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

Abstract

An X-ray transparent electrochemical cell for operando bench-top X-ray diffraction in reflection geometry is presented. Dense glassy carbon (Sigradur-G) is used as an X-ray transparent window. The cell and dedicated sample holder are easy to handle and cost efficient thanks to their simple designs. To demonstrate the performance of this new Swagelok-type operando cell, diffractograms were collected during cycling of the cathode material Li x Mn 2 O 4 (x 1) in a lithium-ion battery. During charging/delithiation, three spinel phases with evolving lattice parameters were found. This observation confirms the expected mixed two-phase and solid-solution behaviour and thereby validates our experimental setup. The presented low-cost setup may enable further battery research units to access operando X-ray diffraction data for characterization of structural phenomena during battery cycling and degradation mechanisms during prolonged cycling, which will lead to improvement of the battery technology.

Experimental Considerations for Operando Metal‐Ion Battery Monitoring using X‐ray Techniques

“…[17] Finally, fit-for-purpose cells can be designed for reflection geometry, transmission geometry or even allow both. [25,26,[35][36][37][38][39][27][28][29][30][31][32][33][34] As will be discussed later, for such cells a Be window is required for reflection geometry, while other materials (aluminized polymer, glassy carbon etc.) can be used for transmission.…”

“…Compared to other existing designs, [27,28,30,31,39] our cell is built employing Swagelok® union parts (nut, sealing rings, etc.) which allows the cell to be tight, hermetic, dismountable, reusable and easy to clean.…”

Understanding the (De)Sodiation Mechanisms in Na‐Based Batteries through Operando X‐Ray Methods

“…In such experiments, a surface layer with an angle‐ and composition‐dependent depth is sampled instead of the entire depth of the working electrode as in transmission geometry. The available cell designs include a reusable Swagelok‐type cell with a Be window, [201] a reusable cell with glassy carbon windows, [202] a reusable cell with a graphite dome as the window, [109] a disposable coin cell with a Kapton window [203] and a pouch cell with an Al/Ti metal foil window [192] . The similarities between the cell designs for X‐ray diffraction/scattering and absorption make parallel XRD and XAS experiments possible on some beamlines.…”

Using In-Situ Laboratory and Synchrotron-Based X-ray Diffraction for Lithium-Ion Batteries Characterization: A Review on Recent Developments

“…Another approach can be the generation of an air gap between the Be window and the electrochemically active part of the cell, so as to prevent Be reactivity at high voltage [27]. Alternative solutions include dense glassy carbon, because of its rigidity and electrical conductivity [32], or polymer materials such as Kapton or Mylar, because of their low cost, non-toxicity, and flexibility [33]. However, because of their poor sealing properties, their use can lead to a potential risk of leaking of the liquid electrolyte and consequent contamination from atmosphere [16].…”