Quantifying total superoxide, peroxide, and carbonaceous compounds in metal–O2 batteries and the solid electrolyte interphase

article Quantifying total superoxide, peroxide, and carbonaceous compounds in metal–O2 batteries and the solid electrolyte interphase published yes Bettina Schafzahl author Eléonore Mourad author Lukas Schafzahl author Yann K. Petit author Anjana R. Raju author Musthafa Ottakam Thotiyl author Martin Wilkening author Christian Slugovc author Stefan Alexander Freunberger author A8CA28E6-CE23-11E9-AD2D-EC27E66974250000-0003-2902-5319 Passivation layers on electrode materials are ubiquitous in nonaqueous battery chemistries and strongly govern performance and lifetime. They comprise breakdown products of the electrolyte including carbonate, alkyl carbonates, alkoxides, carboxylates, and polymers. Parasitic chemistry in metal–O2 batteries forms similar products and is tied to the deviation of the O2 balance from the ideal stoichiometry during formation/decomposition of alkaline peroxides or superoxides. Accurate and integral quantification of carbonaceous species and peroxides or superoxides in battery electrodes remains, however, elusive. We present a refined procedure to quantify them accurately and sensitively by pointing out and rectifying pitfalls of previous procedures. Carbonaceous compounds are differentiated into inorganic and organic ones. We combine mass and UV–vis spectrometry to quantify evolved O2 and complexed peroxide and CO2 evolved from carbonaceous compounds by acid treatment and Fenton’s reaction. The capabilities of the method are exemplified by means of Li–O2 and Na–O2 cathodes, graphite anodes, and LiNi0.8Co0.15Al0.05O2 cathodes. https://research-explorer.ista.ac.at/download/7287/8049/O2 TIOC_fin_incl_SI.pdf application/pdfno ACS2018 eng ACS Energy Letters 2380-8195 2380-819510.1021/acsenergylett.7b01111 31170-176 yes B. Schafzahl et al., “Quantifying total superoxide, peroxide, and carbonaceous compounds in metal–O2 batteries and the solid electrolyte interphase,” ACS Energy Letters, vol. 3, no. 1. ACS, pp. 170–176, 2018. Schafzahl, Bettina, et al. “Quantifying Total Superoxide, Peroxide, and Carbonaceous Compounds in Metal–O2 Batteries and the Solid Electrolyte Interphase.” ACS Energy Letters, vol. 3, no. 1, ACS, 2018, pp. 170–76, doi:<a href="https://doi.org/10.1021/acsenergylett.7b01111">10.1021/acsenergylett.7b01111</a>. Schafzahl, Bettina, Eléonore Mourad, Lukas Schafzahl, Yann K. Petit, Anjana R. Raju, Musthafa Ottakam Thotiyl, Martin Wilkening, Christian Slugovc, and Stefan Alexander Freunberger. “Quantifying Total Superoxide, Peroxide, and Carbonaceous Compounds in Metal–O2 Batteries and the Solid Electrolyte Interphase.” ACS Energy Letters. ACS, 2018. <a href="https://doi.org/10.1021/acsenergylett.7b01111">https://doi.org/10.1021/acsenergylett.7b01111</a>. Schafzahl, B., Mourad, E., Schafzahl, L., Petit, Y. K., Raju, A. R., Thotiyl, M. O., … Freunberger, S. A. (2018). Quantifying total superoxide, peroxide, and carbonaceous compounds in metal–O2 batteries and the solid electrolyte interphase. ACS Energy Letters. ACS. <a href="https://doi.org/10.1021/acsenergylett.7b01111">https://doi.org/10.1021/acsenergylett.7b01111</a> B. Schafzahl, E. Mourad, L. Schafzahl, Y.K. Petit, A.R. Raju, M.O. Thotiyl, M. Wilkening, C. Slugovc, S.A. Freunberger, ACS Energy Letters 3 (2018) 170–176. Schafzahl B, Mourad E, Schafzahl L, et al. Quantifying total superoxide, peroxide, and carbonaceous compounds in metal–O2 batteries and the solid electrolyte interphase. ACS Energy Letters. 2018;3(1):170-176. doi:<a href="https://doi.org/10.1021/acsenergylett.7b01111">10.1021/acsenergylett.7b01111</a> Schafzahl B, Mourad E, Schafzahl L, Petit YK, Raju AR, Thotiyl MO, Wilkening M, Slugovc C, Freunberger SA. 2018. Quantifying total superoxide, peroxide, and carbonaceous compounds in metal–O2 batteries and the solid electrolyte interphase. ACS Energy Letters. 3(1), 170–176. 72872020-01-15T12:13:52Z2021-01-12T08:12:46Z