Precise 3D imaging using dark-field X-ray microscopy under a structured illumination

Precise 3D imaging using dark-field X-ray microscopy under a structured illumination

Synchrotron X-ray tomography provides scientists a powerful tool for obtaining three-dimensional, high-resolution images of ordered materials. But successfully performing synchrotron tomography typically involves a complex and tedious process. For instance, the selected sample and its containment vessel must be rotated together in tiny incremental steps under a focused X-ray beam, over a full 360-degree rotation. And during this full rotation an extremely precise alignment between the crystalline lattice and rotational axis must be continuously maintained. Failure to meet this challenging protocol frequently introduces errors that seriously degrade the tomographic images.

In pursuit of a more efficient and reliable approach, a research team recently combined dark-field X-ray microscopy (DFXM) with a technique called structured illumination. This combination allows the sample and sample environment to remain stationary throughout the imaging process, resulting in quicker setup times, faster data collection, and a more robust path to achieving high-quality 3D images. The new imaging technique was performed on a pnictide superconductor at beamline 6-ID-C of the Advanced Photon Source (APS), a U.S. Department of Energy (DOE) Office of Science user facility at DOE’s Argonne National Laboratory.

The experimental results demonstrate the practicality of the less complex, yet still powerful, modified DFXM technique, opening up a new approach for scientists to obtain accurate 3D imaging at sub-micrometer resolutions.

3D imaging generally entails using some sort of rotation or translation. Medical CT scanners, for example, revolve an X-ray beam and detectors around a stationary patient. During each revolution the X-rays image a “slice” of the patient’s interior, and a computer then combines multiple slices to form a three-dimensional body image.

Synchrotron tomography reverses this process by fixing the X-ray beam’s direction, which then scans an incrementally rotating sample. Unfortunately, this arrangement introduces complexities that frequently lead to imaging errors. This is partly due to the sophisticated equipment that rotates with the sample, such as containment vessels for maintaining the sample at high or low temperatures, at extreme pressures, or within high magnetic fields. A servomotor then rotates both the sample and containment vessel, a complicated arrangement that not only requires long setup times but also provides multiple paths for mechanical deviations.

Read more on APS website

Protein pH is key for improving texture in meat alternatives

Protein pH is key for improving texture in meat alternatives

Researchers have found that the pH of proteins significantly influences the texture of plant-based meat, in a multidisciplinary study where the ESRF has taken part. The results are out now in Food Hydrocolloids.

Consumption of meat, especially of red meat, represents a significant share of the global greenhouse emissions, in particular CO2, methane and nitrous oxide. Per kilo, beef generates 99.48 kilograms of carbon dioxide equivalent emissions, according to a Science publication from the University of Oxford.

Consequently, a plant-based diet is starting to take a prominent place in western countries. However, trying to mimic the desired textural properties typical of the hierarchical structure of fibers in animal meat has proven to be a challenge.

Today, manufacturers use high-moisture extrusion (HME) to recreate the right texture from plant proteins, such as soy or pea. During HME, proteins go under hydration, heat and shear, and this causes molecular changes that lead to anisotropic (directionally aligned) structures.

Recently, scientists have focused on alkalinization and acidification of water used during extrusion to control protein structure and texture, a process called protein pH-shifting.

Now a team led by the Wageningen University and in collaboration with food manufacturing company Unilever, TU Delft, the ESRF and ISIS, has investigated how pH-shifting during the HME of a soy protein concentrate affects the material’s structure across different scales, from nanometers to millimeters.

They used a multidisciplinary approach, which included Small Angle X-ray Scattering, carried out at the ESRF, and Small Angle Neutron Scattering at ISIS, to look into the nanoscale properties and magnetic resonance imaging and diffuse reflectance for the macroscale structure. “The multiscale nature of meat alternatives makes it necessary to use different methods, SAXS being one of the critical methods here”, explains John van Duynhoven, professor at Wageningen University,   senior scientist at Unilever and co-corresponding author of the publication.

At the ESRF’s ID02, they analysed how protein nano-aggregates change in size and structure depending on pH conditions during extrusion. They found that depending on pH levels, the aggregates further organize in particulate or fibrillar networks.

Read more on ESRF website

Diamond will host a pioneering AI-driven drug discovery consortium

Diamond will host a pioneering AI-driven drug discovery consortium

Diamond will be the base for OpenBind, an AI-driven drug discovery centre which will make the UK a world-leader in drug innovation and advancement.

With its unparalleled XChem facilities, Diamond will be a global hub for AI-driven drug discovery. This will lead to the prospect of tackling previously untreatable diseases and dramatically reducing the cost of drug discovery and development. The project is backed by up to £8 million of investment from DSIT’s newly established Sovereign AI unit, a key driver in the government’s AI Opportunities Action Plan.

The consortium will close critical data gaps by using new AI models to find potential new drugs and help create better treatments for diseases. It will also help scientists use engineering biology to solve bigger problems, like making enzymes that can break down plastic waste.

The main aim is to create the world’s largest collection of data on how drugs interact with proteins, the building blocks of the body. Using automated chemistry and high-throughput X-ray crystallography, the consortium will generate more than 500,000 protein-ligand structures over a period of five years. This is twenty times greater than anything collected in the last 50 years.

OpenBind will offer a core dataset that will drive progress across scientific and technological areas, including predicting molecular structures, designing new molecules and improving research workflows. It will work in tandem with other new methods in order to reduce trial-and-error experimentation, guide better decision-making, and support more efficient exploration of chemical possibilities.

At Diamond Light Source, a joint venture between the UK government through STFC and the Wellcome Trust, we are proud to be at the forefront of the UK’s ambition to lead the world in AI-driven drug discovery. OpenBind represents an exciting step forward in harnessing our unique capabilities to generate the high-quality data that AI needs to revolutionise healthcare, helping to cement the UK’s position as a global hub for bioscience innovation.

