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Inorganics 2017, 5, 25 6 of 17 The drawback of the solid-state reaction is the lengthy procedure of calcination that leads usually to bigger particles, and already reported above this is at expense of the rate capability. In the mechanical activation (MA) method, a high energy ball milling step is introduced before thermal treatment. This step aims at forming an intimate mixture of the reactants that effectively reduces the thermal treatment time and temperature, thus arresting the undesirable crystal growth. Some studies have highlighted the effectiveness of MA process for the synthesis of small and phase-pure particles of LiFePO4 [21–23] and C-LiFePO4 [24]. Even with a limited amount of carbon (2 wt %) appropriate for commercial batteries, the capacity of LiFePO4 obtained after jet milling and wet milling reached 157 mAh·g−1 at 0.1C, 120 mAh·g−1 at 10C, without capacity fading after 60 cycles [21]. A review on the synthesis of nanosized electrode materials with layered and spinel structure by mechanical activation and studies of their properties can be found in [25]. The mean particle size obtained in this process is 50–200 nm. To prevent the particles coarsening during the MA, the MA can be realized in the presence of inert compound. In particular, LiCoO2 powder with grain size 50 nm was obtained by such a technique [26]. Note, however, that the milling process can deteriorate the surface layer. It is thus important to check that the thermal treatment after the milling cures the problem by re-crystallizing the surface layer. In addition, there is a tendency of the nanoparticles to agglomerate to form typically 100 nm-thick secondary particles. The mechano-fusion is an efficient way to coat the particle. Here, the smaller particles of the coating material are projected on the larger particles of the active element that have been already synthesized, in order to anchor the coating particles on the surface of the active particles. This process was used to coat LiMn1.5Ni0.5O4 with LiFePO4, which was impossible via the traditional sol–gel method. The LiFePO4 formed a protective layer against the electrolyte [27], which improved significantly the electrochemical properties. In addition, the coating particles were also electrochemically active in this case. 3. Electrochemistry of Nanostructured Cathodes As a general rule, the electrochemical properties of cathodes are governed by the microstructure of the material, especially the local environment of active redox centers, i.e., the transition metal ions in cathode oxides. Thus, the long range order favors the formation of well-defined phases upon lithium insertion, while short range order modified deeply the charge–discharge profiles with absence of phase transition, i.e., formation of voltage plateaus [1]. In the following, we present several examples that emphasize the properties of nanomaterials used as cathodes in lithium batteries. 3.1. Thermodynamic Approach For a given redox couple, the potential of an intercalation electrode considered as solution of guest A in the host latticePDF Image | Nanotechnology of Positive Electrodes for Li-Ion Batteries
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