Synchrotron Source Research Articles

X‐Ray Absorption and X‐Ray Emission Spectroscopy Study of a Molybdenum Disulfide Anode in a Sodium‐Ion Half‐Cell

The development of efficient anodes for sodium‐ion batteries requires a deep understanding of the electrochemical processes involved. Herein, X‐ray spectroscopy is used to study changes in the electronic structure of MoS2 nanosheets coupled with few‐layered graphene at early stages of battery life. Working electrode is combined with a sodium plate and a solution of NaClO4 in ethyl carbonate/dimethyl carbonate in a homemade cell having an X‐ray transparent window. X‐ray absorption spectra at the S K‐edge and Mo L3‐edge are recorded using a synchrotron source, X‐ray emission S Kα and Mo Lα spectra are obtained on a laboratory spectrometer for initial powder and electrode material at different potentials of the cell. Analysis of the spectra shows the occupation of the initially empty orbitals of MoS2 by sodium electrons as a result of the interaction of the components of the sodium‐ion half‐cell. Ex situ X‐ray photoelectron spectroscopy measurements of a fully discharged electrode material reveal partial transformation of hexagonal MoS2 to disordered tetragonal MoS2 coated with a surface electrolyte interphase layer. The obtained results indicate that coupling MoS2 to graphene prevents the breaking of Mo–S bonds when Na+ ions are first introduced, which may promote stable battery performance.

Development of crystal optics for X-ray multi-projection imaging for synchrotron and XFEL sources.

X-ray multi-projection imaging (XMPI) is an emerging experimental technique for the acquisition of rotation-free, time-resolved, volumetric information on stochastic processes. The technique is developed for high-brilliance light-source facilities, aiming to address known limitations of state-of-the-art imaging methods in the acquisition of 4D sample information, linked to their need for sample rotation. XMPI relies on a beam-splitting scheme, that illuminates a sample from multiple, angularly spaced viewpoints, and employs fast, indirect, X-ray imaging detectors for the collection of the data. This approach enables studies of previously inaccessible phenomena of industrial and societal relevance such as fractures in solids, propagation of shock waves, laser-based 3D printing, or even fast processes in the biological domain. In this work, we discuss in detail the beam-splitting scheme of XMPI. More specifically, we explore the relevant properties of X-ray splitter optics for their use in XMPI schemes, both at synchrotron insertion devices and XFEL facilities. Furthermore, we describe two distinct XMPI schemes, designed to faciliate large samples and complex sample environments. Finally, we present experimental proof of the feasibility of MHz-rate XMPI at the European XFEL. This detailed overview aims to state the challenges and the potential of XMPI and act as a stepping stone for future development of the technique.

Sheet-on-sheet fixed target data collection devices for serial crystallography at synchrotron and XFEL sources

Serial crystallography (SX) efficiently distributes over many crystals the radiation dose absorbed during diffraction data acquisition, enabling structure determination of samples at ambient temperature. SX relies on the rapid and reliable replacement of X-ray-exposed crystals with fresh crystals at a rate commensurate with the data acquisition rate. `Solid supports', also known as `fixed targets' or `chips', offer one approach. These are microscopically thin solid panes into or onto which crystals are deposited to be individually interrogated by an X-ray beam. Solid supports are generally patterned using photolithography methods to produce a regular array of features that trap single crystals. A simpler and less expensive alternative is to merely sandwich the microcrystals between two unpatterned X-ray-transparent polymer sheets. Known as sheet-on-sheet (SOS) chips, these offer significantly more versatility. SOS chips place no constraint on the size or size distribution of the microcrystals or their growth conditions. Crystals ranging from true nanocrystals up to microcrystals can be investigated, as can crystals grown in media ranging from low viscosity (aqueous solution) up to high viscosity (such as lipidic cubic phase). Here, we describe our two SOS devices. The first is a compact and lightweight version designed specifically for synchrotron use. It incorporates a standard SPINE-type magnetic base for mounting on a conventional macromolecular crystallography goniometer. The second and larger chip is intended for both X-ray free-electron laser and synchrotron use and is fully compatible with the fast-scanning XY-raster stages developed for data collection with patterned chips.

