Bridging the Thickness Gap: Advanced Soft X-ray Imaging Unlocks 3D Magnetic Textures

Magnetic materials underpin our high-tech lifestyles and will play key roles in the production of clean energy and next-generation computing technologies. Studying natural magnetic materials can offer insights into animal behaviour, the role of Earth’s magnetic field over time and the formation of the solar system itself. The behaviour of magnetic materials is governed by their underlying magnetisation configuration, including magnetic domains (local areas of uniform magnetisation) and defects such as domain walls.

With magnetic systems varying from the macroscopic scale down to single atoms, and occurring in everything from natural magnetite through to carefully designed topological chiral magnets, researchers require an array of techniques to study them. Exploring magnetic textures on the order of the magnetic exchange length requires spatial resolutions of tens of nanometres or lower.

However, while using a combination of high spatial resolution soft X-ray imaging and electron microscopy allows the analysis of thin samples (≲300 nm) and surfaces, investigation of thicker samples has been limited to hard X-ray dichroic imaging, limiting 3D studies to thin films for most materials, including transition metal magnets.

In work recently published in Physical Review X, an international team of researchers led by Dr Claire Donnelly of the Max Planck Institute for Chemical Physics of Solids has developed a soft X-ray imaging technique for thicker magnets, closing this “thickness gap”. Their work reveals previously inaccessible 3D magnetic textures, and is an exciting development with a range of applications, including the study of naturally occurring magnetic rocks, transition-metal based permanent magnets for energy harvesting, and chiral magnets for spintronics.

Read more on Diamond website

Image: (a) Schematic of the ptychography setup. (b) Ptychographic phase projections measured with RCP and LCP x rays, with the difference giving the XMCD signal, indicating the projection of the magnetization (anti)parallel to the x-ray beam.

520-million-year-old worm fossil solves mystery of how modern insects, spiders and crabs evolved

X-ray computed tomography (XCT) studies on Diamond’s I13-2 beamline reveal beautiful ancient structures

A new study led by researchers at Durham University, published in Nature, have uncovered an incredibly rare and detailed fossil, named Youti yuanshi, that gives a peek inside one of the earliest ancestors of modern insects, spiders, crabs and centipedes.

This fossil dates back over 520 million years to the Cambrian period, when the major animal groups we know today were first evolving.

This fossil belongs to a group called the euarthropods, which includes modern insects, spiders and crabs. What makes this fossil so special is that the tiny larva, no bigger than a poppy seed, has its internal organs preserved in exceptional quality.

Using advanced scanning techniques of synchrotron X-ray tomography at Diamond Light Source, the UK’s national synchrotron science facility, researchers generated 3D images of miniature brain regions, digestive glands, a primitive circulatory system and even traces of the nerves supplying the larva’s simple legs and eyes.

Read more on Diamond website

Image: Side-on view of Youti yuanshi, showing internal organ systems.

Credit: Emma J. Long

Pushing Boundaries in Piezoceramics: The Impact of Strontium Acceptor Dopants

Conventional PZT piezoceramics – used in everything from spark generators and parking sensors to medical ultrasonics – can’t function at high temperatures, limiting their industrial applications. They’re also lead-based materials, which face legal restrictions due to their toxicity to people and the environment. In light of these issues, there is considerable interest in developing lead-free, high temperature piezoelectric materials. BiFeO3-BaTiO3 (BF-BT) ceramics are promising candidates, and researchers at the University of Manchester have been seeking to understand the mechanisms of how we can process and modify the composition of these materials to improve their properties. In work recently published in the Journal of Materiomics, they investigated the unusual technique of adding strontium as an acceptor dopant. Although the strontium disrupted the microstructure – as expected – the team found that, in small amounts, it still improved the ferroelectric and piezoelectric properties. This work demonstrates that acceptor dopants can be used to tune piezoelectric properties, and that strontium-doped BF-BT ceramics are potential candidates for high temperature lead-free piezoelectric materials.

Developing Lead-Free Piezoceramics for Extreme Condition

Increasing demand for applications in piezoelectric sensors, accelerometers and transducers has created considerable interest in high temperature piezoceramics. Conventional lead-based ceramics have two important limitations. Firstly, their low Curie temperature (TC) means they can only be used at temperatures below 200°C. Secondly, they have strong toxic effects on the environment and human health, and their use is increasingly restricted.

