Speaker
Description
Accelerating the discovery of next-generation battery materials requires not only faster synthesis routes, but also characterization workflows capable of extracting reliable structural and mechanistic information from large numbers of samples. This work was carried out within the framework of MAITENA $^{1-4}$, the Materials Acceleration and Innovation plaTform for ENergy Applications at CIC energiGUNE, which integrates automated synthesis, high-throughput characterization, electrochemical testing, and data-driven analysis for battery-materials development. Synchrotron techniques are particularly powerful in this context, providing the resolution, sensitivity, and time-resolved capabilities needed to connect automated materials preparation with phase analysis, redox chemistry, and reaction mechanisms under operating conditions.
In this work, synchrotron X-ray diffraction was used as a central tool to support the development of high-throughput characterization strategies for Fe-Mn-based cathode materials $^5$. In the $NaFe_{1-y}$$MnyPO_4$ system, samples prepared using an automated microwave-assisted solvothermal module $^2$ were analyzed through synchrotron diffraction and processed using FullProfAPP $^4$ to build the phase diagram of the $NaFe_{1-y}$$MnyPO_4$ system. These data contributed to the design, optimization, and scientific validation of a multi-sample holder for high-throughput powder diffraction measurements, providing a practical route to accelerate phase identification, structural refinement, and phase-diagram construction in automated battery-materials workflows.
Beyond high-throughput screening, synchrotron techniques were also applied to investigate the functioning mechanism of the high-voltage spinel $LiFe_{0.5}$$Mn_{1.5}$$O_4$ $^6$. Synchrotron X-ray diffraction and dual Fe/Mn K-edge X-ray absorption spectroscopy, including operando measurements during electrochemical cycling, were used to follow the structural evolution and transition-metal redox processes of this defect-prone cathode. Combined with complementary neutron diffraction and Mössbauer spectroscopy, these measurements revealed how Fe defect chemistry influences the electrochemical response and contributes to structural irreversibility during cycling.
Overall, this work highlights two complementary roles of synchrotron facilities in battery research: enabling high-throughput structural characterization within automated materials-acceleration platforms, and providing operando insight into complex degradation mechanisms. By integrating MAITENA-based automated synthesis, multi-sample synchrotron measurements, and streamlined refinement tools such as FullProfAPP, this approach contributes to the development of data-rich workflows for the rational design and optimization of sustainable electrode materials.
References:
1. Ismail M, Bustinza A, Monterrubio I, et al. Toward the Accelerated Discovery of Electroactive Materials for Li-Ion and Na-Ion Batteries:
MAITENA Platform. In: Electrochemical Society Meeting Abstracts 247. The Electrochemical Society, Inc.; 2025:8-8. https://iopscience.iop.org/article/10.1149/MA2025-0118mtgabs/meta
2. Monterrubio I, Orive J, Ismail M, et al. Affordable Automated Modules for Lab‐Scale High‐Throughput Synthesis of Inorganic Materials. Chem
– Eur J. 2025;31(52):e02072. doi:10.1002/chem.202502072
3. Ismail M, Angeles Cabañero M, Orive J, et al. ADEL: an automated drop-cast electrode setup for high-throughput screening of battery materials. Digit Discov. 2025;4(4):943-953. doi:10.1039/D4DD00381K
4. Arcelus O, Rodríguez-Carvajal J, Katcho NA, et al. FullProfAPP: a graphical user interface for the streamlined automation of powder diffraction data analysis. Appl Crystallogr. 2024;57(5). https://journals.iucr.org/paper?iu5063
5. Ismail M. Accelerate Li-ion and Na-ion Battery Development: Bridging Automated Experimental Methods with Theoretical and Operando
Insights. Published online October 24, 2025. doi:10/78342
6. Ismail M, Fehse M, Serrano-Sevillano J, et al. Operando Tracking of Fe Migration in Defect-Engineered LiFe0.5Mn1.5O4 Spinel Cathodes.
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