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From the screening of existing silicon anode materials in the literatures, the preparation methods for promising Si anode materials and their prospects have been offered.
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It covers not only the technics of high purity silicon materials, including the predominant Siemens process of electronic-grade silicon, but also the techniques of silicon film anodes, which consists of butyl-capped silicon precursor, the template methods of nanostructure, magnetron sputtering, ball-milling. Another hot issue is on the preparation methods for silicon anode materials with high performance.
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Various influencing factors of volume variation of silicon anode materials have been reviewed, which consist of discharging voltage, amorphous or crystalline type, tube or pore microstructure, interlayer adhesion, buffering and protective layer materials and conductive agents. One of key problem is how to stabilize the performances of Si anode materials. Like other anode materials with higher capacities, silicon materials as anodes remain serious problems for their large volume variations and poor cyclabilities during cycling. With the rapid progress and wide application of Li-ion batteries, commercial graphite anode can not satisfy the increasing demand for higher capacities. To determine the associated crystallographic phases, X-ray diffraction and Raman spectroscopy are performed. Their progression and related enthalpies are discussed. In air three phase transformations appear (at 330, 410 and 600.C) while in 0.5 %H2/Ar four phase transformations are observed (at 389, 471, 730 and 758.C). Measurements are carried out in ambient air and in 0.5 %H2/Ar. The second part presents TFC investigations on lithium manganese oxide (LMO) thin films. To the best of our knowledge, the presented TFC is the only existing technique combining the aspects "thin films" h and "high-temperature calorimetry." The first part of this article describes the newly developed TFC system. Thereby, the atmosphere can be controlled. Temperature ramps from room temperature up to 1000.C are applied to perform calorimetric thin-film investigations. The key component is a high-temperature stable piezoelectric langasite (La3Ga5SiO14) resonator serving as a highly sensitive planar temperature sensor.Deviations in its frequency are related to temperature fluctuations caused by phase transformations and used to calculate the related enthalpies. Thin-Film Calorimetry (TFC) as presented in this work is a novel analytical tool to determine phase transformation temperatures and enthalpies of thin films and thin-film sequences.