Green cement: Electric heating to contribute to climate neutrality

Green cement: Electric heating to contribute to climate neutrality

HZDR researchers involved in research project on decarbonization of the cement industry

The cement industry is one of the largest producers of carbon dioxide. It is responsible for up to eight percent of global man-made emissions – almost three times as much as the global air traffic. To reduce this share and become climate-neutral, the industry is relying on technological innovations. The international project “ECem”, in which scientists from the Helmholtz Zentrum Dresden-Rossendorf (HZDR) are also involved, is pursuing a promising approach. With the help of electric heating technologies for the energy-intensive process of calcination, the partners from science and industry want to drastically reduce CO2 emissions in cement production. The project started in the fall of 2024 and will run for three and a half years. It is funded by the Innovation Fund Denmark with 21 million Danish crowns (about 2.8 million euros).

Calcination is one of the most important process steps in the production of cement. Limestone is heated to approximately 1450°C in a large furnace and converted into clinker, the main component of cement, by thermal decomposition. This chemical process is responsible for a large proportion of the CO2 emissions released by the cement industry as a whole. Two-thirds of the CO2 is produced during the decomposition of the limestone, a process known as decarbonization, and is therefore unavoidable. The remaining third is due to the enormous energy consumption required to reach the high temperatures. Fossil fuels such as coal or gas are usually used for this purpose.

The „ECem“ (Electric calciner technologies for cement plants of the future) research project is now taking on this industrial heating process. The goal is to develop a more climate-friendly alternative. To this end, the project partners, led by the Danish cement company FLSmidth, including the Danish Institute of Technology, the University of Aalborg, the companies European Energy and Cementos Argos, as well as the HZDR, want to develop two different electric heating technologies.

Metal balls give limestone the necessary material properties

While the Danish partners in the project are working on the development of an infrared radiant heating system, scientists at the HZDR Institute for Fluid Dynamics are researching an electrical solution based on inductive heating. The team first wants to set up a laboratory experiment in which induction coils generate a high-frequency field to heat the material in a container. In a later stage, a rotating kiln will be modeled in a further experimental setup with key data that closely approximates industrial conditions. The challenge is that materials such as limestone, which consists mainly of calcium carbonate, are actually unsuitable for induction heating due to their poor electrical conductivity.

To overcome this obstacle, the team wants to mix so-called susceptors into the raw material to be heated. These are components designed to efficiently convert the electric energy into heat and transfer it to the material. An important task is to find the right material that can function robustly as a susceptor at high temperatures and under harsh industrial conditions. Possible candidates must have a high melting point, must not react with the limestone and should be abrasion-resistant. Forming the susceptors into a shape, for example as metal balls, would have the advantage of combining the calcination and grinding processes into a single step. Investments in the electrification of industrial processes could, in addition to avoiding CO2, have further positive effects such as increasing efficiency or improving product quality, thus giving the respective companies a competitive advantage in the global markets. 

Read more on HZDR website

Image: Functional diagram of the inductive heating of a rotary kiln reactor in cement production: so-called susceptors are added to compensate for the poor electrical conductivity of the raw material. These components, shaped as metal balls in the picture, efficiently convert the energy transferred by induction into heat and distribute it evenly throughout the vessel.

Source: HZDR / B.Schröder

Young Scientist Award for Patrick Heighway

Young Scientist Award for Patrick Heighway

“Patrick Heighway deserves the prestigious prize for his pivotal role in measuring X-ray diffraction at extreme pressures and temperatures at the HED-HiBEF Instrument”, says Emma McBride from Queen’s University, Belfast and chairperson of the User Organization Executive Committee (UOEC).

His work combines experimental data with molecular dynamics simulations to provide critical insight into the nature of release pathways of shock compressed materials, kinematics of plasticity, and the fundamental interaction of grains in compressed polycrystalline materials. This work is important for many different fields, including geophysics, fundamental material science, shock and plasma physics, the search for novel materials, and understanding pathways to fusion energy.

The European XFEL Young Scientist Award recognises young researchers who are at the beginning of their career but are already making outstanding contributions to research at the European XFEL.

The winner will receive a monetary award of 2,000 Euro and was invited to give a talk as part of the plenary session of the European XFEL User Meeting on 21 January 2025 in Hamburg.

For the first time, the European XFEL User Organization Executive Committee awards as well prizes to posters presented this year at the European XFEL Users’ Meeting about exciting research performed with radiation from European XFEL. Poster prizes were awarded to Daniele Ronchetti (CFEL), Calum Prestwood and Carolina Camarda (both European XFEL).

Their topics were “Elastic scattering enhancement via transient resonances” (Ronchetti), “Tracking atomic populations and transitions in x-ray heated mid-Z transition metals” (Prestwood), and “Electronic properties of Ferropericlase (Mg,Fe)O obtained from dynamic compression experiments using DiPOLE100-X at European XFEL” (Camarda).

Read more on European XFEL website

Simultaneous experiment unlocks new collaborative research potential utilising a joint AI platform

Simultaneous experiment unlocks new collaborative research potential utilising a joint AI platform

Diamond Light Source’s I22 beamline and the ISIS Neutron and Muon Source’s Larmor instrument demonstrate the potential afforded using a cutting-edge technique.

In a groundbreaking experiment, a robotic sample preparation platform, driven by artificial intelligence (AI) was used to undertake simultaneous experiments at both Diamond Light Source, the UK’s National Synchrotron, and the ISIS Neutron and Muon Source, the UK’s National Neutron and Muon Source. While collaborative research between these two science facilities, located on the Harwell campus in South Oxfordshire, is common, this particular experiment has pushed new boundaries with the experiments being performed at the same time on identical robotic set-ups which were in direct communication with each other. 

