Funded by the European Union
Welcome to NanED news page where you can find out about the Nan ED project's progress as well as events, and related news at a national and international level.
The first paper involving the work of one of NanED PhD students is already out! A research group led by CRISMAT-CNRS laboratory synthesized a series of self-doped compounds Cu2+xMn1-xGeS4 through Cu substitution to Mn. Using a combination of powder X-ray diffraction, high resolution transmission electron microscopy and precession-assisted electron diffraction tomography, they evidenced that the materials are composed of interconnected enargite- and stannite-type structures, via the formation of nanodomains with a high density of coherent interfaces. The complex crystal chemistry of such nanocomposites rises the issue of the role of the two structures and of their interfaces in the mechanism governing their electrical and thermal conductivities. Sara Passuti (ESR12 working at CRISMAT CNRS in Caen France) has analyzed and identified the structure of both stannite and enargite nanodomains using 3D ED in these complex intergrown nanocomposites. The paper is just out on Angewandte Chemie. Well done Sara!
Great participation of the NanED team at the 33rd European Crystallographic Meeting (ECM33) held in Versailles France from the 23rd to the 27th of August 2022. Several supervisors were involved in the congress as chairs and speakers in different sessions and NanED PhD students presented 9 posters in different sessions from electron crystallography to metallorganic framework, from organic crystals to macromolecules. Their posters have attracted a lot of interest and discussion. The participation in the congress has been very fruitful with the opening of possible collaboration.
Laura Gemmrich Hernandez, NanED PhD student working at Johannes Guthenberg University in Mainz on structural investigation of cement hydration mechanism by electron crystallography, won two poster prizes at ECM33! One in the electron crystallography session shared with the other NanED PhD student Sara Passuti offered by Nanomegas and another offered by CHARMAMAT LABEX in the field of advanced and functional materials. Laura’s poster was about "Structure solution using 3DED of beam and vacuum sensitive Metal Organic Frameworks" and describes the structure modification of two new porous metal phosphonates built by an organic acid linker in the TEM vacuum. Thanks to 3D ED it has been possible to determine their structures during the transformation process induced by the TEM vacuum and by the electron beam. Congratulation to Laura!
Sara Passuti, NanED PhD student working at CNRS in Caen on electron crystallography of nanodomains in functional materials, won a poster prize at ECM33 in the electron crystallography session offered by Nanomegas! Sara’s poster was about “3D scanning precession electron diffraction analysis of nanodomains in thin films” and describes a procedure about how collect 3D ED data of structure solution quality across a thin film. This procedure should allow to determine the modifications of the crystal structure in different portion of a thin film. Congratulation to Sara!
From the 25th to the 27th of May 2022, the NanED project had its first Workshop, held in Prague at the Institute of Physics of the Czech Academy of Sciences.
The workshop's main goal was to teach NanED PhD students how to collect reliable 3D ED data and how to process these data for a successful structure solution and refinement. The workshop was divided into morning theoretical sessions and afternoon practical sessions to learn how to use all the available structure analysis software for 3D ED. Together with most of the NanED supervisors, we had two invited speakers from outside the project, Prof. Tim Gruene from Vienna University a crystallographer expert in the use of SHELX and Dr Gerhard Hofer of Stockholm University a master in protein crystallography. It was the first we gathered together in person and it has been a fantastic experience for all of us.
Working on beam-sensitive and hydrated samples is a complex process. Therefore, Laura Gemmrich Hernandez (ESR08) is currently focused on optimizing the data acquisition routines and sample preparation to get quality data that can lead to the structure solution of such materials.
Currently, the project is focused on microscope management, cryoEM, and data processing of many different types of challenging, organic as well as inorganic, samples; such as hydrated, beam sensitive, and disordered materials. The cryoEM training has included a visit to the BASF in Ludwigshafen (Germany) to learn and practice the vitrification and cryotransfer procedures for these types of samples.
Establishing new crystal tracking routines requires a deep understanding of the hardware, software and 3DED technique and its limitations. Due to that, the work of Marco Santucci (NanED ESR9) is focused in mastering the microscope, with a special eye on the “hidden parameters” that allow the microscope to work. This deep knowledge is necessary to figure out how to handle a basic 3DED experiment, translate it in an automated and technically flexible approach by scripting as well as to improve it.
Marco is focused in the management of the machine, the data collection and processing of organic and inorganic samples, due to their intrinsically different beam stability. Regarding the scripting, Marco is learning Python and DigitalMicrograph© in order to be flexible and synchronize every element of our TEM machines during the data acquisition. Thanks to these acquired competences, Marco will develop a routine to set automatically the best eucentric height, a key parameter for sample mechanical stability during our experiments. At the same time, Marco is also learning how to model disordered crystals and simulate their diffuse scattering using DISCUS, thanks to a visit to the Prof. Rheinard Neder at the FAU in Erlangen.
The current objective in the context of Sara Passuti’s (ESR12 @ CNRS) research project is to implement new strategies for diffraction dataset acquisitions for thin films. Differently from a classical Rotation Electron Diffraction (RED) experiment, the beam is scanned across a pre-defined area going from the coating to the substrate of the thin film or vice versa for every tilt angle.
This way, differences in the lattice parameters in distinct areas of the sample could be highlighted and different domains could be identified.
The main issues concern the optimization of the dataset acquisition protocol, making it faster and more efficient, as well as the sorting of the acquired patterns in order to have separated datasets to analyze for different areas of the sample.
The PhD students Sara Passuti (left) and Erica Cordero-Oyonarte (right) just started at Crismat in Caen their NanED adventure. Sara will work on the project, “Electron crystallography of nanodomains in functional materials” focusing on materials with amazing properties whose crystallography is extremely difficult due to too small ordered domains. Meanwhile, Erica's project is “Electron crystallography of nanoparticles” which involves studying the limiting size of a 3D ED experiment.
Our Supervisor Philippe Boullay explains 3D ED facilities at the Crismat research center in CNR Caen, France
This project has received funding from the European Union’s Horizon 2020 research and innovation programme under the Marie Skłodowska Curie grant agreement No 956099.