LiXEdrom: Innovative measuring chamber for X-ray study of liquid jets
Close-up of the liquid-jet.
Schematic drawing of the LiXEdrom setup for X-ray
absorption and X-ray emission
spectroscopy on the liquid-jet
Until now, the only way to study liquids by soft X-ray emission spectroscopy (XES) has been through a membrane window. Now, researchers of Helmholtz-Zentrum Berlin have carried out an XES study of a free micro-liquid jet on the synchrotron.
X-rays are the medium of choice for many scientific studies. When you shine them on a sample, they literally shed light on the material’s structure, providing loads of information about it. Unfortunately, this mostly applies to solids only, since the sample has to be in a vacuum for the entire time it is being irradiated with soft X-rays. For liquids, that means you have to remove all the water. In the case of biological samples such as proteins, however, this destroys their natural environment. The solution to this problems has always been to measure liquids through membranes. These membranes keep the evacuated side separate from the non-evacuated side. The trouble is, one can never really be sure whether or not membrane effects are distorting the measurement results.
At Helmholtz-Zentrum Berlin (HZB), Emad Aziz, head of a junior research group, has shown that liquids can be investigated by X-ray emission spectroscopy without using membranes after all. At the synchrotron source BESSY II, the group has built a special setup – the LiXEdrom. It is unique in that the liquid is shot as a jet through the X-ray beam. The jet from the nozzle becomes so thin and, at 80 metres per second, so fast that the vacuum can be maintained without the need of a membrane.
“On our LiXEdrom, we create a vacuum in the liquid chamber of up to 10-6 millibar, and can now perform both absorption and emission measurements, giving us even more precise information about the structure of a material,” says Emad Aziz. It also allows a clear “view” of elements that possess absorption and emission energies similar to the energies of the membrane materials, and would therefore overlap with the membrane in the spectrum when measured. This concerns above all carbon and nitrogen – precisely those elements of interest in biological samples.
In their first measurements, published in Chemical Physics (DOI: 10.1016/JChemPhys.2010.08.023) and selected for the cover, the group demonstrated they can achieve energy resolutions on their LiXEdrom comparable to those of the latest high resolution XES spectrometers. For water, they have proven that results obtained from an earlier setup were not overlapped by disturbing membrane effects. They have also studied the electronic structure of nickel ions, unhampered by a risk of deposits on a membrane wall distorting the results. For many applications such as protein studies, this is a significant step towards obtaining reliable structural information.
Original paper in Chem. Phys., DOI 10.1016/JChemPhys.2010.08.023
„High Resolution X-ray Emission Spectroscopy of Water and Aqueous Ions Using the Micro-Jet Technique”, K.M. Lange et al.
- Battery research with the HZB X-ray microscopeNew cathode materials are being developed to further increase the capacity of lithium batteries. Multilayer lithium-rich transition metal oxides (LRTMOs) offer particularly high energy density. However, their capacity decreases with each charging cycle due to structural and chemical changes. Using X-ray methods at BESSY II, teams from several Chinese research institutions have now investigated these changes for the first time with highest precision: at the unique X-ray microscope, they were able to observe morphological and structural developments on the nanometre scale and also clarify chemical changes.
- BESSY II: New procedure for better thermoplasticsBio-based thermoplastics are produced from renewable organic materials and can be recycled after use. Their resilience can be improved by blending bio-based thermoplastics with other thermoplastics. However, the interface between the materials in these blends sometimes requires enhancement to achieve optimal properties. A team from the Eindhoven University of Technology in the Netherlands has now investigated at BESSY II how a new process enables thermoplastic blends with a high interfacial strength to be made from two base materials: Images taken at the new nano station of the IRIS beamline showed that nanocrystalline layers form during the process, which increase material performance.
- Hydrogen: Breakthrough in alkaline membrane electrolysersA team from the Technical University of Berlin, HZB, IMTEK (University of Freiburg) and Siemens Energy has developed a highly efficient alkaline membrane electrolyser that approaches the performance of established PEM electrolysers. What makes this achievement remarkable is the use of inexpensive nickel compounds for the anode catalyst, replacing costly and rare iridium. At BESSY II, the team was able to elucidate the catalytic processes in detail using operando measurements, and a theory team (USA, Singapore) provided a consistent molecular description. In Freiburg, prototype cells were built using a new coating process and tested in operation. The results have been published in the prestigious journal Nature Catalysis.