A new method based on x‐ray diffraction (XRD), thermogravimetry (TG), and gas chromatography (GC), has been developed for the quantitative analysis of silver oxide cathode materials. This method takes into account (i) the existence of, a newly discovered oxygen deficient phase of silver oxide, and (ii) the occurrence of the solid‐state reverse disproportionation reaction between and Ag to form during the TG procedure. In this analysis procedure we use the general formula, (δ is the degree of oxygen deficiency in ), to represent a mixture of and . The weight fractions of , , and Ag were determined by XRD and that of by XRD and/or GC. The degree of oxygen deficiency, δ, was then determined from TG weight loss data. This new comprehensive analysis method is being used to determine compositional changes (aging) in silver oxide cathodes and to relate the changes to battery performance degradation problems. Oxygen deficiency in is a major cause of the high thermal instability seen in many silver oxide cathodes.
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