Blowing in the wind

Monitoring dust from legacy mine tailings to keep communities safe

Queen’s university researchers have studied dust blown from legacy mine tailings at the Giant Mine in Yellowknife, NWT and determined vital information to inform future remediation efforts.

Using the CLS@APS, the researchers were able to determine the chemical form of arsenic in dust particles sourced from the Giant Mine tailings which intermittently blow into nearby communities.

“The synchrotron is really useful for looking at dust because you have this really tiny micron scale beam that you can focus on individual dust particles and get really good data,” said Queen’s researcher Alex Bailey, who conducted the study as part of her Master’s.

Giant Mine is a decommissioned gold mine located 5 km North of Yellowknife that is currently being remediated. The main concern around this site is the existence of toxic-to-humans arsenic trioxide which was formed as a byproduct of ore processing in the 1950s and 60s. Arsenic trioxide had been previously found in local soils and lake sediments, and there was a concern from local residents that arsenic trioxide may be present in dust generated from surface tailings which intermittently blows into the community. It was important for the wellbeing and peace of mind of nearby community members to understand what dust from these tailings might carry.

By analyzing dust-sized material from the surface of the mine tailings and dust captured from a strategic location using detailed mineralogical analysis, synchrotron, and more conventional techniques, the team was able to identify what forms the arsenic would take and its implications for human health.

Read more on the CLS website

Image: Alex Bailey at the APS synchrotron collecting uXRD and uXRF data for sieved tailings dust samples

Promising new extra-large pore zeolite

An international research team, led in Spain by CSIC scientist Miguel A. Camblor, has discovered a stable aluminosilicate zeolite with a three dimensional system of interconnected extra-large pores, named ZEO-1.

Zeolites are crystalline porous materials with important industrial applications, including uses in catalytic processes. The pore apertures limit the access of molecules into and out of the inner confined space of zeolites, where reactions occur.

The research, published in Science, proved that ZEO-1 possesses these “extra-large” pores of around 10 Å (1 angstrom equals one ten billionth of a meter), but also smaller pores of around 7 Å, which is actually the size of traditional “large” pores.

Because of its porosity, strong acidity and high stability, ZEO-1 may find applications as a catalyst in fine chemistry for the production of pharmaceutical intermediates, in controlled substance release, for pollution abatement or as a support for the encapsulation of photo- or electroactive species (they react to light or an electric field).

“The crossings of its cages delimit super boxes, open spaces that can be considered nanoreactors to carry out chemical reactions in their confined space”, explains Miguel A. Camblor, researcher at the Instituto de Ciencia de Materiales de Madrid – CSIC.

To prove that this new zeolite may be useful in applications involving bigger molecules, researchers measured the adsorption to the inner surface of the zeolite of the dye Nile red – a big molecule. Moreover, they tested its performance in fluid catalytic cracking of heavy oil, a process the world still relies on to produce fuels. In both processes, the new zeolite performed better than the conventional large pore zeolite used nowadays.

This research is the result of an international collaboration between eight research centers in China, the USA, Sweden and Spain. The team was led by Fei-Jian Chen (Bengbu Medical College, China), Xiaobo Chen (China University of Petroleum), Jian Li (Stockholm University) and Miguel A. Camblor (Instituto de Ciencia de Materiales de Madrid, CSIC).

Structure determination with synchrotron light

The zeolite was discovered following a high-throughput screening methodology. The structure solution was challenging because the zeolite has a very complex structure, with a small crystal size (<200nm) but an exceedingly large cell volume.

“The combination of electron diffraction data with synchrotron powder X-ray diffraction data collected at the MSPD beamline of the ALBA Synchrotron and the Argonne National Laboratory (USA) made possible the accurate structure determination of ZEO-1″, says Camblor.

Read more on the ALBA website

Image: A perspective view of the extra-large pore of ZEO-1 along (100)

APS helps Pfizer create Covid-19 antiviral treatment

Pharmaceutical company Pfizer has announced the results of clinical trials of its new oral antiviral treatment against COVID-19. The new drug candidate, Paxlovid, proved to be effective against the SARS-CoV-2 virus, which causes COVID-19, according to results released by Pfizer on Nov. 5.

