X-ray imaging of gigahertz ferroelectric domain dynamics

2018/03/062018/03/12

A team of researchers has made an important advance in broadening our understanding of light-induced mesoscale dynamics using the U.S. Department of Energy’s Advanced Photon Source (APS) at Argonne National Laboratory. Time-resolved x-ray diffraction microscopy, aided by a newly developed dynamical phase-field method (DPFM), revealed how lattice waves can be excited by light pulses and the resulting local structural changes among mesoscopic domains in ferroelectrics, a widely utilized material for sensors, nanoscale positioners, and information storage devices.

Light interaction with matter offers a new way of controlling material properties by harnessing energy transport and conversion in functional materials without contact on ultrafast time scales. However, the desired dynamical control is complicated by the inhomogeneous response of real materials. The ultrafast dynamics depend not only on the intrinsic properties of the compound but also, strongly, on mesoscale structures such as surfaces, domains, interfaces, and defects that govern the coupling between various degrees of freedom.

Figure: Schematic illustration of spatially-resolved pump-probe experiment and domain configuration of a BaTiO3 single crystal sample. The inset shows a unit cell of BaTiO3.

Examining the crystallisation during additive biomanufacturing

2018/03/052018/03/07

A research group from the University of Manchester has used wide-angle X-ray diffraction (XRD) in one of the first studies to investigate the evolution of crystallinity and crystal orientation in polycaprolactone (PCL) during 3D printing.

The team has developed a new extrusion-based printing machine, the Plasma-assisted Bioextrusion System (PABS). Extrusion-based techniques are widely used due to their versatility and simplicity, and their ability to print a range of materials in a cell-friendly environment, with high precision. PABS uses a novel approach for biomanufacturing and tissue engineering, combining screw-assisted extrusion, pressure-assisted extrusion and plasma jetting.

Figure: Conceptual material transition from extrusion-based filament printing to the partial replacement of a knee joint via 3D scaffolding.
Credit: Fengyuan Liu, Wajira Mirihanage, Paulo Bartolo, Medical Engineering Research Centre, the University of Manchester

The microstructure of a parrotfish tooth contributes to its toughness

2018/02/082018/02/15

During a 2012 visit to the Great Barrier Reef off the coast of Australia, ALS staff scientist Matthew Marcus became intrigued with parrotfish. “I was reminded that this is a fish that crunches up coral all day and is responsible for much of the white sand on beaches,” Marcus said. “But how can this fish eat coral and not lose its teeth?” So Marcus teamed up with Pupa Gilbert, a biophysicist at the University of Wisconsin–Madison, and an international team of researchers she assembled, to understand how parrotfish teeth work.

Because conventional microscopes can overlook the unique orientation of crystals in tooth enamel, the team used the technique called polarization-dependent imaging contrast (PIC) mapping that Gilbert invented, which uses the photoemission electron microscopy (PEEM) Beamline 11.0.1 at the ALS. The PIC maps allowed them to visualize the orientation of individual crystals of fluorapatite, the main mineral component of parrotfish teeth.

Separate experiments used tomography (Beamline 8.3.2) and microdiffraction (Beamline 12.3.2) to further analyze the crystal orientations and strains in the teeth.

>Read more on the ALS website

Image: (extract) PIC maps acquired at the tips of four different parrotfish teeth show that they consist of 100-nm-wide, microns-long crystals, bundled into “fibers” interwoven like warp and weft fibers in fabric. These fibers gradually decrease in average diameter from 5 μm at the back of a tooth to 2 μm at the tip. Intriguingly, this decrease in size is spatially correlated with an increase in hardness and stiffness. The orientation angle of the crystals is color-coded (chart at bottom).