Professor Gianluigi Botton, CEO of Diamond Light Source

The consortium will be led by some of the world’s leading scientific minds including Professor Frank von Delft, principal scientist of the macromolecular crystallography I04-1 beamline and the XChem facility at Diamond, as well as the University of Oxford’s Professor Charlotte Deane and Nobel laureate David Baker, head of the Institute for Protein Design at the University of Washington.

Read more on Diamond website

Image: Professor Frank von Delft, Diamond’s principal scientist of the MX I04-1 beamline and the XChem facility

Hydrophobic thin-film catalysts for enhanced CO₂ conversion

Hydrophobic thin-film catalysts for enhanced CO₂ conversion

In a major step toward sustainable CO₂ conversion, researchers from the University of Antwerp, Ghent University, and the ALBA Synchrotron studied how interfacial properties—especially hydrophobicity—affect electrocatalyst performance in gas diffusion electrodes.

Using advanced atomic layer deposition (ALD), they developed a high-efficiency indium sulfide (In₂S₃) catalyst for CO₂ electroreduction to formate. Published in Advanced Energy Materials, the study achieved promising results for industrial application at high current densities.

The electrochemical reduction of carbon dioxide (eCO₂R) is an emerging field that bridges renewable energy and carbon capture, offering a route to transform CO₂ into value-added chemicals and fuels. One of the most promising products is formate, a versatile molecule with industrial applications ranging from chemicals and pharmaceuticals to hydrogen storage and fuel cells. In this context, achieving high selectivity and efficiency in eCO₂R under industrially relevant conditions is becoming increasingly relevant.

However, despite extensive research, a clear understanding of the fundamental electrochemical properties and performance of eCO₂R remains challenging due to the complexity of their composite layers.

In this study, researchers investigated eCO₂R performance by carefully tailoring the surface wettability of indium sulfide (In₂S₃) thin films. Using both thermal (T-) and plasma-enhanced (PE-) atomic layer deposition (ALD) methods, they fabricated uniform In₂S₃ catalyst layers on gas diffusion electrodes (GDEs). Synchrotron light was then used to characterize the film structures, revealing that precise control over hydrophobicity is a critical parameter for efficient formate production.

The characterization of the In₂S₃ thin films’ composition, morphology, and hydrophobicity involved a combination of techniques, including X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), X-ray fluorescence (XRF), and contact angle measurements. Grazing-incidence wide-angle X-ray scattering (GIWAXS) at the NCD-SWEET beamline of the ALBA Synchrotron enabled the characterization of the films’ crystallographic structure, providing detailed insights into the distinct differences arising from the two ALD methods.

The team found that while T-ALD preserved the hydrophobicity of the gas diffusion electrode substrate, PE-ALD induced hydrophilicity due to differences in crystallinity and surface morphology. This difference in wettability profoundly impacted performance. The hydrophobic T-In₂S₃ thin films facilitated better CO₂ gas access and led to superior reaction rates and reduced hydrogen evolution. Specifically, the T-In₂S₃ catalysts achieved a Faradaic efficiency for formate of 93% at a current density of 1 A cm⁻², benchmarks considered necessary for industrial application. Furthermore, researchers revealed that the higher the hydrophobicity of the thermal ALD films, the more efficient the formate electrosynthesis, suggesting a crucial role for this interfacial property in facilitating efficient CO₂ mass transport.

In conclusion, this study demonstrates how interfacial engineering through atomic layer deposition techniques can improve electrocatalyst performance. By establishing the relationship between hydrophobicity and enhanced CO₂ conversion efficiency, these findings provide a valuable framework for developing next-generation industrial catalysts and integrated processes for formate production.

Read more on ALBA website

Stabilising fleeting quantum states with light

Stabilising fleeting quantum states with light

Quantum materials exhibit remarkable emergent properties when they are excited by external sources. However, these excited states decay rapidly once the excitation is removed, limiting their practical applications. A team of researchers from Harvard University and the Paul Scherrer Institute PSI have now demonstrated an approach to stabilise these fleeting states and probe their quantum behaviour using bright X-ray flashes from the X-ray free electron laser SwissFEL at PSI. The findings are published in the journal Nature Materials.

Some materials exhibit fascinating quantum properties that can lead to transformative technologies, from lossless electronics to high-capacity batteries. However, when these materials are in their natural state, these properties remain hidden, and scientists need to gently ask for them to pop up. One way they can do this is by using ultrashort pulses of light to alter the microscopic structure and electronic interactions in these materials so that these functional properties emerge. But good things do not last forever – these light-induced states are transient, typically persisting only a few picoseconds, making them difficult to harness in practical applications. In rare cases, light-induced states become long-lived. Yet our understanding of these phenomena remains limited, and no general framework exists for designing excited states that last.

A team of scientists from Harvard University together with PSI colleagues overcame this challenge by manipulating the symmetry of electronic states in a copper oxide compound. Using the X-ray free electron laser SwissFEL at PSI, they demonstrated that tailored optical excitation can induce a ‘metastable’ non-equilibrium electronic state persisting for several nanoseconds – about a thousand times longer than they usually last for. 

Steering electrons with light

The compound under study, Sr14Cu24O41 – a so-called cuprate ladder – is nearly one-dimensional. It is composed of two distinct structural units, the ladders and chains, representing the shape in which copper and oxygen atoms organise. This one-dimensional structure offers a simplified platform to understand complex physical phenomena that also show up in higher-dimensional systems. “This material is like our fruit fly. It is the idealised platform that we can use to study general quantum phenomena,” comments experimental condensed matter physicist Matteo Mitrano from Harvard University, who lead the study. 

One way to achieve a long-lived (‘metastable’) non-equilibrium state is to trap it in an energy well from which it does not have enough energy to escape. However, this technique risks inducing structural phase transitions that change the material’s molecular arrangement, and that is something Mitrano and his team wanted to avoid. “We wanted to figure out whether there was another way to lock the material in a non-equilibrium state through purely electronic methods,” explains Mitrano. For that reason, an alternative approach was proposed.