Scientists at Pfizer created Paxlovid with the help of the ultrabright X-rays of the Advanced Photon Source (APS), a U.S. Department of Energy (DOE) Office of Science user facility at DOE’s Argonne National Laboratory.

“Today’s news is a real game-changer in the global efforts to halt the devastation of this pandemic,” said Albert Bourla, chairman and chief executive officer of Pfizer, in a company press release. ​“These data suggest that our oral antiviral candidate, if approved or authorized by regulatory authorities, has the potential to save patients’ lives, reduce the severity of COVID-19 infections and eliminate up to nine out of 10 hospitalizations.”

DOE invests in user facilities such as the APS for the benefit of the nation’s scientific community, and supports biological research as part of its energy mission. This research has been critical in the fight against COVID-19. The DOE national laboratories formed the National Virtual Biotechnology Laboratory (NVBL) consortium in 2020 to combat COVID-19 using capabilities developed for their DOE mission, and that consortium helps support research into antiviral treatments such as Paxlovid.

Work to determine the structure of the antiviral candidate was done at the Industrial Macromolecular Crystallography Association Collaborative Access Team (IMCA-CAT) beamline at the APS, operated by the Hauptman-Woodward Medical Research Institute (HWI) on behalf of a collaboration of pharmaceutical companies, of which Pfizer is a member.

As a member of IMCA-CAT, Pfizer routinely conducts drug development experiments at the APS, and the process of narrowing down and zeroing in on this drug candidate was performed over many months, according to Lisa Keefe, executive director of IMCA-CAT and vice president for advancing therapeutics and principal scientist at Hauptman-Woodward Medical Research Institute. IMCA-CAT, she said, delivers quality results in a timely manner, much faster than the home laboratories of the companies themselves can do.

Read more on the APS website

Image: The IMCA-CAT beamline at the Advanced Photon Source, where work was done to determine the structure of Pfizer’s new COVID-19 antiviral treatment candidate.

Credit: Lisa Keefe, IMCA-CAT/Hauptman-Woodward Medical Research Institute

Laurent Chapon to lead Argonne’s Advanced Photon Source

Laurent Chapon has been appointed director of the Advanced Photon Source (APS). Chapon will lead the Photon Sciences Directorate at the U.S. Department of Energy’s Argonne National Laboratory through a massive upgrade of the user facility.

Lemont, IL – October 7, 2021 – The U.S. Department of Energy’s (DOE) Argonne National Laboratory has named Laurent Chapon as associate laboratory director for Photon Sciences and director of the Advanced Photon Source (APS), a DOE Office of Science User Facility at Argonne. He will begin his new role on January 10, 2022.

Chapon will join Argonne from Diamond Light Source in the United Kingdom, where he has been the director of physical sciences since 2016. Chapon led the scientific strategy in this division and oversaw five of Diamond’s eight science groups, which encompasses 22 X-ray beamlines and two electron microscopes. He led groups dedicated to technological advancements in optics, metrology and detectors technology at the facility and oversaw the Project Office, User Office, and Experiment Hall groups.

As part of Argonne’s senior management team, Chapon will lead the APS through a time of extraordinary change. The APS Upgrade project will result in a transformed facility that will generate X-ray beams up to 500 times brighter than those it currently delivers. This will require a year-long shutdown of the APS, currently scheduled to begin in April of 2023, and will keep the facility at the forefront of the world’s light sources for scientific discovery.

Read more on the Argonne National Laboratory website

Image: Laurent Chapon

Credit: Lise Chapon

Probing the Structure of a Promising NASICON Material

As physicists, materials scientists, and engineers continue striving to enhance and improve batteries and other energy storage technologies, a key focus is on finding or designing new ways to make electrodes and electrolytes.  One promising avenue of research involves solid-state materials, making possible batteries free of liquid electrolytes, which can pose fire and corrosion hazards.  An international group of researchers joined with scientists at Argonne National Laboratory to investigate the structure of crystalline and amorphous compounds based on the NASICON system, or sodium super-ion conductors. The work (using research carried out at the U.S. Department of Energy’s Advanced Photon Source [APS] and published in the Journal of Chemical Physics) reveals some substantial differences between the crystalline and glass phases of the NAGP system, which affect the ionic conductivity of the various materials.  The investigators note that the fraction of non-bridging oxygen (NBO) atoms appears to play a significant role, possibly altering the Na+ ion mobility, and suggest this as an area of further study.  The work provides fresh insights into the process of homogeneous nucleation and identifying superstructural units in glass ― a necessary step in engineering effective solid-state electrolytes with enhanced ionic conductivity. 