Materials based on bismuth ferrite (BF) combine strong ferro/antiferromagnetism and high spontaneous polarization (>100 mC/cm2) with a high ferroelectric Curie temperature of around 825 °C.

Senior author Dr David Hall, from the University of Manchester, said:

For many years now, we’ve been working with Ionix Advanced Technologies, a spin-out company from the University of Leeds. Ionix uses piezoelectric compositions to generate ultrasound for high temperature applications. It’s very similar to the way ultrasound is used for medical imaging, but in this case, it’s used for inspecting structural components like cooling systems that can operate up to nearly 400 °C. There are similar applications in high temperature processing systems operating at around 580 °C. At the moment, there isn’t a lead-free material that can match that performance.

We’ve been working on a lead-free BiFeO3–BaTiO3 (BF-BT) solid solution. In principle, if you make a piezoelectric device from this compound it would operate up to very high temperatures, and then it could have applications in the real world as a piezoelectric electromechanical transducer material.

Read more on Diamond website

The big switch on: solar panels fully operational at Diamond

Recently installed solar panels that cover the entire roof of Diamond Light Source are now fully operational.  Diamond’s roof covers an area of 32,000m2  which offers an exceptional opportunity to maximise energy efficiency through these panels. 

The energy generated by the solar panels is an annual supply of 2.3GWh/y​. This output amounts to around 5% of the facility’s total annual energy consumption and will mean yearly savings of some half a million pounds. This will additionally contribute to energy savings of more than £2M per year. 

The installation was part of a larger roof maintenance project which presented the opportunity to install a 2.7MW solar panel array.  

Since Diamond’s construction in 2005, the organisation has enhanced the efficiency of existing equipment and limited the amount of equipment needed to run without affecting machine operation. These steps are central to Diamond’s prioritisation of sustainability in all areas of the construction and operation of the facility. Areas of focus have been waste reduction, use of low-carbon electricity supply where possible and the introduction of photovoltaic panels. 

Read more on Diamond website

Students wowed at Oxfordshire’s science event of the year

For the first time in eight years the UK’s world-leading science and innovation campus at Harwell welcomed thousands of school children to explore world-leading science up close.

On Tuesday 25th and Wednesday 26th 2024, Harwell commenced its open week by welcoming over 2,000 students, ranging from primary school to sixth form.

The students had the unique opportunity to go behind the scenes and discover some of the world’s most cutting-edge research through taking part in space-themed escape rooms, hands-on arts and crafts, lectures, and interactive workshops and tours with the UK’s national laboratories operated by the Science and Technology Facilities Council (STFC).

Diamond Light Source hosted tours and workshops, guiding groups around the synchrotron and explaining how the machine functions. Younger children had the opportunity to learn about the synchrotron’s different magnets and made a beaded “magnet” bracelet to take home.  

Across the site, students also met the scientists and technicians who are responsible for the biggest breakthroughs and discoveries on the UK’s behalf that have included in recent years the Nobel prize winning work of recording gravitational waves from the collision of black holes and also the detection of the Higgs boson at the Large Hadron Collider in CERN.

The culmination of the week will be on Saturday June 29th when Harwell opens its doors to the public. The public day is a family-friend event designed for people of all ages and backgrounds.

Read more on Diamond website

International community gathers for Diamond’s Magnetic Materials Group User Meeting

Last week, over 100 scientists from across the international research community attended the first in a series of in person User Meetings taking place in 2024 at Diamond, the UK’s national synchrotron science facility.

The Magnetic Materials Group (MMG) User Meeting, incorporating a Theory of Soft X-ray Spectroscopy Workshop, took place from Monday 3rd – Wednesday 5th June. Delegates heard talks from invited speakers from across Europe who shared their latest research results in areas such as altermagnetism, spin textures, strong correlated systems and functional materials. Diamond scientists presented on the facilities of the MMG, which enable a wide range of polarised X-ray based research into novel materials and phenomena. This included a presentation on one of the Diamond-II upgrade flagship beamlines I17, which will offer Coherent Soft X-ray Imaging and Diffraction (CSXID) and is currently in design phase.

Sarnjeet Dhesi, Diamond’s Science Group Leader for the MMG, says, “It was fantastic to see our user community network and discuss new collaborations that could be enabled by upgrades to our facilities. “

Lightsources.org was one of the event sponsors, along with ELMITEC and BESTEC, and supported the MMG User Meeting by providing the poster prizes. A panel chosen by the organising committee selected the three best posters and Prof. Kevin Edmonds, a Diamond User Committee representative from University of Nottingham, and Silvana Westbury, Project Manager for Lightsources.org, presented the prizes at the end of the meeting.

