High-caliber research launches NSLS-II beamline into operations

Pratt & Whitney conduct the first experiments at a new National Synchrotron Light Source II beamline.

A new experimental station (beamline) has begun operations at the National Synchrotron Light Source II (NSLS-II)—a U.S. Department of Energy (DOE) Office of Science User Facility at DOE’s Brookhaven National Laboratory. Called the Beamline for Materials Measurement (BMM), it offers scientists state-of-the-art technology for using a classic synchrotron technique: x-ray absorption spectroscopy.

“There are critical questions in all areas of science that can be solved using x-ray absorption spectroscopy, from energy sciences and catalysis to geochemistry and materials science,” said Bruce Ravel, a physicist at the National Institute of Standards and Technology (NIST), which constructed and operates BMM through a partnership with NSLS-II.

X-ray absorption spectroscopy is a research technique that was developed in the 1980s and, since then, has been at the forefront of scientific discovery.

“The reason we’ve used this technique for 40 years and the reason why NIST built the BMM beamline is because it adds a great value to the scientific community,” Ravel explained.

The first group of researchers to conduct experiments at BMM came from jet engine manufacturer Pratt & Whitney. Senior Engineer Chris Pelliccione and colleagues used BMM to study the chemistry of jet engines.

>Read more on the National Synchrotron Light Source II (NSLS-II) website

Image: Pratt & Whitney Senior Engineer Chris Pelliccione (left) with NIST’s Bruce Ravel (right) at BMM’s workstation.

Understanding reaction pathways leading to MnO2 polymorph formation

Computational driven design of materials has provided guidelines for designing novel materials with desired properties, especially for metastable materials, which may have superior functionalities than its stable counterparts [1]. However, the synthesis of these metastable materials is usually challenging. The current computational approaches are not able to predict reaction pathways passing through intermediate or metastable phases. As a consequence, the synthesis of many compounds still remains Edisonian, meaning that repeated iteration is usually required to find the reaction conditions needed for synthesizing targeted materials with desired properties. To reduce the amount of cost and effort during this discovery process, a predictive theory for directing the synthesis of materials is necessary.

In the recent article “Understanding Crystallization Pathways Leading to Manganese Oxide Polymorph Formation [2]”, researchers from SLAC, LBNL, MIT, Colorado School of Mines, and NREL combined theory and experimental approaches to develop and demonstrate a theoretical framework that guides the synthesis of intermediate/metastable phases. This ab initio-computation based framework calculates the influence of particle size and solution composition on the stability of polymorph (substances having the same composition but different crystallographic structures), and predicts the phases that will appear along the different reaction pathways.

>Read more on the SSRL at SLAC website

Image (extract): (a) Size-dependent phase diagram of MnO2 polymorphs. The three arrows mark the reaction progression from nano-size to bulk at different potassium concentrations. (b-d) The evolution of x-ray scattering pattern with time along [K+] = 0 M (b), 0.2 M (c), and 0.33M (d). The identities and the fractions of the phases are marked in the subfigure to the right. (e-f) Electron beam diffraction patterns of the δ” phase and δ’ phase harvested from [K+] = 0 M and 0.2 M, respectively. See all figures here.

A designed material untangles long-standing puzzle

This approach could lead to new materials with emergent physics and unique electronic properties, supporting broader research efforts to revolutionize modern electronics.

When atoms or molecules assemble to form bulk matter, new properties (such as conductivity and ferromagnetism) that didn’t exist in the constituent parts can emerge from the whole. Similarly, stacking atomically thin layers into nanostructures (heterostructures) can give rise to a rich variety of emergent phases not found in bulk materials.

Materials that exhibit emergent phenomena (“quantum materials”) often feature multiple phases with simultaneous phase transitions. A great deal of effort is currently being expended to disentangle such transitions, to discover what drives them and to ultimately harness them in new materials with desired functionalities. Most of these efforts have relied on external perturbations (light, pressure, etc.) to decouple the transitions. In this work, researchers found a way to do this intrinsically, through layer-by-layer design of stacking sequences with mismatched periodicities.

>Read more on the Advanced Light Source website

Image: (a) Rare-earth (RE) nickelates (RENiO3) host multiple types of entangled orderings. This illustration depicts a magnetic ordering (spin directions indicated by yellow arrows) and a charge ordering (a checkerboard of two nickel oxidation states, indicated by sphere size and color) in bulk RENiO3 (RE and O atoms omitted for clarity). 
Please find the entire image here.

Research shows how to improve the bond between implants and bone

Research carried out recently at the Canadian Light Source (CLS) in Saskatoon has revealed promising information about how to build a better dental implant, one that integrates more readily with bone to reduce the risk of failure.

