Modern synchrotron beamlines support increasingly complex experiments, but their operation remains strongly dependent on facility-specific control interfaces and workflows. This reliance creates a significant barrier to entry for new users and limits the portability of experimental procedures across beamlines. Here, we present a minimal, agent-agnostic orchestration architecture for AI-assisted beamline operation, deployed at Advanced Light Source beamline 5.3.1. The approach introduces a capability-based abstraction layer that exposes beamline functionality as a set of predefined operations. Within this framework, AI agents translate natural-language user requests into structured experimental plans composed of these capabilities. All plans are executed through the Bluesky Queue Server, ensuring deterministic operation within existing control and safety constraints without modification of the underlying beamline control system. The framework is defined by three key elements: (i) a portable capability layer that decouples user intent from beamline-specific implementation, (ii) a hybrid interaction framework combining AI-assisted workflow composition with graphical user interface (GUI)-based monitoring and control, and (iii) constrained execution that restricts all actions to predefined capabilities and requires user approval prior to execution. We demonstrate the architecture using grazing-incidence scattering (GISAXS), multi-edge X-ray absorption spectroscopy (XANES), and cross-beamline deployment scenarios. In each case, the system generates physically meaningful experimental plan, adapts to local hardware constraints, and preserves experimental intent across different instruments. These results demonstrate a practical and scalable approach for integrating AI into synchrotron experimentation, enabling intent-driven, portable, and safe beamline operation.
The advent of fourth-generation synchrotron radiation sources has enabled advanced coherent X-ray techniques. However, high-flux pink-beam operation introduces significant computational challenges for wave-optics-based coherence analysis. Conventional approaches, such as Monte Carlo sampling of the electron beam or direct diagonalization of the cross-spectral density, become computationally prohibitive when extended to broadband spectra. In this work, we develop an integrated computational framework that combines Monte Carlo brightness convolution for efficient wavefront matrix construction, hierarchical incremental singular value decomposition to overcome memory bottlenecks in coherent mode decomposition, and spectral-spatial decomposition to extract a global orthogonal basis for rapid broadband propagation. The reliability of the proposed method is validated through comparison with Synchrotron Radiation Workshop (SRW) simulations and experimental measurements performed at the HEPS Hard X-ray Coherent Scattering (HXCS) beamline. Furthermore, the framework is applied to analyze chromatic aberrations in compound refractive lens focusing systems, quantitatively evaluating focal-spot broadening and coherence degradation inherent to pink-beam operation. The proposed framework provides a practical and scalable tool for the design and optimization of high-flux pink-beam coherent experiments at modern synchrotron facilities.
The tender X-ray (2.0-4.0 keV) region provides access to the K-edges of light- and mid-Z elements that are central to catalysis, energy materials and soft condensed matter, but direct single-shot spectral diagnostics in this range are technically challenging. Ruled gratings typically offer limited resolving power, while scattering-based approaches suffer from low efficiency in an on-line geometry. We demonstrate that a bent-crystal spectrometer on the SwissFEL Aramis beamline can be adapted to provide indirect single-shot spectral diagnostics for tender X-ray operation by measuring the natural third harmonic of 2.1 and 2.5 keV self-amplified spontaneous emission pulses at 6.3 and 7.5 keV, respectively. The scaled third-harmonic spectra reproduce the bandwidth obtained from independent monochromator scans of the fundamental, yielding a relative bandwidth of ΔE/E ≃ 3.1‰ at 2.5 keV. An autocorrelation analysis of 2400 shots gives an upper limit on the instrumental resolution better than 6 × 10-5 at 7.5 keV. The two-dimensional spectral images further reveal the transverse-mode structure and provide sensitive real-time feedback for optimizing free-electron laser performance in the tender X-ray regime.
Here, we review the capabilities of beamline I16 at Diamond Light Source after nearly 20 years of operation and continuous development. I16 is an X-ray scattering beamline operating in the 2.46-16 keV energy range with energy scans with a resolution of 1 meV. The beamline is equipped with a six-circle kappa diffractometer, offering flexible experimental geometries and support for a variety of ancillary equipment. Available equipment includes cryostats and cryofurnaces that span temperatures from 4.2 K to 700 K, which can be combined with applied electric fields, permanent magnets up to 1 T, and uniaxial strain cells. A range of detectors is mounted on the diffractometer arm, including a photon-counting area detector and an avalanche photodiode, both compatible with crystal analyzers for polarization analysis. Diamond single-crystal phase retarders provide full control of the incident X-ray polarization. These capabilities establish I16 as a state-of-the-art instrument for resonant and non-resonant X-ray scattering, multi Bragg coherent diffraction imaging, and grazing-incidence small- and wide-angle X-ray scattering. Together, they allow for studies of complex electronic, magnetic and structural phenomena in single crystals and thin films. We also outline the software infrastructure supporting experiment planning, data acquisition and rapid on-the-fly data analysis, and discuss ongoing developments and the anticipated benefits of the upgrade to a fourth-generation source.