Scientists observe nanowires as they grow

2018/02/082018/02/22

X-ray experiments reveal exact details of self-catalysed growth for the first time

At DESY’s X-ray source PETRA III, scientists have followed the growth of tiny wires of gallium arsenide live. Their observations reveal exact details of the growth process responsible for the evolving shape and crystal structure of the crystalline nanowires. The findings also provide new approaches to tailoring nanowires with desired properties for specific applications. The scientists, headed by Philipp Schroth of the University of Siegen and the Karlsruhe Institute of Technology (KIT), present their findings in the journal Nano Letters. The semiconductor gallium arsenide (GaAs) is widely used, for instance in infrared remote controls, the high-frequency components of mobile phones and for converting electrical signals into light for fibre optical transmission, as well as in solar panels for deployment in spacecraft.

To fabricate the wires, the scientists employed a procedure known as the self-catalysed Vapour-Liquid-Solid (VLS) method, in which tiny droplets of liquid gallium are first deposited on a silicon crystal at a temperature of around 600 degrees Celsius. Beams of gallium atoms and arsenic molecules are then directed at the wafer, where they are adsorpted and dissolve in the gallium droplets. After some time, the crystalline nanowires begin to form below the droplets, whereby the droplets are gradually pushed upwards. In this process, the gallium droplets act as catalysts for the longitudinal growth of the wires. “Although this process is already quite well established, it has not been possible until now to specifically control the crystal structure of the nanowires produced by it. To achieve this, we first need to understand the details of how the wires grow,” emphasises co-author Ludwig Feigl from KIT.

Image: A single nanowire, crowned by a gallium droplet, as seen with the scanning electron microscope (SEM) of the DESY NanoLab.
Credit: DESY, Thomas Keller

Liquid crystal molecules form nano rings

2018/02/062018/02/07

Quantised self-assembly enables design of materials with novel properties

At DESY’s X-ray source PETRA III, scientists have investigated an intriguing form of self-assembly in liquid crystals: When the liquid crystals are filled into cylindrical nanopores and heated, their molecules form ordered rings as they cool – a condition that otherwise does not naturally occur in the material. This behavior allows nanomaterials with new optical and electrical properties, as the team led by Patrick Huber from Hamburg University of Technology (TUHH) reports in the journal Physical Review Letters.

The scientists had studied a special form of liquid crystals that are composed of disc-shaped molecules called discotic liquid crystals. In these materials, the disk molecules can form high, electrically conductive pillars by themselves, stacking up like coins. The researchers filled discotic liquid crystals in nanopores in a silicate glass. The cylindrical pores had a diameter of only 17 nanometers (millionths of a millimeter) and a depth of 0.36 millimeters.

There, the liquid crystals were heated to around 100 degrees Celsius and then cooled slowly. The initially disorganised disk molecules formed concentric rings arranged like round curved columns. Starting from the edge of the pore, one ring after the other gradually formed with decreasing temperature until at about 70 degrees Celsius the entire cross section of the pore was filled with concentric rings. Upon reheating, the rings gradually disappeared again.

Image: Stepwise self-organisation of the cooling liquid crystals. (Extract, see the entire image here)
Credit: A. Zantop/M. Mazza/K. Sentker/P. Huber, Max-Planck Institut für Dynamik und Selbstorganisation/Technische Universität Hamburg; Quantized Self-Assembly of Discotic Rings in a Liquid Crystal Confined in Nanopores, Physical Review Letters, 2018; CC BY 4.

ID23-EH2: Gearing up for serial crystallography

2018/01/292018/02/01

ID23-EH2 is up and running, catering to small samples and serial crystallography experiments. Its small beam and unique diffractometer are the trademarks of this new MX beamline.

“This is amazing”, says David Drew, a user from Stockholm University, on the new ID23-EH2. “There is a perfect beam line to be screening LCP crystals. After 5 years working on this… it is amazing to be able to speed up finding the best spot to collect”, he adds. Drew and his team are on ID23-EH2. They are the first users since ID23-EH2 opened for business this month and have just started the experiment. He works with his team in transport proteins, which carry nutrients across membrane proteins and are important drug targets.

>Read more on the ESRF website

Picture: Max Nanao with the users from the University of Stockholm (Sweden).

