The Advanced Photon Source
a U.S. Department of Energy Office of Science User Facility

Structural Science (XSD-SRS)

Recent Research Highlights

A Crystal Mismatch Generates Magnetism
Thin films are ubiquitous in computer chips and other electronic devices. Researchers have recently begun tuning the properties of these films by growing them on substrates with different crystal structures. A particularly interesting case is the lanthanum-cobalt oxide, LaCoO3, or LCO for short. As a bulk crystal, LCO is not magnetic, but thin films of LCO grown on certain substrates exhibit ferromagnetic ordering. Previous attempts to explain this induced magnetism have been unable to incorporate the fact that the atomic arrangement, or crystal symmetry, of epitaxial LCO film is distinct from that of both its bulk phase and its substrates. This symmetry mismatch leads to additional structural distortions in LCO thin films, as observed in x-ray experiments performed at the U.S. Department of Energy’s Advanced Photon Source (APS) and elsewhere.
11-ID-D
Setting a New Course for Extracting Uranium from Seawater
Work by a team of researchers from Oak Ridge National Laboratory (ORNL) and The University of Chicago shows that the polymeric adsorbent materials that bind uranium behave nothing like scientists had believed. The results, detailed in a paper published in Energy & Environmental Science, highlight data made possible with x-ray absorption fine structure spectroscopy performed at the Materials Research Collaborative Access Team beamline 10-BM-B at the U.S. Department of Energy’s Advanced Photon Source (APS), as well as pair distribution function data collected at the X-ray Science Division beamline 11-ID-B, also at the APS, which is an Office of Science User Facility at Argonne National Laboratory.
11-ID-B
Crystals Could Reveal a New Spin on Quantum Physics
Crystals Could Reveal a New Spin on Quantum Physics: Physicists would like to know whether a theorized new state of matter, called a quantum spin liquid, actually exists. One multi-institution group of researchers, using the U.S. Department of Energy’s Advanced Photon Source at Argonne National Laboratory, thinks they may have found a rare state very similar to a quantum spin liquid.
11-BM-B, 15-ID-B,C,D
Composite Battery Boost
New composite materials based on selenium (Se) sulfides that act as the positive electrode in a rechargeable lithium-ion (Li-ion) battery could boost the range of electric vehicles by up to five times, according to groundbreaking research carried out at the U.S. Department of Energy’s Advanced Photon Source at Argonne National Laboratory. The studies of the materials demonstrated that they have the potential to pack five times the energy density of conventional batteries.
11-ID-C
Revealing Porous Materials’ Behavior under Pressure
X-ray experiments at the U.S. Department of Energy’s Advanced Photon Source could help researchers design valuable porous materials for high-pressure applications.
17-BM-B
Keeping Li-Ion Batteries from Fading Away
The rechargeable lithium-ion batteries in our smartphones, laptops, and various other personal electronic devices make them completely portable, allowing us to unplug so long as the batteries are charged. But rechargeable batteries don't last forever, and the more times they're recharged, the less energy they store.
11-ID-B
Gold Nanocrystal “Double” Hints at Other Shape-Changing Particles
Chemically the same, graphite and diamonds are as physically distinct as two minerals can be, one opaque and soft, the other translucent and hard. What makes them unique is their differing arrangement of carbon atoms. Polymorphs, or materials with the same composition but different structures, are common in bulk materials. Now a new study in Nature Communications that describes results from studies at synchrotron x-ray light sources, including two U.S. Department of Energy user research facilities, confirms they exist in nanomaterials, too.
11-ID-B
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, identified and characterized two niobium tungsten oxide materials that demonstrate much faster charging rates and power output than conventional lithium electrodes.
9-BM-B,C, 17-BM-B
The First Capture of Neon in an Organic Environment
In a new study, researchers from the Cambridge Crystallographic Data Centre (CCDC) and the U.S. Department of Energy’s (DOE’s) Argonne National Laboratory have teamed up to capture neon within a porous crystalline framework. Neon is well known for being the most unreactive element and is a key component in semiconductor manufacturing, but this is the first time neon has ever been studied within an organic or metal-organic framework. The results, which include critical studies at the Advanced Photon Source (APS), a DOE Office of Science user facility at Argonne, also point the way towards a more economical and greener industrial process for neon production.
17-BM-B
A New Family of Quasicrystals