In this compound, the chain units hold a high density of electronic charge, while the ladders are relatively empty. At equilibrium, the symmetry of the electronic states prevents any movement of charges between the two units. A precisely engineered laser pulse breaks this symmetry, allowing charges to quantum tunnel from the chains to the ladders. “It’s like switching on and off a valve,” explains Mitrano. Once the laser excitation is turned off, the tunnel connecting ladders and chains shuts down, cutting off the communication between these two units and trapping the system in a new long-lived state for some time that allows scientists to measure its properties.

Cutting-edge fast X-ray probes

The ultra-bright femtosecond X-ray pulses generated at the SwissFEL allowed the ultrafast electronic processes governing the formation and subsequent stabilisation of the metastable state to be caught in action. Using a technique known as time-resolved Resonant Inelastic X-ray scattering (tr-RIXS) at the SwissFEL Furka endstation, researchers can gain unique insight into magnetic, electric, and orbital excitations – and their evolution over time – revealing properties that often remain hidden to other probes. 

“We can specifically target those atoms that determine the physical properties of the system,” comments Elia Razzoli, group leader of the Furka endstation and responsible for the experimental setup. 

This capability was key to dissecting the light-induced electronic motion that gave rise to the metastable state. “With this technique, we could observe how the electrons moved at their intrinsic ultrafast timescale and hence reveal electronic metastability,” adds Hari Padma, postdoctoral scholar at Harvard and lead author of the paper.

Read more on PSI website

Image: Laser pulses trigger electronic changes in a cuprate ladder, creating long-lived quantum states that persist for about a thousand times longer than usual.

Credit: Brad Baxley/Part to Whole

Uncovering hidden light-matter interactions at the nanoscale

Uncovering hidden light-matter interactions at the nanoscale

Progress in nanoscience increasingly depends on our ability to control light at spatial and temporal scales matching those characteristic of nanostructures. In particular, controlling the polarization of light is essential for investigating materials whose properties depend not only on how much light they absorb, but also on the specific orientation of the electric field. Such polarization-sensitive effects are central to the behavior of magnetic and chiral materials, which are of great interest across condensed matter physics, chemistry, and materials science.

At visible wavelengths, artificial structures with dimensions comparable or smaller than the wavelength of the light can be used to shape its intensity or polarization with nanoscale precision. However, in the extreme ultraviolet (EUV), where the wavelengths are much shorter, no comparable tools exist. To overcome this limitation, an international team led by researchers at the TIMER beamline of the FERMI free-electron laser (FEL) has developed a breakthrough method. By combining their unique instrument with a tailored configuration of the FEL, they created a novel type of transient grating in which it is not the intensity, but the polarization of the light that varies periodically. Imagine this as a series of stripes where the electric field rotates in opposite directions from one stripe to the next, with inter-stripe spacing as small as 43 nanometers. Unlike artificial structures, this grating is not static, but exists for the same time duration of the FEL pulses, enabling the ultrafast dynamics of the material illuminated by the light pulse to be probed.

The researchers then tested how a thin film of a magnetic alloy (CoGd) responds to this polarization-modulated grating, comparing it with the response induced by an intensity-modulated grating. In the case of intensity-modulated gratings, the signal was dominated by thermal effects, such as heat-induced vibrations (Fig. 1a). In contrast, the polarization grating suppressed this thermo-elastic background, revealing an otherwise hidden signal (Fig. 1b). Numerical simulations showed that this signal can be attributed to helicity-dependent magnetic effects, that is, to changes in the magnetization directly induced by the circular polarization of light. This suggests that polarization-modulated gratings can be used to selectively trigger and monitor non-thermal, ultra-fast magnetic dynamics that were previously inaccessible.

By enabling precise control of light polarization on nanometer length and femtosecond time scales, this new methodology opens exciting opportunities for studying a wide range of materials. These include systems with complex magnetic structures, topological phases, or valley-dependent properties — fields of growing interest in materials science. This approach adds a powerful new tool to the expanding field of ultrafast EUV and X-ray spectroscopy and paves the way for investigating fundamental processes in condensed matter physics with unprecedented precision.

Read more on Elettra website

Better batteries for implantable medical devices

Better batteries for implantable medical devices

With electric vehicles, the challenge for battery makers is straightforward: make batteries that can hold more energy, so the vehicles they power can go further on each charge.

However, for companies that make rechargeable batteries for implantable medical devices – think pacemakers, cardiac defibrillators – safety trumps all else. Yes, these batteries need to last, but that lifespan cannot come at the expense of a patient’s health.

For that reason, the batteries currently used in these devices have anodes that operate at a higher voltage than ones in regular lithium-ion batteries. The anode is the component inside a battery that releases lithium ions and electrons when power is being drawn, and that takes up ions and electrons during charging. In most lithium-ion batteries, the anode is made of graphite.

“They’re amazing batteries, but the energy density is pretty small,” says Eric McCalla, an associate professor in McGill University’s Department of Chemistry. “As a result, there are some applications for which they simply don’t hold enough energy.”

McCalla and his team recently made a breakthrough that could change that. In an earlier study, the group demonstrated that adding a small amount of an element called neodymium to the anode resulted in a whopping 20% increase in the battery’s energy density. In this new study, they used the Canadian Light Source at the University of Saskatchewan to explore why such a small amount of the element could yield such a large increase in energy storage.

“What we think is happening is that when you add a small amount of these really big ions it doesn’t just disrupt the atoms around it, it disrupts atoms over a large distance,” says McCalla. The CLS’s HXMA beamline enabled them to see that the element they added disturbed the entire structure of the anode — even at such small amounts.

“They (neodymium ions) do a lot of local damage, which actually turns out to have benefit,” says McCalla. “Locally we damage the structure, but in a way that it opens up some other spots for lithium to go in and out (thereby increasing the battery’s energy density”.