2017 ANSTO, Australian Synchrotron Stephen Wilkins Medal awarded

2017/11/272017/12/07

Leonie van ‘t Hag has been awarded the Australian Synchrotron S. Wilkins Medal for her PhD thesis

The award recognises her research to improve the method to crystallise proteins and peptides in order to study their structure, using a technique called crystallography. “Leonie’s insights into crystallisation processes could significantly help the development of treatments for a variety of illnesses,” said Australian Synchrotron Director, Professor Andrew Peele.

Most solid material in the world is made of crystalline structures. Crystals are made up of rows and rows of atoms or molecules stacked up like boxes in a warehouse, in different arrangements.

The science of determining these atomic or molecular structures from crystalline materials is called crystallography.

X-Rays reveal the biting truth about parrotfish teeth

2017/11/152017/11/29

Interwoven crystal structure is key to coral-crunching ability

So, you thought the fictional people-eating great white shark in the film “Jaws” had a powerful bite. But don’t overlook the mighty mouth of the parrotfish – its hardy teeth allow it to chomp on coral all day long, ultimately chewing and grinding it up through digestion into fine sand. That’s right: Its “beak” creates beaches. A single parrotfish can produce hundreds of pounds of sand each year.

Now, a study by scientists – including those at the Department of Energy’s Lawrence Berkeley National Laboratory (Berkeley Lab) – has revealed a chain mail-like woven microstructure that gives parrotfish teeth their remarkable bite and resilience.

The natural structure they observed also provides a blueprint for creating ultra-durable synthetic materials that could be useful for mechanical components in electronics, and in other devices that undergo repetitive movement, abrasion, and contact stress.

Matthew Marcus, a staff scientist working at Berkeley Lab’s Advanced Light Source (ALS) – an X-ray source known as a synchrotron light source that was integral in the parrotfish study – became intrigued with parrotfish during a 2012 visit to the Great Barrier Reef off of the coast of Australia.

>Read More on the ALS website

Image: Scientists studied the microstructure of the coral-chomping teeth of the steephead parrotfish, pictured here, to learn about the fish’s powerful bite.
Credit: Alex The Reef Fish Geek/Nautilus Scuba Club, Cairns, Australia

New insights about malaria parasites infection mechanisms

2017/10/042017/10/26

Unraveled details about how the malaria parasite acts after invading the red blood cells.

This highlight has been possible thanks to two advanced microscope techniques combination: X-ray fluorescence microscopy and soft X-rays tomography, this one conducted in ALBA Synchrotron. Infected red blood cells image analysis offer new information that could yield new drugs design against malaria, an illness that claims over 400.000 lives each year.

Plasmodium falciparum causes the malaria disease. This parasite, transmitted through mosquito sting, infects red blood cells of its victim. Once inside, it uses hemoglobin (the protein in charge of oxygen transport) as a nutrient. When it is digested, iron is released in a form of heme molecules. These heme molecules are toxic to the parasite, but it has a strategy to make them harmless: it packs heme in pairs and finally they are packed forming hemozoin crystals. In this way, poisonous iron is locked up and no longer will be a threat for the parasite.

>Read More on the ALBA website

Infographic: Model for biochemistry processes that occur inside the parasite. The parasite takes the hemoglobin from the red blood cell (RBC)
1 and digests it inside the digestive vacuole (DV)
2. as a consequence, heme groups are released
3. and HDP protein packages them in pairs (heme dimers)
4. finally, in the crystallization process these dimers are converted in hemozoin crystals
5. blue arrow points out the suggested feedback mechanism that regulates hemoglobin degradation.

Focusing on microbeam: Initial installment of CRLs at CHESS

2017/08/142017/10/16

A great challenge is to direct x-rays into a very small, very clean footprint while maintaining high photon flux.

A great challenge at many x-ray beamlines is to direct x-rays into a very small, very clean footprint while maintaining high photon flux. This is especially important when illuminating very small samples, as in protein microcrystallography where crystals can be on the order of a micron across and diffract weakly compared to larger crystals. Any excess scatter in these conditions will contribute unwanted noise and decrease the overall signal-to-noise ratio – an important measure of data quality. Consider an experiment where you first must take the water from a firehose and somehow get a water thread thinner than a human hair without any mist! That is akin to the scale of creating x-ray microbeam at CHESS.