The simultaneous experiment was driven by two Automated Formulation Laboratories (AFLs), which after a two-year delay with customs, finally made it to the Harwell Campus. They were then installed and operated autonomously on Diamond’s I22 and ISIS’s Larmor small-angle scattering beamlines. The AFLs were produced by research teams from The National Institute of Standards and Technology (NIST), based in Gaithersburg, Maryland, USA, shipped to the Rutherford Appleton Laboratory and then installed at Diamond and ISIS. 

Dr Gregory Smith, from ISIS, said:

We have discussed using the autonomous formulation laboratory for experiments at ISIS for many years, and it was only recently that we considered the idea of running neutron and X-ray measurements in parallel at ISIS and Diamond. Getting one piece of bespoke equipment on site to run an experiment is challenging enough, but it took great effort from many staff here at RAL, from support staff to scientists to engineers, to manage this. I was pleased to finally manage to get the AFLs here and use them as intended, and the exciting results produced by the NIST team justified all this work, resulting in a truly unique experiment.

The experiment investigated paint formulations, making use of small angle scattering to determine properties of the system. The AFL machines, one red and one blue, were linked together across computer networks and worked concurrently, capturing multiple modalities of the formulations synthesised. 

The project had two objectives; the researchers from NIST were testing the AI and robotic elements of the machines, whilst also working on an industrially relevant question – in this case “what is the optimal formulation of a given paint system?”. 

By using both small angle X-ray scattering (SAXS) at the I22 beamline and small angle neutron scattering (SANS) at Larmor, the experiment proved more effective in both the utilisation of beamtime as well as the quality of data collection. SAXS data can be collected more quickly than SANS data, which allowed the experimental team to rule out formulations that weren’t of interest. This allowed a more complete dataset from the significant formulations in a shorter amount of time, as the team could gather insights from the different parts of the system with each technique. Diamond and ISIS offered the unique opportunity for both formulation labs to work in unison at the neutron and X-ray facilities, a situation that is currently only possible in two locations in the world.

Tim Snow, principal software scientist working on Diamond’s I22 beamline, said: 

It is a really good example of both facilities working together to exploit our unique capabilities, acquiring the best data for our users.

The robotic element of the AFL prepares liquid mixtures via pipetting and transfers those mixtures to a measurement cell. Following a SANS or SAXS experiment, the data is analysed by an AI software algorithm. The AI algorithm looks at the collected data to work out what mixture to make next and subsequently what scan to conduct next.  

Read more on Diamond website

Image: The red Automated Formulation Laboratory (AFL) in place on Diamond’s I22 beamline.

Understanding the Role of Manganese in Fuel Production Catalysts

Understanding the Role of Manganese in Fuel Production Catalysts

SCIENTIFIC ACHIEVEMENT

Using specialized equipment at the Advanced Light Source (ALS), including a custom-built reaction cell, researchers uncovered the role of manganese in cobalt manganese oxide catalysts used for fuel production.

SIGNIFICANCE AND IMPACT

This work opens the door to improved catalyst designs that could decrease the production of harmful methane byproducts in a common petrochemical process. 

Sustainable fuel production

First developed in the 1920s, the Fischer-Tropsch synthesis remains a common chemical process used to convert carbon monoxide and hydrogen from coal into liquid hydrocarbons, or fuel. Cobalt is an efficient catalyst for this reaction, and its combination with manganese has been known for decades to further improve the process by promoting the preferential production of long-chain hydrocarbons over methane, a contributor to climate change. However, the molecular scale origin for why manganese improves the efficiency of this reaction remains unclear.

In this work, researchers uncovered the role of manganese in cobalt-manganese-oxide systems by combining well-defined model catalysts with advanced x-ray spectroscopy techniques. These results provide a platform for how customized equipment can answer challenging scientific questions and set the stage for new catalyst designs that may further decrease the production of methane during Fischer-Tropsch synthesis.

Custom-built instrumentation

Numerous studies have investigated the mechanisms for catalytic performance in cobalt-manganese-oxide systems, proposing particular interfaces, mixed oxides, or nanostructures as reasons for the improved efficiency. However, due to the heterogeneity of widely used powder catalysts, resulting in separated domains of cobalt and manganese, the molecular-scale mechanism of these catalysts remains under debate. To circumvent this, the researchers created model catalysts of well-defined cobalt-manganese-oxide nanocrystals and films where the components were intermixed at the sub-nanometer scale.

The model catalysts were investigated using ambient-pressure x-ray photoelectron spectroscopy (APXPS) at Beamline 9.3.2, which is equipped with commercial instrumentation uniquely designed for ambient-condition experiments that mimic real reaction conditions (this instrumentation was previously developed by the researchers, is now available at Beamline 9.0.2 and Beamline 11.0.2, and induced the application of APXPS at other synchrotron facilities). Similarly, to achieve realistic reaction conditions for x-ray absorption spectroscopy (XAS), a custom-built reaction cell was designed for Beamline 8.0.1, allowing experiments that typically occur under high vacuum to be performed under ambient pressure. The challenging and iterative process of perfecting this reaction cell was key to the success of this study, and the reaction cell is now available to other ALS users.

The magic of manganese

Using the custom-built reaction cell for XAS, the researchers were able to observe the real-time breakdown of carbon monoxide during the introduction of hydrogen to the cobalt-manganese-oxide catalyst at ambient conditions. Next, APXPS showed a significant increase in CHx hydrocarbon species after the addition of carbon monoxide and hydrogen on the cobalt-manganese-oxide catalyst surface–which was in stark contrast to the systems without manganese, where the production of cobalt carbide was more dominant instead. In other words, these results demonstrated that the addition of manganese creates more CHx, which ultimately allows for the production of more long-chain hydrocarbons.

