MYSTIIC at BESSY II: New X-ray microscope put into operation
The first image taken by MYSTIIC: a standard image used to calibrate and measure the resolution of the new STXM. © HZB
The pictures below illustrate the capabilities of correlative in situ microscopy, using the example of (Mo,V,Te,Nb)Ox - a catalyst. This figure shows NEXAFS-TXM at U41 in different gas atmospheres, the data show changes in the electronic states of the elements involved. © C.Pratsch/HZB ; T. Lunkenbein/FHI
Correlative microscopy images of the same sample site within the transmission electron microscope (TEM). © K. Dembélé/FHI
The same sample under a full-field transmission X-ray microscope TXM at the U41 beamline at BESSY II, HZB) in a gas atmosphere. © C. Pratsch/HZB
A new X-ray microscope has started operation at the Energy Materials in situ Lab (EMIL). It is a scanning transmission X-ray microscope designed to examine both sample surfaces and bulk sample. With the soft X-ray light from BESSY II, it is even possible to localise individual elements and chemical compounds; the spatial resolution is below 20 nanometres.
The Energy Materials in situ Lab (EMIL) is directly connected to two beamlines at BESSY II, which provide intense synchrotron radiation for research. One beamline provides hard X-rays, the other soft X-rays for the experiments at EMIL. EMIL is operated jointly by HZB and the Max Planck Society (MPG) . Now, an HZB team has set up a new scanning transmission X-ray microscope (STXM) at the soft X-ray beamline in the BESSY II experimental hall. It was named MYSTIIC - Microscope for x-raY Scanning Transmission In-situ Imaging of Catalysts.
Higher precision and more options
Compared to other X-ray microscopes, the STXM MYSTIIC at EMIL offers even higher precision and more options for scanning surfaces and investigating bulk samples in transmission. In particular, MYSTIIC will also allow to observe chemical processes in gas/liquid cells in the future. "It is like filming the processes taking place during catalysis," says HZB expert Dr Markus Weigand, who is in charge of the instrument. The implementation of a gas mixing system, which is being developed together with the AC department of the Fritz Haber Institute (FHI) of the Max Planck Society, is currently in progress in order to analyse how different gases (for example CO2, CH4, H2 etc.) chemically change the surface of a catalyst on the nanoscale. The new microscope will thus contribute significantly to CatLab's approach on knowledge and understanding in order to develop novel catalyst.
Testing the instrument with friendly users
"Initially, we want to test the instrument with HZB teams or users we know (friendly users)," explains Weigand. For example, HZB researcher Dr Tristan Petit will be the first to investigate so-called MXenes with MYSTIIC. MXenes can absorb and store large amounts of electrical energy very fast. "We want to scan the surfaces of MXene particles with MYSTIIC and find out which elements are involved in certain chemical processes. This will help us to better understand the amazing properties of this class of materials," Petit explains. He and his team are currently preparing the installation of special sample cells for investigations on catalysis, electrochemistry and electrocatalysis. Sample heating up to 1000 °C is also planned. In the future, routines will be developed in collaboration with the FHI that will make it possible to use the same cells for electron microscopy studies in order to combine energy and spatial resolution on the same sample.
Upgrades in mind
The instrument is designed with upgrades to expand capabilities in mind, which will include advanced operando cells and x-ray cameras systems to enable resolving structures of even a few nanometres using ptychographic methods.
MYSTIIC: Energy materials and environmental sciences
Up to now, there have been two X-ray microscopes at BESSY II with very different purposes. Another STXM (MAXYMUS), operated by MPI-IS, focuses on magnetism and time resolution. Nanoscale NEXAFS* spectromicroscopy of energy materials (see examples below) and tomography – for example of shock frozen cells - in the soft and tender X-ray regime can be examined in Prof. Dr. Gerd Schneider's group. MYSTIIC at EMIL is particularly suitable for resolving questions related to energy materials research and environmental sciences.
External users are invited to apply for beam time at MYSTIIC at EMIL from the first call for 2022.
*NEXAFS: Near Edge X-ray Absorption Fine Structure.
- What Zinc concentration in teeth revealsTeeth are composites of mineral and protein, with a bulk of bony dentin that is highly porous. This structure is allows teeth to be both strong and sensitive. Besides calcium and phosphate, teeth contain trace elements such as zinc. Using complementary microscopy imaging techniques, a team from Charité Berlin, TU Berlin and HZB has quantified the distribution of natural zinc along and across teeth in 3 dimensions. The team found that, as porosity in dentine increases towards the pulp, zinc concentration increases 5~10 fold. These results help to understand the influence of widely-used zinc-containing biomaterials (e.g. filling) and could inspire improvements in dental medicine.
- Fascinating archaeological find becomes a source of knowledgeThe Bavarian State Office for the Preservation of Historical Monuments (BLfD) has sent a rare artefact from the Middle Bronze Age to Berlin for examination using cutting-edge, non-destructive methods. It is a 3,400-year-old bronze sword, unearthed during archaeological excavations in Nördlingen, Swabia, in 2023. Experts have been able to determine how the hilt and blade are connected, as well as how the rare and well-preserved decorations on the pommel were made. This has provided valuable insight into the craft techniques employed in southern Germany during the Bronze Age. The BLfD used 3D computed tomography and X-ray diffraction to analyse internal stresses at the Helmholtz-Zentrum Berlin (HZB), as well as X-ray fluorescence spectroscopy at a BESSY II beamline supervised by the Bundesanstalt für Materialforschung und -prüfung (BAM).
- Element cobalt exhibits surprising propertiesThe element cobalt is considered a typical ferromagnet with no further secrets. However, an international team led by HZB researcher Dr. Jaime Sánchez-Barriga has now uncovered complex topological features in its electronic structure. Spin-resolved measurements of the band structure (spin-ARPES) at BESSY II revealed entangled energy bands that cross each other along extended paths in specific crystallographic directions, even at room temperature. As a result, cobalt can be considered as a highly tunable and unexpectedly rich topological platform, opening new perspectives for exploiting magnetic topological states in future information technologies.