Optical ​“tweezers” combine with X-rays to enable analysis of crystals in liquids

Understanding how chemical reactions happen on tiny crystals in liquid solutions is central to a variety of fields, including materials synthesis and heterogeneous catalysis, but obtaining such an understanding requires that scientists observe reactions as they occur.

By using coherent X-ray diffraction techniques, scientists can measure the exterior shape of and strain in nanocrystalline materials with a high degree of precision. However, carrying out such measurements requires precise control of the position and angles of the tiny crystal with respect to the incoming X-ray beam. Traditionally, this has meant adhering or gluing the crystal to a surface, which in turn strains the crystal, thus altering its structure and potentially affecting reactivity.

>Read more on the Advanced Photon Source at Argonne Laboratory website

Image: Scientists have found a way to use “optical tweezers” by employing lasers, a mirror and a light modulator to anchor a crystal in solution. The “tweezers” have made it possible to conduct X-ray diffraction measurements of a crystal suspended in solution.
Credit: Robert Horn/Argonne National Laboratory.

A new molecule could help put the STING on cancer

The protein STING (stimulator of interferon genes) is a component of the innate immune system. It plays a major role in the immune response to cancer, and abnormal STING signaling has been shown to be associated with certain cancers. Immunomodulatory approaches using agonists to target STING signaling are therefore being investigated as anticancer treatments. However, the compounds in clinical trials typically are injected intratumorally in patients with solid cancers. In this study, researchers discovered a novel STING agonist, known as an amidobenzimidazole (ABZI), which can be given by intravenous injection and could therefore potentially open up its evaluation as a treatment for hard-to-reach cancers. Using x-ray diffraction data collected at the U.S. Department of Energy’s Advanced Photon Source (APS), researchers from GlaxoSmithKline (GSK) investigated ABZI compounds and STING. Their results, published in the journal Nature, may have important implications for anticancer immunotherapy.

STING is a protein that mediates innate immunity, and one function of the STING signaling pathway is in mobilizing an immune response against tumors. STING proteins can be activated by cyclic dinucleotides, small molecules that are made by the cytosolic DNA sensor, cGAS, upon sensing of DNA leaking out of the nucleus as a result of DNA damage, including that which might be associated with cancer development.

>Read more on the Advanced Photon Source at Argonne National Lab.

Figure: X-ray crystal structure of the STING protein bound to one of the new molecules.

New technique for two-dimensional material analysis

Discovery allows scientists to look at how 2D materials move with ultrafast precision.

Using a never-before-seen technique, scientists have found a new way to use some of the world’s most powerful X-rays to uncover how atoms move in a single atomic sheet at ultrafast speeds.

The study, led by researchers at the U.S. Department of Energy’s (DOE) Argonne National Laboratory and in collaboration with other institutions, including the University of Washington and DOE’s SLAC National Accelerator Laboratory, developed a new technique called ultrafast surface X-ray scattering. This technique revealed the changing structure of an atomically thin two-dimensional crystal after it was excited with an optical laser pulse.
>Read more on the Advanced Photon Source at Argonne website
>Another article is also available on the Linac Coheren Light Source at SLAC website

Image: An experimental station at SLACs Linac Coherent Light Source X-ray free-electron laser, where scientists used a new tool they developed to watch atoms move within a single atomic sheet.
Credit: SLAC National Accelerator Laboratory

Unleashing perovskites’ potential for solar cells

Perovskites — a broad category of compounds that share a certain crystal structure — have attracted a great deal of attention as potential new solar-cell materials because of their low cost, flexibility, and relatively easy manufacturing process. But much remains unknown about the details of their structure and the effects of substituting different metals or other elements within the material. Now, researchers using the U.S. Department of Energy’s (DOE’s) Advanced Photon Source (APS) have been able to decipher a key aspect of the behavior of perovskites made with different formulations: With certain additives there is a kind of “sweet spot” where sufficient amounts will enhance performance and beyond which further amounts begin to degrade it. The findings were detailed in the journal Science.
Conventional solar cells made of silicon must be processed at temperatures above 1,400 degrees Celsius, using expensive equipment that limits their potential for production scale-up. In contrast, perovskites can be processed in a liquid solution at temperatures as low as 100 degrees, using inexpensive equipment. What’s more, perovskites can be deposited on a variety of substrates, including flexible plastics, enabling a variety of new uses that would be impossible with thicker, stiffer silicon wafers.

