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Caractérisation et évolution du mécanisme électrochimique d'électrodes négatives à base d'étain et d'antimoine

Abstract : This thesis takes place following on from the results obtained by C. Marino on a conversion type material TiSnSb. The interesting electrochemical performance of TiSnSb vs. Li are due to a close mixture of the lithiated species at the end of the discharge. All the interfaces between lithiated antimony phase (Li3Sb), lithiated tin phase (Li7Sn2) and titanium nanoparticles are optimized, leading to a facilitated charge transfer, which assures the rebuilding of TiSnSb on charge. In this context, the main objective was to try to create same type of mixture at the end of the discharge, with an adjustable nature and amount of elements leading to an effective conversion reaction. Through numerous tests, it was proved that the pristine fingerprint material created by the intermetallic crystalline compound play a key role in the conversion mechanism, which is tricky to reproduce by some other ways.The synthesis was oriented toward SnSb to evaluate the role of titanium in the good performance of TiSnSb. Tin antimony alloy was completely investigated as negative electrode material, from the synthesis to the electrochemical mechanism at 25°C and 60°C at the first cycle and its evolution throughout the cycling. Furthermore, failure mechanism was also identified.A new synthetic route for the intermetallic compounds as electrode active materials was developed by using the microwaves. The synthesis takes place directly under air, without oxide formation in a record time of one minute for 1 gram of SnSb. Electrochemical performance of microwave-SnSb were compared with that of SnSb prepared by mecanosynthesis.The electrochemical mechanism of SnSb, poorly described in the literature was reinvestigated. Considering the complexity of the electrochemical mechanism, operando XRD and 119Sn Mossbauer spectroscopy were both performed on SnSb and on the simple mixture of Sn+Sb. Analysis of galvanostatic measurements of SnSb alloy, Sn+Sb mixture and Sb vs. Li was completed to identify the mechanism and understanding failure mechanism.The last part of the thesis was devoted to the ageing mechanism of SnSb depending on the cycling temperature. The cycling duration was 6 months and one year at 60°C and 25°C respectively. These long cycling highlighted some original phenomena, never described in the literature, which are still under investigation.
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Submitted on : Tuesday, April 3, 2018 - 1:04:08 PM
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Philippe Antitomaso. Caractérisation et évolution du mécanisme électrochimique d'électrodes négatives à base d'étain et d'antimoine. Matériaux. Université Montpellier, 2016. Français. ⟨NNT : 2016MONTT195⟩. ⟨tel-01757065⟩



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