LiFePO 种合成方法汇编(参考略).docVIP

LiFePO4 150种合成方法汇编 大力李 2009-12-6 1 LiFePO4 and C-LiFePO4 were prepared using stoichiometric Li2CO3 (99.95%), FeC2O4·H2O (99%), NH4H2PO4 (98%), and glucose (99%). The starting materials were first precalcined at 400 ?C for 6 h in flowing ultra-pure Ar in order to decompose the carbonate, oxalate, and ammonium. After cooling down, the decomposed mixtures were pressed into pellets ( 20mm, L 10mm, 10 kN) and transferred to quartz tubes, which were then sealed in vacuum. The vacuum-sealed sampleswere then calcined in amuffle furnace. The quartz tubes with the samples were removed fromthe furnace and immediately put intowater. The product LiFePO4 was obtained by removal from a broken quartz tube. In this paper, the notations NC and WQ represent samples prepared by natural cooling and by water quenching treatment, respectively. 参考略 2 A LiFePO4/carbon compositewas synthesized from stoichiometric quantities of FePO4·4H2O, LiOH·H2O and a proper amount of citric acid. The mixture underwent the following three processes: (i)high-energy ball milling taken by two steps, by primary ball milling (coarse grinding) for 3 h and secondary ball milling (fine grinding) for 6 h with zirconia balls; (ii) spray-drying, and (iii) thermal treatment under flowing nitrogen at 450 ?C for 1 h and then at 675 ?C for 8h. 3 The FePO4 precursor was prepared as follows. The stoichiometric amounts of H3PO4 and FeNO3·9H2O were dissolved in distilled water. To obtain the FePO4 colloid, the dissolved aqueous solution was recipitated by adding an NH3 solution of 5 mol L?1, under an argon atmosphere, with continuous stirring at 50 ?C and a pH of 1.0–2.0. The co-precipitation mixture was then pressure-filtrated at 20MPa, dried under vacuum at 80 ?C for 6 h, washed, dried again under vacuum at 80 ?C for 6 h, and ground, yielding the final product. 4 LiFePO4 was prepared by the solid-state reaction of Li2CO3 (99.9%, Fluka), Fe(II)C2O4 . H2O (99%, Aldrich) and (NH4)2HPO4 (99%, Fluk