Journal of Power Sources 185 (2008) 1386–1391 Contents lists available at ScienceDirect Journal of Power Sources journal homepage: www.elsevier.com/locate/jpowsour Electrochemical behaviour of tin borophosphate negative electrodes for energy storage systems Atef Y. Shenouda a, , Hua Kun Liu b a Central Metallurgical Research and Development Institute (CMRDI), Tebbin, Helwan, Helwan, Egypt b Institute for Superconducting and Electronic Materials, ARC Centre of Excellence for Electromaterials Science, University of Wollongong, NSW 2522, Australia article info Article history: Received 3 July 2008 Received in revised form 12 August 2008 Accepted 16 August 2008 Available online 27 August 2008 Keywords: Lithium battery negative electrode Tin borophosphate electrode Antimony doping abstract Tin borophosphate compounds doped with antimony, Sn 2 BP 1-x Sb x O 6 (x = 0–0.3), have been prepared and studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transmission infrared spectroscopy (FTIR), electrochemical impedance spectroscopy (EIS), and cyclic voltammetry (CV) and galvanostatic measurements. XRD patterns of all the samples were indexed to the tetragonal system. The EIS showed that the conductivities are enhanced by antimony doping. It was observed that the Warburg impedance coefficient ( w ) was 1163.265 cm 2 s -0.5 for the Sn 2 BP 0.9 Sb 0.1 O 6 (x = 0.1) sample, and this was the lowest value compared to those of the other samples. Sn 2 BP 0.9 Sb 0.1 O 6 (x = 0.1) showed the highest specific discharge capacity of 1050 mAh g -1 among all the samples and a reversible capacity of 540 mAh g -1 at the 150th cycle. © 2008 Elsevier B.V. All rights reserved. 1. Introduction Tin oxide compounds (TOC) have been suggested as high capacity anode materials for lithium-ion batteries [1,2]. Their rechargeability is based on the reversibility in the electrochemi- cal reactions involving structurally related phases of Li–Sn alloys [3]. The alloy phase is believed to be dispersed in an oxide matrix consisting primarily of the decomposition products formed dur- ing the first Li intercalation reaction. The most notable deficiencies of tin oxide compounds are their irreversible capacity loss in the first charge cycle and their poor cyclability relative to carbon-based anodes. The TOC that delivers the best electrochemical perfor- mance is reported with SnB 0.56 P 0.40 Al 0.42 O 0.36 composition [4]. The synthesis of this compound is difficult because of the high melting point of the Al 2 O 3 raw material, necessitating processing tempera- tures as high as 1100 C. Special equipment and care are also needed to reduce the evaporative loss of volatile components such as B 2 O 3 and P 2 O 5 . In this investigation, BPO 4 was used instead to reduce the volatility problem of B 2 O 3 and P 2 O 5 . BPO 4 reacts with SnO at ele- vated temperatures to form Sn 2 BPO 6 , which was used as a model TOC anode in rechargeable lithium test cells. Its electrochemical performance is comparable with those of Sn 2 B 2 O 5 and Sn 2 P 2 O 7 , which are TOCs with only one glass formation promoter (B or P). There has been a resurgence of interest in the use of lithium-alloy Corresponding author. Tel.: +20 25010642; fax: +20 25010639. E-mail address: ayshenouda@yahoo.com (A.Y. Shenouda). anodes because of their low first cycle capacity losses [5]. Most recent implementations have addressed the major deficiency of bulk alloys (material fragmentation consequent upon the large vol- ume changes in intercalation and de-intercalation) by dispersing the active material as ultra-fine particles in a suitable matrix [6–8]. The matrix is often an inactive phase, but an active host material may also be used [9]. The effectiveness of this approach is deter- mined by the ability of the matrix to restrain the particle growth of the active phase. It is in this latter category that TOCs may still hold an edge over the multiphase alloy systems. Three tin compounds, namely Sn 2 P 2 O 7 , Sn 2 B 2 O 5 , and Sn 2 BPO 6 , have been prepared by melt-quenching the appropriate reaction mixtures [10]. The borate glass was the easiest to form, but it was visually the least homogeneous and delivered the poorest electro- chemical performance. Hence, the amount of B in any glassy TOC should be carefully controlled to reach a balance between the ease of synthesis and electrochemical performance. Although similar alloying and de-alloying mechanisms were involved in charge and discharge reactions, Sn 2 P 2 O 7 and Sn 2 BPO 6 cycled much better than Sn 2 B 2 O 5 at the current density of 20 mA g -1 . When the cells were cycled at higher current and a higher discharge potential limit (150 mA g -1 and 1.4 V, respec- tively), Sn 2 BPO 6 displayed the best capacity retention relative to Sn 2 P 2 O 7 and Sn 2 B 2 O 5 . This is perhaps due to the robustness of the BPO 6 4- structure in charge and discharge reactions. The major advantage of TOC over carbonaceous anodes is their large specific capacities on either the gravimetric or volumet- ric basis. They are, however, hampered by the large irreversible 0378-7753/$ – see front matter © 2008 Elsevier B.V. All rights reserved. doi:10.1016/j.jpowsour.2008.08.042