Subsurface hardening of Al irradiated with ultrafast infrared laser

The effect of femtosecond laser shock peening on a model Al-0.3Mn alloy was investigated experimentally and numerically by molecular dynamics. Micro-diffraction experiments performed at synchrotron source revealed the depth profiles of the residual stress and the stored energy of dislocations, a measure of local plasticity. The depth of the maximum compressive stress did not coincide with that of the maximum dislocation energy, which was found at the surface. The interaction between the laser and the metal was simulated with LAMMPS using a two-temperature molecular dynamics package. The model accurately described the equation of state of aluminum and showed nearly equal resolved shear stresses on all slip systems at the wavefront. The dislocation density at a depth of 1 μm, predicted by the Meyers' model [1], was higher than the experimental data, suggesting possible recovery due to the increased temperature of the sample after repeated shock loading.

Advances in hard X-ray RIXS toward meV resolution in the study of 5d transition metal materials

Resonant inelastic X-ray scattering (RIXS) has played a pivotal role in advancing our understanding of spin-orbit physics in 5d transition metal materials. The progress in RIXS techniques has closely paralleled improvements in energy resolution, which have enabled the study of very low-lying excitations and led to the discovery of numerous new phenomena with significant scientific and technological implications. The multi-bend achromat (MBA) lattice upgrade of third-generation synchrotron sources, such as the Advanced Photon Source (APS), heralds a transformative era by introducing enhancements in brilliance and emittance. These advancements provide an opportunity to push the boundaries of RIXS techniques, meeting the challenges at the research frontiers of material science. This article aims to highlight key instrumental and technical advancements that enable the achievement of meV resolution in RIXS and discuss the impact of such high-resolution RIXS on exploring spin-orbit physics in 5d transition metal materials.

Laboratory x-ray nano-computed tomography for biomedical research

High-resolution x-ray tomography is a common technique for biomedical research using synchrotron sources. With advancements in laboratory x-ray sources, an increasing number of experiments can be performed in the lab. In this paper, the design, implementation, and verification of a laboratory setup for x-ray nano-computed tomography is presented using a nano-focus x-ray source and high geometric magnification not requiring any optical elements. Comparing a scintillator-based detector to a photon counting detector shows a clear benefit of using photon counting detectors for these applications, where the flux of the x-ray source is limited and samples have low contrast. Sample contrast is enhanced using propagation-based phase contrast. The resolution of the system is verified using 2D resolution charts and using Fourier Ring Correlation on reconstructed CT slices. Evaluating noise and contrast highlights the benefits of photon counting detectors and the contrast improvement through phase contrast. The implemented setup is capable of reaching sub-micron resolution and satisfying contrast in biological samples, like paraffin embedded tissue.

The prototypical major cluster merger Abell 754

Context. Abell 754 is a rich galaxy cluster at z = 0.0543 and is considered the prototype of a major cluster merger. As many dynamically unrelaxed systems, it hosts diffuse radio emission on megaparsec-scales. Extended synchrotron sources in the intra-cluster medium (ICM) are commonly interpreted as evidence that a fraction of the gravitational energy released during cluster mergers is dissipated into nonthermal components. Aims. Here, we aim to use new MeerKAT UHF- and L-band observations to study nonthermal phenomena in Abell 754. These data are complemented with archival XMM-Newton observations to investigate the resolved spectral properties of both the radio and X-ray cluster emission. Methods. For the first time, we employed the pipeline originally developed to calibrate LOFAR data to MeerKAT observations. This allowed us to perform a direction-dependent calibration and obtain highly sensitive radio images in UHF and L bands that capture the extended emission with unprecedented detail. By using a large XMM-Newton mosaic, we produced thermodynamic maps of the ICM. Results. Our analysis reveals that the radio halo in the cluster center is bounded by the well-known shock in the eastern direction. Furthermore, in the southwest periphery, we discover an extended radio source that we classify as a radio relic that is possibly tracing a shock driven by the squeezed gas compressed by the merger, outflowing in perpendicular directions. The low-luminosity of this relic appears compatible with direct acceleration of thermal pool electrons. We interpret the observed radio and X-ray features in the context of a major cluster merger with a nonzero impact parameter. Conclusions. Abell 754 is a remarkable galaxy cluster showcasing exceptional features associated with the ongoing merger event. The high quality of the new MeerKAT data motivates further work on this system.