Preventing collisions during automated sample exchange is critical for synchrotron beamlines, particularly for complex cryogenic in-vacuum endstations where recovery from hardware damage may take days. GoniOwl , a compact convolutional neural network (CNN) model, classifies sample-pin presence on the goniometer from a live camera feed on the long-wavelength macromolecular crystallography beamline I23 at Diamond Light Source. Trained on over 8700 manually verified images spanning two years of routine operation and augmented for robustness to illumination changes, camera shifts and occlusions, the model achieves >99% accuracy with millisecond-level inference. A confidence-gating mechanism routes uncertain predictions to a fail-safe path requiring operator confirmation, ensuring suitability for machine-protection control. Integrated via Experimental Physics and Industrial Control System ( EPICS ) process variables, GoniOwl runs in real time within the automated sample-change sequence. In shadow-mode deployment, the CNN matched or exceeded both the legacy histogram method and operator confirmations, which each achieved 96% accuracy. A closed-loop disagreement-audit workflow automatically collects divergent cases for targeted retraining and verification. The approach is readily transferable to other beamline environments where camera-based vision systems can provide an additional software machine protection layer.
X-ray spectrometers with high count rate capability are becoming essential to provide higher speeds in synchrotron measurements, like in X-ray fluorescence mapping (XFM). Monolithic multichannel silicon drift detectors (SDDs) enable the creation of dense and high-performance matrices to reach this goal. In this paper we show the results of the development of ASCANIO, a 16-channel backscattering X-ray spectrometer based on SDD monolithic modules. The solid angle and count-rate uniformity in X-ray detection have been optimized thanks to a `tilted' configuration of the SDD units. ASCANIO underwent preliminary testing in the laboratory, where the system achieved around -42°C with an internal pressure of 5.1 × 10-6 mbar. During further verification of its spectroscopic performance, the spectrometer showed resolutions as low as 134 eV FWHM at the Mn Kα peak. After preliminary testing the full system was commissioned on beamline P06 at PETRA III (DESY). Here the effects of the tilted configuration could be observed, and the system achieved a 20 Mcps cumulative output count rate with a dead time of 20%. As a demonstration of ASCANIO's usability, an example use case is demonstrated, where ASCANIO was used for an XFM analysis of a biological sample.
Diamond is extremely well suited for synchrotron X-ray refractive optics. The effectiveness of diamond refractive lenses, fabricated by pulsed laser ablation, is demonstrated here for the focusing, collimation, and expansion of high-energy, undulator-source X-ray beams in the 40-70 keV photon energy range. The design of the lens elements and their mounting scheme allow the convenient feature of stacking both one-dimensionally and two-dimensionally focusing elements together in a self-aligning manner within the same holder for astigmatic manipulation, when needed. The CuCrZr alloy frames embedding the diamonds are suitable for thermal management, while possessing hardness. Collimating lenses, placed following a high-heat-load monochromator, are employed to increase the throughput of a subsequent narrow-angular-acceptance high-energy-resolution monochromator, after which the X-rays are focused to deliver a beam to coherent diffraction experiments on a long beamline. Also motivated and proposed is the concept of a convex beam-expander, which might seem counterintuitive given that it has higher attenuation on-axis. However, for high-energy X-rays from a low-emittance source on a long beamline, convex diamond beam-expanders could be practical. A proof-of-principle test result of this idea is presented.
The first water-cooling nano multilayer Kirkpatrick-Baez mirror system in the Structural Dynamics beamline (ID23) at High Energy Photon Source (HEPS) has been implemented. An Invar gantry is engineered to achieve a balance between light weight and stability. The cooling system, including eutectic gallium-indium (eGaIn), copper braids and a cooling water circuit with a multi-bend copper pipe in a compact space, decouples movement and mitigates vibration. The mirror cooling holders introduce less than 0.5 nm RMS height error and 0.1 µrad RMS slope error in the mirror surface shapes. A series of stability tests is applied to verify the mechanism structure. In a 1 h test assessment using a water-cooling flow of 4.5 L min-1, the system demonstrated a positional stability of 5.96 nm and an angular stability of 86.76 nrad from 1 Hz to 500 Hz. The focal spot size of 13.39 nm × 15.15 nm (H × V) at a photon energy of 21.8 keV demonstrates the system's performance.
