Abstract
New concepts for Li-ion batteries are of growing interest for high-performance applications. One aim is the search for new electrode materials with superior properties and their detailed characterization. We demonstrate the application of X-ray photoelectron spectroscopy (XPS) to investigate electrode materials (LiCoO2, LiCrMnO4) during electrochemical cycling. The optimization of a “quasi in situ” analysis, by transferring the samples with a transport chamber from the glove box to the XPS chamber, and the reliability of the experiments performed are shown. The behavior of characteristic chemical species at the electrodes and the changes in oxidation states of LiCrMnO4 during cycling is discussed. The formation of Cr6+ is suspected as a possible reason for irreversible capacity loss during charging up to complete Li deintercalation (approximately 5.2 V).
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Mizushima K, Jones PC, Wiseman PJ, Goodenough JB (1980) Mater Res Bull 15:783–789
Whittingham MS (2004) Chem Rev 104:4271–4301
Ohzuku T, Brodd RJ (2007) J Power Sources 174:449–456
Kawai H, Nagata M, Tukamoto H, West AR (1999) J Power Sources 81–82:67–72
Sigala C, Verbaere A, Mansot JL, Guyomard D, Piffard Y, Tournoux M (1997) J Solid State Chem 132:372–381
Nikolowski K, Bramnik NN, Ehrenberg H (2008) Ionics 14:121–124
Suzuki S, Tomita M, Okada S, Arai H (1996) J Phys Chem Solids 57:1851–1856
Briggs D, Grant JT (2003) (eds) Surface analysis by Auger and X-ray photoelectron spectroscopy. IM Publications, Chichester
Dahéron L, Dedryvère R, Martinez H, Ménétrier M, Denage C, Delmas C, Gonbeau D (2008) Chem Mater 20:583–590
Edstrom K, Gustafsson T, Thomas JO (2004) Electrochim Acta 50:397–403
Cheng R, Borca CN, Pilet N, Xu B, Yuan L, Doudin B, Liou SH, Dowben PA (2002) Appl Phys Lett 81:2109–2111
Ünveren E, Kemnitz E, Hutton S, Lippitz A, Unger WES (2004) Surf Interface Anal 36:92–95
Grohmann I, Kemnitz E, Lippitz A, Unger WES (1995) Surf Interface Anal 23:887–891
Beyreuther E, Grafström S, Eng LM, Thile C, Dörr K (2006) Phys Rev B 73:155425
Andersson AM, Abraham DP, Haasch R, MacLaren S, Liu J, Amine K (2002) J Electrochem Soc 149:A1358–A1369
Wu C, Wang Z, Wu F, Chen L, Huang X (2001) Solid State Ionics 144:277–285
Acknowledgements
Financial support from the Deutsche Forschungsgemeinschaft (DFG) is gratefully appreciated. The authors would also like to thank A. Thomas for assistance with the sample preparation.
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Oswald, S., Nikolowski, K. & Ehrenberg, H. Quasi in situ XPS investigations on intercalation mechanisms in Li-ion battery materials. Anal Bioanal Chem 393, 1871–1877 (2009). https://doi.org/10.1007/s00216-008-2520-z
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DOI: https://doi.org/10.1007/s00216-008-2520-z