In situ X-ray diffraction analysis of (CFx)n batteries: signal extraction by multivariate analysis

(CFx)n cathode reaction during discharge has been investigated using in situ X‐ray diffraction (XRD). Mathematical treatment of the in situ XRD data set was performed using multivariate curve resolution with alternating least squares (MCR–ALS), a technique of multivariate analysis. MCR–ALS analysis successfully separated the relatively weak XRD signal intensity due to the chemical reaction from the other inert cell component signals. The resulting dynamic reaction component revealed the loss of (CFx)n cathode signal together with the simultaneous appearance of LiF by‐product intensity. Careful examination of the XRD data set revealed an additional dynamic component which may be associated with the formation of an intermediate compound during the discharge process.