A radially accessible tubular in situ X‐ray cell for spatially resolved operando scattering and spectroscopic studies of electrochemical energy storage devices. Issue 5 (16th September 2016)

• Record Type: Journal Article
• Authors: Liu, Hao; Allan, Phoebe K.; Borkiewicz, Olaf J.; Kurtz, Charles; Grey, Clare P.; Chapman, Karena W.; Chupas, Peter J.
• Is Part Of: Journal of applied crystallography. Volume 49:Issue 5(2016)
• Page Start: 1665
• Page End: 1673
• Publication Date: 2016-09-16
• Subjects: in situ X‐ray electrochemical cells -- energy storage -- batteries -- capacitors -- spatial resolution; Crystallography -- Periodicals; 548.05
• DOI: 10.1107/S1600576716012632
• Languages: English
• ISSNs: 0021-8898

Abstract

Abstract : Spatially resolved X‐ray scattering and spectroscopy measurements, to separately probe and map reactions of individual components and regions within an operating electrochemical device, are enabled by the development of a tubular in situ cell. Abstract : A tubular operando electrochemical cell has been developed to allow spatially resolved X‐ray scattering and spectroscopic measurements of individual cell components, or regions thereof, during device operation. These measurements are enabled by the tubular cell geometry, wherein the X‐ray‐transparent tube walls allow radial access for the incident and scattered/transmitted X‐ray beam; by probing different depths within the electrode stack, the transformation of different components or regions can be resolved. The cell is compatible with a variety of synchrotron‐based scattering, absorption and imaging methodologies. The reliability of the electrochemical cell and the quality of the resulting X‐ray scattering and spectroscopic data are demonstrated for two types of energy storage: the evolution of the distribution of the state of charge of an Li‐ion battery electrode during cycling is documented using X‐ray powder diffraction, and the redistribution of ions between two porous carbon electrodes in an electrochemical double‐layer capacitor is documented using X‐ray absorption near‐edge spectroscopy.