In parallel to the experiments, other researchers on the team used computer modelling to calculate how much easier it is for lithium to move when the neodymium ions are nearby. “That really locked down this mechanism, where we’re able to make new sites where lithium wants to go.”

Being able to do their experiment “in situ” at the HXMA beamline was critical, says McCalla. “We had the battery running while we were running the experiment, so we didn’t have to take the cell apart and scrape the sample out and hope that it was stable in air,” he says. In previous attempts, the researchers found that the material degraded when it was removed from the battery. “Being able to do it in the battery, doing the measurement right on the beamline, that made all the difference.”

In this study, McCalla and his team were focused on increasing the amount of energy a battery can hold without compromising safety. Now they’re shifting their focus to increasing the battery lifespan. They identified some instability related to the electrolyte, which they think could impact its long-term use. “There’s definitely continued work that needs to happen, to make these commercially viable. But already the gains that we’ve made show that the energy (produced by the new type of battery) would enable new or different medical applications.”

Read more on CLS website

Exploring the molecular relationship between glycated proteins and cancer cells

Exploring the molecular relationship between glycated proteins and cancer cells

Sugar molecules in our bodies, derived primarily from food, can spontaneously adhere to various proteins, a process called glycation. Glycation can form dangerous Advanced Glycation End Products (AGEs) that lead to various pathologies like Alzheimer’s disease and diabetes, but it can also disable proteins that help cancer cells proliferate. In the early 2000s, scientists discovered that an enzyme called fructosamine-3-Kinase (FN3K) reverses protein glycation. That has made FN3K a valuable target for drug developers hoping to control when and where glycation occurs. 

The data needed for such work has been lacking. But a new study published in Nature Communications involving high-resolution structures determined from data collected at the Advanced Photon Source (APS), a U.S. Department of Energy (DOE) Office of Science user facility at DOE’s Argonne National Laboratory, reveals how FN3K deglycates a protein. These findings can serve as the basis for structure-based and in silico drug design targeting FN3K.

Glycation normally occurs in the bloodstream, but it can happen quickly and spontaneously wherever sugar levels are high. One place would be a tumor microenvironment, where cancer cells require the energy from sugar to proliferate. 

Proliferation of cancer cells is also aided by a protein called NRF2 (nuclear factor erythroid 2-related factor 2). This transcription factor regulates genes involved in cell growth and survival. It can both suppress and promote tumors, depending on the type of cancer and what stage it’s in. Early on, it’s thought to suppress tumors; later, it’s thought to promote them. 

When NRF2 is glycated, it loses its stability and is rendered ineffective at protecting cancer cells. But NRF2 can regain this detrimental function when the sugar is removed—deglycated—by the enzyme FN3K, according to a 2019 study. This study opened two new ways of thinking about how to limit cancer cell proliferation: targeting NRF2 directly or modulating its activity through FN3K—a back door approach that would prevent the enzyme from deglycating NRF2.

With the 2019 study in mind, the scientists behind the current research set out to explore the therapeutic potential of FN3K. They determined a series of crystal structures of human FN3K (HsFN3K) in its unbound, or apo, form. Some variation of a deglycating enzyme occurs in nearly every form of life; the human form is the only one to feature the amino acid tryptophan near its core catalytic site. 

The scientists also determined crystal structures of HsFN3K bound to an analog of glycated NRF2 and the nucleotide ATP triggering different catalytic states—ATP prior to phosphorylation, ADP following phosphorylation, and AMPPNP, an ATP analog, for comparison. The X-ray diffraction data were collected at the Northeast Collaborative Access Team (NE-CAT) beamline at 24-ID-E of the APS.

With careful scrutiny of such high-resolution structures, the team deciphered what no one had seen before. In the pre-catalytic state, the tryptophan recognized the ATP, then flipped 180 degrees. That caused a conformational change in the sugar moiety on the NRF2 analog that made it receptive to phosphorylation; addition of the phosphate destabilized the sugar half and removed it from the protein. Had the resolution been any lower, scientists would not have perceived and recognized the importance of the tryptophan flip. Analyzing their structures, they found that it did not occur with ADP or AMPPNP; it only happened with ATP. 

What about tryptophan? To investigate its role, the team substituted a different amino acid to see if deglycation would still take place. It didn’t, leading the team to hypothesize that tryptophan may function as an ATP sensor, promoting HsFN3K’s kinase activity, even though it’s not part of the usual kinase classical active site players. But one tryptophan substitution gave the opposite result—changing it to a histidine, present in several versions of this enzyme from other species, made HsFN3K unusually hyperactive.

These findings have broad implications for advancing scientific knowledge and conducting basic research. The scientists hypothesize that in humans, evolution enhanced cellular homeostasis by slowing down HsFN3K’s glycating activity through tryptophan, creating an advantageous baseline level of glycation.

As for basic research, many scientists use a derivative of ATP that doesn’t trigger phosphorylation (AMPPNP) to study how ATP interacts with proteins without bothering with catalytic reaction. Only one atom distinguishes ATP from AMPPNP, but that one atom makes all the difference in the world, according to the authors of this study. They found that AMPPNP sits slightly differently from ATP in HsFN3K, preventing the tryptophan from flipping. While they don’t believe that their findings invalidate studies using AMPPNP, they do believe that in some cases, scientists should be careful how they interpret findings. 

Read more on Argonne website

Image: A representation of the crystal structure of HsFN3K in complex with ATP and the sugar mimic substrate DMF. The typical kinase fold is shown with its N-lobe in blue and C-lobe in green. DMF is positioned next to ATP in the catalytic site, both shown in stick representation. Tryptophan W219, shown with electron density shown as a mesh, is in a flipped conformation induced by the ATP binding (top inset), while in the presence of ADP it does not flip (bottom inset). The sugar (DMF) conformation is also different in the two states, underscoring the precise placement of the molecules involved for a productive reaction and providing important mechanistic insights into glycation by FN3K.