Winners were:

1st prize 🏅 went to Myron Huzan for their poster on ‘Quantifying the influence of 3d-4s mixing on linearly coordinated metal ions.’

Image: Prof. Kevin Edmonds, a Diamond User Committee representative from University of Nottingham (left), and Silvana Westbury, Project Manager for Lightsources.org (centre), presenting 1st prize to Myron Huzan (right)

Credit: Stefania Mazzorana/Diamond

2nd prize🏅, for their poster on ‘The magnetic order and excitations in GdRu2Si2’, went to George Wood.

3rd prize🏅, for their poster on ‘Strain modulated charge ordered transitions in a highly-correlated electron material’, went to Diego Barlettani.

Diamond’s next User Meeting, which is the Spectroscopy Group User Meeting, takes place this week (registration for this event is now closed). Future User Meetings covering Extreme Conditions as well as Imaging and Microscopy will take place later in the year. Keep an eye on the Diamond and Lightsources.org websites to find out when registration opens for these in person events.  

To learn more about the Magnetic Material Group, visit the Diamond website

Revolutionising research: DIAD delves into dentistry

The innovative design of Diamond’s Dual Imaging and Diffraction (DIAD) beamline provides valuable opportunities for biomedical materials science

Diamond is home to an ever-evolving array of beamlines and instruments, allowing scientists from a wide variety of disciplines to collect high-quality, high-resolution data for their groundbreaking research. In materials science, X-ray imaging and tomography experiments can determine the 3D microstructure of samples, while X-ray diffraction techniques offer the phase composition and stress distribution. Most synchrotron beamlines are designed to offer one or the other, with a few that can do both – but not at the same time. Switching between the modes can be complicated and time consuming. Diamond’s Dual Imaging and Diffraction beamline (DIAD) provides both imaging and diffraction capabilities in one instrument. Its novel dual beam design operates with two independent beams meeting at the sample position, one setup for imaging and one for diffraction. By constantly switching between the two modes, DIAD enables in situ and in operando measurements and time-resolved studies. Understanding the complex structure of tooth enamel, the factors involved in its decay and potential strategies for its remineralisation exemplify some outstanding tasks in biomedical materials science that can benefit from the dual beamline approach. In work recently published in Chemical & Biomedical Imaging, a group of researchers from the University of Oxford and the University of Birmingham (led by Professor Alexander Korsunsky) detail a proof-of-concept study that demonstrated how the unique capabilities of DIAD can be used to consider different options for remineralisation and to grade them in terms of how well they work.

Teeth: nature’s nanostructured marvels

Human teeth are a miracle of biological engineering. Their remarkable strength and resilience come from a combination of hard external enamel over an interior of flexible dentine. On the microscopic scale, enamel is built from nanoscale hydroxyapatite (HAp) crystallites, bundled together into micron-scale rods with surrounding inter-rod regions. Delving deeper into the extraordinary structure of teeth provides valuable insights for the development of strong, bio-inspired materials. However, as we’re all aware, teeth aren’t impervious, and can rot away under the onslaught of an acid-provoking modern diet. Unlike those of some other animals (such as rodents), human teeth don’t regenerate. Once they are damaged, we must face the pain of a “drill and fill” repair, or the fitting of synthetic prosthetic replacements. 

Project lead Prof Alexander Korsunsky, from the University of Oxford, said:

Teeth are a fascinating example of nature’s hierarchical structuring from the nanoscale. Whereas bone and dentine, the inner part of the tooth, remain vascularised and living – meaning constantly renewing, changing, rebuilding, remodelling – enamel is one part of the human body that doesn’t. Nature effectively builds pieces of stone subjected to extreme thermal, chemical and mechanical attack, that can last up to 100 years. In our first major research project we set out to understand the processes involved in dental caries and how they interact with the structure of teeth. Now that another major four-year project has been awarded, we are out to explore what could be done to reverse caries and remineralise enamel.