The ALS data was complemented by computational density functional theory (DFT) calculations. DFT demonstrated that manganese helps with the production of long-chain hydrocarbons because manganese oxide binds with hydrogen, making it unavailable for reacting with CHx to stop propagation, resulting in less methane and more long-chain hydrocarbons. Moving forward, this work paves the way for improved catalyst designs that can make these reactions even more efficient.

Read more on ALS website

Developing new drugs to battle resurgence of malaria

Developing new drugs to battle resurgence of malaria

With a warming climate comes the threat of expanding habitats for mosquitos that carry malaria, but researchers are using sophisticated synchrotron techniques in the quest for new treatments for the deadly disease.

While most cases of Malaria occur in sub-Saharan Africa, Central and South America, and Southeast Asia, “mosquito areas are spreading,” explained Dr. Oluwatoyin Asojo, adjunct professor of biochemistry and cell biology at The Geisel School of Medicine at Dartmouth College in Lebanon, New Hampshire. Warmer temperatures are helping the mosquitos return to breeding grounds “in places where we haven’t seen it (malaria) since the early part of the 20th century,” like North America and parts of Europe.

According to the World Health Organization’s most recent World Malaria Report, there were 262 million cases of the disease worldwide in 2023 and 597,000 deaths. Almost all the deaths occurred in Africa.

Given the risk of new malaria spread and growing drug resistance to conventional quinine-based therapeutics, new options are needed “so we’ll have an arsenal of tools ready,” she said. Asojo is part of an international team of scientists and students using the Canadian Light Source (CLS) at the University of Saskatchewan to study treatments targeting the malaria-causing parasite Plasmodium vivax (P. vivax). The challenge with P. vivax is that it can remain dormant in the human liver for years or even decades, then enter the blood and cause symptoms.

The team recently found a compound (IMP-1088) that binds in the parasite with an enzyme called N-myristoyltransferase or NMT, which also occurs naturally in humans. This binding inhibits all stages thus disrupting P. vivax’s lifecycle.

Read more on CLS website

Tearing down bacterial membranes with new antibiotics

Tearing down bacterial membranes with new antibiotics

Crystallography reveals how an E. coli drug candidate inhibits an essential enzyme

According to the UN Environment Programme, bacteria resistant to existing antibiotics cause approximately one million deaths each year — a toll expected to soar ten times higher by 2050 if researchers don’t develop alternative therapies. Some bacteria, including some strains of the gut pathogen Escherichia coli or the lung pathogen Klebsiella pneumoniae, are resistant to multiple antibiotics, limiting treatment options. These species belong to a category called ‘Gram-negative’ that do not retain a violet ‘Gram’ dye very well when stained and viewed under the microscope. Members of this group possess two bacterial membranes, the outer of which is studded with fatty carbohydrates called lipopolysaccharides (LPS) that play an essential role in reinforcing the membrane’s integrity. Douglas Huseby, a microbiologist at Uppsala University in Sweden, and his colleagues are designing drug candidates that obstruct LPS synthesis. AstraZeneca previously developed a compound called AZ-1 that could inhibit this pathway but found that it underperformed. After screening other molecules with inhibitory potential, Huseby and his team found one with a similar structure to AZ-1. By merging the two molecules into one, the team developed a potent blocker. X-ray crystallography experiments at Diamond’s I04-1 beamline revealed that the new drug inhibits an essential enzyme by binding to part of the active site. After tweaking the molecule to improve its properties, the team repeated their crystallography work to confirm it bound to the same site on the enzyme. Preclinical tests in mice show a single dose of the drug is safe and effective, underscoring the drug’s encouraging potential. 

No antibiotic is invulnerable to bacterial resistance. Regardless of what bacterial components the drugs target, bacteria evolve defences against every class of the drugs. Now more than ever, clinicians need novel antibiotics that target new microbial features, slowing down the emergence of resistant, untreatable superbugs, but new antibiotics have not completed the journey from the lab to the clinic since the 1970s.

During the mid-20th century, scientists turned to nature to discover antibiotics, but that has become untenable today. “Each new antibiotic you find is about ten times harder to find than the previous one,” Huseby said. Today, scientists focus more attention on designing new antibiotics instead.

Attacking bacteria from the outside

The enzymes that synthesize the fatty sugar lipopolysaccharide (LPS) present an alluring, fresh target. LPS is found on the outer surface of Gram-negative bacteria, which have a thin cell wall and two cell membranes. Several Gram-negative bacteria cause severe infections in humans and have evolved resistance to multiple antibiotics. These include Escherichia coli, a common cause of diarrhoea, and Klebsiella pneumoniae, a tough-to-treat superbug behind pneumonia and meningitis.

LPS is essential in Gram-negative bacteria, as it reinforces the structural integrity of Gram-negative bacteria’s outer membrane, as noted in Mechanism of outer membrane destabilization by global reduction of protein content. Owing to its importance, enzymes involved in its synthesis make good targets for drug design. What’s more, humans lack this synthesis pathway, meaning drugs could theoretically kill bacteria without having collateral effects by disrupting human proteins.

LPS anchors to the outer surface of the bacteria using a fatty molecule called lipid A, and the enzyme that synthesizes this anchor, LpxH, is present in 70% of Gram-negative bacteria, so Huseby and his colleagues wanted to design an antibiotic that could inhibit this enzyme. Since this enzyme is conserved in many species, drugs that target it could potentially have broad-spectrum use, much like the cephalosporin drugs used to treat many Gram-negative microbes. (New agents for the treatment of infections with Gram-negative bacteria: restoring the miracle or false dawn?)

Merging medicines

AstraZeneca already developed a drug candidate that inhibits LpxH called AZ1; however, the compound was only effective in bacteria if the researchers turned off their efflux pumps — portals on the surface that jettison antibiotics (Novel Antibacterial Targets and Compounds Revealed by a High-Throughput Cell Wall Reporter Assay). “It’s not uncommon that you aren’t able to overcome the efflux problem,” Huseby said.