Reliable monitoring of the incident X-ray beam intensity and position is essential in soft X-ray microspectroscopy, where beam instabilities directly affect data normalization and achievable spatial resolution. Conventional beam diagnostics are often implemented using offline detectors located far from the sample or by measuring downstream on empty regions of the sample support membrane, not fully reflecting the experimental conditions experienced during measurements. In this work, the development of functionalized soft X-ray optical elements based on monolithic silicon carbide (SiC) diode detectors, enabling real-time in situ beam diagnostics directly within a scanning transmission X-ray microscopy (STXM) setup, is presented. Two complementary device geometries are investigated: order-sorting aperture (OSA)-based detectors and center-stop-based detectors. The devices are fabricated using plasma-focused-ion-beam milling and substrate thinning, allowing the integration of optical and sensing functionalities with minimal changes to the beamline and endstation setup. The performance of the functionalized optics is experimentally validated at the PolLux STXM beamline of the Swiss Light Source. The devices provide simultaneous access to the transverse beam position and the incident beam intensity I0 through the unfocused 0th-order component. Using this component, the OSA detector enabled simultaneous measurements of the intensity and transverse displacement of the beam from the focused beam illuminating the sample. Between 700 and 1000 eV, the SiC measured current exhibited linear correlation to the avalanche photodiode (APD) signal, with coefficient of determination R2 = 0.997. Position-sensitive detection was possible with a four-sector diode, where all sectors were electrically continuous and beam responsive, while gaps between the quadrants were insensitive. These results demonstrate the feasibility of SiC-based functionalized X-ray optics as beam diagnostic tools for soft X-ray microscopy and spectroscopy.
Experiment proposals at synchrotron facilities serve as the primary gateway for instrument access. They currently lack the standardized and granular topic metadata necessary for tasks such as classification and review, and, broadly speaking, reuse. This paper defines and tests the feasibility of a real-time topic classification service for experiment proposals using an open-source machine-learning model and domain experts for the evaluation phase. We applied the OpenAlex topic classification model to 5384 experiment proposals and selected 209 of them to each be independently evaluated by three domain experts to assess the performance and utility of the model. Analysis of the evaluations reveals a general consensus among the reviewers regarding the model's predictions, with a Krippendorff's alpha of 0.572. We also find that 74.2% of the proposals had at least one topic that was unanimously deemed relevant, which suggests that the model performs well enough to be used in a live setting with real-time verification. However, we do not recommend using it in automated environments without human oversight, given the proposal-based precision score of 56.0%. By aligning the data infrastructure of photon and neutron facilities with the OpenAlex ecosystem, we also lay the groundwork for the eventual inclusion of proposals and experiment reports into OpenAlex, which is necessary for a complete record of a research activity.
Commissioning of a synchrotron hard X-ray nanoprobe beamline traditionally requires months of iterative alignment after hardware installation, during which operational knowledge accumulates but remains inaccessible to non-specialist users. To address this, we present a browser-based virtual commissioning platform for the Korea Light Source ID10 Hard X-ray Nanoprobe beamline (first light 2029) that allows beamline scientists to design, test and refine alignment procedures, scan plans and experimental workflows years before the first photon arrives. Specifically, the platform integrates a Monte Carlo ray-tracing engine, a standard Experimental Physics and Industrial Control System ( EPICS )/ Bluesky control stack, and a multilingual natural-language interface within a single deployable package, which we name HANBIT (Hybrid Agent-driven Natural-language Beamline Interactive Toolkit). Users can interactively explore parameter trade-offs, such as the effect of the secondary source aperture on beam size versus photon flux. The Monte Carlo engine reproduces the overall Shadow4 beam-profile shape and is validated against SPECTRA undulator spectra, source size and divergence. The natural language processing (NLP) agent achieves 98.2% automated action-identification accuracy across 228 test cases in Korean, English and Japanese, whereas expert review of the same responses yields an acceptance rate of 67.3%. We identify this 30.9 percentage-point gap as a central finding: automated accuracy does not guarantee operational acceptability, and closing it is the key challenge for deployment-grade natural-language beamline control. We further validate the zero-change hardware transition strategy that the beamline pursues on three real hardware subsystems, confirming that at the validated device layers the control code and scan plans operate unchanged on the real devices; the integration of the remaining parts, such as high-rate area detectors, which awaits the detector hardware, is also discussed.