Boosting energy storage: the role of lithium distribution in battery performance

Boosting energy storage: the role of lithium distribution in battery performance

An international research team from several institutions, including the ALBA Synchrotron, has come up with a new way to improve nickel-rich positive electrodes for lithium-ion batteries. Published in Nature Communications, the study sheds light on how lithium positioning impacts the electrochemical stability of the electrodes. The team also identified two optimized nickel-rich materials that open the door to more durable and effective lithium-ion battery systems.

As demand for rechargeable batteries grows, the need for sustainable and cost-effective materials to improve their lifespan and performance becomes increasingly critical. The next-generation lithium-ion batteries are being designed with new cathode active materials for high-performance energy storage that avoid hazardous materials like cobalt. Among the most promising positive electrode candidates are nickel-rich layered oxide materials. However, these materials face significant challenges in long-term stability due to structural degradation. A crucial yet frequently overlooked factor affecting their stability is the precise positioning of lithium atoms within the lattice—a characteristic extremely difficult to determine due to lithium’s weak interaction with standard X-ray methods.

A recent study published in Nature Communications addresses this challenge with advanced characterization techniques, including synchrotron X-ray and neutron diffraction, to analyse and optimize lithium distribution within nickel-rich electrodes. This work was a collaborative effort involving scientists from Shenzhen and Shanxi Universities (China), ICN2, and ICREA (Spain) alongside scientists from the ALBA Synchrotron, the Institute Laue-Langevin (France), the Karlsruhe Institute of Technology (Germany) and the UM6P (Morocco).

By adjusting lithium incorporation and adding multiple high-valence dopants (Nb⁵⁺, W⁶⁺, Mo⁶⁺), researchers identified two electrode materials with better durability and stability. The optimization of the material performance was also achieved by creating superlattice domains, that is ensuring that the distribution of the lithium ions is not random. Small changes in lithium occupancy in nickel-rich positive electrodes can significantly enhance electrochemical performance.  

Researchers examined the internal structure of these electrodes with a variety of techniques and synchrotron facilities. In particular, researchers monitored the real-time structural evolution of the nickel-rich positive electrodes during battery operation using in situ synchrotron X-ray diffraction (SXRD) at the MSPD beamline at ALBA. The high-resolution diffraction patterns provided by this beamline allowed the tracking of lithium positioning as well as of their phase transitions and lattice changes.

“The ability to study electrodes under operating conditions was critical to show how lithium occupancy influences stability and performance, which are both key parameters for the development of more durable Li-ion battery materials”, says Alexander Missyul, beamline scientist at MSPD.

This work identified two optimized electrode materials with important gains in battery cyclability. The first, with a lithium content of 1.08, stabilized the lithium/nickel exchange, and improved mechanical durability. The second, with a lithium content of 1.20, promoted oxygen redox activity, which helped electrode integrity at higher voltages. Both materials demonstrated a capacity retention of over 90% after extended cycling, significantly outperforming conventional nickel-rich electrodes.

Read more on ALBA website

Caught in the frame: the birth of nanostructures

Caught in the frame: the birth of nanostructures

A team led by prof. Magdalena Parlińska-Wojtan from the Institute of Nuclear Physics of the Polish Academy of Sciences conducted advanced research on the process of electrodeposition of metallic nanostructures, using unique microscopic techniques in a liquid environment. International cooperation, including the Silesian University of Technology, the University of Warsaw, the SOLARIS Center, ETH Zurich, and the Fritz Haber Institute in Berlin, resulted in a publication in the prestigious journal Nano Letters.

Modern microscopes and a special electrochemical flow cell allowed scientists from the IFJ PAN to observe the process of creating metal nanoparticles with unprecedented precision. This is a step towards better design of future materials – from fuel cells to advanced sensors. 

Electrodeposition is the process of depositing a metal layer on the surface of an electrode immersed in an electrolyte under the influence of voltage. Although known for a long time, until now it has been difficult to observe its course in detail in real time. Thanks to a special flow cell, in which a microscopic volume is separated by two very thin membranes (and one of them is additionally equipped with electrodes), it became possible to track the formation of a platinum-nickel (PtNi) nanolayer. 

The experiment recorded two mechanisms: direct growth of the PtNi layer on the electrode and the formation of nanoparticles in solution and their deposition on the electrode surface, especially where the electron beam reached. More detailed observations showed that the nanostructures have a spherical shape and a dendritic surface. 
In the next stage of the experiment, carried out in cooperation with the Fritz Haber Institute (Max Planck Gesellschaft), the reaction parameters were modified, which allowed for the recording of nucleation and the growth and dissolution cycles of nanoparticles. Observations showed that the growth rate prevailed over dissolution, thanks to which a durable layer was created. 

Further studies were conducted in the STXM microscope at the SOLARIS center in Krakow. Although the resolution of STXM is lower than TEM, the STXM microscope allows for more precise chemical analysis. It was determined that the PtNi layer consists of metallic platinum and nickel(II) oxide. 

The research opens up new possibilities for controlled synthesis of nanostructures that can be used in energy, electronics and medicine. The recognition of the importance of the work was the inclusion of a graphic from the publication on the cover of the 40th issue of Nano Letters.

Read more on SOLARIS website

Clay emerges as a natural semiconductor

Clay emerges as a natural semiconductor

Vermiculite, a natural occurring clay mineral, can be a 2D wide band-gap semiconductor with unique electronic and magnetic properties, according to a study partially carried out at the ESRF and which is out now in the journal npj 2D Materials and Applications. The work at the ESRF focused on deciphering the structure of vermiculite, ensuring that it retained the features of semiconductors at the atomic level.

Vermiculite has long been used in insulation, construction, and environmental applications (like water purification and CO₂ capture); however, it had never been explored as a material for nanoelectronics or spintronics.

Now a team led by NTNU, in collaboration with the ESRF’s BM01, has successfully found that it can function as a 2D semiconductor. “Quantum technology is often associated with synthetic materials that have been developed in advanced, completely clean environments,” says Professor Jon Otto Fossum from NTNU’s Department of Physics. “We have found a naturally occurring clay material with sought-after properties for use in quantum technology,” he adds.

