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The Analytical Scientist / App Notes / 2020 / The 1Der for operando XRD measurements

The 1Der for operando XRD measurements

09/25/2020

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The operando (operating) technique enables real-time X-ray diffraction (XRD) characterization of the crystalline phases in battery electrodes. The structural evolution of phases can be tracked during the charge-discharge cycling of the battery. The ion-exchange reaction can be studied under varying operating conditions for a deeper understanding of battery performance, stability and lifetime.

Pouch cells are often used in battery technology research and are increasingly being used for integration into e.g. automotive applications, due to the benefits of cheap and versatile production. Pouch cells can be fabricated with varying thicknesses, sizes and shapes. Used cells are easy to store and recycle.
 
On the Empyrean XRD system, pouch cells are easy to study in transmission geometry and their flat, often rectangular shape also allows for mapping of measurements at different positions across the battery cell. The 1Der detector is a truly versatile option for this set up, enabling operando battery measurements alongside other more conventional experiments.

The transmission configuration for studying a pouch cell is shown in Figure 1. A commercial pouch cell employing a LiFePO4 cathode and a graphite anode is measured during 5 complete cycles of charge/ discharge. It is held in a specially designed pouch cell holder on a programmable X-Y-Z sample stage. Ag radiation is used for maximum penetration through the cell and the finest data quality is assured by the special focussing mirror incident beam optic tuned to Ag Kα wavelength. The versatile 1Der detector completes the configuration. With its automatically tuneable energy window, the 1Der can select a narrow window around Ag radiation energy, for a fast powder diffraction scan.

Figure 1. Empyrean configuration for transmission incorporating Ag X-ray tube, focussing mirror and the 1Der detector. The pouch cell battery is mounted in a pouch cell holder on a programmable X-Y-Z stage.

>> Download the Full Application Note as a PDF

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