The study of the mechanical behaviour of carbonate rocks has benefited from the evolution of experimental tools, due to their complex multi-scale microstructure. Triaxial cells transparent to X-rays have emerged and allowed in situ investigation of progressive failure developments and their link with microstructure. We conducted a series of 4D X-ray computed tomography mechanical tests on porous Saint-Maximin limestone at the PSICHE beamline of Synchrotron SOLEIL. Tests were performed using an in-house-developed triaxial press, Modulo. Volumes were scanned using a helical acquisition and reconstructed at 2.83 µm. They were then analysed using digital volume correlation. Volumetric strain and shear strain magnitude maps were computed using a 100 voxels gauge length with Paraview. Additionally, we computed porosity maps based on mean grey levels, at the same gauge length. Analysis of total and normalized incremental strain maps was carried out. We also compared volumetric strain maps with the initial porosity maps. Each step of the procedure is described herein. The errors on strain and porosity are discussed.
The reaction kinetics and structure of alkali-activated binders are known to be affected by their calcium (Ca) contents. However, the intrinsic difference between high Ca and low Ca alkali-activated systems, especially at the atomic scale, has not been fully investigated. Here, we compare local atomic ordering and reaction kinetics of blast furnace slag and metakaolin as representatives of high and low Ca systems, respectively. In situ X-ray pair distribution function (PDF) analysis and isothermal calorimetry were utilized in parallel to investigate the evolution of local structure in these systems. Isothermal calorimetry results showed contrasting reaction kinetics of high Ca (alkali-activated slag) and low Ca (alkali-activated metakaolin) systems, where the latter shows no induction period. The evolution of specific PDF peaks is related to the main binder gels in each respective system and can be used to track their reaction kinetics, exhibiting excellent correlation with the cumulative heat data (R2 > 0.97). Finally, and most importantly, the PDF results revealed that the atomic ordering of N-A-S-(H) gel is limited up to ∼10 Å, whereas C-(N)-A-S-H gel grew up to ∼40 Å, which suggests that there is an intrinsic difference in the formation mechanism and local structures of dominant gels formed in high and low Ca systems.
The development of fourth-generation synchrotrons, including the Diamond-II upgrade, promises 10-100× flux increases, reaching up to 1012 photons s-1 mm-2 at the detector, across a broad range of energies from 20 to 100 keV. To exploit fully these impressive photon fluxes and high X-ray energies, readout chips must achieve high frame rates and dynamic ranges, while the use of high-Z sensor materials is essential. To address these challenges, the UK's Science and Technology Facilities Council has developed DynamiX, a test structure for a novel two-stage charge cancellation circuit on a 65 nm CMOS process with a dynamic range from single photon(s) per pixel per frame to >9000 photons per pixel per frame (1011-1012 photons s-1 mm-2) at 20 keV photon energy. The application-specific integrated circuit has 16 ×16 pixels on 110 µm pitch and is hybridized with 2 mm thick Redlen high-flux cadmium zinc telluride (HF-CdZnTe). Data are read out at 534000 frames per second over a 14 Gbps serialiser and frames are assembled and saved with a custom data acquisition system. Measurements were made on the Diamond Light Source (DLS) B16 Test Beamline using monochromatic X-ray beams of different sizes and energies to evaluate the detector performance. A sub-pixel beam of size ∼60 µm × ∼15 µm was used to probe pixels to measure single photons with a noise performance of σ = 5.7 ± 0.1 keV. These single photons are used to calibrate the test pulse and pixel cancellation packet sizes. The linearity of the detector response under increasing flux was measured from <1 photon per pixel per frame to ∼109 photons s-1 mm-2 at 20 keV with an r.m.s. linearity of 6.2%. A polychromatic X-ray set was used to reach higher fluxes of ∼3 × 1010 photons s-1 mm-2 (20 keV equivalent), yielding an r.m.s. linearity of 3.2%. Finally, the full sensor area was used to image a rotating slitted disc at 534000 frames per second.
A metrology method dedicated to position monitoring and correction for the ptychography setup at the High Energy Photon Source (HEPS, Beijing, China) beamline ID09 is proposed. The sophisticated design of the Invar interferometer metrology frame ensures optimal performance within the compact environment between the focal spot and the sample setup. The measurement method and error analysis are described in detail. The sample setup achieves a positional stability of less than 2 nm RMS from 1 Hz to 500 Hz. The 12.3 nm reconstruction resolution of 2D ptychography at 12.4 keV demonstrates that the interferometer metrology strategy is available.
