Fast X-ray Nanotomography with Sub-10 nm Resolution as a Powerful Imaging Tool for Nanotechnology and Energy Storage Applications.

In the last decade, transmission X-ray microscopes (TXMs) have come into operation in most of the synchrotrons worldwide. They have proven to be outstanding tools for non-invasive ex and in situ 3D characterization of materials at the nanoscale across varying range of scientific applications. However, their spatial resolution has not improved in many years, while newly developed functional materials and microdevices with enhanced performances exhibit nanostructures always finer. Here, optomechanical breakthroughs leading to fast 3D tomographic acquisitions (85 min) with sub-10 nm spatial resolution, narrowing the gap between X-ray and electron microscopy, are reported. These new achievements are first validated with 3D characterizations of nanolithography objects corresponding to ultrahigh-aspect-ratio hard X-ray zone plates. Then, this powerful technique is used to investigate the morphology and conformality of nanometer-thick film electrodes synthesized by atomic layer deposition and magnetron sputtering deposition methods on 3D silicon scaffolds for electrochemical energy storage applications.

Fast Electrochemical Storage Process in Sputtered Nb2O5 Porous Thin Films.

The formation of a thin film electrode exhibiting high capacity and high rate capabilities is challenging in the field of miniaturized electrochemical energy storage. Here, we present an elegant strategy to tune the morphology and the properties of sputtered porous Nb2O5 thin films deposited on Si-based substrates via the magnetron sputtering deposition technique. Kinetic analysis of the redox reactions is studied to qualify the charge storage process, where we observe a non-diffusion-controlled mechanism within the porous niobium pentoxide thin film. To improve the surface capacity of the Nb2O5 porous electrode, the thickness is progressively increased up to 0.94 µm, providing a surface capacity close to 60 µAh·cm-2 at 1 mV·s-1. The fabrication of high energy density miniaturized power sources based on the optimized T-Nb2O5 films could be achieved for Internet of Things applications requiring high rate capability.