“There are millions of dental and orthopedic implants placed every year in North America and a certain number of them always fail, even in healthy people with healthy bone,” said Kathryn Grandfield, assistant professor in the Department of Materials Science and Engineering at McMaster University in Hamilton.

A dental implant restores function after a tooth is lost or removed. It is usually a screw shaped implant that is placed in the jaw bone and acts as the tooth roots, while an artificial tooth is placed on top. The implant portion is the artificial root that holds an artificial tooth in place.

Grandfield led a study that showed altering the surface of a titanium implant improved its connection to the surrounding bone. It is a finding that may well be applicable to other kinds of metal implants, including engineered knees and hips, and even plates used to secure bone fractures.

About three million people in North America receive dental implants annually. While the failure rate is only one to two percent, “one or two percent of three million is a lot,” she said. Orthopedic implants fail up to five per cent of the time within the first 10 years; the expected life of these devices is about 20 to 25 years, she added.

“What we’re trying to discover is why they fail, and why the implants that are successful work. Our goal is to understand the bone-implant interface in order to improve the design of implants.”

>Read more on the Canadian Light Source website

X-Ray Experiment confirms theoretical model for making new materials

By observing changes in materials as they’re being synthesized, scientists hope to learn how they form and come up with recipes for making the materials they need for next-gen energy technologies.

Over the last decade, scientists have used supercomputers and advanced simulation software to predict hundreds of new materials with exciting properties for next-generation energy technologies.

Now they need to figure out how to make them.

To predict the best recipe for making a material, they first need a better understanding of how it forms, including all the intermediate phases it goes through along the way – some of which may be useful in their own right.

Now experiments at the Department of Energy’s SLAC National Accelerator Laboratory have confirmed the predictive power of a new computational approach to materials synthesis. Researchers say that this approach, developed at the DOE’s Lawrence Berkeley National Laboratory, could streamline the creation of novel materials for solar cells, batteries and other sustainable technologies.

>Read more on the Stanford Synchrotron Radiation Lightsource at SLAC website

Image: In an experiment at SLAC, scientists loaded ingredients for making a material into a thin glass tube and used X-rays (top left) to observe the phases it went through as it was forming (shown in bubbles). The experiment verified theoretical predictions made by scientists at Berkeley Lab with the help of supercomputers (right).
Credit: Greg Stewart/SLAC National Accelerator Laboratory

Magnetization ratchet in cylindrical nanowires

A team of researchers from Materials Science Institute of Madrid (CSIC), University of Barcelona and ALBA Synchrotron reported on magnetization ratchet effect observed for the first time in cylindrical magnetic nanowires (magnetic cylinders with diameters of 120nm and lengths of over 20µm).

These nanowires are considered as building blocks for future 3D (vertical) electronic and information storage devices as well as for applications in biological sensing and medicine. The experiments have been carried out at the CIRCE beamline of the ALBA Synchrotron. The results are published in ACS Nano.

The magnetic ratchet effect, which represents a linear or rotary motion of domain walls in only one direction preventing it in the opposite one, originates in the asymmetric energy barrier or pinning sites. Up to now it has been achieved only in limited number of lithographically engineered planar nanostructures. The aim of the experiment was to design and prove the one-directional propagation of magnetic domain walls in cylindrical nanowires.

>Read more on the ALBA website

Image: (extract) Unidirectional propagation of magnetization as seen in micromagnetic simulations and XMCD-PEEM experiments. See entire image here.

Dark-field X-ray microscopy provides surprising insight on ferroelectrics

Thanks to the unique capabilities of in-situ dark-field X-ray microscopy, scientists have now been able to see the complex structures hidden deep inside ferroelectric materials. The results, published today in Nature Materials, contradict previous studies in which only the surface was studied. This revolutionary new technique will be the main feature of a new beamline for the new EBS machine currently being built at the ESRF.

“Until now we could only see the surface of the material; dark-field x-ray microscopy is like creating a window to its interior”, explains Hugh Simons, assistant professor at the Technical University of Denmark and corresponding author of the study. “It provides incredible contrast for even the subtlest structures inside these materials, giving us a much clearer picture of how they work”, he adds.

Simons, together with the team of ID06 – the beamline where the technique is being developed – studied the ferroelectric material BaTiO3, which is used every day in cars, computers and mobile phones. By imaging their internal structure at the same time as they applied an electric field on it, they could see how these internal structures behave and change dynamically.

>Read more on the European Synchrotron (ESRF) website

Image: (extract) Crosssectional dark-field x-ray microscopy maps of the embedded BaTiO3 grain. (…) the reconstructed strain map reveals the structural relationship between domain clusters. Full picture here.
Credit: H. Simons.

Brookhaven Lab scientist receives Early Career Research Program Funding

Valentina Bisogni, an associate physicist at the U.S. Department of Energy’s (DOE) Brookhaven National Laboratory, has been selected by DOE’s Office of Science to receive significant research funding as part of DOE’s Early Career Research Program.

