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1 Supporting Information Anion Redox Chemistry in the Cobalt Free 3d Transition Metal Oxide Intercalation Electrode Li[Li 0.2 Ni 0.2 Mn 0.6 ]O 2 Kun Luo a, Matthew R. Roberts a, Niccoló Guerrini a, Nuria Tapia-Ruiz a, Rong Hao a, Felix Massel b, David M. Pickup c, Yi-Sheng Liu d, Jinghua Guo d, Alan V. Chadwick c, Laurent C. Duda b, Peter G. Bruce a * a Departments of Materials and Chemistry, University of Oxford, Parks Road, Oxford OX1 3PH, UK. b Department of Physics and Astronomy, Division of Molecular and Condensed Matter Physics, Uppsala University, Box 516, S Uppsala, Sweden. c School of Physical Sciences, University of Kent, Canterbury, Kent CT2 7NH, UK. d Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA 94720, United States. peter.bruce@materials.ox.ac.uk 1

2 Figure S1. Powder diffraction patterns for Li[Li 0.2Ni 0.2Mn 0.6]O 2 fitted using an R m model. The + indicates observed data; solid line indicates calculated profile. Tick marks show allowed reflections. a) Powder X-ray diffraction data. The dotted box indicates the superstructure peaks. b) Powder neutron diffraction data. Red tick marks correspond to peak positions of the vanadium sample holder. 2

3 Table S1. Refined Structure of Li[Li 0.2Ni 0.2Mn 0.6]O 2 Atom Site x y z Occupancy Uiso (Å 2 ) Li(1)/Ni(1) 3b (2)/0.032(2) (7) Li(2)/Ni(2)/Mn(1) 3a (2)/0.168(2)/ (2) O(1) 6c (1) (1) Li[Li 0.2Ni 0.2Mn 0.6]O 2 space group R m. a = (7) Å, c = (6) Å, χ 2 = 5.467, wrp = 3.03%, Rp = 3.21% Figure S2. In-situ X-ray diffraction patterns of Li[Li 0.2Ni 0.2Mn 0.6]O 2 during the 1 st cycle. a - The structure of Li[Li 0.2Ni 0.2Mn 0.6]O 2. b - In situ X-ray diffraction patterns in the region of o and o. c - The charge-discharge curve for Li 1.2Ni 0.2Mn 0.6O 2. 3

4 Figure S3. Negative ion Time of Flight Secondary Ion Mass Spectrometry (TOF-SIMS) images of 18 O labelled Li[Li 0.2Ni 0.2Mn 0.6]O2 cathode before charge. 4

5 Calculation of the expected percentages of 16/18 O 2 and C 16/18 O 2 16/18 O 2: The 16/16 O 2, 16/18 O 2 and 18/18 O 2 ratios presented in Table 1 were calculated based on the probabilities of their formation given the amounts of 18 O and 16 O observed in Li[Li 0.2Ni 0.2Mn 0.6]O 2 by TOF-SIMS. C 16/18 O 2: The CO 2 arises from decomposition of the electrolyte solvent due to attack by oxygen species emitted from the lattice. We assume that the oxygen from the material is released in a reduced state probably as superoxide O 2-. Freunberger et al. proposed possible mechanisms for the PC decomposition process in the presence of superoxide O 2-, in which several types of Li-organic compounds could be formed according to following process. 1 2O 2- - O 2 + 3e - (1) (2) As implied by the products shown in equation 2, it is possible that when attacked by superoxide the PC can undergo a series of chain reactions that do not involve reaction with further released oxygen. It is proposed that these products then decompose to form CO 2 and H 2O at high potential on charging (>4 V). Therefore we propose the following simplified decomposition reaction (assuming n = 1) at high potentials caused by O 2-. CH 3C 2H 3O 2CO - (PC) + 4O 2 4CO 2 + 3H 2O + 4e - (3) Based on this assumption we calculated the predicted ratios of CO 2 that are formed containing 18 O. This was carried out by considering the probability of the CO 2 containing 18 O given the ratio of 18 O/ 16 O contained in the lattice (from TOF-SIMS) and 16 O in PC electrolyte. It is clear that the numbers in Table 1 in the main paper do not match exactly and we believe this is likely because of possible propagating reactions that take place after the ring opening of PC caused by superoxide reported previously