Scientists looked into exfoliating the material, because it has a layered structure and resembles that of graphite, which is used to make graphene. Until now, no one had explored it as a 2D material since it is very difficult to delaminate.

With help of in-situ diffraction experiments, the researchers established the way to reduce the material to a few atomic layers and discovered that its exfoliated form reveals semiconducting and antiferromagnetic properties. Nanosheets also have a high surface to volume ratio, which makes it interact more with light or electric fields. Due to their size, nanosheets can be integrated into thin films.

Dmitry Chernyshov, scientist in charge of BM01, explains the importance of this single-layered form: “The discovery of an antiferromagnetic ground state of vermiculite was only possible with its exfoliated form; it opens a route towards potential applications that would also require single nanosheets of this layered material”.

600 million tons of vermiculite

The exfoliation procedure was carried out at NTNU and optimized in three consecutive experiments at BM01, where synchrotron X-ray diffraction experiments solved the structural characterization of this clay and helped to establish a technology protocol in-situ to make its functional exfoliated form.

Unlike synthetic semiconductors, vermiculite is widely available, inexpensive and environmentally friendly, with global reserves estimated at 600 million tons. “Because of these features, it could help create sustainable, scalable materials for nanoelectronics and quantum technologies”, concludes Barabara Pacáková, the first author of the paper.

Read more on ESRF website

Symposium celebrates Claudio Pellegrini, pioneer of SLAC’s X-ray laser

Symposium celebrates Claudio Pellegrini, pioneer of SLAC’s X-ray laser

Leading researchers met at SLAC on Pellegrini’s 90th birthday to honor his ongoing scientific legacy and to explore the future of X-ray free-electron laser science.

Ask anyone about Claudio Pellegrini – distinguished professor emeritus of physics at the University of California, Los Angeles, and adjunct professor of photon science at the Department of Energy’s SLAC National Accelerator Laboratory – and they are quick to share their heartfelt admiration. They describe a gentle giant, widely regarded for his influential work and noble character; a charismatic and curious leader who ushered in a whole new way of doing science; a mentor, friend and someone who has become a father or grandfather figure to many in the accelerator and free-electron laser science community.

On May 9, 2025, on Pellegrini’s 90th birthday, SLAC hosted a special symposium to honor his ongoing scientific legacy. 

Among Pellegrini’s many accomplishments, one moment in time stands out. At a workshop on fourth generation light sources in 1992, he proposed to use SLAC’s historic linear accelerator to build an X-ray free-electron laser. That visionary idea became reality in 2009 when SLAC turned on its Linac Coherent Lightsource (LCLS), the world’s first free-electron laser producing “hard,” or very high-energy, X-rays.

Click through the photo carousel to learn more about the development of the LCLS idea, Pellegrini’s contributions, and what his colleagues had to say about his legacy at the May 9 symposium.

When LCLS came online, it was a revolutionary new facility. With its unprecedented flashes of X-ray light that each only last a few millionths of a billionth of a second and are a billion times brighter than those produced by any previous source, researchers could now do science they could only dream of before. For example, LCLS allowed them to take snapshots of atoms and molecules at work and string them together in molecular movies that reveal chemical reactions and other fundamental ultrafast processes in real time in materials, technology and living things.  

While the goal behind Pellegrini’s proposal was clear from the beginning, it was also apparent that turning it into a working machine would be an extraordinary technological challenge. “It didn’t seem to be impossible, but we certainly needed to do our homework,” Pellegrini remembers. “It took a place like SLAC with its technical capabilities and the collective effort of many talented people in many places to make it happen.” 

Since 2009, similar light sources have been developed around the world. Meanwhile, at SLAC, recent and future upgrades to LCLS ensure that its capabilities keep defining and pushing the frontiers of X-ray science and technology.

The symposium was organized by Uwe Bergmann, Martin L. Perl Endowed Professor of ultrafast X-ray science at the University of Wisconsin, Madison, together with LCLS’s Leilani Conradson, Samira Morton and Brandon Tan.

Read more SLAC website

 Turning Non-Magnetic Materials Magnetic with Atomically Thin Films

 Turning Non-Magnetic Materials Magnetic with Atomically Thin Films

The rules about magnetic order may need to be rewritten. Researchers have discovered that chromium selenide (Cr₂Se₃) – traditionally non-magnetic in bulk form – transforms into a magnetic material when reduced to atomically thin layers. This finding contradicts previous theoretical predictions, and opens new possibilities for spintronics applications. This could lead to faster, smaller, and more efficient electronic components for smartphones, data storage, and other essential technologies.

An international research team from Tohoku University, Université de Lorraine (Synchrotron SOLEIL), the National Synchrotron Radiation Research Center (NSRRC), High Energy Accelerator Research Organization, and National Institutes for Quantum Science and Technology successfully grew two-dimensional Cr₂Se₃ thin films on graphene using molecular beam epitaxy. By systematically reducing the thickness from three layers to one layer and analyzing them with high-brightness synchrotron X-rays, the team made a surprising discovery. This finding challenges conventional theoretical predictions that two-dimensional materials cannot maintain magnetic order.

“When we first observed the ferromagnetic behavior in these ultra-thin films, we were genuinely shocked,” explains Professor Takafumi Sato (WPI-AIMR, Tohoku University), the lead researcher. “Conventional theory told us this shouldn’t happen. What’s even more fascinating is that the thinner we made the films, the stronger the magnetic properties became—completely contrary to what we expected.”

While three-dimensional Cr₂Se₃ crystals exhibit antiferromagnetism (where magnetic moments cancel each other out), the two-dimensional versions transform into ferromagnetic materials. Even more remarkably, the ferromagnetic transition temperature increases as the films become thinner.

Through micro-ARPES analysis of electronic states, researchers identified the mechanism behind this phenomenon: conduction electrons injected from the graphene substrate across the interface into Cr₂Se₃ are the decisive factor enabling high-temperature ferromagnetism in these ultra-thin films.