Read more on Diamond website

Understanding Stainless Steel’s Resistance to Hydrogen Embrittlement

Stainless steel is one of our most versatile materials. Its hygienic qualities ensure the safety of medical instruments and implants, and its corrosion-resistant properties make it indispensable in industries from construction to food processing. The corrosion resistance arises from the alloy’s chromium content, as the chromium forms a passive film on the surface that can self-heal in the presence of oxygen, shielding the bulk of the material from corrosion. However, the stability of the passive film can be affected by hydrogen absorption, leading to microstructure embrittlement that lowers the stress required for cracks to occur and propagate in the metal. A challenge for the hydrogen energy industry is that high-performance metallic materials are highly susceptible to hydrogen embrittlement. One potential candidate for building a safe hydrogen economy infrastructure is super duplex stainless steel (SDSS). 

In work recently published in Applied Surface Science, an international team of researchers used in situ surface-sensitive synchrotron X-ray measurements to investigate the early stages of hydrogen-induced degradation of SDSS occurring at the near surface. Their results show that SDSS’s exceptional resistance to hydrogen embrittlement can be explained by the stability of the passive oxide film, and that the semiconducting property of the passive film plays an important role in hydrogen embrittlement. The authors also conclude that profound in situ experimental characterisation and computational calculation are needed to reveal the complex processes behind material degradation. 

High-Strength, Corrosion-Resistant Steel

Green hydrogen can be used as both a feedstock and energy carrier and has the potential to play a crucial role in the future fossil-free energy landscape. However, high-strength metallic materials are highly susceptible to hydrogen embrittlement (hydrogen-induced material degradation), posing a significant challenge for safe hydrogen storage and transport.

Prof Jinshan Pan, from the KTH Royal Institute of Technology in Sweden, said:

Hydrogen embrittlement is a very important issue for many applications. Different metal materials may have this embrittlement problem. It’s really a hundred-years-old challenge. In many cases, the metal surface has a passive film, like an oxide, that allows materials to be used in practice, because otherwise the metals themselves are active.

Read more on Diamond website

The Mona Lisa of fossils secretly visits Diamond

The feathered limbs, pointed teeth and sharp claws of the oldest known bird-like dinosaurs, the Archaeopteryx, have fascinated naturalists and palaeontologists including Charles Lyell and Charles Darwin who propelled the species to fame especially following publication of his theory of evolution.  

So, when a precious 150-million-year-old Ostromia crassipes fossil – formerly known as a specimen of Archaeopteryx – arrived at Diamond Light Source in a high security operation, it naturally caused a great deal of excitement. The rare fossil, which is usually housed at the renowned Teylers Museum in the Netherlands, was brought to Diamond so scientists and students could discover more about its features, including the colour of its feathers. The specimen was studied on the I18 beamline, using its microfocus X-ray, and this was the first time it had been examined in such detail.

Collection manager at the museum, Tim de Zeeuw, described the fossil as the Mona Lisa of the museum’s collection. The Jurassic fossil is so precious, it was secretly brought to the UK by a special transport team and was kept under lock and key around the clock, even while on the beamline at Diamond.  

The new research will be the subject of a forthcoming paper and is a collaboration between the University of Utrecht and Teylers Museum. Lead author, Edgar Mulder, a master’s student at the university explained that it was a bit of dream come true to get time to examine the fossil at Diamond and the team worked through the night to get as much information as possible.  

The fossil was found in Jachenhausen, a village in southeastern Germany in 1855. When it was discovered, it was thought to be a pterosaur until 1970 when it was identified as an Archaeopteryx.

Professor Dr Anne S. Schulp at the University of Utrecht, said,

In 2017, it was concluded that this sample was more closely related to the Chinese Anchiornis and given the name Ostromia. This new research at Diamond is helping to further determine its features. It is particularly important as the Archaeopteryx and other ‘early birds’ play a key role in the origin of birds.

The Archaeopteryx is called the ‘first true bird’ and is about the same size as a magpie at around 20 inches from head to tail. This Ostromia fossil shows the knee region, part of the wing, claws, ribs, lower stomach bones, and feather imprints. 