The team decided to search for compounds with inhibitory potential. After screening multiple hits, they landed on a molecule called JEDI-852. This candidate caught their attention because some bacteria in their screen evolved resistance to it by mutating their LpxH gene, suggesting this compound targets the enzyme.

Unexpectedly, JEDI-852 and AZ1 showed striking similarities. By observing the molecules side by side, Huseby’s team noticed that they share a common core. They decided to synthesize a merged version, with unique functional groups from AZ1 at one end and ones from JEDI-852 at the other. Their newly fashioned molecule, which they called JEDI-1444, proved superior at inhibiting LpxH than AZ1. It even worked in bacteria with functioning efflux pumps, suggesting it is potent enough to kill bacteria even if they expel some of the drug from the cell.

Read more on Diamond website

Image: X-ray crystallography experiments at Diamond’s I04-1 beamline revealed that the new drug, JEDI-1444, binds to the LPS-synthesizing enzyme in the same place as substrates, suggesting it may interfere with the active site. Image credit: Douglas Huseby; adapted from the PNAS publication in accordance with CC-BY 4.0 license.

Nanoislands on silicon with switchable topological textures

Nanoislands on silicon with switchable topological textures

Nanostructures with specific electromagnetic patterns promise applications in nanoelectronics and future information technologies. However, it is very challenging to control those patterns. Now, a team at HZB examined a specific class of nanoislands on silicon with interesting chiral, swirling polar textures, which can be stabilised and even reversibly switched by an external electric field.

Ferroelectrics at the nanoscale exhibit a wealth of polar and sometimes swirling (chiral) electromagnetic textures that not only represent fascinating physics, but also promise applications in future nanoelectronics. For example, ultra-high-density data storage or extremely energy-efficient field-effect transistors. However, a sticking point has been the stability of these topological textures and how they can be controlled and steered by an external electrical or optical stimulus.

New perspectives:

A team led by Prof. Catherine Dubourdieu (HZB and FU Berlin) has now published a paper in Nature Communications that opens up new perspectives. Together with partners from the CEMES-CNRS in Toulouse, the University of Picardie in Amiens and the Jozef Stefan Institute in Ljubljana, they have thoroughly investigated a particularly interesting class of nanoislands on silicon and explored their suitability for electrical manipulation.

Nanoislands on silicon

“We have produced BaTiO3 nanostructures that form tiny islands on a silicon substrate,” explains Dubourdieu. The nano-islands are trapezoidal in shape, with dimensions of 30–60 nm (on top), and have stable polarisation domains. “By fine tuning the first step of the silicon wafer passivation, we could induce the nucleation of these nanoislands,” says Dong-Jik Kim, a scientist in Dubourdieu’s team.

Read more on HZB website

Image: Artistic representation of the center down-convergent polarization field. It results from the compression of the polarization flux by the sidewalls of the nanoislands. The texture in each nanoisland resembles a swirling vortex of liquid flowing into a narrowing funnel.

Credit: Laura Canil /HZB

High-Power Laser Facility probes iron at the Earth’s core conditions

High-Power Laser Facility probes iron at the Earth’s core conditions

probe

Scientists have captured unprecedented detail of how iron behaves under extreme conditions approaching those of the core – advancing our understanding of planetary dynamics. Published in Physical Review Letters, these are the first experimental results from the new High-Power Laser Facility (HPLF) at the ESRF.

At the heart of our planet, Earth’s core comprises two distinct sections: a molten outer core that begins around 2,900 km beneath our feet, and a solid inner core starting around 5,150 km. Iron accounts for roughly 85% of the core by weight, combining with nickel and lighter elements to form alloys.

But uncertainties remain over the melting point of iron and its alloys under the extreme pressures of deep Earth. Debates also persist over how iron’s crystal structure may change with depth, which influences its physical and chemical properties at larger scales.

Shocked to the core

Fresh insights into these questions are revealed in new experimental work by Sofia Balugani, PhD student at the ESRF within the InnovaXN programme, in collaboration with the Ecole Polytechnique (LULI Laboratory, France), the First Light Fusion company (UK), and the HPLF team. The researchers “shocked” a tiny iron target (3.5 μm-thick) by firing it with a laser pulse, reaching a pressure of 240 GPa. By coupling the laser with X-rays, they recorded a bulk temperature measurement of 5,340K, the first of its kind for iron’s melting plateau under such extreme conditions. A melting point of 6200K was extrapolated for the even higher pressures of the inner core boundary (ICB).

“After three years of PhD research, this work fulfills my long-standing interest in planets, allowing me to study materials crucial to planets and their properties under extreme conditions, such as those on Earth,” says Balugani.

The research helps refine models of the Earth’s core’s behaviour. That’s because HPLF is optimised for this type of X-ray absorption experiment, which enabled the team to simultaneously track temperature alongside changes in the local order of iron. The findings rule out a transition in iron’s lattice structure to a high-temperature bcc (body-centred cubic) phase, which is observed in some other metals under shock compression such as copper and gold.

Instead, iron remains in the denser hcp (hexagonal close-packed) phase. The results may interest astrophysicists searching for exoplanets, given the importance of the core in generating a geomagnetic field and driving plate tectonics – both of which are key to supporting habitable conditions on Earth.

Read more on ESRF website

Image: The High-Power Laser Facility at the ESRF.

Credit: S. Candé.

Diamond celebrates 14,000th paper – A breakthrough in lithium-ion battery research

Diamond celebrates 14,000th paper – A breakthrough in lithium-ion battery research

A new understanding of the role oxygen plays could revolutionise battery development

Diamond Light Source stands as one of the leading research facilities globally, driving scientific advancements. The 14,000th paper published as a result of innovative experiments undertaken at the UK’s national synchrotron highlights the profound impact science can have in addressing the world’s most urgent challenges. A team of researchers from WMG at the University of Warwick, in collaboration with academic partners in the Faraday Institution’s Degradation and FutureCat projects, has conducted a ground-breaking study that bridges the gap between academic models and real-world battery performance.