Survey of non-thermal electrons around supermassive black holes through polarization flips

Abstract Optically thick non-thermal synchrotron sources notably produce linear polarization vectors that are parallel to projected magnetic field lines on the observer’s screen, although they are perpendicular in well-known optically thin cases. To elucidate the complex relationship between the vectors and fields, and to investigate the energy and spatial distribution of non-thermal electrons through the images, we perform polarization radiative transfer calculations at submillimeter wavelengths. Here the calculations are based on semi-analytic force-free jet models with non-thermal electrons with a power-law energy distribution. In the calculated images, we find a $90{^\circ }$-flip of linear polarization vectors at the base of counter-side (receding) jet near a black hole, which occurs because of large optical depths for the synchrotron self-absorption effect. The $90{^\circ }$-flip of LP vectors is also seen on the photon ring at a high frequency, since the optical depth along the rays is large there due to the light bending effect. In addition, we see the flip of the sign of circular polarization components on the counter-jet and photon ring. Furthermore, we show that these polarization flips are synthesized with large values in the spectral index map, and also give rise to outstanding features in the Faraday Rotation Measure map. Since the conditions of flipping depend on the magnetic field strength and configuration and the energy distribution of electrons, we can expect that the polarization flips will provide us with observational evidence for the presence of non-thermal electrons around the black hole, and a clue to the magnetic driving mechanism of plasma jets.

On the Multi-Layered Adsorption of Alcanols in the Vicinity of Liquid–Vapor Transition at the Saturated Hydrocarbon–Water Interface

Structure of adsorption layer of long-chain monoatomic alcohols: 1-dodecanol and 1-tetracosanol at the interfaces n-hexane – water and n-hexadecane – water in the vicinity of “liquid – vapor” thermotropic phase transition is investigated by the method of X-ray reflectometry at synchrotron source. Model-independent structural data obtained on the adsorption layers under investigation deviate considerably from the structural parameters which have been proposed previously within a model-based representation and discussed in previous publications on said systems. It is shown that in the low-temperature mesophase the adsorption film consists of a Gibbs monolayer, a transitional liquid region with thickness of two to three monolayers ~50 Å and an extended (wide up to 200 Å) layer of micelles. Presence of a plane of the closest approach of micellar layer to the adsorption film at the interface is established. Transition to the high-temperature mesophase is followed by liquefying and partial evaporation of alcanol film along with observed depletion of micellar layer down to its complete disappearance.

X-ray circular dichroism measured by cross-polarization x-ray transient grating

Abstract Measuring natural circular dichroism in the x-ray regime to extract stereochemical information from chiral molecules in solution remains a challenge. This is primarily due to technical limitations of the existing synchrotron sources, which hinder access to measurements of local chirality by exploiting core hole electronic transitions. In response to this challenge, we propose an alternative approach: utilizing XFEL-based cross-polarization x-ray transient grating (XTG). This method provides an indirect means to measure x-ray circular dichroism (XCD). Notably, our findings reveal that the signal emerges only once the excited cores have undergone dephasing through relaxation. XTG is now routinely measured in the XUV regime and has recently been made available for hard x-rays. Free electron lasers now offer polarization controls, and XTG can be extended to various polarization states for the two pump beams, making XCD measured by XTG feasible with the current state-of-the-art technology.

Collimation principles of a hollow X-ray microbeam for high-contrast cytoplasm irradiation.

A Monte Carlo simulation was used to assess the performance of a collimated hollow X-ray microbeam for subcellular cytoplasm irradiation. A high-Z coaxial collimation structure with an inner core for nucleus shielding was investigated. Two key performances, the extraction efficiency (cytoplasm dose per unit incident fluence) and the dose contrast (cytoplasm-to-nucleus dose ratio), were evaluated regarding the influences of the material, geometry and physical arrangements of the collimator, target dish and incident beam source. Simulation results demonstrate that a gold coaxial structure with a practical collimation geometry of a 1-mm length, 10-μm inner diameter and 200-μm outer diameter, with the top exit closely attached (with a minimized air gap) to the bottom of a cell dish with a 3-μm thick Mylar film is recommended for cytoplasm irradiation of adherent mammalian cells. For a synchrotron source in the energy range < 10keV, a dose contrast of approximately 100 can be achieved. For a bremsstrahlung source <30-kV tube voltage, a dose contrast of approximately 50-100 can still be achieved. General principles are summarized with further explanations of the performance of the hollow X-ray microbeam.