Read more on Diamond website

Image: Ostromia reconstruction, previously known as the Haarlem Archaeopteryx specimen 

Credit: Mariolanzas CC BY-SA 4.0 

70 Years in the Making: A Historical Virus Sample Reveals a Novel Protein Structure

The world is full of treasure troves of hoarded scientific samples – everything from pressed plants in herbaria and pinned insects in museum drawers to rocks from the Moon and asteroids in air-tight vaults. Generations of scientists have contributed to collecting, preserving and studying such specimens, amassing an immense amount of knowledge about our natural world and how it changes over time. As we develop ever more powerful technologies to explore them, these historical samples can lead us to new discoveries, as an international team of researchers recently found. Their work, published in Nature Communications, began with a 70-year-old viral sample tracked down in a low temperature freezer. This viral sample was of a Nudivirus that are economically important in agriculture, where they are used as biological agents to control some insect pests. However, they can be pests themselves, damaging large-scale crustacean and insect farming efforts. Using X-ray crystallography, the research team solved the lattice structure of a polyhedrin (occlusion body) from Nudiviridae, which adds to our knowledge of how viruses use protein self-assembly to protect themselves from the environment.  

Two families of insect viruses – the double-stranded DNA Baculoviridae and double-stranded RNA cypoviruses – are known for using protein crystals, called polyhedra, to encase virus particles. The notable feature of the polyhedra is their remarkable resilience, protecting the viruses inside from environmental factors such as temperature, light, and water. When insects consume contaminated foliage, the viral polyhedra dissolve in their digestive tracts to produce a new viral infection. New crystals of viral polyhedra grow inside the infected insects, which when they die contaminate more foliage and spread the virus. The Baculoviridae and cypoviruses evolved polyhedra separately, essentially using different proteins to arrive at the same biological solution.

Although Nudiviridae are related to Baculoviridae, they were originally given the prefix nudi- because they were thought to lack the polyhedrin protein. However, recent research has found that at least one genus of nudiviruses form polyhedra that were not previously recognised.

Dr Jeremy Keown at the University of Oxford said:

We were interested in investigating the structure of these nudivirus polyhedra and so we got in touch with Dr Annie Bézier at the Institut de Recherche sur la Biologie de l’Insecte in Tours, who had done some initial characterisation of these samples. She had frozen samples originally purified in the 1960s. We used the I24 beamline to carry out initial X-ray diffraction experiments, and those results showed us that the crystal lattice structure was different from that found in other viruses.

We were able to make a mutant version of the protein that included methionines and that was crucial to our research. It enabled us to grow the cells in a medium containing selenomethionines – a sort of derivatised version of the protein – and that eventually allowed us to solve the structure.

In October 2019, the team returned to Diamond, this time to the new VMXm beamline.

Dr Keown said:

At this point, we were working with large numbers of very small crystals. We had a lot of help from beamline scientists Dr Adam Crawshaw and Dr Jose Trincao, preparing slurries of microcrystals in cryo-EM grids, which we then vitrified. Crystals this small are rapidly destroyed in the X-ray beam, so we collected small wedges of data from lots and lots of crystals. When the Covid-19 pandemic hit, it meant we couldn’t collect data in person, so I dropped samples off at Diamond, and the beamline staff ran the experiments.

Read more on Diamond website

Image : a) Scanning electron micrograph of native ToNV occlusion bodies prepared for diffraction experiments. Images have been cropped but are otherwise unedited. b) A single polyhedrin molecule coloured from the N-terminus (blue) to the C-terminus (red) and annotated with secondary structure features. A calcium ion is shown (green). The dashed line shows the missing loop 171–174. c) The dimeric unit (red and blue chains) of the OB lattice are shown in two orientations. The two-fold symmetric axis is indicated by the black ellipse.

Leading UK Science facilities announce new five-year collaboration

A new five-year agreement to facilitate collaboration between two leading UK Science institutions has been announced.

Diamond Light Source, the UK’s synchrotron light source and the National Physical Laboratory (NPL) aim to bring the two organisations closer together to allow students to learn about each other’s science portfolio. This agreement will drive a closer collaboration through the formation of a Steering Committee that will help shape curriculum content to meet students’ needs.

Commenting on the signing of the Memorandum of Understanding (MoU), Chief Scientist at NPL, DR JT Janssen;

Our goal is to combine our expertise and facilities to accomplish momentous scientific impact.  We want to develop common specialised knowledge and increase the effective use of our facilities; as well as increasing cooperation and mutual support among our students and staff.

In addition to joint meetings, networking and training, the MoU will facilitate the identification of collaborative research and skills development opportunities of mutual or individual interest through a dedicated Steering Committee with representatives from both organisations.