One solution would be to simply block the x-rays down to the size desired, but this has the unfortunate side effect of throwing away vast numbers of photons. Fortunately, x-rays can be manipulated similar to visual light and therefore focused using optical components such as mirrors and lenses. Recently, an optical design of interest at CHESS incorporates the focusing power of x-ray compound refractive lenses (CRLs) to create an x-ray beam on the order of microns across – effectively, a microbeam.

>Read More

Picture: The assembled and aligned lenses in their casing. Two brass pinholes bookend the stack of lenses, which all sit in a v-groove designed to be sub-micrometer in accuracy.

Great experience at BioMAX

2017/06/302018/01/17

“It was a fantastic experience”, Jette Sandholm Kastrup.

On June 30, 2017 Professor Jette Sandholm Kastrup, University of Copenhagen was granted two shifts of beamtime at BioMAX by the Program Advisory Committee (PAC) and the MAX IV Laboratory Management for the project “Molecular recognition of agonists, antagonists and positive allosteric modulators at ionotropic glutamate receptors”.

The ionotropic glutamate receptors (iGluRs) are highly abundant in the central nervous system (CNS) and mediate fast synaptic neurotransmission. Dysfunction of the glutamatergic system has been associated with various diseases in the CNS, e.g. depression, Parkinson’s and Alzheimer’s diseases and epilepsy. The iGluRs are for example considered an attractive and appropriate target for the discovery of cognitive enhancers.

>Read More

X-ray experiments reveal two different types of water

2017/06/262017/10/09

The strangest liquid of all is even more unusual than we thought

Liquid water exists in two different forms – at least at very low temperatures. This is the conclusion drawn from X-ray experiments carried out at DESY and at the Argonne National Laboratory in the US. An international team of researchers headed by the University of Stockholm now reports its findings in the Proceedings of the National Academy of Sciences (PNAS).

The scientists led by Anders Nilsson had been studying so-called amorphous ice. This glass-like form of frozen water has been known for decades. It is quite rare on earth and does not occur in everyday life; however, most water ice in the solar system actually exists in this amorphous form. Instead of forming a solid crystal – as in an ice cube taken from the freezer – the ice takes on the form of disordered chains of molecules, more akin to the internal structure of glass. Amorphous ice can be produced, for example, by cooling liquid water so rapidly that the molecules do not have enough time to form a crystal lattice.

>Read More

Picture: Liquid water has two variants: High Density Liquid (HDL) and Low Density Liquid (LDL) which have now been observed at extremely low temperatures, but can not be bottled. Photo: Gesine Born, DESY

Liquid-phase chemistry: Graphene nanobubbles

2017/04/072017/10/09

X-Ray Photoelectron Spectroscopy (XPS) and X-Ray Absorption Spectroscopy (XAS) provide unique knowledge on the electronic structure and chemical properties of materials.

Unfortunately this information is scarce when investigating solid/liquid interfaces, chemical or photochemical reactions in ambient conditions because of the short electron inelastic mean free path (IMFP) that requires a vacuum environment, which poses serious limitation on the application of XPS and XAS to samples operating in atmosphere or in the presence of a solvent. One promising approach to enable the use of conventional electron spectroscopies is the use of thin membrane, such as graphene (Gr), which is transparent to both X-ray photons and photoelectrons. For these purposes, this work proposes an innovative system based on sealed Gr nanobubbles (GNBs) on a titanium dioxide TiO₂ (100) rutile single crystal filled with the solution of interest during the fabrication stage (Figure 1a).

The formation of irregularly shaped vesicles with an average height of 6 nm and lateral size of a few hundreds of nanometers was proved by using a multi-technique approach involving Atomic Force Microscopy (AFM, see Figure 1b,c,d), Raman (Figure 1e) and synchrotron radiation spectroscopies (Figure 2), which have unequivocally demonstrated the presence of water inside the GNBs and the transition to a flat Gr layer after water evaporation by thermal heating up to 350 °C in ultra high vacuum (UHV).

>Read More