The effort, now in its ninth year, is designed to bolster the nation’s scientific workforce by providing support to exceptional researchers during the crucial early career years, when many scientists do their most formative work. Bisogni is among a total of 84 recipients selected this year after a competitive review of proposals. Thirty winners come from DOE national laboratories and 54 from U.S. universities.

“Supporting talented researchers early in their career is key to building and maintaining a skilled and effective scientific workforce for the nation. By investing in the next generation of scientific researchers, we are supporting lifelong discovery science to fuel the nation’s innovation system,” said Secretary of Energy Rick Perry. “We are proud of the accomplishments these young scientists have already made, and look forward to following their achievements in years to come.”

Each researcher will receive a grant of up to $2.5 million over five years to cover their salary and research expenses. A list of the 84 awardees, their institutions, and titles of their research projects is available on DOE’s Early Career Research Program webpage.

>Read more on the NSLS-II at Brookhaven Lab website

Image: Valentina Bisogni is shown preparing samples at NSLS-II’s Soft Inelastic X-ray Scattering beamline, where she will conduct her research funded through DOE’s Early Career Research Program.

The 2018 Julian David Baumert Ph.D. Thesis Award

Maxwell Terban received the 2018 Julian Baumert Ph.D. Thesis Award at this year’s Joint CFN and NSLS-II Users’ Meeting.

Maxwell Terban, a postdoctoral researcher at the Max-Plank Institute for Solid State Research, Stuttgart, is this year’s recipient of the Julian Baumert Ph.D. Thesis Award. Terban was selected for developing new research methods, based around a technique called pair distribution function (PDF), for extracting and analyzing structural signatures from materials. His research incorporated measurements from the now-closed National Synchrotron Light Source (NSLS) and the recently opened National Synchrotron Light Source II (NSLS-II)—a U.S. Department of Energy (DOE) Office of Science User Facility located at Brookhaven National Laboratory.

Each year, the Baumert Award is given to a researcher who has recently conducted a thesis project that included measurements at NSLS or NSLS-II. The award was established in memory of Julian David Baumert, a young Brookhaven physicist who worked on x-ray studies of soft-matter interfaces at NSLS.

Terban holds a bachelor’s degree in chemical engineering from the University of Massachusetts, Amherst, and a master’s degree in materials science and engineering from Columbia University. He graduated with a Ph.D. in materials science and engineering from Columbia University in 2018, and completed his doctoral dissertation under the guidance of Simon Billinge, a professor of materials science and engineering and applied physics and mathematics at Columbia.

>Read more on the NSLSI-II at Brookhaven National Laboratory website

Image: Maxwell Terban, a postdoctoral researcher at the Max-Plank Institute for Solid State Research, Stuttgart, is this year’s recipient of the Julian Baumert Ph.D. Thesis Award.

Molecular Anvils Trigger Chemical Reactions

Tripling the energy storage of lithium-ion batteries

Scientists have synthesized a new cathode material from iron fluoride that surpasses the capacity limits of traditional lithium-ion batteries.

As the demand for smartphones, electric vehicles, and renewable energy continues to rise, scientists are searching for ways to improve lithium-ion batteries—the most common type of battery found in home electronics and a promising solution for grid-scale energy storage. Increasing the energy density of lithium-ion batteries could facilitate the development of advanced technologies with long-lasting batteries, as well as the widespread use of wind and solar energy. Now, researchers have made significant progress toward achieving that goal.

A collaboration led by scientists at the University of Maryland (UMD), the U.S. Department of Energy’s (DOE) Brookhaven National Laboratory, and the U.S. Army Research Lab have developed and studied a new cathode material that could triple the energy density of lithium-ion battery electrodes. Their research was published on June 13 in Nature Communications.

>Read more on the NSLS-II at Brookhaven National Lab website

Image: Brookhaven scientists are shown at the Center for Functional Nanomaterials. Pictured from left to right are: (top row) Jianming Bai, Seongmin Bak, and Sooyeon Hwang; (bottom row) Dong Su and Enyuan Hu.

Insulator metal transition at the nanoscale

An international team of researchers has been able to probe the insulator-conductor phase transition of materials at the nanoscale resolution. This is one of the first results of MaReS endstation of BOREAS beamline.

Controlling the flow of electrons within circuits is how electronic devices work. This is achieved through the appropriate choice of materials. Metals allow electrons to flow freely and insulators prevent conduction. In general, the electrical properties of a material are determined when the material is fabricated and cannot be changed afterwards without changing the material. However, there are materials that can exhibit metal or insulator behaviour depending on their temperature. Being able switch their properties, these materials could lead to a new generation of electronic devices.