Prof. Gianluigi Botton, Chief Executive Officer at Diamond Light Source adds;

This agreement is going to create great opportunities for new science and for both organisations’ scientists and students.  A key objective is to facilitate collaboration around student engagement activities, including using our respective expertise to accomplish valuable scientific training for each other’s student cohorts

Read more on Diamond website

Image: From L to R: (Front Row) CEOs Dr Peter Thompson (NPL) and Prof. Gianluigi Botton (Diamond), and (Second Row) Dr Richard Burguete Postgraduate Institute Director (NPL), Dr JT Janssen, Chief Scientist (NPL), Isabelle Boscaro-Clark, Head of Impact, Communications and Engagement (Diamond), Dr Adrian Mancuso, Physical Sciences Director (Diamond), and Prof. Sir Dave Stuart FRS, Life Sciences Director (Diamond)

Fertilisation under the X-ray beam

After the egg has been fertilized by a sperm, the surrounding egg coat tightens, mechanically preventing the entry of additional sperm and the ensuing death of the embryo. A team from the Karolinska Institutet has now gained this new insight through measurements at the X-ray light sources BESSY II, DLS and ESRF. 

Fertilization in mammals begins when a sperm attaches to the egg coat, a filamentous extracellular envelope that sperm must penetrate in order to fuse with the egg. Now an international team of researchers has mapped in detail the structure and function of the protein ZP2, an egg coat filament component that plays a key role in regulating how egg and sperm interact with each other at fertilization.

“It was known that ZP2 is cleaved after the first sperm has entered the egg, and we explain how this event makes the egg coat harder and impermeable to other sperm,” says Luca Jovine, Professor at the Department of Biosciences and Nutrition, Karolinska Institutet, who led the study. “This prevents polyspermy – the fusion of multiple sperm with a single egg – which is a fatal condition for the embryo.”

The changes in the egg coat after fertilization are also crucial to female fertility by ensuring the protection of the developing embryo until this implants in the uterus. The new knowledge may therefore have implications for the development of non-hormonal contraceptives that interfere with the formation of the egg coat. Moreover, the study explains egg coat-associated forms of female infertility. 

“Mutations in the genes encoding egg coat proteins can cause female infertility, and more and more such mutations are being discovered,” explains Luca Jovine. “We hope that our study will contribute to the diagnosis of female infertility and, possibly, the prevention of unwanted pregnancies.”

Read more on HZB website

“Stripy” algae tell us more about possibilities in material design

As we celebrate the 155th anniversary of the periodic table this March, we mark the milestone during British Science Week 2024 by shedding light on the chemical building blocks of an amazing sea creature.  

The light generated by Diamond Light Source is one of the most powerful in the world, able to detail almost all the elements on the periodic table at a molecular level. And a recent discovery about tiny organisms means big news for biogeochemists.  

The ability to see the elemental composition of microorganisms is only possible with the brilliant X-ray light available at synchrotrons like Diamond. When the elements were classified 155 years ago, with creation of the periodic table, it would have been impossible to imagine today’s groundbreaking technology. Being able to pinpoint the location of almost any element means scientists can discover things like the miniscule stripes of calcium and strontium on a sea-dwelling organism.  

And why is this level of detail important? By working at this atomic scale, learning how even the tiniest creature are formed, scientists can translate this knowledge to bigger things, like better medicines, cures for viruses, and advanced engineering possibilities.  

In a paper from the Environmental Science: Processes and Impacts of the Royal Society of Chemistry, users from Diamond Light Source, University of Sheffield and the Institute of Environmental Science and Technology (ICTA) at Universitat Autònoma de Barcelona studied marine algae on our I14 beamline. This study was part of a year in industry student project.  

With the high-resolution X-ray techniques, the scientists have learnt some interesting details about coccolithophores, which is a type of marine plankton.  

These organisms create their own outer shells called coccoliths, which are made up of calcium carbonate (the same material as chalk) as well as some other minor elements like strontium. The researchers created a high-resolution 3D image of the surprisingly stripy chemical makeup of these structures leading to new findings about how they are formed.  

This single-celled algae can be found in the sunlight zone of the ocean. They use chlorophyll to capture the sunlight and use photosynthesis to turn it into energy. This means they consume carbon dioxide and release oxygen.  

Coccolithophores are ecologically important and hugely contribute to the marine biological pump, the mechanism that takes carbon away from the atmosphere and the land, transporting it to the ocean interior and seafloor sediments.  