Table-Top Ultrafast Soft X-Ray Spectroscopy Toward Synchrotron-like in-Situ Photoelectrochemical Measurements

Advancements in in-situ X-ray capabilities have enabled the measurement of electrochemical systems in more realistic operating conditions. While these measurements have progressed our understanding of electrochemical reactions from carrier dynamics to reaction mechanisms to degradation processes, they have mostly been limited to synchrotron facilities. However, performing in-situ table-top measurements has remained a challenge in the field. Table-top XUV spectrometers based on high-harmonic generation (HHG) are powerful tools for measuring ultrafast electronic and structural properties of photoelectrocatalysts ex-situ. However, extending the accessible energy range of HHG-based spectrometers beyond 300 eV is difficult due to inherent physical scaling laws. Laser-produced plasma sources can extend into the soft X-ray range to cover the water window. This capability could enable in-situ studies of photocatalysts, but their inherent source fluctuations have prevented ultrafast studies in the past. In this work, we employ methods pioneered by HHG-based setups to create a novel laser-produced plasma technique for table-top time-resolved measurements in the soft X-ray regime (200 – 1000 eV). We combine EMCCD detection, background-free self-referencing, edge-referencing analysis, amongst other advances, to reduce shot-to-shot noise so that sub-mOD signals are detectable. This presentation will also describe the technical advances pioneered at synchrotron sources that have enabled in-situ X-ray measurements of electrochemical systems. These advancements have inspired the effort to achieve the first table-top soft X-ray measurements in device-relevant liquid environments, enabling the correlation of photocatalyst properties, such as electron and hole energies and polarons, with photoelectrochemical product formation.

Towards the Direct Observation of the Local and Electronic Structure Evolution of Positive Electrode Materials by X-Ray Raman Scattering and X-Ray Emission Spectroscopy

The emergence of high brilliance synchrotron sources and the availability of more sophisticated infrastructure have opened doors to advanced material characterization, enabling a profound understanding of new processes and mechanisms in battery research. [1] More specifically, non-resonant Valence-to-Core X-ray emission spectroscopy (VtC-XES) and X-ray Raman scattering (XRS) stand out as complementary photon-in/photon-out X-ray spectroscopy techniques. The unique capability of these techniques lies in their access to soft X-ray edges using a hard X-ray beam, providing comprehensive information on both the electronic and local structure, due to their high sensitivity to local structure and coordination. [2,3] In this work, two different families of materials with different compositions and crystal structures are studied using XES and XRS.The first part focuses on the detailed study of oxygen substituted KVPO4F1-xOx (x = 0, 0.25, 0.5, 0.75, 1) using VtC-XES combined to ab initio theoretical calculations. The average working potential increases with increasing oxygen content by activating the V3+/4+ and V4+/5+ redox couples and replacing the VO4F2 “ionic” entity by {V=O}O5 unit with a highly “covalent” vanadyl-type bond. [4] VtC-XES allowed us to distinguish the contributions of V-F, V-O, and V=O bonds in the local environment, with spectral intensities highly correlated to the F- and O2- anionic composition. In addition, specific spectral evolutions are also associated to the presence of highly covalent V=O bonds, strongly influencing the electrode potential of the material.The second part examines a series of electrochemically obtained LiyNiO2 layered oxide materials (y = 0.02, 0.25, 0.33, 0.5, 0.67, 1.0). VtC-XES performed at the Ni Kβ emission line allows to study the local structure evolution around Ni, whereas XRS spectroscopy at both the O K-edge and Ni L2,3 L-edges gives an access to the interplay between Ni and O through the hybridized states of Ni 3d and O 2p. [5] This work provides a survey on both the cationic and anionic redox processes, and unveils the underlying phenomena related to the charge compensation processes occurring in this material.Overall, we present a comprehensive study of different polyanionic and layered oxide positive electrode materials using complementary X-ray spectroscopic techniques to probe both the local and electronic structures. We demonstrate that they allow to follow and understand evolution and changes in the local structure in materials of intricate crystal structures.AcknowledgementThis work was supported by the DESTINY Marie Skłodowska-Curie Actions COFUND PhD Programme (Grant Agreement #945357) co-funded by the European Union's Horizon2020 research and innovation program and the Synchrotron SOLEIL. ANR is also acknowledged for funding the RS2E network through the STORE-EX Labex Project ANR-10-LABX-76-01. Alistore-ERI network is also acknowledged.

Characterizing electron-collecting CdTe for use in a 77 ns burst-rate imager.