The diagnostics and laser infrastructure of the Soft X-ray Port (SXP) at the European X-ray Free Electron Laser are presented. Designed as a supplementary open port, SXP aims to enhance the research capabilities alongside the existing baseline instruments at the SASE3 soft X-ray undulator exploiting the high repetition rate operation enabled by superconducting acceleration cavities. These instruments already support studies in atomic, molecular and non-linear optics (SQS), as well as condensed matter physics (SCS). The inception of SXP is largely motivated by the community involved in time-resolved X-ray photoelectron spectroscopy (tr-XPES), focusing on material science dynamics at surfaces and interfaces. The dedicated endstation equipped with a time-of-flight momentum microscope allows for simultaneous recording of energy- and angle-resolved photoelectron distributions in a pump-probe setting, employing two synchronized femtosecond laser systems meant to cover a broad spectrum from the infrared to the extreme ultraviolet region. The alignment laser system, pump-probe laser transport, including the in-coupling optics, and the installed photon arrival-time monitor are described. Under the present operating conditions, however, the photon arrival-time monitor does not yet provide routine single-shot timing corrections, so the currently demonstrated temporal benchmark is obtained in situ at the tr-XPES endstation. Measurements on a patterned Au reference sample show that the laser spot sizes can be characterized directly and that sidebands yield an X-ray/optical cross-correlation of about 58 fs (FWHM). These measurements define the spatial and temporal instrument response currently achieved for pump-probe experiments at SXP.
Grazing-incidence (GI) scattering techniques are widely used to characterize thin films, offering high surface sensitivity and insight into morphology and structure. However, these approaches typically provide statistical averaged information due to elongated footprint or limited spatial resolution due to beam size. Here we introduce a method that combines structured illumination with GI X-ray scattering and leverages our computational imaging approach to resolve local structural details. We demonstrate that our method captures local features of an organic semiconductor thin film without the need for sample rotation as in tomography. The method expands GI techniques from statistical averaging to high-resolution imaging, thereby providing the capability for detailed analysis of local material properties, such as domain shape, orientation and polymorphism, which are critical for advancing material design towards more efficient and tailored materials.
Not fully grasping the concepts of relativity can lead to misunderstandings about the fundamental background of synchrotron emission. Here we deal with some intriguing cases, in which the relevant `speed of light' is not the invariant c but the speed with respect to a moving object. This specifically affects two pillars of synchrotron radiation: the Lorentz length contraction and the Doppler shift. We propose a teaching strategy relying on new versions of simple `thought' experiments. Besides putting synchrotron radiation on solid foundations, the approach amazingly leads to a unique link-described by Einstein as `remarkable'-between special relativity and quantum mechanics.
Metal fuels such as iron are promising carbon-free energy carriers for a sustainable energy system, where energy release occurs via combustion in metal flames. Apart from the design of the appropriate burners, another challenge is to control the oxidation process and gain direct insight into the kinetics and the mechanism of metal oxidation in flames. Optimizing the combustion process to release the stored energy is crucial, but in situ analysis of metal flames remains a real chemical engineering and physical chemistry challenge. Here, we demonstrate an in situ approach with synchrotron X-ray radiation allowing identification and quantification of iron (oxide) phases during the combustion process that is adaptable for various combustion modes and conditions. Using quick scanning X-ray absorption spectroscopy, we were able to track the oxidation state of iron and thus the structure along the visual flame cross-section. Strong gradients in oxidation state and phase composition across and beyond the flame front were found. The flame front determined by visualization with an optical camera corresponds to the formation of FeO, while the main combustion product Fe3O4 was mainly formed outside the visible flame zone.
Wavefront characterization is essential for diagnosing, interpreting and mitigating performance limitations at X-ray free-electron lasers (XFELs). However, the dramatic increase in thermal load and data throughput at high repetition rates makes established wavefront characterization methods difficult to implement effectively. Here, we demonstrate that X-ray speckle arising from beamline optics can enable fast, robust and sensor-free wavefront metrology at next-generation XFEL facilities. Combining this approach with a statistical formulation of X-ray speckle tracking, we quantify local wavefront fluctuations within pulse trains at the European XFEL. We find that shot-to-shot wavefront fluctuations are predominantly planar phase tilts with distinct statistical signatures across intra- and inter-train timescales. The dominant source of wavefront error is periodic at frequencies consistent with known mechanical oscillation modes of the photon transport optics, while intra-train fluctuations correlate with instabilities in the electron bunch trajectory. Our results establish a practical framework for high-repetition-rate wavefront characterization and diagnostics at next-generation XFELs.