Their work, recently published in Joule, used a trio of synchrotron techniques – Resonant Inelastic soft X-ray Scattering (RIXS), hard and soft X-ray absorption spectroscopy (XAS) – to investigate the charge compensation mechanism of lithium-ion (Li-ion) battery cathodes during high-voltage operation. This study demonstrates that oxygen plays a significant role through a metal-ligand redox process, emphasising the importance of focusing on surface passivation strategies to mitigate oxygen reactivity with electrolytes, reducing degradation and enhancing safety. By using pilot-line fabricated pouch cells, this work aligns fundamental research with commercial applications and offers crucial insights to improve energy density and cycling stability.

Challenges and Opportunities for High-Energy-Density Batteries

The global transition to a low-carbon future requires the development of low-cost, reliable and long-range electric vehicles, with Li-ion batteries playing a crucial role. However, traditional models of the electronic charge compensation mechanism in layered metal oxide cathodes are insufficient for developing next-generation batteries with increased energy density through high-voltage operation.

Prof Louis Piper explained:

When we talk about trying to increase the energy density of a battery, what that means is being able to remove as many electrons as possible, In a lithium-ion battery, Li-ions move between the anode and a cathode, releasing an equal number of electrons as current. In a commercial layered metal oxide battery, we can pull out about two-thirds of the accessible lithium ions, and therefore, two-thirds of the available electrons. That means the battery is always below its theoretical capacity, but it’s engineered that way to prevent the degradation that occurs when you pull more out. Replacing cobalt with nickel increases the practical capacity of the battery, but it pushes it closer to the point where you see accelerated degradation. Traditional models attribute charge compensation solely to transition metal oxidation, but if that’s true then why does replacing cobalt with nickel change things, and why do we have more problems with safety and oxygen loss as we increase the energy density? We need a better understanding of the metal-ligand redox process to develop safe, stable, higher performance Li-ion cells.

Innovating Battery Research with Real-World Testing

WMG is home to a Battery Scale-Up pilot facility, a suite of cell production equipment covering the full production process cell assembly and testing. It allows researchers to manufacture battery cells in a variety of different formats.

Read more on Diamond website

Image: Graphical abstract of the publication

Metastable marvel: X-rays illuminate an exotic material transformation

Metastable marvel: X-rays illuminate an exotic material transformation

A flash of light traps this material in an excited state indefinitely, and new experiments reveal how it happens.

A dry material makes a great fire starter, and a soft material lends itself to a sweater. Batteries require materials that can store lots of energy, and microchips need components that can turn the flow of electricity on and off.

Each material’s properties are a result of what’s happening internally. The structure of a material’s atomic scaffolding can take many forms and is often a complex combination of competing patterns. This atomic and electronic landscape determines how a material will interact with the rest of the world, including other materials, electric and magnetic fields, and light.

Scientists at the U.S. Department of Energy’s (DOE) Argonne National Laboratory, as part of a multi-institutional team of universities and national laboratories, are investigating a material with a highly unusual structure — one that changes dramatically when exposed to an ultrafast pulse of light from a laser.

“Together, these complementary facilities are accelerating our understanding of metastable state creation.” — Argonne Physicist Haidan Wen

After the pulse, the material is caught in an exotic state outside of equilibrium, or stability. Called metastable, these states are an exciting and largely unexplored phenomenon in materials science, and they could find application in information storage and processing. 

The team of scientists created the metastable state in 2019 and characterized the material before and after its transition. Using a combination of advanced X-ray and ultrafast laser capabilities, their recent experiments reveal the evolution of the material’s structure during the transition. The researchers captured the entire process in detail across several orders of magnitude in time, ranging from the picosecond to microsecond scales (trillionths to millionths of a second).

In particular, the team is investigating metastability in a class of materials called ferroelectrics, which play an important role in sensing and memory applications. Understanding these transitions in ferroelectrics could eventually inform the design of materials for next-generation microelectronics.

Metastable states

“Most of the materials used in technology are in equilibrium — or their lowest energy state — so that a technology can work reliably without wild variations in performance,” said Venkatraman Gopalan, professor at Pennsylvania State University and an author on the study. ​“However, this is very restrictive, since amazing properties may lurk just beyond equilibrium.”

The challenge is that nonequilibrium states are generally short-lived. Metastable states, however, are nonequilibrium states that persist for a very long time. Diamond, for example, is a metastable state of carbon. We say they’re forever, but over the course of billions of years, diamonds decay into graphite, a more stable state of carbon. 

“It’s sort of like throwing a ball up a cliff, and instead of it returning to the ground, the ball gets stuck on a ledge on the cliff wall,” Gopalan said. If the pathway to the ground is blocked by the ledge, the ball will rest there in a metastable state.

The scientists created the starting phase in this experiment by combining alternating layers of two materials — a ferroelectric and a nonferroelectric. The configurations of the electrons within the different layers compete with each other, resulting in a swirling pattern of vortices in the electronic structure across the material. This internal frustration blocks pathways that the material might otherwise take to return to equilibrium after being excited by the laser pulse.

Read more on Argonne website

Image: Illustration of the material’s transition, with time represented from left to right. A laser pulse (left) sends the material into disorder (middle). Out of this so-called soup phase emerges a highly ordered phase called a supercrystal (right).

Credit: Argonne National Laboratory

A Close Look at a Copper-Titanium Catalyst Under CO2 Hydrogenation

A Close Look at a Copper-Titanium Catalyst Under CO2 Hydrogenation

A major facet of transitioning from fossil fuels to green and renewable energy solutions involves the removal, capture and storage of carbon dioxide (CO2) from the environment. One method is by CO2 hydrogenation, which requires a catalyst to spur the reaction, frequently including metal-oxide catalysts in which metal-support interactions (MSIs) play an important role. 