Read more on KEK website

Image: In 1966, Mermin and Wagner theoretically predicted that while ferromagnetic order can be stabilized in three-dimensional systems, it cannot be sustained in two-dimensional isotropic systems due to thermal fluctuations (left: 3D, right: 2D).

Credit: Takafumi Sato et al.

Catching “Hydrogen Spillover” onto a Catalytic Surface

Catching “Hydrogen Spillover” onto a Catalytic Surface

Researchers uncovered the precise mechanism of hydrogen spillover (H2 splitting and migration) onto a catalytic surface by watching it happen under various conditions at the Advanced Light Source (ALS).

The research lays the foundation for designing more efficient catalysts and storage materials essential for next-generation hydrogen energy technologies.

Hydrogen on the move

The splitting and migration of molecular hydrogen (H2) over a catalytic surface (a process known as “hydrogen spillover”) is a fundamental yet elusive phenomenon in catalysis that affects a wide range of uses, from hydrogenation (which can be used to upgrade or purify crude oil components) to energy storage (when bonded to a metal, hydrogen can be stored in the solid state). Despite its importance, direct experimental evidence capturing the real-time mechanistic steps of hydrogen spillover remains scarce.

In particular, tungsten oxide (WO3), a widely used catalytic material, exhibits dynamic interactions with hydrogen, yet the precise nature of these interactions has been a subject of long-standing debate, especially for distinguishing the chemical dynamics occurring on the surface from those in the bulk.

This research was driven by the need to resolve these ambiguities using ambient-pressure x-ray photoelectron spectroscopy (APXPS), which provides direct spectroscopic evidence of the spillover process as it unfolds. By integrating experimental observations with theoretical models, the researchers unlocked a comprehensive understanding of how hydrogen interacts with reducible oxide surfaces and influences their catalytic properties.

Operando APXPS at the ALS

This study focused on WO3 thin films “decorated” with Pt metal clusters that facilitate hydrogen activation and dissociation. To directly visualize the stepwise evolution of hydrogen spillover on WO3, the researchers employed APXPS at ALS Beamline 9.3.2, a technique pioneered at the ALS and uniquely suited for studying solid–gas interfaces in real time under realistic (“operando”) reaction conditions.

APXPS detected the oxidation states of tungsten and the presence of surface hydrogen species as the samples were exposed over time to hydrogen gas at various temperatures. The tunable incident photon energy allowed selective analysis of different elements (including differentiating between various hydrogen species—molecular, protonic, or hydride-like) at variable depths, enabling the researchers to track hydrogen-induced changes with high precision. The ability to collect real-time spectra while exposing the sample to hydrogen enabled the detection of intermediates that would be difficult to observe with other methods.

Furthermore, by combining the APXPS experimental observations with first-principles-based microkinetic modeling and simulations, the researchers gained a comprehensive understanding of the reaction mechanisms underlying hydrogen spillover.

Read more on ALS website

Image: Artistic depiction of a tungsten trioxide (WO3) surface (purple/red) “decorated” with a platinum nanocluster (metallic gray). Green arrows trace the evolution of hydrogen (white) from gas form (H2) to dissociation into H+ on the platinum, to spillover (migration) onto the WO3 surface, and, at elevated temperatures, desorption as water vapor (H2O) and diffusion into the bulk.

The great planetary reset: Mapping glass pearls

The great planetary reset: Mapping glass pearls

Their days were numbered, all manner of Cretaceous life in kingdom plantae and animalia. Those that survived the impact winter became our modern groups of terrestrial and aquatic plants, animals, and marine plankton. Scientists want to understand how the Chicxulub asteroid that hit Earth 66 million years ago changed the conditions for life on the planet and veiled the sun for so many years, leading to the extinction of the dinosaurs. Secrets to this understanding are locked in the asteroid’s physical composition. An international research group has now produced a unique elemental map of the spherules formed by the asteroid impact, with data from MAX IV’s Balder and NanoMAX beamlines. The findings may better explain the aerosol cloud formation that catalysed extinction-level climate change.

The Chicxulub asteroid impact in the Gulf of Mexico, known as the Cretaceous–Paleogene (K–Pg) boundary event, marks the epoch demarcation, and the 5th mass extinction in the geological record. The asteroid carved a 200 kilometre-wide, kilometre-deep crater, globally dispersing a clay sediment layer abundant in platinum group elements (PGEs), namely iridium, osmium, and platinum. The ejected molten debris from the vaporized asteroid was preserved in the sediment as glass-like pearls called microspherules.

Major questions have remained about the spherule composition and chemical information, possible carrier elements of the idium in the spherules, and processes that occurred during global distribution after impact. To address these open questions, scientists from Sweden, Colombia, the U.S.A., and United Kingdom investigated spherules from Gorgonilla Island off the west coast of Colombia.

“We were surprised to find such a major heterogeneity, with that I mean that the composition of one spherule from another, is very different, with silica and calcium dominating in some, while others are full of iron. However, the major surprise was finding the elements that we were searching for, the rare iridium,” said Vivi Vajda, Professor of Palaeontology and Head of the Paleobiology department at the Swedish Museum of Natural History. “With the super-high-resolution mapping at NanoMAX, we could see the iridium in the form of tiny shards, in shapes of needles and triangles.”

Structural data collected from the spherules included use of X-ray fluorescence (XRF) microscopy at NanoMAX beamline and X-ray absorption spectroscopy (XAS) and X-ray absorption near edge structure (XANES) at Balder beamline at MAX IV. Results revealed the presence of PGEs and identified metallic carrier elements such as cobalt, nickel, lead and others. “We have been able to resolve a major enigma showing that iridium most likely has been transported in a mineral with copper and zinc, possibly minerals new to science,” explained Vajda.