Just as fishing experts know that casting a line in the right spot hooks the big catch, scientists from the U.S. Department of Energy Office of Science's (DOE-SC's) Ames Laboratory used an algorithm they developed, and the high-brightness x-ray beams from the DOE-SC's Argonne National Laboratory Advanced Photon Source to hone in on just the right spot for discovering a new family of rare-earth quasicrystals.
11-ID-C
Developing Protections against Chemical Warfare Agents
Chemical warfare agents that could be deployed against both soldiers and civilians have been a grave concern since World War I, when they were first used. Research on methods to defeat these weapons has been a focus of scientists since that time. Now, a multi-institution collaboration of scientists from U.S. federal research institutions and U.S. universities is studying how the use of zirconium (Zr)-based metal organic frameworks (MOFs) and niobium (Nb)-based polyoxometalates (POMs) may be effectively used in gas masks to capture and decompose dangerous chemical agents like Sarin, notably used in a subway terrorist attack in Japan in 1995.
17-BM-B
Cementing the Structure of CSHs
Portland cement concrete is all around us, in the sidewalks we walk on, the buildings we live and work in, and the roads our vehicles ride on. One of the most versatile and useful building materials ever created, it is so commonplace that we hardly ever think of it (unless we happen to trip and scrape our knees on it). Yet surprisingly, although we worry about carbon emissions from cars, airplanes, and power plants, this everyday, seemingly innocent material is also a hidden and largely ignored global warming culprit.
11-ID-C
Forging the Links to Building Better Metal Oxides
Metal oxides such as titanium dioxide (TiO2) are fascinating and versatile substances that can be used in many applications, including photovoltaic devices, batteries, and other vital technologies. But the utility of a particular material for a particular purpose may be limited, and common techniques to chemically "fine tune" their properties to fit specific parameters, such as doping or surface coating, are not always practical or effective. A group of researchers from a diverse set of institutions decided to try a different strategy by cross-linking metal oxide molecules with boron to create clusters of hybrid networks with new chemical and electrical properties and then characterizing the material at the U.S. Department of Energy’s Advanced Photon Source. Their work, which was published in Nature Materials, opens possibilities for the precise tailoring of such materials for specific purposes.
10-BM-A,B, 11-ID-B
A Step Toward Better “Beyond Lithium” Batteries
A step towards new, "beyond lithium" rechargeable batteries with superior performance has been made by a multi-institution, international collaboration of scientists who used a variety of research techniques and facilities including the U.S. Department of Energy’s Advanced Photon Source (APS) at Argonne National Laboratory. The research was published in the journal Nature Materials.
11-ID-B
Hints from Hemoglobin Lead to Better Carbon Monoxide Separation
Carbon monoxide (CO) is an insidious poison because it loves the iron in our blood; it pushes oxygen out of iron-based hemoglobin, leading to painful asphyxiation. This affinity for iron comes in handy in a newly created material that can absorb carbon monoxide far better than other materials, with potential applications in industrial processes like syngas production, where CO is a key player, and reactions where CO is an unwanted contaminant. A number of characterization and measurement techniques contributed to this groundbreaking research, including critical experiments at the U.S. Department of Energy’s Advanced Photon Source.
11-BM-B, 17-BM-B
A Gold Alloy with an Extra Electron
A novel gold compound with an “extra” electron compared to its chemical cousins is predicted to be a 3D Dirac semimetal, a relatively new class of electronic materials in which electrons behave as though they are massless, leading to high mobilities and unusual physics. The discovery, made at the U.S. Department of Energy’s Advanced Photon Source (APS), expands the search for possible thermoelectric materials (which make up Peltier coolers and thermoelectric generators) to include compounds with gold-gold bonds that stabilize "abnormal" electron counts. Such materials have very fast-moving electrons that could be used in circuits. Alternatively, these semimetals may have applications for solid-state cooling or heating.
11-BM-B
Water Adsorption in Metal-Organic Frameworks
Crystallographic evidence of the importance of water loading effects on a metal-organic framework that does not experience large-scale structural changes has been revealed by researchers using the U.S. Department of Energy’s Advanced Photon Source, with the potential for increasing their usefulness in important industrial and even medical applications.
