Preparation of nano-crystalline Li0.5La0.5TiO 3 perovskite material using citrate-nitrate redox reaction by the combustion technique is reported. The role of the ammonium nitrate concentration used to co-precipitate the Li0.5La0.5Ti-citrate precursor is revealed by ATD/TG, XRD, SEM-EDX and HRTEM techniques. Thermo-gravimetric analysis data show how the intensity of the exothermic peak associated with the citrate-nitrate redox reaction decreases until disappearance as the citrate/nitrate molar ratio increases. The XRD study indicates that a single-phase cubic Li0.5La0.5TiO3 phase is formed at 350 C when the citrate/nitrate ratio varies between 0.13 and 0.17. The formed Li0.5La0.5TiO3 powders show an average particle size of 15-20 nm. Electrochemical impedance spectroscopy technique reveals a relative high ionic conductivity inside the grain for the nanometric Li0.5La0.5TiO3 material, with values of around 10-4 S/cm at room temperature. © 2013 Elsevier Ltd and Techna Group S.r.l. All rights reserved.401 PART A249256Armand, M., Tarascon, J.M., Building better batteries (2008) Nature, 451Scrosati, B., Garche, J., Lithium batteries: Status, prospects and future (2010) Journal of Power Sources, 195, pp. 2419-2430Bruce, P.G., Scrosati, B., Tarascon, J.M., Nanomaterials for rechargeable lithium batteries (2008) Angewandte Chemie International Edition, 47, pp. 2930-2946Meethong, N., Huang, H.-Y.S., Carter, W.C., Chiang, Y.-M., Size-dependent lithium miscibility gap in nanoscale Li 1-xFePO4 (2007) Electrochemical and Solid-State Letters, 10, pp. 134-A138Stramare, S., Thangadurai, V., Weppner, W., Lithium lanthanum titanates: A review (2003) Chemistry of Materials, 15, pp. 3974-3990Fergus, J.W., Ceramic and polymeric solid electrolytes for lithium-ion batteries (2010) Journal of Power Sources, 195, pp. 4554-4569Kitaoka, K., Kozuka, H., Hashimoto, T., Yoko, T., Preparation of La0.5Li0.5TiO3 perovskite thin films by the sol-gel method (1997) Journal of Materials Science, 32, pp. 2063-2070Vijayakumar, M., Pham, Q.N., Bohnke, C., Lithium lanthanum titanate ceramic as sensitive material for pH sensor: Influence of synthesis methods and powder grains size (2005) Journal of the European Ceramic Society, 25, pp. 2973-2976Pechini, M.P., (1967) Method of Preparing Lead and Alkaline Titanates and Niobiates and Coating Method Using the Same to Form A Capacitor, USA, p. 697Vijayakumar, M., Inaguma, Y., Mashiko, W., Crosnier-López, M.-P., Bhonke, C., Synthesis of fine powders of Li3xLa2/3-xTiO 3 perovskite by a polymerizable precursor method (2004) Chemistry of Materials, 16, pp. 2719-2724Pham, Q.N., Bohnke, C., Lopez, M.P.C., Bohnke, O., Synthesis and characterization of nanostructured fast ionic conductor Li0.30La0.56TiO3 (2006) Chemistry of Materials, 18, pp. 4385-4392Behera, S.K., Barpanda, P., Pratihar, S.K., Bhattacharyya, S., Synthesis of magnesium-aluminium spinel from autoignition of citrate-nitrate gel (2004) Materials Letters, 58, pp. 1451-1455Werde, G.V.K.V., Mondelaers, D., Rul, H.D., Bael, M.K.V., Mullens, J., Poucke, L.C.V., The aqueous solution-gel synthesis of perovskite Pb(Zr 1-xTix)O3 (PZT) (2007) Journal of Materials Science, 42, pp. 624-632Purohit, R.D., Saha, S., Tyagi, A.K., Nanocrystalline thoria powders via glycine-nitrate combustion (2001) Journal of Nuclear Materials, 288, pp. 7-10Chakrabarti, N., Maiti, H.S., Chemical synthesis of PZT powder by auto-combustion of citrate-nitrate gel (1997) Materials Letters, 30, pp. 169-173Marinsek, M., Zupan, K., Maeek, J., Ni-YSZ cermet anodes prepared by citrate/nitrate combustion synthesis (2002) Journal of Power Sources, 106, pp. 178-188Jain, S.R., Adiga, K.C., Verneker, V.R.P., A new approach to thermochemical calculations of condensed fuel-oxidizer mixtures (1981) Combustion and Flame, 40, pp. 71-79Zupan, K., Kolar, D., Marinsek, M., Influence of citrate-nitrate reaction mixture packing on ceramic powder properties (2000) Journal of Power Sources, 86, pp. 417-422Folly, P., Mädera, P., Propellant chemistry (2004) CHIMIA International Journal for Chemistry, 58, pp. 