Crystal Structure of a Lightweight Borohydride from Submicrometer Crystallites by Precession Electron Diffraction

Abstract

We demonstrate that precession electron diffraction at low-dose conditions can be successfully applied for structure analysis of extremely electron-beam-sensitive materials. Using LiBH4 as a test material, complete structural information, including the location of the H atoms, was obtained from submicrometer-sized crystallites. This demonstrates for the first time that, where conventional transmission electron microscopy techniques fail, quantitative precession electron diffraction can provide structural information from submicrometer particles of such extremely electron-beam-sensitive materials as complex lightweight hydrides. We expect the precession electron diffraction technique to be a useful tool for nanoscale investigations of thermally unstable lightweight hydrogen-storage materials.

3D electron diffraction techniques

“…1(a)], unless several PED patterns are collected from different zones. A 3D set of reflection intensities can be built by merging data from different zone axes and several structures could be solved in this way (Gjønnes et al, 1998;Gemmi et al, 2003Gemmi et al, , 2010Boullay et al, 2009;Hadermann et al, 2010Hadermann et al, , 2012Klein, 2011). However, orienting the crystal in many different zone axes is tedious and time consuming.…”

Structure solution and refinement of metal-ion battery cathode materials using electron diffraction tomography

“…For the subsequent refinement, on the other hand, high-quality intensities are necessary. Intensity scaling between the different datasets is then a refineable parameter, as implemented by Hadermann et al (2012) for separate precession electron diffraction patterns to refine the structure of LiBH 4 , and which can be extended to scaling of full EDT datasets, being, after the reconstruction, still only intensity versus hkl lists. In such case, for EDT datasets, there will in general be enough common reflections to allow the scaling for kinematical refinement.…”

Structure analysis of materials at the order–disorder borderline using three-dimensional electron diffraction

“…ED has also been successfully applied to incommensurate materials (Palatinus et al, 2011;Steciuk et al, 2016), and to macromolecules (Shi et al, 2013;Yonekura et al, 2015;Clabbers et al, 2017;de la Cruz et al, 2017;Xu et al, 2018;Lanza et al, 2019) and other structures of biological relevance (Rodriguez et al, 2015;Zee et al, 2019). Additionally, compared with X-rays, electrons can locate more easily light atoms such as Li (Hadermann et al, 2011(Hadermann et al, , 2012Kolb et al, 2011;Drozhzhin et al, 2016) and H (Palatinus et al, 2017;Clabbers et al, 2019), possibly employing refinement algorithms that take into consideration the dynamical scattering (Palatinus et al, 2013(Palatinus et al, , 2015.…”