The Keck-PAD (pixel array detector) was developed at Cornell as a burst-rate imager capable of recording images from successive electron bunches (153 ns period) from the Advanced Photon Source (APS). Both Si and hole-collecting Schottky CdTe have been successfully bonded to this ASIC (application-specific integrated circuit) and used with this frame rate. The facility upgrades at the APS will lower the bunch period to 77 ns, which will require modifications to the Keck-PAD electronics to image properly at this reduced period. In addition, operation at high X-ray energies will require a different sensor material having a shorter charge collection time. For the target energy of 40 keV for this project, simulations have shown that electron-collecting CdTe should allow >90% charge collection within 35 ns. This collection time will be sufficient to sample the signal from one frame and prepare for the next. 750 µm-thick electron-collecting Schottky CdTe has been obtained from Acrorad and bonded to two different charge-integrating ASICs developed at Cornell, the Keck-PAD and the CU-APS-PAD. Carrier mobility has been investigated using the detector response to single X-ray bunches at the Cornell High Energy Synchrotron Source and to a pulsed optical laser. The tests indicate that the collection time will meet the requirements for 77 ns imaging.

Correcting directional dark field x-ray imaging artefacts using position dependent image deblurring and attenuation removal

In recent years, a novel x-ray imaging modality has emerged that reveals unresolved sample microstructure via a “dark-field image”, which provides complementary information to conventional “bright-field” images, such as attenuation and phase-contrast modalities. This x-ray dark-field signal is produced by unresolved microstructures scattering the x-ray beam resulting in localised image blur. Dark-field retrieval techniques extract this blur to reconstruct a dark-field image. Unfortunately, the presence of non-dark-field blur such as source-size blur or the detector point-spread-function can affect the dark-field retrieval as they also blur the experimental image. In addition, dark-field images can be degraded by the artefacts induced by large intensity gradients from attenuation and propagation-based phase contrast, particularly around sample edges. By measuring any non-dark-field blurring across the image plane and removing it from experimental images, as well as removing attenuation and propagation-based phase contrast, we show that a directional dark-field image can be retrieved with fewer artefacts and more consistent quantitative measures. We present the details of these corrections and provide “before and after” directional dark-field images of samples imaged at a synchrotron source. This paper utilises single-grid directional dark-field imaging, but these corrections have the potential to be broadly applied to other x-ray imaging techniques.

Probing particle acceleration in Abell 2256: From 16 MHz to gamma rays

Merging galaxy clusters often host spectacular diffuse radio synchrotron sources. These sources can be explained by a non-thermal pool of relativistic electrons that are accelerated by shocks and turbulence in the intracluster medium. The origin of the pool and details of the cosmic ray transport and acceleration mechanisms in clusters are still open questions. Due to the often extremely steep spectral indices of diffuse radio emission, it is best studied at low frequencies. However, the lowest frequency window available to ground-based telescopes (10−30 MHz) has remained largely unexplored as radio frequency interference and calibration problems related to the ionosphere become severe. Here, we present LOFAR observations from 16 to 168 MHz targeting the famous cluster Abell 2256. In the deepest-ever images at decametre wavelengths, we detected and resolved the radio halo, radio shock, and various steep spectrum sources. We measured standard single power-law behaviour for the radio halo and radio shock spectra, with spectral indices of α = −1.56 ± 0.02 from 24 to 1500 MHz and α = −1.00 ± 0.02 from 24 to 3000 MHz, respectively. Additionally, we found significant spectral index and curvature fluctuations across the radio halo, indicating an inhomogeneous emitting volume. In contrast to the straight power-law spectra of the large-scale diffuse sources, the various AGN-related sources showed extreme steepening towards higher frequencies and flattening towards low frequencies. We also discovered a new fossil plasma source with a steep spectrum between 23 and 144 MHz, with α = −1.9 ± 0.1. Finally, by comparing radio and gamma-ray observations, we ruled out purely hadronic models for the radio halo origin in Abell 2256, unless the magnetic field strength in the cluster is exceptionally high, which is unsupportable by energetic arguments and inconsistent with the knowledge of other cluster magnetic fields.

Imaging inter - and intra-particle features in crystalline cathode materials for Li-ion batteries using nano-focused beam techniques at 4th generation synchrotron sources

Imaging inter - and intra-particle features in crystalline cathode materials for Li-ion batteries using nano-focused beam techniques at 4th generation synchrotron sources

Multidimensional Analysis of the Adult Human Heart in Health and Disease Using Hierarchical Phase-Contrast Tomography.