Because of their high ionic conductivity, materials with a NASICON structure are prime candidates for a solid electrolyte in sodium-ion batteries.  They can be prepared by a glass-ceramic route, which involves the crystallization of a precursor glass, giving them the usefulness of moldable bulk materials.  In this work, the research team specifically studied the NAGP system [Na1+xAlxGe2-x(PO4)3] with x = 0, 0.4 and 0.8 in both crystalline and glassy forms. Working at several different facilities, they used a combination of techniques, including neutron and x-ray diffraction, along with 27Al and 31P magic angle spinning and 31P/23Na double-resonance nuclear magnetic resonance spectroscopy.  The glassy form of NAGP materials was examined both in its as-prepared state and after thermal annealing, so that the changes on crystal nucleation could be studied.

Neutron powder diffraction measurements were performed at the BER II reactor source, Helmholtz-Zentrum Berlin, using the fine resolution powder diffractometer E9 (FIREPOD), followed by Rietveld analysis.  Further neutron diffraction observations were conducted at the Institut Laue-Langevin using the D4c diffractometer and at the ISIS pulsed neutron source using the GEM diffractometer.  X-ray diffraction studies were performed at X-ray Science Division Magnetic Materials Group’s beamline 6-ID-D of the APS, an Office of Science user facility at Argonne National Laboratory. 

Read more on the APS website

Image: Fig. 1. NASICON crystal structure showing the tetrahedral P(4) phosphate motifs (purple), octahedral GeO6 motifs (cyan) and Na+ ions (green). Oxygen atoms are depicted in red.

Researchers discover foam “Fizzics”

Chemical engineers at the University of Illinois Chicago and UCLA used the U.S. Department of Energy’s Advanced Photon Source (APS) in answering longstanding questions about the underlying processes that determine the life cycle of liquid foams. The breakthrough in understanding how liquid foams dissipate could help improve the commercial production and application of foams in a broad range of industries and could lead to improved products. Findings of the research were featured in the Proceedings of the National Academy of Sciences of the United States of America.

Foams are a familiar phenomenon in everyday lives — mixing soaps and detergents into water when doing dishes, blowing bubbles out of soapy water toys, sipping the foam off a cup of lattes or milk shake. Liquid foams can occur in a variety of natural and artificial settings. While some foams are produced naturally, as in bodies of water creating large ocean blooms on the beaches, others arise in industrial processes. In oil recovery and fermentation, for example, foams are a byproduct.

Whenever soapy water is agitated, foams are formed. They are mostly gas pockets separated by thin liquid films that often contain tiny molecular aggregates called micelles. Oily dirt, for example, is washed away by hiding in the water-phobic cores of micelles. In addition, fat digestion in our bodies relies on the role of micelles formed by bile salts.

Over time, foams dissipate as liquid within the thin films is squeezed out. Soap and detergent molecules that are by very nature amphiphilic (hydrophilic and hydrophobic) aggregate within water to form spherical micelles, with their outward-facing heads being hydrophilic and water-phobic tails forming the core.

Read more on the ANL website

Image: Micellar foam films show grayscale intensity variations that correspond to rich nanoscopic topography mapped using IDIOM protocols.

Credit: Chrystian Ochoa and Vivek Sharma/UIC

Tiny Chip-Based Device Performs Ultrafast Manipulation of X-Rays

Researchers from the U.S. Department of Energy’s Advanced Photon Source (APS) and Center for Nanoscale Materials at Argonne National Laboratory have developed and demonstrated new x-ray optics that can be used to harness extremely fast pulses in a package that is significantly smaller and lighter than conventional devices used to manipulate x-rays. The new optics are based on microscopic chip-based devices known as microelectromechanical systems (MEMS).

“Our new ultrafast optics-on-a-chip is poised to enable x-ray research and applications that could have a broad impact on understanding fast-evolving chemical, material and biological processes,” said research team leader Jin Wang from the X-ray Science Division Time Resolved Research (TRR) Group at the APS. “This could aid in the development of more efficient solar cells and batteries, advanced computer storage materials and devices, and more effective drugs for fighting diseases.”