6 Quantification of electron transfer (charge capacity) due to O removed from the lattice This was estimated based on the CO 2 and O 2 evolved, as described above. The following assumptions were used: CO 2: As discussed above, we simplified the process of CO 2 evolution as equation (3). Combining equation (1) and (3), the electron transfer through CO 2 is calculated. O 2: As discussed in the main paper, the vast majority of the O 2 gas detected in Region 3 arises directly from O released from the lattice. 2O 2- O 2 + 4e - (4) The electron transfer associated with the O 2 generation was quantified using equation (4). 6

7 Figure S4. Schematic diagrams showing the SXAS electronic transitions from the O1s to the empty states on each of the transition metals in Li[Li 0.2Ni 0.2Mn 0.6]O 2. (The diagrams show one electron energies and hence do not distinguish energetically between spin-up and spin-down states). The O K-edge SXAS for the pristine Li[Li 0.2Ni 0.2Mn 0.6]O 2 material, Figure 6a, is dominated at low energy by two peaks. The possible O K-edge SXAS transitions anticipated to these unoccupied states are given in Figure S4. The dominant transition metal ion in Li[Li 0.2Ni 0.2Mn 0.6]O 2 is Mn 4+ 3d 3, so there are 7 possible SXAS transitions associated with Mn 4+, 3 spin-down t 2g, 2 spin-up and 2 spin-down e g, with 0.6 Mn present per formula unit this implies we would expect 4.2 transitions per formula unit. For Ni 2+ 2 spin-down e g transitions gives 0.4 transitions per formula unit. Therefore, Mn 4+ accounts for ~91 % of the expected SXAS transitions to the unoccupied states and hence it dominates the spectrum. This is confirmed by comparing the SXAS spectrum for Li[Li 0.2Ni 0.2Mn 0.6]O 2, Figure 6a, with the O K-edge SXAS for MnO 2 from the literature, which shows that the spectra are almost identical, with two peaks at the same energies and with almost the same intensity ratio. 3 The lower energy peak has been assigned to the spin-down t 2g and spin-up e g transitions with the higher energy peak arising from the spin-down e g transitions. 3a, 4 7

8 Reference 1. Freunberger, S. A.; Chen, Y. H.; Peng, Z. Q.; Griffin, J. M.; Hardwick, L. J.; Barde, F.; Novak, P.; Bruce, P. G., Reactions in the Rechargeable Lithium-O 2 Battery with Alkyl Carbonate Electrolytes. J Am Chem Soc 2011, 133 (20), Aurbach, D.; Daroux, M.; Faguy, P.; Yeager, E., The Electrochemistry of Noble-Metal Electrodes in Aprotic Organic-Solvents Containing Lithium-Salts. J Electroanal Chem 1991, 297 (1), (a) de Groot, F. M. F.; Grioni, M.; Fuggle, J. C.; Ghijsen, J.; Sawatzky, G. A.; Petersen, H., Oxygen 1s X-Ray-Absorption Edges of Transition-Metal Oxides. Phys Rev B 1989, 40 (8), ; (b) Gilbert, B.; Frazer, B. H.; Belz, A.; Conrad, P. G.; Nealson, K. H.; Haskel, D.; Lang, J. C.; Srajer, G.; De Stasio, G., Multiple scattering calculations of bonding and X-ray absorption spectroscopy of manganese oxides. J Phys Chem A 2003, 107 (16), Yoon, W. S.; Balasubramanian, M.; Yang, X. Q.; Fu, Z. G.; Fischer, D. A.; McBreen, J., Soft X- ray absorption spectroscopic study of a LiNi 0.5Mn 0.5O 2 cathode during charge. J Electrochem Soc 2004, 151 (2), A246-A251. 8

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