Read more on Diamond website  

Image : False colour scanning electron micrographs of different coccolithophore species

Exploring Matter at or under Extreme Conditions at Diamond

We’re all familiar with ice – water frozen into its solid state, at or below 0°C at standard atmospheric pressure (1 atm, or 101.325 kPa). But this naturally occurring crystalline solid (officially known as ice Ih or ice one h) is just one of at least nineteen phases of ice, each with a different packing geometry. The less familiar phases (polymorphs) occur at different pressures and temperatures. The ice polymorphs have differing densities, crystalline structures, and proton ordering. These strange phases of ice are just one example of what happens to matter at extremely high pressures.

The physical and chemical properties of a material depend on its structure and the distances between its atoms. Pressure has far more of an effect on interatomic distances than temperature, so varying the pressure is a powerful tool for exploring the relationship between structure and properties. Fundamental insights can be used, for example, to inform the design of new materials or to help explain phenomena such as volcanic eruptions that originate from processes deep in the Earth. 

Further, the electronic structure of a material can be very different under pressure, giving rise to extraordinary effects. An insulator such as ice can become a metal or conductor (e.g. Ice XVII, or Superionic water), and metals can become insulators. E.g. Sodium, a pale grey, shiny metal transforms into a glass-like transparent insulator under pressure. Changing electron configurations at high pressure gives elements a different reactivity and chemistry, almost reinventing the periodic table.

Annette Kleppe, Principal Beamline Scientist on Diamond’s I15 beamline, said;

High-pressure devices are superbly suitable for tuning structural and electronic properties of materials. In fact, pressure can change the electronic properties so dramatically that it adds a whole new dimension to the periodic table. High-pressure, when combined with different experimental analysis techniques, is a powerful tool for understanding natural phenomena or designing novel materials, for example. High-pressure research topics range from low-temperature physics to high-temperature Earth and planetary science.

It’s no wonder researchers want to explore these extreme conditions, and Diamond has several facilities to accommodate them. I15 is our dedicated Extreme Conditions beamline, dedicated to X-ray powder diffraction experiments at extreme pressures and temperatures. Users can also carry out high-pressure experiments on beamline I18 (Microfocus Spectroscopy), I19 (Small Molecule Single Crystal Diffraction), and I22 (Small Angle Scattering and Diffraction). 

Dr Dominique Laniel from the University of Edinburgh said; 

Single crystal X-ray diffraction studies of organic molecular solids – the basic building blocks of life – have mostly been confined to pressures below 10 GPa. It is hypothesised that beyond that pressure (equivalent to 100,000 bar), the void space in these solids approaches zero, a turning point in the behaviour of molecular structures. Zero void space meaning that further compression is expected to change the intramolecular and intermolecular bonding interactions . A multidisciplinary team from the Centre for Science at Extreme Conditions at the University of Edinburgh set out to test this theory and push the boundary for high-pressure investigations on this type of molecular solid using the simple amino acid glycine.

Lewis Clough is a joint PhD student between Diamond and the University of Edinburgh. He worked with colleagues from Edinburgh, studying the behaviour of the alpha polymorph of glycine, which persists to at least 50 GPa. Using high-pressure single-crystal diffraction on I15, the team achieved the highest single-crystal pressure data set collected at Diamond on an organic material.

For the experiment, a tiny 50 μm-sized single crystal of α-glycine was loaded into a diamond anvil cell (DAC), a pocket-sized high-pressure apparatus, in which the crystal was compressed between the tips of two diamonds. Using an X-ray energy of 78 keV – significantly higher than standard for single crystal diffraction experiments – the team collected very high-quality data and solved the structure to the highest pressures of 51-52 GPa.

Read more on Diamond website

Image: Photograph of a single crystal of α-glycine compressed to 52.76 GPa in a diamond anvil cell. A section of the crystal structure determined at this pressure is overlaid on the crystal, showing the layers that increase in proximity upon compression, revealing a network of inter-layer hydrogen bonding interactions.

Power of Movement in Plants

Published in Nature, researchers from Aarhus University and the Technical University of Munich used Diamond’s eBIC facility to uncover new insights into what drives movement in plants.

Auxins are hormones playing a central role and controlling nearly all aspects of plant growth and development. Charles Darwin observed that plants could grow directionally in response to environmental stimuli such as light or gravity. In his book, The Power of Movement in Plants, published in 1880, Darwin showed that the part of the plant responding to such a stimulus differs from the part that perceives it. He proposed that some kind of ‘influence’ must travel from the perception site to the response area. However, Darwin was unable to identify the influence. 