In new results published in The Optical Society OSA) journal Optics Express, the researchers demonstrated their new x-ray optics-on-a-chip device (Fig. 1), which measures about 250 micrometers and weighs just 3 micrograms, using the TRR Group’s 7-ID-C x-ray beamline at the APS. The tiny device performed 100 to 1,000 times faster than conventional x-ray optics, which that tend to be bulky.

Read more on the APS website

Image: Fig. 1. The photograph shows two MEMS elements on a single chip (A), with the active elements of 250 µm × 250 µm, and the micrograph (B) highlighting the size of the diffractive element, as compared to a section of human hair (C).

Strong and resilient synthetic tendons produced from hydrogels

Human tissues exhibit a remarkable range of properties. A human heart consists mostly of muscle that cyclically expands and contracts over a lifetime. Skin is soft and pliable while also being resilient and tough. And our tendons are highly elastic and strong and capable of repeatedly stretching thousands of times per day. While limited success has been achieved in producing man-made materials that can mimic some of the properties of natural tissues (for instance polymers used as synthetic skin for wound repair) scientists have failed to create artificial materials that can match all the outstanding features of tendons and many other natural tissues. An international team of researchers has transformed a standard hydrogel into an artificial tendon with properties that meet and even surpass those of natural tendons. This new material was examined via electron microscopy and x-ray scattering to reveal the microscopic structures responsible for its outstanding features. The x-ray measurements were gathered at the U.S. Department of Energy’s (DOE’s) Advanced Photon Source (APS). The researchers have shown that their new hydrogel-based material can be modified to mimic a variety of human tissues and could also potentially be adapted to non-biological roles. Their results were published in the journal Nature.

Read more on the APS website

Image: Fig. 1. SEM images (left) showing the deformation of the mesh-like nanofibril network during stretching and corresponding in situ SAXS patterns (right). Scale bars, 1 μm (SEM images); 0.025 Å−1 (SAXS images)

Credit: From M. Hua et al., Strong tough hydrogels via the synergy of freeze-casting and salting out,” Nature 590, 594 (25 February 2021). © 2021 Springer Nature Limited

Under wraps: X-rays reveal 1,900-year-old mummy’s secrets

Researchers used the powerful X-rays of the Advanced Photon Source to see the preserved remains of an ancient Egyptian girl without disturbing the linen wrappings. The results of those tests point to a new way to study mummified specimens.

The mummified remains of ancient Egyptians hold many secrets, from the condition of the bodies to the artifacts placed within the burial garments. Now a team of researchers has found a way to unwrap those secrets, without unraveling the mummies themselves.

Three years ago, researchers from Northwestern University, in preparation for an exhibit on campus, carefully transported a 1,900-year-old mummy to the Advanced Photon Source (APS), a U.S. Department of Energy (DOE) Office of Science User Facility at DOE’s Argonne National Laboratory. There scientists used powerful X-ray beams to peer inside the layers of linen and resin to examine the 2,000-year-old bones and objects buried within.

Read more on the Argonne National Laboratory website

Image: In 2017, Stuart Stock, center, of Northwestern University, talks with Rachel Sabino, right, of the Art Institute of Chicago while Argonne scientist Ali Mashayekhi, left, makes adjustments to the apparatus holding a 1,900-year-old Egyptian mummy.

Credit: Mark Lopez / Argonne National Laboratory.

A kappa diffractometer for intermediate X-ray energies at APS beamline 29-ID

An ultra-high vacuum, non-magnetic kappa geometry diffractometer has been designed and commissioned for the resonant soft x-ray scattering (RSXS) branch of the X-ray Science Division (XSD) Intermediate Energy X-ray (IEX) beamline 29-ID at the Advanced Photon Source (APS). Beamline 29-ID is managed by the XSD Magnetic Materials Group; the APS is an Office of Science user facility at Argonne National Laboratory. There were three main design goals for this diffractometer: kappa geometry, non-magnetic, and high-precision. The kappa geometry was chosen to allow for a large q-range and space for a sample environment (electric or magnetic fields). Non-magnetic components were used for all the components above and including the κ-arm to avoid disturbing magnetic or electric fields during experiments. Lastly, the diffractometer precision requirement of a sphere of confusion (SOC) of less than 50 µm was a key driving factor for this instrument in terms of rotation stages and machining precision.