Vanadium Dioxide (VO2) is one such material. It can switch from an insulating phase to a metallic phase just above room temperature, a feature exploited already for sensors. However, the reason why the properties of this material change so dramatically has been a matter of scientific debate for over 50 years.

One of the challenges in understanding why and how this switch occurs is due to a process called phase separation. The insulator-metal phase transition is similar to the ice to liquid transition in water. When ice melts, both liquid and solid water can coexist in separate regions. Similarly, in VO2, insulating and metallic regions of the material can be coexisting at the same time during the transition. But unlike water, where the different regions are often large enough to see with the naked eye, in VOthis separation occurs on the nanoscale and it is thus challenging to observe. As a result, it has been hard to know if the true properties of each phase, or the mixture of both phases, are being measured.

>Read more on the ALBA Synchrotron website

Image: (extract, original here) reconstructed holograms at the vanadium and oxygen edges (518, 529, and 530.5 eV) used to encode the intensities of the three color channels of an RGB (red, green, blue) image. At 330 K, an increase in intensity of the green channel, which probes the metallic rutile phase (R) through the d∥ state, is observed in small regions. As the sample is heated further, it becomes increasingly clear that the blue channel, which probes a intermediate insulating M2 phase, also changes but in different regions. At 334 K, three distinct regions can be observed corresponding to the insulating monoclinic M1, M2, and metallic R phases. As the temperature increases, the R phase dominates. The circular field of view is 2 μm in diameter. (taken from Vidas et al, Nanoletters, 2018).

Video presentation of thesis at NanoMAX

In April 2018, Karolis Parfeniukas (image) defended the first thesis to be fully completed at one of the new MAXIV beamlines called NanoMAX Here’s an interview with Karolis about this project making zone plates to improve focusing of the X-ray beam. Thesis from KTH university, Royal Institute of Technology in Stockholm. PLease watch here the presentation of his research at MAX IV Laboratory:

>Read more here about MAX IV Laboratory

Rational optimization of organic solar-cell materials

Taking additive manufacturing’s heart beat

Additive manufacturing, or 3D printing, builds objects by adding layers and it is emerging as a more flexible and reliable way of manufacturing complex structures in the aerospace, engineering and biomedical industries. A British team is at the ESRF’s ID19 to see into the heart of the process and understand it.

“I would not want to ship this equipment on an aeroplane”, Chu Lun Alex Leung said, scientist from the University of Manchester. “It was too precious to leave it in the hands of third parties”, he added. Instead of coming to the ESRF by aeroplane, Leung and his colleagues endured the 12-hour drive in a rental van all the way from Oxfordshire (UK) to the ESRF to make sure their unique equipment arrived safely.

Leung was referring to the laser additive manufacturing (LAM) process replicator, or LAMPR for short, a machine himself and colleagues at the Research Complex at Harwell have developed that 3D prints polymers, metals and ceramics while ESRF’s X-rays probe the heart of the process – the melting and solidification of powders to form complex 3D printed components.

>Read more on the European Synchrotron website

Image: The team on the beamline, next to the laser additive manufacturing (LAM) process replicator. Front row: Margie P. Olbinado, Yunhui Chen. Back row: Sam Tammas-Williams, Lorna Sinclair, Peter D. Lee, Chu lun alex Leung, Samuel Clark, Sebastian Marussi.
Credit: C.Argoud

World’s strongest bio-material outperforms steel and spider silk

Novel method transfers superior nanoscale mechanics to macroscopic fibres

At DESY’s X-ray light source PETRA III, a team led by Swedish researchers has produced the strongest bio-material that has ever been made. The artifical, but bio-degradable cellulose fibres are stronger than steel and even than dragline spider silk, which is usually considered the strongest bio-based material. The team headed by Daniel Söderberg from the KTH Royal Institute of Technology in Stockholm reports the work in the journal ACS Nano of the American Chemical Society.

The ultrastrong material is made of cellulose nanofibres (CNF), the essential building blocks of wood and other plant life. Using a novel production method, the researchers have successfully transferred the unique mechanical properties of these nanofibres to a macroscopic, lightweight material that could be used as an eco-friendly alternative for plastic in airplanes, cars, furniture and other products. “Our new material even has potential for biomedicine since cellulose is not rejected by your body”, explains Söderberg.

The scientists started with commercially available cellulose nanofibres that are just 2 to 5 nanometres in diameter and up to 700 nanometres long. A nanometre (nm) is a millionth of a millimetre. The nanofibres were suspended in water and fed into a small channel, just one millimetre wide and milled in steel. Through two pairs of perpendicular inflows additional deionized water and water with a low pH-value entered the channel from the sides, squeezing the stream of nanofibres together and accelerating it.

>Read more on the PETRA III at DESY website

Image: The resulting fibre seen with a scanning electron microscope (SEM).
Credit: Nitesh Mittal, KTH Stockholm