Darwin’s ‘growth accelerating substance’ was identified in 1926 as the hormone auxin. Later research identified that auxin is the growth factor that determines almost all plant responses to environmental changes. Directional transport of the auxin molecule between cells is required to ensure that the auxin response occurs in the correct part of the plant.

It wasn’t until the 1990s that scientists identified the proteins involved in the process. PIN-FORMED (PIN) proteins are auxin transporters, and they are essential for the development of auxin gradients within plant tissues that guide plant growth. They’re named from the distinct needle-like ‘pin’ form, without shoots or flowers, into which plants with dysfunctional PIN proteins grow. Even then, how PIN proteins fold, how they recognise substrates and inhibitors and the molecular mechanism behind transport have remained unknown.

Now researchers from Aarhus University and the Technical University of Munich have used single particle cryo-EM at eBIC to provide the first structural basis of auxin transport by PIN proteins.

Read more on Diamond website

Image: PIN8 is a 40 kDa membrane protein that transports the plant hormone Auxin. It forms a homodimer with each monomer containing two domains: transporter (green) and scaffold (blue). In the transporter domain a distinct crossover (red) is localized at the middle of the membrane plane that defines the auxin binding site. Below the structure are show 8 representative 2D classes from the data collected at eBIC that resulted in 3 distinct conformations solved. To the left are shown a schematic of the transport of Auxin (IAA) with two key conformations coloured that summarizes the transport mechanism as described by the data obtained at eBIC.

From Theory to Confidence: Building Trust in Twistronics Models

A UK collaboration explored the transformative impact of twist angles on the electronic structure of 2D materials

A single sheet of graphene, composed of a single layer of carbon atoms in a hexagonal pattern, is a semimetal. However, adding a second sheet of graphene, twisted at a slight angle to the first, can give rise to very different electronic properties, depending on the angle. At the ‘magic’ angle of about 1.1°, for example, a twisted bilayer sheet of graphene is a superconductor. The same effect is seen in other 2D materials, giving rise to a new field of study – twistronics – seeking to both understand and exploit the relationship between twist angles and novel electronic properties. In work recently published in Nano Letters, researchers from the University of Warwick and the National Graphene Institute at the University of Manchester used spatially-resolved angle-resolved photoemission spectroscopy (ARPES) on Diamond’s I05 beamline to study the twist-dependent band structure of twisted-bilayer, monolayer-on-bilayer, and double-bilayer graphene. Their results show good agreement between experimental measurements and theoretical simulations, confirming that the models can be used to explore the electronic band structure and emergent transport and optical properties of twisted-few-layer graphenes. 

Prof Neil Wilson at the University of Warwick opens by noting that;

Twistronics is a new concept in 2D materials, in condensed matter physics. When you have two atomically thin layers next to each other, their properties depend on the twist angle between them. This happens because of changes to the electronic structure, and there has been a huge amount of research on twistronics – putting two layers together at different twist angles and seeing what happens to the optical properties and electrical properties. You’re working with two very small pieces of 2D material stacked on top of each other, typically only a few micrometres across, which is fine for optical measurements and electrical transport measurements. However, that makes it extremely challenging to study the electronic structure directly.

To get a good look at the electronic structure of these exciting materials, Prof Wilson’s group at the University of Warwick worked with researchers from the National Graphene Institute and Diamond’s I05 beamline. Prof Roman Gorbachev’s group at the National Graphene Institute is a world leader in fabricating these complex samples.

Senior Beamline Scientist Matthew Watson explains;

Angle-resolved ARPES allows us to measure directly the electronic structure of the 2D materials. It allows us to determine both the energy and momentum of the electrons within the material, which gives us directly the electronic structure which underpins the optical properties and the transport properties. And the I05 nano-branch endstation delivers spatially-resolved ARPES from ultra-small spots, on the micrometre length scales we have in these 2D samples.

Read more on Diamond website

Image: Electronic structures of twisted double bilayer graphene at large (left) and “magic” (centre) twist angles, showing the emergence of a flat band at the top, which is at the heart of the various phenomena that emerge in this system. Data measured at I05 at Diamond and reported in Nunn et al.

Credit: Matthew Watson