Journal of Alloys and Compounds 479 (2009) 875–878 Contents lists available at ScienceDirect Journal of Alloys and Compounds journal homepage: www.elsevier.com/locate/jallcom Sol–gel synthesis and electrochemical properties of CuV 2 O 6 cathode material Cao Jun-qi a , Wang Xian-you a, , Tang Anping a , Wang Xin a , Wang Ying b , Wu Wen a a School of Chemistry, Key Laboratory of Environmentally Friendly Chemistry and Applications of Minister of Education, Xiangtan University, Xiangtan, Hunan 411105, China b School of Chemical Engineering and Pharmacy, Wuhan Institute of Technology, Hubei 430070, China article info Article history: Received 18 August 2008 Received in revised form 21 January 2009 Accepted 22 January 2009 Available online 6 February 2009 Keywords: CuV2O6 Lithium ion battery Sol–gel method Copper–vanadium-oxides Cathode material abstract The CuV 2 O 6 cathode material was successfully synthesized using the NH 4 VO 3 and the alkaline copper carbonate (CuCO 3 ·Cu(OH) 2 ·xH 2 O, malachite) as the starting reagents by a citrate sol–gel route. The struc- tures and electrochemical properties of CuV 2 O 6 synthesized at different temperature were characterized by X-ray diffraction (XRD), thermogravimetry/differential thermogravimetry (TG/DTG), scanning electron microscopy (SEM) and electrochemical measurements. The results showed that the sample prepared at 550 C had small particle size, and thus revealed higher initial discharge capacity (403 mAh g -1 ) and better cycle performance than that prepared by the conventional solid-state method. © 2009 Elsevier B.V. All rights reserved. 1. Introduction In the past few years, vanadium-based materials, such as V 2 O 5 , silver–vanadium-oxides (SVO, typically Ag 2 V 4 O 11 ) and copper–vanadium-oxides (CVO, typically CuV 2 O 6 and Cu 2 V 2 O 7 ), drew great interests of researchers for their high lithiated charac- teristics [1–5]. Especially, Ag 2 V 4 O 11 has achieved a commercial suc- cess as solid-state cathode material in primary (non-rechargeable) lithium power sources for implantable biomedical devices [6]. Fur- thermore, recent studies showed that the copper–vanadium-oxides have delivered even more electrochemical capacity than SVO as reported [7–9]. The cathode material Cu 2 V 2 O 7 could deliver an attractive specific capacity near 500mAh g -1 [10] while the CuV 2 O 6 could deliver the highest discharge specific capacity among all the CVO series, more than the Ag 2 V 4 O 11 material used in commercial Li/SVO batteries. Like NiV 2 O 6 [11,12], Li 1+x V 3 O 8 [13] and other vanadium-based materials, the synthesizing technique played the important func- tion to their electrochemical performances. As reported, the NiV 2 O 6 material synthesized by Fuentes et al. [11] was used as an anode material (potential plateau was 0.5 V vs. Li + /Li) whereas the NiV 2 O 6 material synthesized by Andrukaitis et al. [12] was used as a cath- ode material for lithium battery (potential plateau was about 1.5V vs. Li + /Li). As for the synthesis of CuV 2 O 6 , there were three methods reported in the literatures until to now. Eguchi et al. reported high temperature solid-state method [7]. CuO and V 2 O 5 powders, which Corresponding author. Tel.: +86 732 8293043; fax: +86 732 8292282. E-mail address: wxianyou@yahoo.com (X.-y. Wang). has been preheated at 750 C and 650 C for 24 h, respectively, were mixed at a molar ratio of 1:1 in an agate mortar and the mixture was pressed (200 MPa) into pellets. Pellets were heated at 620 C on a platinum plate for 48.5 h under air atmosphere. It required large energy consumption, long reaction time, and the resultant prod- ucts exhibited low capacity. Besides, the co-precipitation method was reported by Wei et al. [14]. The stoichiometric and oxygen defi- cient CuV 2 O 6 was synthesized, but the electrochemical properties of CuV 2 O 6 have not been reported yet. Recently, Cao et al. put for- ward the soft chemistry method to synthesize the -CuV 2 O 6 [8]. The -CuV 2 O 6 was obtained from V 2 O 5 gel and Cu 2 O powders. Although as-prepared CuV 2 O 6 could deliver the specific capacity of nearly 350 mAh g -1 in the discharge current density of 30 mA g -1 , its usage is limited because the V 2 O 5 gel could not be cosmically manufactured. In this work, CuV 2 O 6 was successfully synthesized via sol–gel method for the first time. Synthesized technique and electrochem- ical performance of the as-prepared CuV 2 O 6 material was studied in detail. 2. Experimental 2.1. Preparation of CuV2O6 The CuV2O6 was synthesized by a sol–gel route based on citric acid using NH4VO3 as a vanadium source. Citric acid was employed as chelating reagent in the sol–gel process to provide the mixing of anion at the molecular level. Starting materials were of analytical grade. The NH4VO3 and the alkaline copper carbonate (CuCO3·Cu(OH)2·xH2O) powders were dissolved completely in citric acid solution on the molecular ratio of 2:1:3 in vigorous magnetic stirring at 80 C. The color of the transparent solution varied from salmon pink, khaki, dark blue to greenish black at the end. Then, the resultant sol was heated in a beaker over a hot plate for dryness 0925-8388/$ – see front matter © 2009 Elsevier B.V. All rights reserved. doi:10.1016/j.jallcom.2009.01.095