A pEek on the lab

A primary focus of our lab is the elucidation of complex sodium storage mechanisms in disordered carbonaceous anodes (hard carbons). While sodium insertion into hard carbon has long been a subject of debate, our facility utilizes operando NMR to provide real-time, non-destructive evidence of the multi-stage sodiation process.

The transition from ionic to metallic character is a critical signature of "pore-filling." Our lab specializes in identifying the Knight shift—a significant frequency shift (typically appearing around 800–1100 ppm for sodium) caused by the interaction between the 23Na nuclei and the conduction electrons of these metallic-like clusters. By distinguishing these clusters from bulk sodium dendrites (which appear at higher shifts), we provide vital insights into battery safety and initial Coulombic efficiency (ICE). Our operando capabilities allow us to track these species during actual charge-discharge cycles, revealing the reversibility of pore-filling and the structural evolution of the Solid Electrolyte Interphase (SEI) at the atomic scale.

Using an all-encompassing, non-destructive small-angle X-ray scattering methodology, we obtain unique nano-structural insights into materials. Through exploitation of integrated, advanced experiment orchestration and automated data workflows, turn-around time is minimized both for static samples, as well as for (highly customizable) in-situ and operando experiments. Over the eight years of its existence, the MOUSE lab has measured over 4000 samples for 200+ internal and external projects, and has contributed nanostructural insights to about 60 papers to date.

The thermochemical analysis unit is equipped with a thermogravimetric analyzer (TGA) operating under air or inert (Ar or N2) atmosphere, enabling the investigation of thermal stability and decomposition behavior. Mass changes are recorded as a function of temperature and time, while a coupled differential scanning calorimetry (DSC) system simultaneously measures heat flow associated with endothermic and exothermic transitions. In addition, the unit is interfaced with a gas chromatography–mass spectrometry (GC–MS) system, allowing the identification and analysis of evolved gaseous species during thermal treatment. The combined TGA–DSC–GC–MS setup provides a comprehensive thermochemical characterization by correlating mass loss, thermal events, and gas-phase composition.

The operando-SAXS cell is designed to enable in situ small-angle X-ray scattering measurements during electrochemical operation under realistic battery conditions. The cell geometry is based on a modified 2032-type configuration, incorporating X-ray transparent windows. The working electrode consists of a carbon-based electrode paired with a sodium counter/reference electrode, separated by an ion-permeable separator and assembled under inert conditions. The compact design allows integration into the SAXS test stand and precise alignment with the incident X-ray beam. Operando measurements are performed at room temperature (25 °C), enabling real-time monitoring of nanoscale structural evolution in the electrode material during cycling. This setup provides direct insight into structure–property relationships and dynamic changes occurring during cycling. 

BioLogic systems are high-precision analytical instruments. When testing coin cells, they are primarily used for High Precision Coulometry (HPC) and differential capacity analysis (dQ/dV). The hardware features ultra-high resolution (often 24-bit) and low current ranges, which are essential for detecting minute parasitic reactions or phase changes in new electrode materials.

In three-electrode cell configurations, BioLogic can be used for Electrochemical Impedance Spectroscopy (EIS) measurements. It can actively control the potential of the working electrode relative to the reference while simultaneously measuring the impedance of the individual electrodes.