15-ID-B,C,D, 17-BM-B
A Deeper Look into Bio-Inspired Catalysts
Developing hydrogen as a fuel is important for both economic and environmental reasons. This work carried out at the U.S. Department of Energy’s Advanced Photon Source advances our understanding of the charge-separation dynamics that occur in bio-inspired photocatalytic systems for the hydrogen evolution reaction.
9-BM-B,C, 11-ID-D
Faking Photosynthesis to Make Hydrogen Fuel
Humans can learn a lot from plants. With energy from the sun, protein catalysts in plants efficiently split water to generate oxygen, storing the energy as carbohydrates. Scientists would like to perform a similar trick, using solar energy to split water and produce hydrogen fuel. Hydrogen fuel burns clean, producing only water as a byproduct, but splitting water is not an efficient task for humans. Researchers have taken baby steps toward artificial photosynthesis, building solar-powered water-splitting catalysts in the laboratory, but so far these catalysts remain far less efficient than their vegetal counterparts. One reason it's difficult to improve catalytic efficiency is that scientists don't fully understand the catalysts’ water-splitting mechanism.
11-ID-D
Improving the Braids that Bind Uranium from Seawater
Nuclear power is one of the best ways currently available to supply clean, baseload electric power to the U.S. over the long term. But reserves of good uranium ore to fuel those plants are diminishing. By 2100 there will not be enough recoverable uranium left in terrestrial mines to meet the demands of existing power plants. However, if we cannot mine uranium on land, we may be able to sift it from the sea: The oceans contain huge reserves of uranium dissolved in seawater. State-of-the-art polymer fabrics soaked in seawater can recover 7 to 8 grams of uranium over a span of 30 days.
11-ID-B
A Strange Phenomenon that Helps and Hurts Lithium-Ion Battery Performance
New research offers the first complete picture of why a promising approach of stuffing more lithium into battery cathodes leads to their failure. A better understanding of this could be the key to smaller phone batteries and electric cars that drive farther between charges.
11-ID-B, 20-BM-B
Supercrystal: A Hidden Phase of Matter Created by a Burst of Light
"Frustration" plus a pulse of laser light resulted in a stable "supercrystal" created by a team of researchers from two U.S. universities and three U.S. Department of Energy national laboratories, including Argonne National Laboratory.
7-ID-B,C,D, 11-ID-D, 33-BM-C, 33-ID-D,E
Growing the Skinniest Magnets
Growing the Skinniest Magnets: Experiments performed at the U.S. Department of Energy’s Advanced Photon Source could lead to much smaller, more powerful computers and other magnetic devices.
17-BM-B
Disordered Crystals Are Promising for Future Battery Technology
Tiny, disordered particles of magnesium chromium oxide may hold the key to new magnesium battery energy storage technology, which could possess increased capacity compared to conventional lithium-ion batteries, find researchers who studied the material utilizing ultra-bright x-ray beams from the U.S. Department of Energy’s Advanced Photon Source.
4-ID-C, 10-BM-A,B, 11-ID-B
Custom-Built MOFs for Catalytic Enzyme Encapsulation
Metal-organic frameworks (MOFs) are handy crystalline constructs that combine metallic ions with organic molecules to form a structure featuring molecular “cages” or channels that can trap other atoms or molecules to filter, store, or otherwise separate them from the surrounding environment. One common potential use for MOFs is in catalysis, but the immobilization of enzymes is challenging because of leaching and aggregation that can decrease catalytic efficiency. With the help of structural studies performed at the U.S. Department of Energy’s Advanced Photon Source (APS), a group of experimenters has devised several new MOFs designed to encapsulate enzymes with high catalytic efficiency and recyclability. Their work was published in Nature Communications.
17-BM-B
For Lithium-Ion Cathodes, Partial Order Up
As the lithium-ion industry continues to grow, so does the use of cobalt or nickel, straining scarce metal resources. To sustain this continued growth, development of new cathodes with high energy densities made from Earth-abundant elements will be necessary. Users of the U.S. Department of Energy’s Advanced Photon Source report two new inexpensive lithium-ion cathode materials with extraordinary potential as cathodes in lithium-ion batteries.
11-ID-B, 20-BM-B
An Earth-Bound Amino Acid that May Be Common in Outer Space
Of the many amino acids essential for life, glycine has both the fewest number of atoms and the greatest known number of polymorphs (unique structural forms). Although scientists have long recognized that glycine displays multiple polymorphs, the exact structure of several of these forms has remained a mystery. Now a research team has uncovered the precise molecular arrangement of one of these mysterious structural phases, which they have dubbed glycine dihydrate, or GDH. The researchers deduced the structure of GDH by applying computational analysis to powder x-ray diffraction measurements collected at the U.S. Department of Energy’s Advanced Photon Source (APS) at Argonne National Laboratory.
