whereas a surface oxidised layer is formed by outwards diffusion of Fe, then the vacancies so created order themselves giving rise to the maghemite-magnetite phase transition, will be examined in great detail. We will discuss, on robust statistical basis, the calculation of kinetic and diffusion constants, the temperature effect on the lattice constant and on the thickness of the surface oxidised layer; the different possible structural models for the cubic-maghemite NPs. We thank for support Fondazione Cariplo (2009-0289).

In situ observation of rapid reactions in nanoscale Ni–Al multilayer foils using synchrotron radiation

The observation of rapid reactions in nanoscale multilayers present challenges that require sophisticated analysis methods. We present high-resolution in situ x-ray diffraction analysis of reactions in nanoscale foils of Ni0.9V0.1–Al using the Mythen II solid-state microstrip detector system at the Material Science beamline of the Swiss Light Source Synchrotron at Paul Scherrer Institute in Villigen, Switzerland. The results reveal the temperature evolution corresponding to the rapid formation of NiAl intermetallic phase, vanadium segregation and formation of stresses during cooling, determined at high temporal (0.125 ms) and angular (0.004°) resolution over a full angular range of 120°.

Hydrostatic levelling systems: Measuring at the system limits

Three hydrostatic displacement monitoring system applications in Switzerland are discussed; the first concerns experience gained monitoring the foundation of the Albigna dam, the second relating to the underground stability of the Swiss Light Source synchrotron and the third concerning the deformation of a bridge near the city of Lucerne. Two different principles were applied, the Hydrostatic Levelling System (HLS) using the “half-filled pipe principle” developed by the Paul Scherrer Institute and the Large Area Settlement System (LAS) using the “differential pressure principle”. With both systems ground deformations induced by tidal forces can be seen. However, high accuracy of single sensors is not sufficient. A well-designed configuration of the complete system is equally important. On the other hand there are also limits imposed by installation logistics and by the environmental conditions. An example is the bridge monitoring application, where the acceleration along the bridge due to the passage of heavy trucks limits the feasibility of using hydrostatic levelling measurements.

A rotating filter for the wiggler beamline at the Swiss Light Source

The advent of high-current, medium-energy storage rings and small-gap wigglers for the production of intense hard X-ray beams implies a high absorbed heat load in the filter, which removes long-wavelength radiation. A rotating filter assembly based on a commercially available crucible of glassy-carbon is described for use with a high-power wiggler beamline at the Swiss Light Source synchrotron facility.

Structural studies of strain-symmetrised modulation-doped Si/SiGe structures grown by molecular beam epitaxy

In this work, we present recent achievements on the low-temperature (∼300 °C) molecular beam epitaxial growth of high Ge content Si/SiGe modulation-doped multiple quantum well structures on Si 0.5Ge 0.5 pseudosubstrates. High-resolution X-ray reflectivity and diffraction experiments performed at the Swiss Light Source synchrotron, as well as analysis by transmission electron microscopy, showed very good control of the growth parameters and interface r.m.s. roughness as low as 0.4 nm.