Background Current clinical imaging modalities such as CT and MRI provide resolution adequate to diagnose cardiovascular diseases but cannot depict detailed structural features in the heart across length scales. Hierarchical phase-contrast tomography (HiP-CT) uses fourth-generation synchrotron sources with improved x-ray brilliance and high energies to provide micron-resolution imaging of intact adult organs with unprecedented detail. Purpose To evaluate the capability of HiP-CT to depict the macro- to microanatomy of structurally normal and abnormal adult human hearts ex vivo. Materials and Methods Between February 2021 and September 2023, two adult human donor hearts were obtained, fixed in formalin, and prepared using a mixture of crushed agar in a 70% ethanol solution. One heart was from a 63-year-old White male without known cardiac disease, and the other was from an 87-year-old White female with a history of multiple known cardiovascular pathologies including ischemic heart disease, hypertension, and atrial fibrillation. Nondestructive ex vivo imaging of these hearts without exogenous contrast agent was performed using HiP-CT at the European Synchrotron Radiation Facility. Results HiP-CT demonstrated the capacity for high-spatial-resolution, multiscale cardiac imaging ex vivo, revealing histologic-level detail of the myocardium, valves, coronary arteries, and cardiac conduction system across length scales. Virtual sectioning of the cardiac conduction system provided information on fatty infiltration, vascular supply, and pathways between the cardiac nodes and adjacent structures. HiP-CT achieved resolutions ranging from gross (isotropic voxels of approximately 20 µm) to microscopic (approximately 6.4-µm voxel size) to cellular (approximately 2.3-µm voxel size) in scale. The potential for quantitative assessment of features in health and disease was demonstrated. Conclusion HiP-CT provided high-spatial-resolution, three-dimensional images of structurally normal and diseased ex vivo adult human hearts. Whole-heart image volumes were obtained with isotropic voxels of approximately 20 µm, and local regions of interest were obtained with resolution down to 2.3-6.4 µm without the need for sectioning, destructive techniques, or exogenous contrast agents. Published under a CC BY 4.0 license Supplemental material is available for this article. See also the editorial by Bluemke and Pourmorteza in this issue.

Archaeometry at synchrotrons: how to get the most out of ancient materials

X-rays techniques are widely utilised in the field of archaeometry because of the numerous advantages they present. Using X-rays, structural and chemical details of specimens can be assessed while preserving artefacts integrity, with the additional benefit of requiring little or no sample preparation procedures. Synchrotron sources produce high-intensity, highly collimated beams whose energy can be easily tuned over broad ranges going from the IR to the X-rays. Their peculiarities include unbeatable spatial resolution, enhanced elemental selectivity, and extraordinary chemical sensitivity. In recent years, synchrotron beams have achieved a significant evolution thanks to several factors, such as advancements in source and optics design, acquisition of higher-level technical and scientific expertise, etc. This has ignited an increasing interest in synchrotron-based techniques which are expanding more and more, approaching always new frontiers. This work presents the main characteristics of synchrotrons and aims to help the unfamiliar readers in the non-trivial choice between laboratory and synchrotron sources for their scientific investigations.

Depth-resolved mechanical behaviour of shot peened 7050-T7451 aluminium surfaces using in-situ synchrotron X-ray diffraction

We have assessed the elasto-plastic (sub)surface behaviour of 7050-T7451 aluminium alloy treated by shot peening using S110 steel shots of 300 μm in diameter and two different intensities, namely Almen intensity (A) of 3.4 (low-intensity) and 10.9 (high-intensity). Shot peening (SP) is a cold work process applied in the aerospace industry to enhance the fatigue tolerance of structural components after machining. The local mechanical response within the SP-induced layer was depth profiled at room temperature by performing an X-ray micro-diffraction experiment in transmission geometry at a synchrotron source, during tensile loading of the specimen to rupture. The presence of a SP-induced layer in the specimen is evidenced by compressive longitudinal lattice strains (∼-540 με for low-intensity and ∼-4200 με for high-intensity at 0.1 mm from the surface for the 311 reflection), parallel with respect to the applied load, i.e. perpendicular to the direction of impact of the steel shots, and also by higher values of the Full-Width-at-Half-Maximum (FWHM) of the diffraction peaks than those measured in the bulk material, due to the local plastic deformation induced by shot peening. High-intensity shot peening produced a higher surface roughness (Sa ∼13 μm), and also two times thicker deformed surface layer (∼0.4 mm), than low-intensity shot peening (Sa ∼2 μm and ∼0.2 mm thick deformed layer). For both shot peening conditions, the local yield stress of the surface layer and bulk material were similar, however the severely affected layers exhibit a non-linear elastic behaviour when applying loads lower than the yield stress of the material. Beyond yielding, the presence of SP-induced layers is mainly evidenced by the relatively higher value of the FWHM near-surface compared to the bulk (∼20 % higher for low-intensity and ∼40 % for high-intensity), due to the initial plastic deformation accumulated during shot peening and additional plasticity during loading of the specimen.