Operando 3D Visualization of MgTR-Derived SiOₓ–Graphite Li-ion Battery Andes Using Synchrotron X-ray Tomography
Pedro Alonso-Sanchez a, Manuel Abillan Miñana a, Federico Cova b, Valeria Blanco c
a 1Instituto de Nanociencia y Materiales de Aragón (INMA), CSIC-Universidad de Zaragoza, Zaragoza 50009, Spain
b ALBA Synchrotron Light Facility, Carrer de la Llum 2-26, Cerdanyola del Vallès, 08290, Spain.
c Institut de Ciència de Materials de Barcelona (ICMAB), CSIC, Carrer dels Til·lers sn, Bellaterra, 08193, Spain
Proceedings of MATSUS Spring 2026 Conference (MATSUSSpring26)
G6 Operando and Correlative Characterization of Sustainable Materials and Interfaces
Barcelona, Spain, 2026 March 23rd - 27th
Organizers: Florian Hausen and Svetlana Menkin
Invited Speaker, Valeria Blanco, presentation 296
Publication date: 15th December 2025

Diatom microalgae naturally produce intricately patterned SiO₂ (SiO₃) frustules with hierarchical porosity and species-specific morphologies that cannot be replicated by conventional synthesis routes. These biogenic silica architectures offer a unique and sustainable template for producing advanced silicon-based materials for Li-ion battery anodes. In this work, frustules obtained from industrially cultured diatoms were converted into nanostructured SiOₓ through a controlled magnesiothermic reduction (MgTR) reaction, preserving their characteristic 3D morphology while generating interconnected porous SiOₓ frameworks. TEM and TEM-EDS analyses confirm uniform Si/O distributions and nanoscale porosity, which together provide mechanically adaptive structures ideal for mitigating volume changes of Si-based negative electrodes during cycling.

The MgTR-derived SiOₓ was subsequently incorporated into upscaled SiOₓ–graphite blended electrodes processed under industrially relevant slurry preparation and coating conditions. To directly link the bio-derived architecture to electrode behaviour, the composite electrodes were investigated operando using synchrotron X-ray computed microtomography (X-ray CT) at the FaXToR beamline (ALBA Synchrotron). The operando measurements reveal the evolution of porosity, particle rearrangement, and mechanical deformation during lithiation and delithiation, highlighting the distinct mesoscale response of diatom-derived SiOₓ within the graphite matrix.

These results demonstrate that diatom-templated silica, when converted via MgTR, provides a structurally resilient and scalable pathway to SiOₓ for blended anodes, and they underscore the importance of operando 3D characterization to guide the rational design of sustainable, high-capacity silicon-based electrodes for Li-ion battery technology.

The authors acknowledge the SUSTBATT (M-ERA.NET), Research Council of Norway, for the financial assistance (Project No. 337463). The authors thank Simon Nilsson for diatoms- from the Swedish Algae Factory, Sweden and Josh Thomas and Henrik Erikson from LiFeSiZE, Sweden, for the scaling up of the electrodes.

© FUNDACIO DE LA COMUNITAT VALENCIANA SCITO
We use our own and third party cookies for analysing and measuring usage of our website to improve our services. If you continue browsing, we consider accepting its use. You can check our Cookies Policy in which you will also find how to configure your web browser for the use of cookies. More info