>Read more on the Advanced Photon Source (APS) website

Image: Perovskite-based solar cells are flexible, lightweight, can be produced cheaply, and could someday bring down the cost of solar energy. Shown here is the type of perovskite solar cell measured at the CNM/XSD Hard X-ray Nanoprobe at the APS.
Credit: Rob Felt

Illuminating a key industrial process

Results of research carried out at the U.S. Department of Energy’s (DOE’s) Advanced Photon Source (APS) may pave the way to improvements in industrial processes based on solvent extraction, which is used in the mining and refinement of technologically important rare earths. The results were published in the journal Physical Review Letters.
Rare earths such as lanthanides, which are elements in the range of atomic number 57 to 71, are not actually rare. They exist in large quantities in the world, but are only found in the form of trace amounts in rocks. Since rare earths are important for a variety of applications (e.g., electronics) their extraction is a major mining-related industry.
A common process by which rare earths are extracted involves dissolving rocks in acids, then shaking up the solution with an organic solvent and a surfactant. Under the right conditions, the desired ions move out of the aqueous phase and into the organic solvent.  This is known as “liquid-liquid extraction” or “solvent extraction,” and is conducted on a large scale by the mining industry. This process also separates heavier lanthanides from lighter lanthanides present in the same solution, because the heavier lanthanides separate more easily. While this fact is known and exploited in industrial separations processes, the nanoscale mechanisms of the separation process are not well understood.

>Read more on the Advanced Photon Source

Image: (a ) Schematic of system studied; positively charged lanthanide ions (blue circles) dissolve in the water, while the negatively charged surfactant molecules (purple) float on the water surface. (b) Data showing how density of ions at the surfactant surface jumps as the concentration of ions in the bulk water increases (Er=erbium, a heavier lanthanide, Nd=neodymium, a lighter lanthanide). The lines thru data are predictions from computer simulations. From M. Miller et al., Phys. Rev. Lett. 122, 058001 (2019).

The first observation of near-room-temperature superconductivity

For decades, room-temperature superconductivity has been one of physics’ ultimate goals, a Holy Grail-like objective that seems to keep drifting within realization yet always stubbornly out of reach. Various materials, theories, and techniques have been proposed and explored in search of this objective, but its realization has remained elusive. Yet recent experimental work on hydrogen-rich materials at high pressures is finally opening the pathway to practical superconductivity and its vast potential. Russell Hemley, a materials chemist at George Washington University in Washington, D.C., first announced evidence of superconductivity at 260 K in May, 2018, and then hints of an even higher 280 K transition in August of that year. Now Hemley, along with a team of researchers from The George Washington University and the Carnegie Institution for Science synthesized several lanthanum superhydride materials that demonstrated the first experimental evidence of superconductivity at near room temperature, and with colleagues from Argonne National Laboratory characterized them at the U.S. Department of Energy’s Advanced Photon Source (APS). Read more

Beam us up

The upgrade of the U.S. Department of Energy’s Advanced Photon Source at Argonne National Laboratory will make it between 100 and 1,000 times brighter than it is today.

That factor is such a big change, it’s going to revolutionize the types of science that we can do,” said Stephen Streiffer, Argonne Associate Laboratory Director for Photon Sciences and Director of the APS. We’ll be able to look at the structure of materials and chemical systems in the interior of things — inside a turbine blade or a catalytic reactor — almost down to the atomic scale. We haven’t been able to do that before. Given that vast change, we can only dream about the science we’re going to do.”
In December, DOE approved the technical scope, cost estimate and plan of work for an upgrade of APS.
The APS upgrade has been in the works since 2010. The upgrade will reveal a new machine that will allow its 5,500 annual users from university, industrial, and government laboratories to work at a higher spatial resolution, or to work faster with a brighter beam (a beam with more X-rays focused on a smaller spot) than they can now.