The complete diffractometer can be seen in Fig. 1(a), shown installed into the RSXS UHV vacuum chamber at 29-ID. The precise SOC (< 50 µm) requirement drove the design method. In order to reach this goal, it was decided that a combination of precision machining, Finite element analysis, and stage precision would be used instead of calibrating an error-correction table. This has the advantage that the upper bound of the SOC requirement can be achieved without any control hardware, making the device more robust.

Read more on the Advanced Photon Source Website

Image: Fig1. (a) Image of the commissioned kappa diffractometer inside the RSXS vacuum chamber on the APS 29-ID beamline with the main components identified. (b) A close up model of the components above the f axis. The model also shows the new thermal break and thermal strap.

New state-of-the-art beamlines for the APS

The two new beamlines will be constructed as part of a comprehensive upgrade of the APS, enhancing its capabilities and maintaining its status as a world-leading facility for X-ray science.

In a socially distanced ceremony this morning at the U.S. Department of Energy’s (DOE) Argonne National Laboratory, leaders from DOE, Argonne and the University of Chicago broke ground on the future of X-ray science in the United States.

Today’s small gathering marked the start of construction on the Long Beamline Building, a new experiment hall that will house two new beamlines that will transport the ultrabright X-rays generated by the Advanced Photon Source (APS) to advanced scientific instruments. It will be built as part of the $815 million upgrade of the APS, a DOE Office of Science User Facility and one of the most productive light sources in the world. The APS, which is in essence a stadium-sized X-ray microscope, attracts more than 5,000 scientists from around the globe to conduct research each year in many fields ranging from chemistry to life sciences to materials science to geology.

Read more on the Argonne National Laboratory website

Image : Artist’s rendition of the Long Beamline Building. The new facility will be built as part of a major upgrade of the APS and will house two new beamlines.

Credit: HDR Architects

Scientists use pressure to make liquid magnetism breakthrough

It sounds like a riddle: What do you get if you take two small diamonds, put a small magneticcrystal between them and squeeze them together very slowly?

The answer is a magnetic liquid, which seems counterintuitive. Liquids become solids under pressure, but not generally the other way around. But this unusual pivotal discovery, unveiled by a team of researchers working at the Advanced Photon Source (APS), a U.S. Department of Energy (DOE) Office of Science User Facility at DOE’s Argonne National Laboratory, may provide scientists with new insight into high-temperature superconductivity and quantum computing.

Though scientists and engineers have been making use of superconducting materials for decades, the exact process by which high-temperature superconductors conduct electricity without resistance remains a quantum mechanical mystery. The telltale signs of a superconductor are a loss of resistance and a loss of magnetism. High-temperature superconductors can operate at temperatures above those of liquid nitrogen (−320 degrees Fahrenheit), making them attractive for lossless transmission lines in power grids and other applications in the energy sector.

Read more on the APS website

Image: APS

Argonne scientists fashion new class of X-ray detector

The original Argonne press release by Jared Sagoff can be read here.

Getting an X-ray at the dentist or the doctor is at best a little inconvenient and at worst a little risky, as radiation exposure has been linked to an increased risk of cancer. But researchers may have discovered a new way to generate precise X-ray images with a lower amount of exposure, thanks to an exciting set of materials that is generating a lot of interest.

Scientists at the U.S. Department of Energy’s (DOE) Argonne National Laboratory and Los Alamos National Laboratory have identified a new class of X-ray detectors based on layered perovskites, a semiconducting material also used in some other types of applications such as solar cells and light-emitting diodes. The detector with the new material is 100 times more sensitive than conventional, silicon-based X-ray detectors.

>Read more on the Advanced Photon Source website.

Image: Two-dimensional (2D) Ruddlesden-Popper phase layered perovskites (BA)2(MA)2Pb3I10 with three layers of inorganic octahedral slab and bulky organics as spacers.

Credit: Image by Dave Tsai/Los Alamos.