Researchers from the U.S. Department of Energy’s (DOE) Brookhaven National Laboratory, Stony Brook University, DOE’s Argonne National Laboratory and several other institutions used a suite of in situ techniques to study the behavior and structural and chemical properties of a Cu@TiOx core@shell catalyst under CO2 hydrogenation. Their work was published in ACS Catalysis.

In a core@shell structure, one type of active system (the core) is encapsulated by a shell of a different material to enhance catalytic performance. These experiments focused on an inverse oxide/metal catalyst configuration using a copper nanowire core with a titanium oxide (titania) shell. Such catalysts have been shown to offer improved stability and activity over the conventional metal/oxide arrangement.

Through the use of an entire range of in situ characterization techniques – including time-resolved experiments with X-ray absorption spectroscopy (XAS), ambient pressure X-ray photoelectron spectroscopy (AP-XPS), environmental transmission electron microscopy (E-TEM), and X-ray diffraction at the 17-BM-B beamline of the Advanced Photon Source, a DOE Office of Science user facility at Argonne – the investigators sought to achieve a comprehensive understanding of the structure and behavior of the Cu@TiOx catalyst under CO2 activation and hydrogenation, a functional picture that cannot be obtained with typical steady state studies.

The dynamic characteristics of this catalyst system became immediately evident even during the standard pretreatment used for CO2 hydrogenation, when the H2 pretreatment at temperatures of above 250 degrees Celsius resulted in cracking of the titania shell and migration of Cu particles from the core to the top of the oxide shell. This, along with other configuration changes, was caused by metal-support interactions. The migrating Cu particles are about 20-40 nm in diameter and are speckled with clusters of TiOx and Cu-Ti-Ox. With this altered structure, the system displayed highly dynamic yet wholly reversible catalytic characteristics that were dependent on temperature and chemical environment.

Read more on Argonne website

Image: E-TEM that match with the XRD results.

Artificial Imagination

Artificial Imagination

A Brookhaven Lab researcher has conceptualized an “exocortex,” an extension of the human brain that will generate inspiration and imagination for scientific discovery

PTON, N.Y. — Artificial intelligence (AI) once seemed like a fantastical construct of science fiction, enabling characters to deploy spacecrafts to neighboring galaxies with a casual command. Humanoid AIs even served as companions to otherwise lonely characters. Now, in the very real 21st century, AI is becoming part of everyday life, with tools like chatbots available and useful for everyday tasks like answering questions, improving writing, and solving mathematical equations.

AI does, however, have the potential to revolutionize scientific research — in ways that can feel like science fiction but are within reach.

At the U.S. Department of Energy’s (DOE) Brookhaven National Laboratory, scientists are already using AI to automate experiments and discover new materials. They’re even designing an AI scientific companion that communicates in ordinary language and helps conduct experiments. And Kevin Yager, the Electronic Nanomaterials Group leader at the Center for Functional Nanomaterials (CFN), has articulated an overarching vision for the role of AI in scientific research.

It’s called a science exocortex — “exo” meaning outside and “cortex” referencing the information processing layer of the human brain. Rather than simple chatbots and scientific assistants, the conceptualized exocortex will be an extension of a scientist’s brain. Researchers will interact with it through conversation, without the need for any invasive brain-computer interfaces.

“An exocortex, realized through software, would serve as a new source of thinking, inspiration, and imagination,” said Yager, whose vision was recently published in Digital Discovery. “If we design and build the exocortex correctly, our interactions with it will feel like those ‘aha’ moments we sometimes have upon waking from sleep or while otherwise ruminating on a problem. You won’t check in with an exocortex; you’ll experience it.”

Yager describes the exocortex as analogous to the layers of the human brain, which developed through the course of human evolution. Over millions of years, the human brain became the information processing masterpiece it is today by accumulating new layers, each one more sophisticated than the last. The bottom of the brain controls basic survival functions, like breathing. Other, more advanced layers tackle increasingly complicated functions, like emotional regulation and language processing. Most importantly, all facets of the brain work together in harmony to form “the human experience.”

“Technologically, we have the potential now to add another, external layer to the brain — one that connects us to AI,” Yager said. “And just like the specialized regions of the brain that coordinate with each other to give emergence to what we call intelligence, the exocortex will integrate individualized AI capabilities to solve a problem or generate creativity.”

An “app store” of AI agents

Compared to the average chatbot, which is a single AI system, the exocortex would be a collection of dozens of AI agents working together — customized to a researcher’s individual needs.

Each agent would be trained to carry out specific science-related tasks. A scientific literature agent, for example, could sift through published papers to find an optimal protocol for an experiment, while another AI agent collects and analyzes data from a running experiment. Additional agents could launch experiments or simulations, compare findings to previous studies, or even propose ideas for subsequent experiments.

All of the agents’ tasks will happen in concert, simultaneously, and without manual intervention, culminating in new insights delivered to the human researcher.

One design aspect of Yager’s proposed exocortex is that the AI agents will communicate with one another in plain English language. This will enable human scientists to study and audit the chains of decisions that lead to a particular AI outcome, providing much-needed opportunities to assess accuracy and exert engineering control.

Yager says the task of building an exocortex is enormous, and the developmental effort should be shared among scientists worldwide, so individual research groups can leverage their own expertise to design new agents. Ideally, scientists will one day have “an app store” from which they can download AI agents that will enhance the abilities of their own exocortex, similar to how downloading new apps adds functionality to phones. Individual AI “apps” could also be efficiently updated and replaced.

“I expect to see a multiplicative effect,” explained Yager. “As scientists simultaneously improve the individual AIs and the foundational exocortex technology, the capabilities of the exocortex will likely grow much faster than people expect.”

