The ID11-L HESEB Soft X-ray beamline and end station significantly enhance soft X-ray research capabilities. Operating in an energy range of 90–1800 eV, extendable to 70–2000 eV, the beamline achieves high performance with an energy resolution of E/ΔE > 8000 and a photon flux of 10 10 to 3.4 × 10 12 photons/s. Its 500 × 250 µm 2 beam spot size allows for precise measurements, including studies on magnetic materials using variable circular polarization. This paper presents the end station’s design, including the receptacle, magnetic sample holder, and ambient pressure capabilities, along with experimental results that demonstrate the beamline’s potential for diverse scientific applications.
SESAME and a consortium of five Helmholtz Centers are designing and installing a state-of-the-art soft X-Ray undulator beamline at the SESAME light source in Amman, Jordan. Funding is provided by the Helmholtz Association over a four year project cycle that started in January 2019. This is an interim report covering the first 36 months of the project where the construction and installation has been almost completed and commissioning and characterization of the beamline is about to start. Additionally, seminars, workshops, and a training program are part of the project aimed at establishing a broad user community.
Transnational access (TNA) to national radiation sources is presently provided via programmes of the European Commission by BIOSTRUCT-X and CALIPSO with a major benefit for scientists from European countries. Entirely based on scientific merit, TNA allows all European scientists to realise synchrotron radiation experiments for addressing the Societal Challenges promoted in HORIZON2020. In addition, by TNA all European users directly take part in the development of the research infrastructure of facilities. The mutual interconnection of users and facilities is a strong prerequisite for future development of the research infrastructure of photon science. Taking into account the present programme structure of HORIZON2020, the European Synchrotron User Organization (ESUO) sees considerable dangers for the continuation of this successful collaboration in the future.
Spectroscopy and imaging of condensed matter have benefited greatly from the availability of intense X-ray beams from synchrotron sources, both in terms of spatial resolution and of elemental specificity. The advent of the X-ray free electron laser (X-ray FEL) provides the additional features of ultra-short pulses and high transverse coherence, which greatly expand possibilities to study dynamic processes and to image non-crystalline materials. The proposed SwissFEL facility at the Paul Scherrer Institute is one of at present four X-ray FEL projects worldwide and is scheduled to go into operation in the year 2017. This article describes a selection of problems in nuclear materials science and technology that would directly benefit from this and similar X-ray FEL sources. X-ray FEL-based experiments are proposed to be conducted on nuclear energy-related materials using single-shot X-ray spectroscopy, coherent X-ray scattering and/or X-ray photon correlation spectroscopy in order to address relevant scientific questions such as the evolution in time of the irradiation-induced damage processes, the deformation processes in nuclear materials, the ion diffusion processes in the barrier systems of geological repositories, the boiling heat transfer in nuclear reactors, as well as the structural characterization of graphite dust in advanced nuclear reactors and clay colloid aggregates in the groundwater near a radioactive waste repository.
Advanced analytical techniques have been used to characterize nuclear materials at the Paul Scherrer Institute during the last decade. The analysed materials ranged from reactor pressure vessel (RPV) steels, Zircaloy claddings to fuel samples. The processes studied included copper cluster build up in RPV steels, corrosion, mechanical and irradiation damage behaviour of PWR and BWR cladding materials as well as fuel defect development. The used advanced techniques included muon spin resonance spectroscopy for zirconium alloy defect characterization while fuel element materials were analysed by techniques derived from neutron and X-ray scattering and absorption spectroscopy.
Synchrotron radiation techniques represent powerful tools to characterize materials down to the nanometer level. This paper presents a survey of the state-of-the-art synchrotron-based techniques which are particularly well-suited for investigating materials properties. Complementary X-ray absorption techniques such as extended X-ray absorption fine structure (EXAFS), X-ray magnetic circular dichroism (XMCD), photoemission electron microscopy (PEEM) are used to address the individual local atomic structure and magnetic moments in Fe-Cr model systems. The formation of atomic clusters/precipitates in such systems is also investigated by means of scanning transmission X-ray microscopy (STXM). Such advanced analytical techniques can not only offer valuable structural and magnetic information on such systems, they can also serve for validating computational calculations performed at different time and length scales which can help improve materials lifetime predictions.
Advanced nuclear plants are designed for long-term operation in quite demanding environments. Limited operation experience with the materials used in such plants necessitate a reliable assessment of damage and residual life of components. Non-destructive condition monitoring of damage is difficult, if not impossible for many materials. Periodic investigation of small samples taken from well defined locations in the plant could provide an attractive tool for damage assessments. This paper will discuss possibilities of using very small samples taken from plant locations for complementary condition monitoring. Techniques such as micro/nano-indentation, micropillar compression, micro bending, small punch and thin strip testing can be used for the determination of local mechanical properties. Advanced preparation techniques such as focused ion beam (FIB) allow the preparation of samples from these small volumes for micro-structural analyses with transmission electron microscope (TEM) and advanced X-ray synchrotron techniques. Modeling techniques (e.g. dislocation dynamics DD) can provide a quantitative link between microstructure and mechanical properties. Using examples from ferritic oxide dispersion strengthened materials the DD approach is highlighted to understand component life assessments.