Crystals, lasers, glasses, and bent molecules: adventures in nonlinear optics

Light is an indispensable scientific tool. For example, laser-based optical sensors can detect oxygen in the environment, proteins in biomedical samples, and process markers in industrial settings, among other applications. However, not all wavelengths of light can be generated by a single laser, which limits what chemicals can be detected with optical sensing. That’s where nonlinear optical crystals can help. By shining multiple lasers with different wavelengths through such crystals, researchers can tune laser beams via frequency conversion and cover more of the optical spectra. This has been a successful approach for wavelengths from ultraviolet to near-infrared(IR), but the mid-IR region has lacked practical nonlinear optical crystals. However, crystals may not be the only game in town. A multi-institution international research team is exploring a possible solution to the crystal problem: cutting-edge glasses containing mercuric iodide. The idea is that these glasses could behave like nonlinear optical crystals, offering an enticing approach to the generation of novel amorphous optical materials. But first, the researchers needed to figure out what these glasses look like at the atomic scale. For that, they went to the U.S. Department of Energy’s (DOE’s) Advanced Photon Source (APS) to collect high-energy x-ray diffraction data. By combining the diffraction data with other structural data and computer modeling, the team uncovered the secrets behind how a glass can act like a crystal.

Nonlinear optical crystals are widely used in photonics applications, but can be challenging to synthesize. To sidestep the need for crystals, scientists have been pursuing glassy materials that can tune lasers. One challenge is that glassy materials with isotropic internal structures aren’t able to perform the frequency conversion necessary to tune lasers. However, glasses with chiral asymmetric properties have nonlinear optical potential. This research team is investigating hybrid molecular/network glasses with non-centrosymmetric mercuric iodide (HgI2).

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

Image: Schematic representation of second harmonic generation as light passes through bent HgI2 molecules adopting a non-random orientation within mesoscopic domains of sulfide glass.

Researchers find what makes chocolate melt in your mouth

Scientists use X-rays to see the true nature of chocolate.

The taste of a silky piece of rich chocolate is one of life’s great pleasures, and producing a smooth mouthfeel is an aspiration of every serious chocolatier.  The characteristics that truly set haute chocolate apart can be seen at the microscale thanks to recent, pivotal research performed by researchers from the University of Guelph at the Advanced Photon Source (APS) located at the U.S. Department of Energy’s (DOE) Argonne National Laboratory.

In a series of studies, University of Guelph researcher Fernanda Peyronel used a technique called ultra-small-angle x-ray scattering (USAXS) to investigate a property called fractal dimension, a particular feature of the geometric configuration of tiny particles of chocolate. “Basically, we’re trying to see whether these particles have a more open or a more closed structure and to correlate that to the mouthfeel experienced by consumers,” Peyronel said.

The USAXS technique allows scientists to resolve particles that range in size from a few hundred nanometers to around 10 micrometers — roughly the limit at which our taste buds can distinguish different textures. The beamline at the APS also accommodates detectors for small-angle x-ray scattering as well as large-angle x-ray scattering. These allow scientists to study their systems from less than a nanometer to around 10 micrometers.

>Read more on the APS at Argonne website

The active role of collagen in building bones

We use our skeleton every day, but our mental model of our bones may look more like a glow-in-the-dark Halloween costume, or a teaching skeleton hanging on a sitcom set, than true anatomy. While these common representations of skeletons focus on the sturdy aspects of bones, the structural frames of actual bones are built by a soft organic portion. To create bones, the human body precipitates calcium phosphate minerals using collagen, a long protein, as scaffolding. Our bodies mineralize calcium phosphate both inside and outside collagen-confined spaces, and scientists are still working to understand how the two types of mineralization occur. Recent research at the U.S. Department of Energy’s Advanced Photon Source (APS) has investigated mineralization rates and shown that collagen structures reduce the energy barriers to mineralization by providing a substrate on which the calcium phosphate can precipitate. Since common bone diseases, such as osteoporosis, hinge on an abnormal calcium phosphate precipitation process, this improved understanding of the role of collagen in precipitation could lead to insight into the treatment of these diseases.

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

Figure (extract, full image here) This scanning electron microscopy image shows calcium phosphate minerals nucleation in both extrafibrillar (purple colored image) and intrafibrillar (green colored image) spaces of collagen matrices. Without polyaspartic acid, extrafibrillar nucleation of calcium phosphate is dominant while with polyaspartic acid, intrafibrillar nucleation mainly occurs.