>Read more on the Advanced Photon Source at Argonne National Laboratory website

Image: A closeup of the magnets that will drive the upgraded APS beams.

Finding unusual performance in unconventional battery materials

Even as our electronic devices become ever more sophisticated and versatile, battery technology remains a stubborn bottleneck, preventing the full realization of promising applications such as electric vehicles and power-grid solar energy storage.  Among the limitations of current materials are poor ionic and electron transport qualities. While strategies exist to improve these properties, and hence reduce charging times and enhance storage capacity, they are often expensive, difficult to implement on a large scale, and of only limited effectiveness.  An alternative solution is the search for new materials with the desired atomic structures and characteristics.  This is the strategy of a group of researchers who, utilizing ultra-bright x-rays from the U.S. Department of Energy’s Advanced Photon Source (APS), identified and characterized two niobium tungsten oxide materials that demonstrate much faster charging rates and power output than conventional lithium electrodes.  Their work appeared in the journal Nature.

Currently, the usual approach for wringing extra capacity and performance from lithium-ion batteries involves the creation of electrode materials with nanoscale structures, which reduces the diffusion distances for lithium ions.  However, this also tends to increase the practical volume of the material and can introduce unwanted additional chemical reactions. Further, when graphite electrodes are pushed to achieve high charging rates, irregular dendrites of lithium can form and grow, leading to short circuits, overheating, and even fires.  Measures to prevent these dendrites generally cause a decrease in energy density.  These issues seriously limit the use of graphite electrodes for high-rate applications.

>Read more on the Advanced Photon Source website

Image: Artist’s impression of rapidly flowing lithium through the niobium tungsten oxide structure. This is a detail of the image, please see here for the entire art work.
Credit: Ella Maru Studio

A super-relaxed myosin state to offset hypertrophic cardiomyopathy

At its most basic level, the proper functioning of the heart depends upon the intricate interaction of proteins that trigger, maintain, and control the muscular contractions and relaxations of this vital organ. Disruption of those interactions can cause serious pathologies such as hypertrophic cardiomyopathy (HCM). Such disruptions can originate with mutations in the primary motor protein involved in heart contraction, ß-cardiac myosin, which can alter the rate of ATP hydrolysis and have been hypothesized to destabilize its super-relaxed state (SRX). Researchers investigated the stabilizing action of mavacamten, a cardiac drug currently in phase 3 clinical trials, on the ß-cardiac myosin super-relaxed state and its possible therapeutic effects on HCM. Their work, which included electron microscopy and low-angle x-ray diffraction at the U.S. Department of Energy’s Advanced Photon Source (APS), was published in Proceedings of the National Academies of Sciences of the United States of America.

Previous work had hinted that a folded state of the myosin protein, seen both in purified form and in isolated filaments and known as the interacting-heads motif or IHM, could be analogous to the SRX state, although this has not yet been demonstrated experimentally. It has been proposed that mutations causing HCM disrupt this state, resulting in a higher percentage of myosin heads being available for interaction with actin and leading to the hypercontractility of cardiac tissue seen in HCM. These investigators, from  MyoKardia, Inc., the Stanford University School of Medicine, the Illinois Institute of Technology, Exemplar Genetics, the Harvard Medical School, and the University of California, San Francisco, first studied this possibility using three separate purified ß-cardiac myosin constructs (25-heptad heavy meromysin [HMM], two-heptad HMM, and short S1), finding that a fraction of their basal ATPase rates were within the range of 0.002-0.004 s-1 which defines the SRX state.

>Read more on the Advanced Photon Source at Argonne National Laboratory

Image: The figure (a) shows a diffraction pattern from untreated muscle compared to treated muscle on the right. Intensification of the x-ray reflections from the treated muscle indicate a highly ordered “super-relaxed” state of myosin motors. Figure (b) shows the myosin heads in the compact “interacting head motif” which the heads adopt in the super-relaxed state allowing them to be packed closely and tightly on the surface of muscle thick filaments.