Of course, making the exocortex a reality won’t be easy. While scientists have designed a plethora of AIs that can interface with a user and complete specific tasks, building a network of AIs that can interact with each other is an entirely new challenge.  

Yager expects each AI agent to require access to a “catalog” of the other agents and their specialized abilities, so they each can send messages describing the work they’ve done and explaining what they need from other AI agents.

“No one knows how to do this yet,” Yager said. Among the challenges is determining the ideal organization of agents. “Should it be a hierarchy where there is a chief with leaders and employees, like how a company operates? Or should it be more fluid, so the AIs figure out the workflow themselves? There is no obvious answer, and this is an exciting research question about the exocortex design that we are investigating.”

The final output of the exocortex will be a result of some sequence of decisions, planning, execution, verification, and summarization, rather than the simple text that a generative chatbot outputs. This extra iteration, promoted by the communication between AI agents and the exocortex structure, will ultimately improve the output and make the AI even more intelligent.

Read more on BNL website

Revolutionising plastic recycling: a breakthrough in enzyme-based depolymerisation

Revolutionising plastic recycling: a breakthrough in enzyme-based depolymerisation

The accumulation of plastic waste in the environment is an ecological disaster and will require multiple solutions to tackle the problem. Despite recent initiatives to close the plastics loop, only 9% of plastic was recycled in 2019, with the remaining waste either incinerated or accumulating in landfills or natural environments, posing hazards to both living and non-living systems. Bioplastics, derived from renewable sources, have been investigated as green alternatives to conventional fossil-based plastics. However, costly synthetic routes and low recyclability continue to challenge the growth of bioplastics. Poly(lactic acid) (PLA) is the most popular polymer for commercial bioplastics, but its recycling is limited by challenging mechanical recycling and slow biodegradation. A team of researchers from King’s College London has developed a generalisable biocatalysis engineering strategy to enhance the use of enzymes to depolymerise a broad class of plastics, in a publication recently published in Cell Reports Physical Science. This novel approach is 84 times faster than the 12-week-long industrial composting process currently used for recycling bioplastic materials 

The problem with plastic waste

The demand for conventional plastics such as Poly(lactic acid) (PLA) or poly(ethylene terephthalate) (PET) is increasing, with 460 million tons produced in 2019; a 230-fold increase from the 2 million tons produced in 1950. Plastic waste is a significant environmental issue, with millions of tons of plastic ending up in natural environments each year. Traditional recycling methods are often inefficient and unable to produce high-quality reusable materials. Bioplastics, derived from biological sources such as corn starch and sugarcane, are seen as a more sustainable alternative. However, current methods of bioplastic production are costly and compete with food-based agriculture for land use. Furthermore, mechanical recycling methods generate CO2 and are incapable of producing high-quality reusable materials, leading many retailers to revert to using oil and fossil-based materials. As an example, it takes up to 84 days at 60°C in industrial composting to recycle PLA, with very little valorisation possible. 

An innovative solution

In this publication, the team of researchers developed a new protocol to recycle PLA. This method involves different component to help depolymerise the material.  

First, they used ionic liquids to solubilise the plastic. Ionic liquids are salts in a liquid state that have unique properties, such as low volatility and high thermal stability. Ionic liquids have been shown to have the ability to solubilise polymers used in common plastics such as PET and PLA. Secondly, they used a commercially available enzyme, a lipase from Candida antarctica (CaLB) to degrade the plastic.  

As the enzyme may not be stable in ionic liquid, the researchers performed some chemical modifications in three different steps to preserve enzyme activity.

Researchers performed circular dichroism at Diamond Light Source on the B23 beamline to ensure that the secondary structure of the enzyme was intact after the chemical modifications. Measurements realised on B23 also showed that the thermostability of the modified protein was higher in ionic liquid (> 80°C) compared to the unmodified protein in aqueous solution. This parameter is important, as heat is required to help depolymerise plastics. 

Read more on Diamond website

Image: Graphical abstract of the publication

Room-temperature serial crystallography experiments with microsecond pulsed beams

Room-temperature serial crystallography experiments with microsecond pulsed beams

Scientists can now scan thousands of protein crystals at room temperature using X-ray microsecond pulses at the ESRF’s serial crystallography beamline, ID29. This capability is of utmost importance for time-resolved studies and drug discovery research at physiological conditions. The results are published in Communications Chemistry.

Studying macromolecular complexes at room temperature has always been challenging because of X-ray damage to the biological samples. Usually this is mitigated by collecting diffraction data at cryogenic conditions, but under these conditions functional dynamics are hindered.

Serial crystallography can provide an alternative way to collect data at physiological conditions with limited X-ray damage andto visualise functional dynamics that become untrapped. Serial femtosecond crystallography at X-ray free electron lasers (XFELs) allow scientists to decode macromolecular structures by acquiring data of tiny protein crystals at room temperature, outrunning the damage thanks to the extremely short pulses on the femtosecond. The transfer of the same technology to 3rd generation synchrotrons has been often limited to longer exposure time, flux and spatial resolution.

At the ESRF, thanks to the Extremely Brilliant Source, the ID29 beamline today has a flux density of ( > 1014 ph/s/µm2), three times higher than 3rd generation synchrotron sources. With this, scientists can deliver X-rays in very short pulses, on the microsecond time resolution, and at a very high repetition rate for macromolecular structure determination at room temperature.

Combined with a slightly polychromatic beam, this allows to measure complete reflections and ultimately accurate structure factor from thousands of microcrystals, even from low redundant datasets. This combination minimizes the sample consumption down to only a few microliters of crystal slurry, in contrast to larger amounts that are frequently needed for serial experiments, and allows complete data to be collected in the fraction of the time.