17-BM-B
How Tantalum Clustering Leads to Charge Density Wave Lattice Distortions in 2H-TaSe2
Researchers using the U.S. Department of Energy’s Advanced Photon Source took a detailed look at high-temperature tantalum behavior to assess its role in potential future superconducting, optoelectronic, and ultrafast electronic devices.
1-ID-B,C,E, 11-ID-C
Unlocking Secrets of Nanoscale Crystal Formation
Highly intense x-ray beams and a clever experimental setup allowed researchers to watch a high-pressure, high-temperature chemical reaction to determine for the first time what controls formation of two different nanoscale crystalline structures in the metal cobalt. The technique, employed at two U.S. Department of Energy x-ray light sources, including the Advanced Photon Source, allowed continuous study of cobalt nanoparticles as they grew from clusters including 10s of atoms, to crystals as large as 5 nanometers. The research provides the proof-of-principle for a new technique to study crystal formation in real time, with potential applications for other materials, including alloys and oxides.
17-BM-B
Newly-Discovered Semiconductor Dynamics May Help Improve Energy Efficiency
Researchers utilizing intense x-ray beams from the U.S. Department of Energy’s Advanced Photon Source (APS) examined the flow of electricity through semiconductors and uncovered another reason these materials seem to lose their ability to carry a charge as they become more densely “doped.” Their results, which may help engineers design faster semiconductors in the future, were published online in the journal ACS Nano.
10-ID-B, 11-ID-D, 12-ID-B
Mix and Match MOF
Inexpensive materials called MOFs, for metal-organic frameworks, pull gases out of air or other mixed gas streams, but fail to do so with oxygen. Now, a team that includes researchers from two U.S. Department of Energy (DOE) national laboratories has overcome this limitation by creating a composite of a MOF and a helper molecule in which the two work in concert to separate oxygen from other gases simply and cheaply. The results, achieved with an assist from the DOE’s Advanced Photon Source (APS) at Argonne, might help with a wide variety of applications, including making pure oxygen for fuel cells, using that oxygen in a fuel cell, removing oxygen in food packaging, making oxygen sensors, or for other industrial processes. The technique might also be used with gases other than oxygen as well by switching out the helper molecule.
11-ID-B
Putting the Heat on an Additive-Manufactured Alloy
As the techniques of additive manufacturing (AM), more popularly known as “3-D printing,” become ever more versatile and applicable for diverse purposes, they sometimes pose unique challenges that are not present with more traditional manufacturing methods. In additive-manufactured metals and alloys, such problems can result in microstructural defects that lead to reduced strength and stress resistance, an issue commonly addressed by post-build heat treatment. But this approach can also have undesirable side effects. Researchers from the National Institute of Standards and Technology used the U.S. Department of Energy’s Advanced Photon Source to examine the AM alloy Inconel 625 (IN625) in an effort to better understand the effects of heat treatment on AM alloy microstructure and phase evolution.
9-ID-B,C, 11-BM-B
Cooking Up New Nanoribbons to Make Better White LEDs
As the world moves away from incandescent light bulbs, light-emitting diodes (LEDs) are growing in popularity. They use significantly less energy and have far longer lifetimes than do the traditional incandescent bulbs, which are being phased out, and they don't contain mercury, as do compact fluorescents. LEDs do have a drawback, however. The phosphors that convert the single color produced by an LED into white light tend to produce a cool, bluish glow instead of the warmer, yellower color most people prefer.
11-BM-B
Hints from Hemoglobin Lead to Better Carbon Monoxide Separation
Carbon monoxide (CO) is an insidious poison because it loves the iron in our blood; it pushes oxygen out of iron-based hemoglobin, leading to painful asphyxiation. This affinity for iron comes in handy in a newly created material that can absorb carbon monoxide far better than other materials, with potential applications in industrial processes like syngas production, where CO is a key player, and reactions where CO is an unwanted contaminant. A number of characterization and measurement techniques contributed to this groundbreaking research, including critical experiments at the U.S. Department of Energy’s Advanced Photon Source.
11-BM-B, 17-BM-B