Read more on MAX IV website

Image: Illustration of Chicxulub asteroid impact in the shallow tropical sea in what´s today the Mexican Gulf. The mixture of target rock, marine plankton, and the asteroid formed a melt that produced droplets which cooled to silica ‘pearls’ enclosing traces of the asteroid.

Credit: Pollyanna von Knorring

Scientists Use AI and X-ray Vision to Gain Insight into Battery Electrolyte

Scientists Use AI and X-ray Vision to Gain Insight into Battery Electrolyte

Artificial intelligence and experimental validation reveal atomic-scale basis for improved ‘water-in-salt’ battery performance

UPTON, N.Y. — A team of scientists from the U.S. Department of Energy’s (DOE) Brookhaven National Laboratory and Stony Brook University (SBU) used artificial intelligence (AI) to help them understand how zinc-ion batteries work — and potentially how to make them more efficient for future energy storage needs. Their study, published in the journal PRX Energy, focused on the water-based electrolyte that shuttles electrically charged zinc ions through the rechargeable battery during charging and use. The AI model tapped into how those charged ions interact with water under varying concentrations of zinc chloride (ZnCl2), a form of salt with high solubility in water.

The AI findings, validated by experiments at Brookhaven Lab’s National Synchrotron Light Source II (NSLS-II), show why high salt concentrations produce the best battery performance.

“AI is an important tool that can facilitate the advancement of science,” said Esther Takeuchi, chair of the Interdisciplinary Science Department (ISD) at Brookhaven Lab and the William and Jane Knapp Chair in Energy and the Environment at SBU. “The research done by this team provides an example of the insights that can be gained by combining experiment and theory enhanced by the use of AI.”

Amy Marschilok, manager of the Energy Storage Division of ISD and a professor of chemistry at SBU, added, “This work could help advance the development of robust zinc-ion batteries for large-scale energy storage. These batteries are particularly attractive for resilient energy applications because the water-based electrolyte is inherently safe and the materials use to make them are abundant and affordable.”

Water in salt

Like all batteries, zinc-ion batteries convert energy from chemical reactions into electrical energy, explained Deyu Lu, a staff scientist in the Theory and Computation Group of Brookhaven Lab’s Center for Functional Nanomaterials (CFN) who led this research.

“However, competing chemical reactions, such as those that split water molecules and produce hydrogen gas, can severely degrade battery performance,” he said. “If any of this energy is used in side reactions, you lose energy that is supposed to do work.”

Lu and his collaborators knew that previous studies had found that water splitting is suppressed in a special zinc chloride electrolyte where the salt concentration is so high it’s referred to as “water-in-salt,” in contrast to more common “salt-in-water” electrolytes. To figure out why the high-salt version was better, they wanted to capture the atomic-scale details of how zinc and chloride ions move and interact with water — and how that affects the electrolyte’s conductivity — at different salt concentrations.

But seeing these atomic-scale details is extremely challenging. So the team turned to a form of computer modeling enhanced by AI vision.

Developing AI vision

“Seeing these complex details would be impossible using conventional computing techniques,” Lu said. “Conventional simulation methods cannot handle the large number of atomic interactions with the desired accuracy to capture the timescales over which such systems evolve. Such calculations require enormous computing power, which would easily take many years.”

So instead of performing all the complex calculations that would be needed to fully simulate the ions’ interactions with water, the team used conventional simulations to generate a small number of simulation data, known as a “training set,” and fed it to an AI program. They used computing resources at the Theory and Computational Facility at CFN, a DOE Office of Science user facility, and Brookhaven Lab’s Scientific Computing and Data Facilities within the Computing and Data Sciences directorate (CDS).

“We needed a little bit of data collected by calculating a small number of interactions to kickstart the process of training an initial model,” said CDS’s Chuntian Cao, first author on the paper. “Then, we ran the model to generate more data to continue to improve the model’s predictions.”

At each step, the scientists ran their results through an ensemble of machine learning (ML) models to assess whether the predictions were accurate. Lu likened the process to calling several friends to help answer questions on “Who Wants to be a Millionaire,” a once-popular TV game show. “If the friends/models all agree, then it looks like you have good chance that you have an accurate prediction,” he noted.

But, as Cao pointed out, “When we find that some predictions have very large deviations in the ensemble of ML models, we return to doing the conventional calculations to get the correct answer. These new corrected data points are then added back to the training data to further refine the ML model.”

This iterative “active learning” process minimized the number of calculations that needed to be run in a computationally expensive way to complete the training of the ML model. And, after several rounds of training, the AI model could make predictions about much larger numbers of atomic interactions over longer and longer timescales.

“Chuntian ran the simulations with several thousands of atoms, a very large system, for hundreds of nanoseconds — an impossible task using the conventional methods. AI/ML is truly a game changer in the study of complex materials,” Lu said.

Stablizing water

The Brookhaven and Stony Brook scientists’ AI model revealed that high zinc chloride concentrations play the key role in stabilizing water molecules, protecting them from splitting.

In pure water, the oxygen atom in one water molecule (H2O) forms two so-called hydrogen bonds with hydrogen atoms in neighboring water molecules. These hydrogen bonds connect the water moleclues in a continuous network that makes the water molecules more reactive and susceptible to splitting, Lu said.

The team found that the number of hydrogen bonds drops rapidly as the zinc chloride concentration increases, disrupting the hydrogen-bond network. In the water-in-salt regime, only about 20% of the hydrogen bonds are left.

“Stabilizing the water molecules is an essential component of why high-concentration water-in-salt electrolytes work so well,” said Cao.

Read more on NSLS-II website

Image: Scientists used AI to model how zinc and chloride ions (gray and green spheres) at different concentrations would interact with and move through water (oxygen and hydrogen represented by red and white spheres) in an aqueous battery electrolyte. The AI-assisted modeling revealed that a high concentration of zinc chloride salt solution stabilizes water in the electrolyte while maintaining sufficiently high conductivity — characteristics that are essential for aqueous zinc-ion battery performance.

Credit: Chuntian Cao / Brookhaven National Laboratory