“Our beamline is the first in the world at a high energy 4th generation synchrotron which is designed to use the high flux density to study macromolecules at room temperature, with a microsecond time resolution”, explains Daniele de Sanctis, scientist in charge of ID29 together with Shibom Basu, EMBL scientist. “The technique, called serial microsecond crystallography (SµX), allows researchers to use less sample to achieve comprehensive structural detail of proteins under physiological conditions and also to visualise molecular movies in action on this time domain. Our work initiates a new future of time-resolved serial microsecond crystallography experiments at 4th generation storage rings, that will ultimately complement X-ray free electron laser (XFEL) experiments.”

A versatile sample environment

One specificity of serial crystallography is the set-up. How do scientists deliver a slurry of hundreds to thousands of microcrystals to the beam? This is a constantly evolving field and ID29 can accommodate different kinds of sample delivery methods with its flexible setup. The researchers applied the unique beam of ID29 to different sample delivery methods: fixed target (foils and chips) and  three different types of high viscosity extruders demonstrating how structures obtained do not present any evident sign of radiation damage. The data quality obtained allows to unambiguously identify the electron density map of ligated molecules.

Read more on ESRF website

Image: Daniele De Sanctis, scientist in charge of the ESRF, and Shibom Basu, from the EMBL, on the beamline.

Credit: S. Candé.

How Enzymes Make New Products Using Greenhouse Gases

How Enzymes Make New Products Using Greenhouse Gases

Humans have been using enzymes to create new products for thousands of years. First it was wine, then cheese. In this tradition, three years ago, a team of scientists tweaked a lyase (HACL/S) to reverse course. Instead of breaking, the enzyme synthesizes novel chemicals through the addition of carbon atoms. 

Now, using the Advanced Photon Source (APS), a U.S. Department of Energy (DOE) Office of Science user facility at DOE’s Argonne National Laboratory, an international team shows how HACL/S enzymes work on an atomic level. Their findings can serve as the basis for increasing the enzymes’ yield and versatility while drawing down as precursors atmospheric carbon dioxide and methane.

HACL/S enzymes were originally discovered for their role in breaking down fatty acids into formyl-CoA (fCoA) and an aldehyde or ketone in mammalian peroxisomes. Since then, scientists have discovered their ability to condense fCoA with various aldehydes and ketones and have one carbon atom added to them. Given the enzyme’s ability to reverse reaction direction from a lyase to a synthase, combined with an abundance of carbon molecules in the atmosphere, HACL/S is an ideal model for biocatalytic production of a variety of new products.  

However, compared to chemical synthetic reactions, biocatalytic production usually produces low yield. The authors of the current research reasoned that if they could manipulate the specificity of these enzymes to accept different kinds of ketones or aldehydes, they could boost the enzymes’ productivity and efficiency.

In order to do that, they first needed to discover how these enzymes worked.

To begin, the team chose from the list of over 100 newly identified proteins six variants of the enzyme that exhibited high activity with aldehyde compounds of different length and formyl-CoA and had amino acid sequences that were diverse enough to cover the HACL/S subfamily. The team synthesized genes for each of the variants, then expressed them in Escherichia coli bacteria.

After purifying the expressed proteins, some members of the international team characterized the enzymes biochemically. Others produced crystals of five enzymes separately and in complexes with acyl-CoA substrates, ThDP cofactor, and ADP. They X-rayed the crystals, diffracted to 1.70–2.70 Å, at beamlines 19-ID – the Structural Biology Center (SBC) – and 23-ID-B – the National Institute of General Medical Sciences and National Cancer Institute Structural Biology Facility (GM/CA) – of the Advanced Photon Source (APS) at Argonne National Laboratory. 

The crystal structures obtained from the X-ray data revealed what computer-predicted models could not: a flexible loop on the C terminus that locked on the cofactor and kept it bound to the enzyme’s active site. When the substrate was added, the loop closed the active site, stabilizing the cofactor and enabling the transfer of the formate compound to the substrate. 

Read more on Argonne website

ALBA participates in CiSMA project to produce 100% recycled steel

ALBA participates in CiSMA project to produce 100% recycled steel

The European project CiSMA, coordinated by the technology centre Eurecat and with a budget of nearly €4.5 million, is to develop 100 percent recycled steel made from scrap and produced in an electric arc furnace to help cut CO2 footprint, boost circular economy and reduce EU’s dependency to critical raw materials in the automotive, professional laundry equipment and other industries.

The European steel industry is targeting a 50 percent reduction in CO2 emissions by 2030 and carbon neutrality by 2050. Electric arc furnace steel production, which replaces the traditional blast furnace process, “will make possible to produce high-performance steels for mass-market products,” says Jaume Pujante, PhD, CiSMA’s technical coordinator and head of the Metals Processing research line in the Metallic and Ceramic Materials Unit at Eurecat. “This will help to cut down emissions by more than 75 percent and use up to 100 percent scrap loads.”

To do this, the project will “tackle the challenge of producing high-performance steel with electric arc furnaces, a technology which is currently limited by the fact that low-performance scrap materials contain unwanted trace elements which adversely affect steel quality” adds Begoña Casas, PhD, CiSMA project coordinator at Eurecat.

CiSMA will maximize the use of low-quality scrap, separating undesired inclusions with a focus on copper. To validate the project’s developments, two pilot tests will be run to verify that the material and process are compliant to the market and also to demonstrate the technologies developed and quantify the environmental improvements compared to the current product.

One of the pilots will test components from a Volvo Cars vehicle and the other will evaluate components for Electrolux Professional washing machines.

The CiSMA project is additionally to “develop technologies that enable introducing these scrap-based, electric arc furnace steel products into mass-market sheet metal consumer goods”, notes Montse Vilaseca, PhD, director of Eurecat’s Metallic and Ceramic Materials Unit.

Read more on ALBA website