 

Topological excitations emerge from a vibrating crystal lattice

It has long been known that the properties of materials are crucially dependent on the arrangement of the atoms that make up the material. For example, atoms that are further apart will tend to vibrate more slowly and propagate sound waves more slowly. Now, researchers from Brookhaven National Laboratory have used Sector 30 at the Advanced Photon Source (APS) to discover “topological” vibrations in iron silicide (FeSi). These topological vibration arise from a special symmetrical arrangement of the atoms in FeSi and endow the atomic vibrations with novel properties such as the potential to transmit sound waves along the edge of the materials without scattering and dissipation. Looking to the future one might envisage using these modes to transfer energy or information within technological devices.

In quantum mechanics, atomic motions in crystals are described in terms of vibrational modes called phonons. Similar to electrons moving in metals, phonons can also propagate through materials. The detailed properties of these excitations determine many of the thermal, mechanical and electronic properties of the material. In 2017, part of the current collaborative team from the Chinese Academy of Science, theoretically predicted the existence of the topological phonons in transition metal monosilicides. As shown in Fig.1, these topological phonons are formed by two Dirac-cones with different slopes and are protected by symmetry. Since the mathematical description of each Dirac-cone is intimately related to the famous Weyl-equation that was originally proposed in high-energy physics, these topological phonons are consequently called double-Weyl excitations.

>Read more on the Advanced Photon Source website

Image: (extract) Schematic view of the double-Weyl phonon dispersion. Full image here.
Credit: Brookhaven National Laboratory

Demonstrating a new approach to lithium-ion batteries

A team of researchers from the University of Cambridge, Diamond Light Source and Argonne National Laboratory in the US have demonstrated a new approach that could fast-track the development of lithium-ion batteries that are both high-powered and fast-charging.

In a bid to tackle rising air pollution, the UK government has banned the sale of new diesel and petrol vehicles from 2040, and the race is on to develop high performance batteries for electric vehicles that can be charged in minutes, not hours. The rechargeable battery technology of choice is currently lithium-ion (Li-ion), and the power output and recharging time of Li-ion batteries are dependent on how ions and electrons move between the battery electrodes and electrolyte. In particular, the Li-ion diffusion rate provides a fundamental limitation to the rate at which a battery can be charged and discharged.

>Read more on the Diamond Light Source website

Molecular Anvils Trigger Chemical Reactions

Spin and charge frozen by strain

In the development of next-generation microelectronics, a great deal of attention has been given to the use of epitaxy (the deposition of a crystalline overlayer on a crystalline substrate) to tailor the properties of materials to suit particular applications. Correlated electron systems provide an excellent platform for the development of new microelectronic devices due to the presence of multiple competing ground states of similar energy. In some cases, strain can drive these systems between two or more such states, resulting in phase transitions and dramatic changes in the properties of the material. Often, the specific mechanism by which strain accomplishes such a feat is unknown. This was precisely the case in lanthanum cobaltite, LaCoO3, which undergoes a strain-induced transition from paramagnet to ferromagnet, until a recent study carried out at the U.S. Department of Energy’s Advanced Photon Source (APS) revealed the intriguing microscopic phenomena at work in this system. These phenomena may play a role in spin-state and magnetic-phase transitions, regardless of stimulus, in many other correlated systems.

Lanthanum cobaltite is a perovskite, which means the structure can be thought of as made up of distorted cubes with cobalt at the cube centers, oxygen at the cube faces, and lanthanum at the cube corners. The cobalt ions have a nominal 3+ valence, meaning they lose three electrons to the neighboring oxygen ions. Bulk LaCoO3 is paramagnetic (that is, having a net magnetization only in the presence of an externally applied magnetic field) above 110 Kelvin, and non-magnetic below that temperature. In its ground state, all the electrons on a given cobalt ion are paired, meaning their magnetic spins cancel each other out. These are so-called low-spin (LS) Co3+ ions, and when all of the cobalt ions are in this form, LaCoO3 is non-magnetic.

