Rapid synthesis of LiCr 0.15 Mn 1.85 O 4 by glycine–nitrate method Ivana Stojković a , Azarnoush Hosseinmardi b , Dragana Jugović c , Miodrag Mitrić d , Nikola Cvjetićanin a, ⁎ a Faculty of Physical Chemistry, University of Belgrade, Studentski Trg 12-16, P.O. Box 137, 11001 Belgrade, Serbia and Montenegro b Institute for Chemistry and Technology of Inorganic Materials, Graz University of Technology, Stremayrgasse 16/III 8010 Graz, Austria c Institute of Technical Sciences, Serbian Academy of Sciences and Arts, Knez Mihajlova 35/IV, 11000 Belgrade, Serbia and Montenegro d The Vinča Institute of Nuclear Sciences, Laboratory for Theoretical and Condensed Matter Physics, P.O. Box 522, 11001 Belgrade, Serbia and Montenegro Received 30 May 2005; received in revised form 7 February 2006; accepted 16 February 2006 Abstract LiCr 0.15 Mn 1.85 O 4 spinel has been successfully synthesized by glycine–nitrate method (GNM). The presence of pure spinel phase was confirmed by long term XRPD measurements and the Rietveld structural refinement. Lattice parameter was estimated to be 8.2338Å. Average particle size of prepared powder material is below 500nm. The BET surface area is 9.6m 2 g - 1 . As a cathode material for lithium batteries LiCr 0.15 Mn 1.85 O 4 shows initial discharge capacity of 110mA h g - 1 and capacity retention of 83% after 50 cycles. © 2006 Elsevier B.V. All rights reserved. Keywords: LiCr 0.15 Mn 1.85 O 4 spinel; Glycine–nitrate method; Rietveld refinement; Cathode material 1. Introduction LiMn 2 O 4 is a promising cathode material for lithium-ion batteries because it delivers high voltage, good capacity and it is a low cost and non-toxic material. Unfortunately, LiMn 2 O 4 spinel shows considerable decrease in capacity during electro- chemical charging–discharging on the 4V plateau. Recently several dominant modes of capacity fade have been proposed. According to Tucker et al. [1] Mn-dissolution and concomitant Li-for-Mn ion exchange at the end-of-discharge are the dominant modes of failure of LiMn 2 O 4 cathode. Shin and Manthiram [2,3] demonstrated that lattice parameter difference Δa between the two cubic phases formed in the two-phase region [4] plays a main role in the capacity fade. Δa causes the development of microstrain which hinders lithium diffusion inside the crystal. The largest improvement in preventing capacity fade has been achieved by substitution of some manganese by other metal cations. These more robust spinels have higher average oxidation state of remaining manganese (>3.5+). This leads to a lower theoretical capacity because of the lower number of lithium ions that can be extracted from the spinel structure before all manganese is oxidized. Not only the choice of M z+ metal cation type but also its amount “x”, is important for obtaining LiM x Mn 2-x O 4 cathode material with adequate initial capacity and high capacity retention. Cr 3+ is among the cations whose substitution for manganese gives highest performance increase [1,5–8]. The best results are obtained for 0.10 < x < 0.20. LiMn 2 O 4 and LiM x Mn 2-x O 4 spinels are usually prepared by time and energy consuming solid state reaction, starting from carbonates and/or oxides [1–3,5,8,9]. Synthesis methods via solution offer homogeneity of the starting state and accordingly lower temperatures and shorter heating times than in solid state reaction. Some of these methods may be complex [10], or even demand special equipment [11,12]. In this work powder material LiCr 0.15 Mn 1.85 O 4 is prepared by rapid glycine–nitrate method (GNM), developed before for synthesis of YBa 2 Cu 3 O 7-x ceramics [13]. GNM was already used by our group [14] and by Zhang et al. [15] for synthesis of LiMn 2 O 4 spinel. Here we have tested the possibility for cheap and fast synthesis of more complex spinel. We have examined Solid State Ionics 177 (2006) 847 – 850 www.elsevier.com/locate/ssi ⁎ Corresponding author. Tel./fax: +381 11 187133. E-mail address: nikcvj@ffh.bg.ac.yu (N. Cvjetićanin). 0167-2738/$ - see front matter © 2006 Elsevier B.V. All rights reserved. doi:10.1016/j.ssi.2006.02.013