Versatile electrochemical cell for Li/Na-ion batteries and high-throughput setup for combined operando X-ray diffraction and absorption spectroscopy

Abstract

A fundamental understanding of de/intercalation processes (single phase versus multi‐phase), structural stability and voltage–composition profiles is pivotal for optimization of electrode materials for rechargeable non‐aqueous batteries. A fully operational setup (electrochemical cells, sample changer and interfacing software) that enables combined quasi‐simultaneous operando X‐ray diffraction (XRD) and absorption (XANES and EXAFS) measurements coupled with electrochemical characterization is presented. Combined XRD, XANES and EXAFS analysis provides a deep insight into the working mechanisms of electrode materials, as shown for the high‐voltage Li insertion cathode material LiMn1.5Ni0.5O4 and the high‐capacity sodium conversion anode material Bi2S3. It is also demonstrated that the cell design can be used for in‐house XRD characterization. Long‐term cycling experiments on both Li and Na electrode materials prove the hermeticity and chemical stability of the design as a versatile operando electrochemical cell.

Operando investigations of lithiation and delithiation processes in a BiVO4 anode material

“…The electrochemical cycling for the operando studies was performed in Swagelok type electrochemical cells with Kapton windows as earlier described. 16 The operando battery cell assembly is identical to that of the home lab coin cells described above. The first 1.5 galvanostatic cycles were followed operando.…”

“…The applied current was chosen to let each dis-/charge to take approximately 10 h. Collection of XANES data (2 min per scan) followed by SXRD data using a Dexela 2923 CMOS twodimensional detector (1 min per scan) was performed in sequence for several cells mounted in an automatized sample changer with 12 positions. 16 Computational details. Total energies were calculated by the projectedaugmented plane-wave (PAW) implementation of the Vienna ab initio simulation package (VASP).…”

Fast operando X-ray pair distribution function using the DRIX electrochemical cell

“…XRS is also a bulk probe, meaning that geometries where multiple battery components are illuminated by the incident X-ray beam may give rise to complex and overlapping XRS data, which cannot be analysed. These requirements make previous battery designs for XAS/ diffraction (Leriche et al, 2010;Sottmann et al, 2016;Borkiewicz et al, 2012) with low angular range and signal purity unsuitable.…”

“…Kapton windows have been replaced by rigid and conductive low-Z elements, like glassy carbon or beryllium, in other cell designs (Leriche et al, 2010;Sottmann et al, 2016;Borkiewicz et al, 2012;Hartung et al, 2015), offering an improved seal, stack pressure and conductivity for in situ XAS and Bragg diffraction experiments. These multipurpose electrochemical cells, AMPIX (Borkiewicz et al, 2012) or Bruker (Leriche et al, 2010), are also based on more standard coin and Swagelok cells, respectively.…”

An electrochemical cell for operando bench-top X-ray diffraction

“…Several designs of X-ray transparent electrochemical cells have been proposed for laboratory and synchrotron XRD in both reflection and transmission geometries. An overview has been given by Sottmann et al (2016). For laboratory XRD in reflection geometry, these include a reusable Swagelok-type cell with a beryllium window (Leriche et al, 2010), a reusable cell with a graphite dome as the window (Shen et al, 2014), a disposable coin cell with a Kapton window (Rhodes et al, 2011) and a pouch cell with an Al/Ti metal foil window (Villevieille et al, 2014).…”