>Read more on the Advanced Photon Source website

Image: Upper left: Resonant x-ray scattering at the cobalt K-edge. Inversion of the spectra at the reflections shown indicates the presence of charge order. Upper right: X-ray diffraction reciprocal space maps at the (002) and (003) reflection indicating the high epitaxial quality of the films. The satellite peaks result from lattice modulations associated with the reduced symmetry in the film. Lower left: Schematic crystal structure of epitaxial LaCoO3 showing the arrangement of cobalt sites with different charge and spin. The circulated charge transfer from oxygen to the different cobalt sites is also shown. Lower right: Calculated total energy as a function of the difference between the in-plane Co-O bond lengths of HS and LS cobalt ions (∆rCo-O).

Freeze-framing nanosecond movements of nanoparticles

New method allows to monitor fast movements at hard X-ray lasers.

A team of scientists from DESY, the Advanced Photon Source APS and National Accelerator Laboratory SLAC, both in the USA, have developed and integrated a new method for monitoring ultrafast movements of nanoscopic systems. With the light of the X-ray laser LCLS at the research center SLAC in California, they took images of the movements of nanoparticles taking only the billionth of a second (0,000 000 001 s). In their experiments now published in the journal Nature Communications they overcame the slowness of present-day two-dimensional X-ray detectors by splitting individual laser flashes of LCLS, delaying one half of it by a nanosecond and recording a single picture of the nanoparticle with these pairs of X-ray pulses. The tunable light splitter for hard X-rays which the scientists developed for these experiments enables this new technique to monitor movements of nanometer size fluctuations down to femtoseconds and at atomic resolution. For comparison: modern synchrotron radiation light sources like PETRA III at DESY can typically measure movements on millisecond timescales.

The intense light flashes of X-ray lasers are coherent which means that the waves of the monochromatic laser light propagate in phase to each other. Diffracting coherent light by a sample usually results in a so-called speckle diffraction pattern showing apparently randomly ordered light spots. However, this speckle is also a map of the sample arrangement, and movements of the sample constituents result in a different speckle pattern.

>Read more on the DESY website

Image: Scheme of the experiment: An autocorrelator developed at DESY splits the ultrashort X-ray laser pulses into two equal intensity pulses which arrive with a tunable delay at the sample. The speckle pattern of the sample is collected in a single exposure of the 2-D detector
Credit: W. Roseker/DESY

Sending electrons on a rollercoaster ride

A first-of-its-kind x-ray instrument for frontier research with high-brightness x-rays is now in operation at Argonne National Laboratory. The new device utilizes a unique superconducting technology that speeds electrons on a path much like that of a rollercoaster.

The insertion device (ID), called a Helical Superconducting Undulator (HSCU), was designed at the Advanced Photon Source (APS), a U.S. Department of Energy (DOE) Office of Science User Facility at DOE’s Argonne National Laboratory. The device has three primary advantages over other types of IDs for producing high-brightness x-rays: (1) it generates a stronger magnetic field than other IDs; (2) it allows researchers to select a single energy from the x-ray beam without using any x-ray optics; and (3) it produces an x-ray beam with circular polarization. Argonne developed the helical undulator with $2 million in funding from the DOE Office of Science.

>Read more on the Advanced Photon Source website

Image: Matthew Kasa and Susan Bettenhausen of the Advanced Photon Source (APS) Accelerator Division Magnetic Devices Group put the finishing touches on installation of the Helical Superconducting Undulator in Sector 7 of the APS storage ring.

Scientists have a new way to gauge the growth of nanowires

In a new study, researchers from the U.S. Department of Energy’s Argonne and Brookhaven National Laboratories observed the formation of two kinds of defects in individual nanowires, which are smaller in diameter than a human hair.

These nanowires, made of indium gallium arsenide, could be useful for a wide range of applications in a field scientists have termed optoelectronics, which encompasses devices that work by converting light energy into electrical impulses. Fiber optic relays are a good example.

The effectiveness of these devices, however, can be affected by tiny defects in their components. These defects, which can change both the optical and electronic properties of these materials, interest scientists who seek to tailor them to boost the functionality of future optoelectronics, including materials that will be able to manipulate quantum information.

>Read more on the NSLS-II website and the Advanced Photon Source website

Image: Argonne and Brookhaven researchers observed two kinds of defects forming in individual nanowires, depicted here. These nanowires are smaller in diameter than a human hair.
Credit: Megan Hill/Northwestern University