374-382Singh, K.A., Pathak, L.C., Roy, S.K., Effect of citric acid on the synthesis of nano-crystalline yttria stabilized zirconia powders by nitrate-citrate process (2007) Ceramics International, 33, pp. 1463-1468Otero, T., Mosqueda, Y., Miilian, C.R., Perez-Cappe, E., Li3xLa2/3-xTiO3 nanoparticles obtained from a low temperature synthesis route (2011) Journal of Nano Research, 14, pp. 107-113Théoret, A., Sandorfy, C., Infrared spectra and crystalline phase transitions of ammonium nitrate (1964) Canadian Journal of Chemistry, 42, pp. 57-62Zhecheva, R.S.E., Gorova, M., Alcántara, R., Morales, J., Tirado, J.L., Lithium-cobalt citrate precursors in the preparation of intercalation electrode materials (1996) Chemistry of Materials, 8, pp. 1429-1440Todorovsky, D.S., Getsova, M.M., Wawer, I., Stefanov, P., Enchev, V., On the chemical nature of lanthanum-titanium citric complexes, precursors of La2Ti2O7 (2004) Materials Letters, 58, pp. 3559-3563Dakanali, M., Kefalas, E.T., Raptopoulou, C.P., Terzis, A., Voyiatzis, G., Kyrikou, I., Mavromoustakos, T., Salifoglou, A., A new dinuclear Ti(IV)-peroxo-citrate complex from aqueous solutions. Synthetic, structural, and spectroscopic studies in relevance to aqueous titanium(IV)-peroxo-citrate speciation (2003) Inorganic Chemistry, 42, pp. 4632-4639Muhlebach, J., Muller, K., Schawarzenbach, G., The peroxo complexes of titanium (1970) Inorganic Chemistry, 9, pp. 2381-2390Hardy, A., D'Haen, J., Bael, M.K.V., Mullens, J., An aqueous solution gel citratoperoxo Ti(IV) precursor: Synthesis, gelation, thermo oxidative decomposition and oxide crystallization (2007) Journal of Sol-Gel Science and Technology, 44, pp. 65-74Kakihana, M., Kobayashi, M., Tomita, K., Petrykin, V., Application of water soluble titanium complexes as precursors for synthesis of titanium containing oxides via aqueous solution processes (2010) Bulletin of the Chemical Society of Japan, 83, pp. 1285-1308Mosqueda, Y., Cappe, E.P., Aranda, P., Ruiz-Hitzky, E., Preparation of an Li0.7Ni0.8Co0.2O 2 electrode material from a new Li-Co-Ni mixed-citrate precursor (2005) European Journal of Inorganic Chemistry, pp. 2698-2705Bretos, I., Jiménez, R., Calzada, M.L., Bael, M.K.V., Hardy, A., Genechten, D.V., Mullens, J., Entirely aqueous solution-gel route for the preparation of (Pb 1-xCax)TiO3 thin films (2006) Chemistry of Materials, 18, pp. 6448-6456Todorovsky, D.S., Getsova, M.M., Vasileva, M.A., Thermal decomposition of lanthanum-titanium citric complexes prepared from ethylene glycol medium (2002) Journal of Materials Science, 37, pp. 4029-4039Oxley, J.C., Smith, J.L., Rogers, E., Yu, M., Ammonium nitrate: Thermal stability and explosivity modifier (2002) Thermochimica Acta, 384, pp. 23-45Oommen, C., Jain, S.R., Ammonium nitrate: A promising rocket propellant oxidizer (1999) Journal of Hazardous Materials, 67, pp. 253-281Korošec, R.C., Kajič, P., Bukovec, P., Determination of water, ammonium nitrate and sodium nitrate content in 'water-in-oil' emulsions using TG and DSC (2007) Journal of Thermal Analysis and Calorimetry, 89, pp. 619-624Banerjee, S., Kumar, A., Devi, P.S., Preparation of nanoparticles of oxides by the citrate-nitrate process. Effect of metal ions on the thermal decomposition characteristics (2011) Journal of Thermal Analysis and CalorimetryPatil, K.C., Hegde, M.S., Rattan, T., Aruna, S.T., Chemistry of Nanocrystalline Oxide Materials: Combustion Synthesis (2008) Properties and Applications, , World Scientific Publishing Co. Pvt. Ltd. SingaporeAkhavan, J., (2004) The Chemistry of Explosives, , R.S.o. Chemistry (Ed.)Chen, C.H., Amine, K., Ionic conductivity, lithium insertion and extraction of lanthanum lithium titanate (2001) Solid State Ionics, 144, pp. 51-57Barsoukov, E., (2005) Impedance Spectroscopy: Theory, Experiment and Applications, , Evegenij Barsoukov, J. Ross Macdonald (Eds.) second edition, John Wiley & Sons, Inc., New JerseyChung, H.-T., Kim, J.-G., Kim, H.-G., Dependence of the lithium ionic conductivity on the B-site ion substitution in (Li0.5 La0.5)Ti1-xM xO3 (M=Sn, Zr, Mn, Ge) (1998) Solid State Ionics, 107, pp. 153-160