Two zirconium alloys (Zr–2.5%Nb) – one oxidized in a pressurized water reactor, the other oxidized in autoclave and used as reference – are analyzed by combining synchrotron-based scanning transmission and fluorescence X-ray microscopy and micro-X-ray absorption spectroscopy (micro-XAS). Two-dimensional zirconium distribution maps recorded on the neutron irradiated and the non-irradiated autoclaved Zr–2.5%Nb alloys clearly allow the localization of the oxide and the metal parts of the interface with a micrometer spatial resolution. Micro-XAS investigations make possible the determination of the speciation of zirconium and niobium both in the oxide and the metal parts of the interface for the irradiated and non-irradiated samples. The coordination environment and/or the valency of zirconium and niobium in the metal and the oxide parts of the interface have been determined for both materials, and interpreted on the basis of comparison with metal and oxide reference compounds.
Silicon carbide (SiC) is investigated as a possible structural material for future nuclear power plants. It is utilized as fibre and/or as matrix in ceramic composite materials. The fibre reinforcement is necessary to provide the required ductility. In this work, the behaviour of pure SiC under irradiation by He implantation is studied. Samples are investigated by means of the extended X-ray absorption fine structure (EXAFS) spectroscopy, performed at the Si K-edge. The Fourier transforms of the EXAFS data indicate a decrease of the Si–Si bond related shells around the absorbing Si. The possible damage features are discussed and the three most probable ones for the irradiation conditions are selected for future modelling work.
X-rays from synchrotron beamlines provide a powerful tool for materials analysis in circumstances where long-term materials degradation under complex loading conditions (e.g., temperature, irradiation, and stress) becomes important. This may occur for advanced gas cooled reactors. Synchrotron X-rays can help to improve lifetime assessments by providing a more in-depth understanding of microstructural damage. This article summarizes results of X-ray absorption fine spectrum analysis and X-ray magnetic circular dichroism synchrotron techniques. They were employed to evaluate various microstructural features, which are important in understanding the lifetime of materials exposed to extreme conditions. Dispersoid strengthening by yttria particles, conditions that produce nanocrystal Zircaloy, and the role of magnetism on the stability of ferritic steels were taken as examples.
X-ray absorption near-edge structure (XANES) spectroscopy is applied to Zr-based alloys ((Zr,x%Nb) with x⩽1wt.%) corroded in steam at 415°C to resolve the niobium speciation in the metal and the oxide parts of their metal/oxide interface. By combining these synchrotron X-ray measurements with additional ab initio calculations of Nb K-edge XANES spectra, this study reveals (i) the presence of Nb0 in the metal and of Nb atoms having valency between +2 and +4 in the oxide as well as (ii) the coexistence of Nb-doped monoclinic and Nb-doped tetragonal zirconia structures within the oxide of the (Zr,1.0%Nb) alloy.
Synergistic synchrotron x-ray absorption experiments using imaging magnetic microspectroscopy, x-ray magnetic circular dichroism, and ab initio calculations on FeCr alloys reveal that the Cr content strongly influences the ferromagnetic microstructure and the Fe magnetic moments. The Cr local structure resolved by extended x-ray absorption fine structure (EXAFS) is also found to be affected by the alloy's composition. Both EXAFS and ab initio calculations show a change in the Cr local atomic structure above 10 at.% Cr content from the distance contraction of the first two coordination shells around the Cr absorbing atom. These results indicate the strong dependence of magnetic and structural properties of these alloys on Cr concentration.
Detailed understanding of the respective roles of solution and surface parameters on the reactions at uranyl solution/Al-(hydr)oxide interfaces is crucial to model accurately the behaviour of U in nature. We report studies on the effects of the initial aqueous uranyl speciation in moderately acidic solutions, e.g. of mononuclear, polynuclear uranyl species and/or (potential) U(VI) colloids, on the sorption of U by large surface areas of amorphous Al-hydroxide. Investigations by Extended X-ray Absorption Fine Structure (EXAFS) and Time-Resolved Laser-induced Fluorescence Spectroscopy (TRLFS) reveal similar U coordination environments on Al-hydroxide for low to moderate U loadings of sorption samples obtained at pH 4–5, independently of the presence of mononuclear or polynuclear aqueous species, or of the potential instability of initial solutions favoring true U-colloids formation. EXAFS data can be interpreted in terms of a dimeric, bidentate, inner-sphere uranyl surface complex as an average of the U surface structures. TRLFS data, however, provide valuable insights into the complex U surface speciation. They indicate multiple uranyl surface species under moderately acidic conditions, as predominant mononuclear and/or dinuclear, inner-sphere surface complexes and as additional minor species having U atoms in a uranyl (hydr)oxide-like coordination environment. The additional species probably occur as surface polymers and/or as adsorbed true U colloids, depending on the aqueous U concentration level (1–100 μM). These results are of importance because they suggest that Al-hydroxide surface characteristics strongly control uranyl surface species in moderately acidic systems.