Overview

High-energy X-ray diffraction (XRD) is a bulk structure characterization technique widely used in materials research taking advantage of the high penetration power into material, large accessible q-range, and small correction factors. In situ measurements study materials under various conditions. Operando studies are essential for the insight of structural change in functional materials during operation to improve their performance. XRD can resolve phase identities and other features, like particle size, microstrain, structural defects, etc. The beamlines operated by the Structural Science (SRS) group offer a wide range of in situ and operando powder XRD and total scattering measurement capabilities with sub-second temporal resolution. The beamlines operate in x-ray transmission geometry with monochromatic beams and area detectors, and in the case of 11-BM with an array of analyzer crystals and scintillators for highest resolution. Most recent developments include an in-line Raman system at 17-BM that allows simultaneous measurement of XRD/PDF and Raman spectroscopy data under controlled temperature and gas environments. 11-ID-B enables studies of surfaces and interfaces with an optional line focusing of a few micrometers in beam height.  11-ID-B utilizes a hexapod to allow highly accurate control of specimen orientation, enabling surface and interface scattering. 11-ID-C employs a heavy-load hexapod stage providing similar capabilities for heavy equipment up to 250 kg. The high-resolution 11-BM beamline now has the option to switch to an area detector for rapid checks on the sample status. The group has a strong emphasis on battery research, and maintains an electrochemistry facility which is accessible 24/7 for all APS users for cell preparation. This eChem Lab offers standard lab equipment plus two Argon atmosphere glove boxes with one dedicated for Sulphur containing materials.

11-BM, 11-ID-B and 17-BM all offer Mail In services.

11-BM
11-BM is dedicated to high-resolution powder diffraction measurements. The instrument operates over the energy range from 25-35 keV, and combines a sagittally focused monochromator with multiple Si crystal analyzers to achieve exceptional resolution and sensitivity. The beamline offers a unique mail-in service for rapid access, and supports on-site user experiments for non-routine powder diffraction measurements. Technical Specifications
11-ID-B

11-ID-B is dedicated to Pair-Distribution-Function (PDF) measurements with area detectors. The instrument operates at high X-ray energies (58.6 keV, 86.7 keV) and is optimized for High throughput measurements and non-ambient / in-situ measurements. Typical configurations may involve a sample changer, cryostream, compact furnace/flow cell, and single-crystal diffuse scattering (under development).

Now accepting Mail In proposals. More information can be found on the mail-in wiki.

 Technical Specifications
11-ID-C
11-ID-C is used for scattering studies at extreme conditions. The high energy X-ray beam (105.7 keV) is highly penetrating and allows a wide coverage of reciprocal space over a small angular scattering range. This is particularly advantageous for experiments that require bulky sample environments (e.g. magnets, cryostats, levitator). Technical Specifications
17-BM-B

17-BM-B is dedicated to rapid acquisition powder diffraction experiments using an area detector, where moderate resolution data can be obtained in fractions of seconds. The versatile set-up can accommodate a wide range of sample environments and is well suited to parametric/in situ/in operando measurements. Standard configurations include a sample changer, cryostream, compact furnace/flow cell, compact pressure cells (<10 GPa, under development). 

Now accepting Mail In proposals. More information can be found on the mail-in wiki.

 Technical Specifications
eChem Lab
The eChem lab is equipped with a state-of-the-art Ar-atmosphere glovebox with fridge/freezer unit, and small and large antechambers. The glovebox is supplied with Li and Na metals, standard electrolytes, coin cell crimping tools and accessories needed to assemble battery cells.  The lab is also equipped with three mobile 8-channel MACCOR® battery cyclers capable of running independent experiments, a single-channel CH Instruments® potentiostat, a vacuum oven, balances, bench space and standard laboratory consumables. Details

 

03.18.2020